data_OLI_25C_CCD _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2329(4) _cell_length_b 8.6152(4) _cell_length_c 5.9362(3) _cell_angle_alpha 90 _cell_angle_beta 90.0397(10) _cell_angle_gamma 90 _cell_volume 421.04(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5966 _cell_measurement_theta_min 3 _cell_measurement_theta_max 38 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.465 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_absorpt_coefficient_mu 17.807 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.048 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Axs Smart-Apex CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8326 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.364 _diffrn_reflns_theta_max 38.472 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 2323 _reflns_number_gt 2238 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART (Bruker-Axs Inc)' _computing_cell_refinement 'SAINT (Bruker-Axs Inc)' _computing_data_reduction 'SAINT (Bruker-Axs Inc)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.327(1) ref 1 0 0 0 1 0 0 0 1 2 0.673(1) pmt -1 0 0 0 -1 0 0 0 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2323 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.00080(4) 0.00047(5) 0.24945(5) 0.00931(6) Uani 1 1 d . . . . . Cu2 Cu 0.13710(4) 0.61875(3) -0.02415(6) 0.01055(7) Uani 1 1 d . . . . . As1 As 0.23729(3) 0.25021(2) 0.01085(4) 0.00695(6) Uani 1 1 d . . . . . O1 O 0.3703(3) 0.2536(2) 0.2197(4) 0.0140(4) Uani 1 1 d . . . . . O1' O 0.3346(3) 0.2773(2) -0.2341(3) 0.0137(4) Uani 1 1 d . . . . . O2 O 0.1315(2) 0.0802(2) 0.0029(3) 0.0096(3) Uani 1 1 d . . . . . O3 O 0.0996(2) 0.3943(2) 0.0517(4) 0.0138(4) Uani 1 1 d . . . . . O4 O 0.3731(2) 0.59687(19) -0.0010(3) 0.0094(3) Uani 1 1 d . . . . . H1 H 0.4117 0.7017 -0.0057 0.011 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01109(12) 0.01377(12) 0.00306(11) -0.00002(8) 0.00008(16) -0.00419(8) Cu2 0.00788(10) 0.01202(11) 0.01175(12) 0.00246(10) 0.00058(10) 0.00040(8) As1 0.00788(9) 0.00838(10) 0.00458(9) 0.00021(7) 0.00005(10) -0.00075(6) O1 0.0149(10) 0.0180(9) 0.0089(8) 0.0045(5) -0.0052(7) -0.0053(7) O1' 0.0199(10) 0.0153(7) 0.0061(7) -0.0021(6) 0.0060(7) -0.0062(7) O2 0.0138(6) 0.0101(6) 0.0048(6) 0.0006(5) -0.0001(7) -0.0045(5) O3 0.0076(6) 0.0100(6) 0.0238(11) -0.0007(6) 0.0016(7) 0.0003(5) O4 0.0101(6) 0.0121(6) 0.0060(6) -0.0002(5) 0.0000(7) 0.0006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.9502(17) . ? Cu1 O2 1.9707(18) 3 ? Cu1 O4 1.9942(18) 4_566 ? Cu1 O4 2.0057(19) 2_545 ? Cu1 O1' 2.348(2) 4_566 ? Cu1 O1 2.390(2) 2_545 ? Cu1 Cu1 2.9616(6) 3 ? Cu1 Cu1 2.9747(6) 3_556 ? Cu2 O4 1.9570(17) . ? Cu2 O3 1.959(2) 3_565 ? Cu2 O1' 1.995(2) 2_554 ? Cu2 O3 2.0090(18) . ? Cu2 O1 2.150(2) 2 ? Cu2 Cu2 3.0603(6) 3_565 ? As1 O1 1.654(2) . ? As1 O1' 1.6770(19) . ? As1 O3 1.6988(18) . ? As1 O2 1.7044(16) . ? O1 Cu2 2.150(2) 2_545 ? O1 Cu1 2.390(2) 2 ? O1' Cu2 1.995(2) 2_544 ? O1' Cu1 2.348(2) 4_665 ? O2 Cu1 1.9706(18) 3 ? O2 O2 2.570(3) 3 ? O2 O4 2.961(2) 2_545 ? O2 O4 2.983(2) 2_544 ? O3 Cu2 1.959(2) 3_565 ? O3 O3 2.526(4) 3_565 ? O4 Cu1 1.9943(18) 4_665 ? O4 Cu1 2.0057(19) 2 ? O4 O4 2.674(3) 3_665 ? O4 H1 0.9578 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.89(7) . 3 ? O2 Cu1 O4 175.50(7) . 4_566 ? O2 Cu1 O4 97.58(7) 3 4_566 ? O2 Cu1 O4 96.90(7) . 2_545 ? O2 Cu1 O4 176.16(7) 3 2_545 ? O4 Cu1 O4 83.91(7) 4_566 2_545 ? O2 Cu1 O1' 93.82(7) . 4_566 ? O2 Cu1 O1' 90.25(8) 3 4_566 ? O4 Cu1 O1' 90.65(7) 4_566 4_566 ? O4 Cu1 O1' 86.19(8) 2_545 4_566 ? O2 Cu1 O1 96.87(8) . 2_545 ? O2 Cu1 O1 89.41(7) 3 2_545 ? O4 Cu1 O1 78.64(8) 4_566 2_545 ? O4 Cu1 O1 94.35(7) 2_545 2_545 ? O1' Cu1 O1 169.15(8) 4_566 2_545 ? O2 Cu1 Cu1 41.21(5) . 3 ? O2 Cu1 Cu1 40.69(5) 3 3 ? O4 Cu1 Cu1 138.10(6) 4_566 3 ? O4 Cu1 Cu1 137.99(5) 2_545 3 ? O1' Cu1 Cu1 92.68(5) 4_566 3 ? O1 Cu1 Cu1 94.13(6) 2_545 3 ? O2 Cu1 Cu1 138.53(6) . 3_556 ? O2 Cu1 Cu1 139.57(5) 3 3_556 ? O4 Cu1 Cu1 42.10(5) 4_566 3_556 ? O4 Cu1 Cu1 41.81(5) 2_545 3_556 ? O1' Cu1 Cu1 87.87(5) 4_566 3_556 ? O1 Cu1 Cu1 85.36(6) 2_545 3_556 ? Cu1 Cu1 Cu1 179.40(3) 3 3_556 ? O4 Cu2 O3 171.14(7) . 3_565 ? O4 Cu2 O1' 90.00(9) . 2_554 ? O3 Cu2 O1' 95.51(10) 3_565 2_554 ? O4 Cu2 O3 92.54(8) . . ? O3 Cu2 O3 79.06(8) 3_565 . ? O1' Cu2 O3 146.95(10) 2_554 . ? O4 Cu2 O1 91.24(8) . 2 ? O3 Cu2 O1 94.17(9) 3_565 2 ? O1' Cu2 O1 103.78(9) 2_554 2 ? O3 Cu2 O1 109.10(9) . 2 ? O4 Cu2 Cu2 131.42(5) . 3_565 ? O3 Cu2 Cu2 40.13(5) 3_565 3_565 ? O1' Cu2 Cu2 127.71(8) 2_554 3_565 ? O3 Cu2 Cu2 38.93(6) . 3_565 ? O1 Cu2 Cu2 105.15(6) 2 3_565 ? O1 As1 O1' 109.33(12) . . ? O1 As1 O3 108.75(11) . . ? O1' As1 O3 109.97(11) . . ? O1 As1 O2 111.96(9) . . ? O1' As1 O2 109.86(9) . . ? O3 As1 O2 106.92(8) . . ? As1 O1 Cu2 126.98(11) . 2_545 ? As1 O1 Cu1 111.77(10) . 2 ? Cu2 O1 Cu1 115.44(9) 2_545 2 ? As1 O1' Cu2 125.78(11) . 2_544 ? As1 O1' Cu1 115.18(10) . 4_665 ? Cu2 O1' Cu1 117.44(9) 2_544 4_665 ? As1 O2 Cu1 124.58(10) . . ? As1 O2 Cu1 127.08(10) . 3 ? Cu1 O2 Cu1 98.11(7) . 3 ? As1 O2 O2 153.27(14) . 3 ? Cu1 O2 O2 49.40(6) . 3 ? Cu1 O2 O2 48.71(6) 3 3 ? As1 O2 O4 86.43(8) . 2_545 ? Cu1 O2 O4 42.26(5) . 2_545 ? Cu1 O2 O4 140.25(8) 3 2_545 ? O2 O2 O4 91.60(9) 3 2_545 ? As1 O2 O4 89.57(7) . 2_544 ? Cu1 O2 O4 139.43(9) . 2_544 ? Cu1 O2 O4 41.51(5) 3 2_544 ? O2 O2 O4 90.13(10) 3 2_544 ? O4 O2 O4 174.27(9) 2_545 2_544 ? As1 O3 Cu2 127.59(10) . 3_565 ? As1 O3 Cu2 124.66(11) . . ? Cu2 O3 Cu2 100.94(8) 3_565 . ? As1 O3 O3 157.7(2) . 3_565 ? Cu2 O3 O3 51.35(7) 3_565 3_565 ? Cu2 O3 O3 49.59(6) . 3_565 ? Cu2 O4 Cu1 120.37(10) . 4_665 ? Cu2 O4 Cu1 127.73(10) . 2 ? Cu1 O4 Cu1 96.09(7) 4_665 2 ? Cu2 O4 O4 146.73(12) . 3_665 ? Cu1 O4 O4 48.23(6) 4_665 3_665 ? Cu1 O4 O4 47.87(6) 2 3_665 ? Cu2 O4 H1 103.7 . . ? Cu1 O4 H1 101.7 4_665 . ? Cu1 O4 H1 103.8 2 . ? O4 O4 H1 109.3 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.96 2.23 2.795(3) 116.4 3_665 O4 H1 O1' 0.96 2.53 2.985(3) 108.9 3_665 _refine_diff_density_max 1.673 _refine_diff_density_min -2.378 _refine_diff_density_rms 0.287 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite 25C ccd in P 21/n CELL .71073 8.2329 8.6152 5.9362 90.0000 90.0397 90.000 ZERR 4 0.0004 0.0004 0.0003 0.0000 0.0010 .00 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z EQIV $6 -x+1/2, y-1/2, -z-1/2 BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O2 O4_$6 BIND O3 O3_$3 HTAB O4 O1_$5 HTAB O4 O1'_$5 L.S. 5 LIST 4 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 1 PLAN 25 WGHT 0.041200 0.200000 BASF 0.67260 FVAR 0.37989 0.97965 CU1 3 -0.000802 0.000472 0.249446 11.00000 0.01109 0.01377 = 0.00306 -0.00002 0.00008 -0.00419 CU2 3 0.137101 0.618746 -0.024152 11.00000 0.00788 0.01202 = 0.01175 0.00246 0.00058 0.00040 AS1 4 0.237286 0.250213 0.010845 11.00000 0.00788 0.00838 = 0.00458 0.00021 0.00005 -0.00075 O1 2 0.370274 0.253638 0.219669 11.00000 0.01494 0.01801 = 0.00894 0.00452 -0.00524 -0.00525 O1' 2 0.334601 0.277272 -0.234110 11.00000 0.01988 0.01529 = 0.00608 -0.00210 0.00601 -0.00616 O2 2 0.131537 0.080222 0.002900 11.00000 0.01379 0.01011 = 0.00476 0.00058 -0.00010 -0.00448 O3 2 0.099594 0.394339 0.051719 11.00000 0.00765 0.01001 = 0.02376 -0.00070 0.00160 0.00031 O4 2 0.373126 0.596873 -0.001020 11.00000 0.01009 0.01210 = 0.00597 -0.00020 0.00001 0.00057 AFIX 3 H1 1 0.411676 0.701723 -0.005680 11.00000 -1.20000 AFIX 0 HKLF 4 REM olivenite 25C ccd in P 21/n REM R1 = 0.0278 for 2238 Fo > 4sig(Fo) and 0.0288 for all 2323 data REM 75 parameters refined using 0 restraints END WGHT 0.0413 0.2000 REM Highest difference peak 1.673, deepest hole -2.378, 1-sigma level 0.287 Q1 1 0.1479 0.6037 -0.0733 11.00000 0.05 1.47 Q2 1 0.0984 0.6735 -0.0588 11.00000 0.05 1.26 Q3 1 0.1797 0.6773 0.0289 11.00000 0.05 1.24 Q4 1 0.1948 0.1776 -0.0467 11.00000 0.05 1.24 Q5 1 0.2907 0.3009 0.0483 11.00000 0.05 1.18 Q6 1 0.1343 -0.1187 -0.0064 11.00000 0.05 1.04 Q7 1 0.2527 0.6131 0.0609 11.00000 0.05 0.96 Q8 1 0.0826 0.3766 0.1032 11.00000 0.05 0.94 Q9 1 0.3694 0.8825 -0.0014 11.00000 0.05 0.93 Q10 1 -0.0547 0.0512 0.2163 11.00000 0.05 0.93 Q11 1 0.2723 0.1794 0.0723 11.00000 0.05 0.91 Q12 1 0.2883 0.2431 0.1768 11.00000 0.05 0.90 Q13 1 0.1731 0.2990 -0.0127 11.00000 0.05 0.88 Q14 1 -0.0009 0.4997 0.2513 11.00000 0.05 0.88 Q15 1 0.3145 0.5950 0.1357 11.00000 0.05 0.87 Q16 1 0.3173 0.2570 -0.1214 11.00000 0.05 0.87 Q17 1 0.3222 0.6172 -0.0207 11.00000 0.05 0.84 Q18 1 -0.0356 -0.0614 0.1922 11.00000 0.05 0.82 Q19 1 0.1686 0.1611 0.0989 11.00000 0.05 0.82 Q20 1 0.0220 0.6011 0.0600 11.00000 0.05 0.79 Q21 1 0.3990 0.1805 0.0753 11.00000 0.05 0.79 Q22 1 0.2144 0.2449 0.0710 11.00000 0.05 0.78 Q23 1 0.5196 0.7625 -0.0509 11.00000 0.05 0.78 Q24 1 0.4000 0.6014 -0.0593 11.00000 0.05 0.77 Q25 1 0.4458 0.2517 -0.1209 11.00000 0.05 0.75 ; _shelx_res_checksum 46458 _shelx_hkl_file ; -1 0 0 1.9045 0.3937 1 0 0 2.8727 0.3086 -2 0 0 198.45 12.83 2 0 0 183.90 10.74 -3 0 0 1.1116 0.3785 3 0 0 0.1702 0.3617 -4 0 0 19.074 1.677 4 0 0 19.407 1.819 -5 0 0 0.6003 0.5291 5 0 0 0.0426 0.5001 -6 0 0 150.96 7.91 6 0 0 140.97 8.70 -7 0 0 0.9271 0.7917 7 0 0 2.3301 0.9150 -8 0 0 3593.75 176.50 8 0 0 3618.31 198.58 -9 0 0 0.3125 0.9842 9 0 0 0.8193 1.1491 -10 0 0 97.353 9.523 10 0 0 82.149 5.980 -11 0 0 1.1810 2.3088 11 0 0 0.0000 1.2236 -12 0 0 59.210 8.171 12 0 0 64.445 5.022 -13 0 0 2.2237 3.0110 -14 0 0 97.715 11.640 0 -1 0 1.5428 0.3724 0 1 0 0.3553 0.0978 -1 -1 0 964.20 45.54 -1 1 0 910.63 28.75 1 1 0 897.26 37.17 -2 -1 0 474.80 22.94 -2 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5 -2 -9 56.050 7.639 5 2 -9 49.187 6.618 -5 -2 9 36.164 5.192 -5 2 9 45.676 5.416 4 -2 -9 54.273 7.341 4 2 -9 53.518 6.714 -4 -2 9 40.250 5.458 -4 2 9 44.995 5.501 3 -2 -9 45.889 6.543 3 2 -9 61.763 7.043 -3 -2 9 36.132 5.288 -3 2 9 44.676 5.373 2 -2 -9 6.6817 3.7558 2 2 -9 10.714 4.054 -2 -2 9 6.3945 3.0536 -2 2 9 11.502 3.203 1 -2 -9 62.051 7.533 1 2 -9 68.147 7.650 -1 -2 9 48.411 6.075 -1 2 9 68.605 6.480 0 -2 -9 64.891 7.873 0 2 -9 65.615 7.480 0 -2 9 45.804 5.926 0 2 9 63.189 6.214 -1 -2 -9 44.878 6.565 -1 2 -9 46.517 6.618 1 -2 9 39.409 5.256 1 2 9 48.964 5.160 -2 -2 -9 6.8094 4.2559 -2 2 -9 3.9154 3.8196 2 -2 9 6.9796 2.8834 2 2 9 6.0008 2.5429 -3 -2 -9 51.900 7.416 -3 2 -9 51.188 6.895 3 -2 9 39.888 5.309 3 2 9 49.581 5.096 -4 -2 -9 56.231 7.863 -4 2 -9 41.878 6.799 4 -2 9 42.633 5.139 4 2 9 49.240 4.873 -5 -2 -9 68.030 9.214 -5 2 -9 75.467 8.831 5 -2 9 65.083 6.394 -6 -2 -9 3.2557 4.3836 -6 2 -9 2.5961 3.8303 6 -2 9 12.970 3.022 6 -3 -9 17.662 5.192 6 3 -9 10.012 3.383 -6 -3 9 7.3839 2.8621 -6 3 9 10.491 3.011 5 -3 -9 92.927 10.533 5 3 -9 100.00 9.83 -5 -3 9 92.693 8.703 -5 3 9 114.80 9.03 4 -3 -9 2.6918 4.0324 4 3 -9 1.8300 3.1919 -4 -3 9 2.1279 2.6812 -4 3 9 0.8937 2.2237 3 -3 -9 53.656 7.203 3 3 -9 61.136 7.129 -3 -3 9 50.645 6.033 -3 3 9 50.347 5.724 2 -3 -9 15.353 4.830 2 3 -9 15.747 4.490 -2 -3 9 21.992 4.139 -2 3 9 21.333 3.681 1 -3 -9 162.91 15.01 1 3 -9 211.56 15.44 -1 -3 9 171.38 13.35 -1 3 9 170.63 12.86 0 -3 -9 8.2032 4.6495 0 3 -9 7.6393 3.9580 0 -3 9 6.9158 3.1919 0 3 9 6.5328 2.7025 -1 -3 -9 252.61 19.96 -1 3 -9 248.01 12.08 1 -3 9 228.15 17.17 1 3 9 244.88 16.65 -2 -3 -9 19.226 5.554 -2 3 -9 22.319 2.846 2 -3 9 19.481 4.032 2 3 9 19.013 3.245 -3 -3 -9 90.416 10.246 -3 3 -9 84.351 9.203 3 -3 9 83.298 7.810 3 3 9 86.990 7.235 -4 -3 -9 0.0000 3.9792 -4 3 -9 0.3405 3.3302 4 -3 9 2.0322 2.4152 4 3 9 1.3087 1.6066 -5 -3 -9 23.375 6.011 -5 3 -9 30.610 5.852 -6 -3 -9 20.833 6.054 -6 3 -9 21.226 5.150 -6 -4 9 3.6069 1.5853 5 -4 -9 21.886 5.373 -5 -4 9 13.066 3.596 -5 4 9 13.300 3.437 4 -4 -9 5.8199 4.4899 -4 -4 9 1.6598 2.4152 -4 4 9 0.5745 2.2875 3 -4 -9 19.662 5.182 -3 -4 9 12.917 3.671 -3 4 9 16.066 3.554 2 -4 -9 2.9791 3.7984 2 4 -9 0.0000 2.9259 -2 -4 9 0.0000 2.3514 -2 4 9 1.0852 2.2769 1 -4 -9 154.68 14.08 1 4 -9 188.95 13.98 -1 -4 9 137.53 12.01 -1 4 9 150.30 11.54 0 -4 -9 5.9050 4.4687 0 4 -9 2.4578 1.6272 0 -4 9 1.2342 2.9578 0 4 9 2.8514 2.2982 -1 -4 -9 157.01 14.28 -1 4 -9 166.26 8.52 1 -4 9 138.08 12.11 1 4 9 152.35 11.34 -2 -4 -9 1.0108 4.1176 -2 4 -9 0.8160 1.7387 2 -4 9 1.6172 2.8195 2 4 9 0.4469 1.7555 -3 -4 -9 11.533 5.064 -3 4 -9 11.842 2.470 3 -4 9 10.884 3.415 3 4 9 9.9907 2.5429 -4 -4 -9 0.5320 4.1920 -4 4 -9 0.6597 3.3302 4 -4 9 1.2448 2.5216 4 4 9 0.0000 1.3938 -5 -4 -9 11.714 5.139 -5 4 -9 15.162 4.426 5 -4 9 13.470 3.373 -6 4 -9 1.1810 2.0322 -5 -5 9 40.016 5.033 4 -5 -9 6.3413 4.5006 -4 -5 9 5.3624 3.0323 -4 5 9 5.2241 2.7876 3 -5 -9 45.655 6.990 -3 -5 9 47.400 5.852 -3 5 9 46.602 5.479 2 -5 -9 49.421 7.097 -2 -5 9 34.739 5.469 -2 5 9 46.878 5.150 1 -5 -9 164.38 14.46 -1 -5 9 157.12 12.74 -1 5 9 168.87 12.10 0 -5 -9 2.1811 4.1708 0 5 -9 0.6384 2.0747 0 -5 9 1.4364 3.0110 0 5 9 2.2343 2.0535 -1 -5 -9 192.09 16.92 -1 5 -9 203.42 12.97 1 -5 9 177.16 14.50 1 5 9 211.31 13.96 -2 -5 -9 35.026 6.426 -2 5 -9 43.112 4.543 2 -5 9 37.611 5.448 2 5 9 38.835 4.415 -3 -5 -9 59.072 8.129 -3 5 -9 56.273 5.607 3 -5 9 55.497 6.426 3 5 9 56.837 5.405 -4 -5 -9 7.9798 4.7985 -4 5 -9 7.0116 2.9578 4 -5 9 8.4905 3.3834 4 5 9 8.2670 2.1386 5 -5 9 28.099 4.586 3 -6 -9 49.613 6.948 -3 -6 9 45.740 5.894 -3 6 9 46.474 5.416 2 -6 -9 0.0000 3.2770 -2 -6 9 0.0958 2.7344 -2 6 9 2.6493 2.2343 1 -6 -9 42.601 6.543 1 6 -9 35.515 4.118 -1 -6 9 34.877 5.352 -1 6 9 33.526 4.458 0 -6 -9 50.421 7.331 0 6 -9 50.273 4.958 0 -6 9 42.931 6.160 0 6 9 58.635 5.671 -1 -6 -9 23.631 5.586 -1 6 -9 25.227 3.628 1 -6 9 26.397 4.884 1 6 9 27.940 3.841 -2 -6 -9 1.2342 3.5217 -2 6 -9 1.0959 2.1811 2 -6 9 2.7663 3.0004 2 6 9 2.9578 2.0215 -3 -6 -9 51.943 7.714 -3 6 -9 48.857 5.128 3 -6 9 53.081 6.511 3 6 9 55.624 5.224 2 -7 -9 9.0650 4.0963 2 7 -9 11.065 2.564 1 -7 -9 148.52 13.41 1 7 -9 133.33 9.82 0 -7 -9 0.0000 3.6707 0 7 -9 0.5107 2.1067 0 7 9 1.5747 1.9258 -1 -7 -9 56.518 7.895 1 7 9 65.817 6.001 -2 -7 -9 10.608 4.373 2 7 9 11.267 2.575 3 0 -10 3.1068 3.6069 2 0 -10 344.66 26.17 1 0 -10 1.5534 3.6707 -1 0 10 0.0000 2.1173 0 0 -10 1.2342 3.7664 0 0 10 0.4894 2.2769 -1 0 -10 2.1705 3.7452 1 0 10 0.0000 1.8939 -2 0 -10 524.32 38.24 -3 0 -10 1.4576 3.6388 3 0 10 0.0000 1.9045 3 1 -10 189.24 15.86 2 -1 -10 45.676 6.746 2 1 -10 57.124 7.065 -2 -1 10 40.888 5.575 -2 1 10 45.400 5.692 1 -1 -10 118.46 11.40 1 1 -10 118.30 11.38 -1 -1 10 113.75 9.81 -1 1 10 112.31 9.59 0 -1 -10 155.34 13.52 0 1 -10 152.37 13.31 0 -1 10 137.58 11.42 0 1 10 139.20 11.22 -1 -1 -10 57.571 7.650 -1 1 -10 57.784 7.373 1 -1 10 50.070 5.969 1 1 10 54.667 5.873 -2 -1 -10 88.267 9.576 -2 1 -10 97.300 9.703 2 -1 10 77.744 7.490 2 1 10 67.626 7.001 3 -1 10 125.48 10.08 3 1 10 127.70 9.88 3 2 -10 47.868 6.341 2 -2 -10 5.4901 4.0431 2 2 -10 7.2137 3.9048 -2 -2 10 4.2772 2.7025 -2 2 10 4.3623 2.6812 1 -2 -10 17.609 5.096 1 2 -10 14.779 4.511 -1 -2 10 15.864 3.735 -1 2 10 15.332 3.405 0 -2 -10 347.17 26.30 0 2 -10 369.55 26.22 0 -2 10 319.64 22.97 0 2 10 336.09 22.65 -1 -2 -10 26.227 5.958 -1 2 -10 34.239 6.001 1 -2 10 36.111 4.990 1 2 10 31.004 4.384 -2 -2 -10 11.714 4.554 -2 2 -10 9.4800 4.1708 2 -2 10 8.0755 2.9898 2 2 10 5.9157 2.4152 3 2 10 22.045 3.447 2 3 -10 53.730 6.618 1 3 -10 99.683 9.895 0 3 -10 5.0539 3.4685 0 3 10 3.8516 2.3726 -1 3 -10 151.63 13.30 1 3 10 143.82 11.11 -2 3 -10 32.536 5.362 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 29444 #===END data_OLI_25C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2294(10) _cell_length_b 8.6120(9) _cell_length_c 5.9358(7) _cell_angle_alpha 90 _cell_angle_beta 90.063(10) _cell_angle_gamma 90 _cell_volume 420.68(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.469 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.822 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2472 _diffrn_reflns_av_unetI/netI 0.0629 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.365 _diffrn_reflns_theta_max 30.027 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1236 _reflns_number_gt 1156 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.337(3) ref 1 0 0 0 1 0 0 0 1 2 0.663(3) pmt -1 0 0 0 -1 0 0 0 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.1646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2008)' _refine_ls_extinction_coef 0.0043(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1236 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.00101(12) 0.00008(16) 0.24932(13) 0.0197(2) Uani 1 1 d . . . . . Cu2 Cu 0.13729(9) 0.61871(9) -0.02426(17) 0.0206(2) Uani 1 1 d . . . . . As1 As 0.23721(7) 0.25035(7) 0.01113(13) 0.01736(19) Uani 1 1 d . . . . . O1 O 0.3704(6) 0.2534(6) 0.2196(9) 0.0224(12) Uani 1 1 d . . . . . O1' O 0.3327(6) 0.2777(7) -0.2356(9) 0.0215(11) Uani 1 1 d . . . . . O2 O 0.1310(5) 0.0807(6) 0.0033(9) 0.0201(9) Uani 1 1 d . . . . . O3 O 0.1003(5) 0.3933(6) 0.0521(11) 0.0250(12) Uani 1 1 d . . . . . O4 O 0.3722(5) 0.5973(5) -0.0018(10) 0.0187(8) Uani 1 1 d . . . . . H1 H 0.4108 0.7022 -0.0064 0.022 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0197(3) 0.0249(4) 0.0146(3) 0.0004(4) -0.0011(5) -0.0041(3) Cu2 0.0163(3) 0.0226(4) 0.0229(4) 0.0025(4) 0.0004(3) 0.0004(3) As1 0.0160(3) 0.0195(4) 0.0165(3) 0.0000(3) -0.0004(3) -0.0005(2) O1 0.021(2) 0.027(3) 0.019(2) 0.0014(19) -0.0044(18) 0.000(2) O1' 0.025(2) 0.021(2) 0.018(2) 0.000(2) 0.0057(19) -0.002(2) O2 0.0212(17) 0.021(2) 0.018(2) 0.000(2) 0.004(2) -0.0065(16) O3 0.0168(18) 0.022(2) 0.036(3) -0.001(3) 0.0015(18) -0.0004(17) O4 0.0180(16) 0.022(2) 0.0165(19) 0.002(2) 0.001(2) 0.0020(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.949(5) . ? Cu1 O2 1.968(5) 3 ? Cu1 O4 1.995(5) 4_566 ? Cu1 O4 2.017(5) 2_545 ? Cu1 O1' 2.354(6) 4_566 ? Cu1 O1 2.388(5) 2_545 ? Cu1 Cu1 2.9598(15) 3 ? Cu1 Cu1 2.9761(15) 3_556 ? Cu2 O4 1.946(4) . ? Cu2 O3 1.964(5) 3_565 ? Cu2 O1' 1.992(6) 2_554 ? Cu2 O3 2.017(5) . ? Cu2 O1 2.149(6) 2 ? Cu2 Cu2 3.0611(15) 3_565 ? As1 O1 1.652(5) . ? As1 O1' 1.679(5) . ? As1 O3 1.686(5) . ? As1 O2 1.703(5) . ? O1 Cu2 2.149(6) 2_545 ? O1 Cu1 2.388(5) 2 ? O1' Cu2 1.992(6) 2_544 ? O1' Cu1 2.354(6) 4_665 ? O2 Cu1 1.968(5) 3 ? O2 O2 2.566(8) 3 ? O2 O4 2.962(7) 2_545 ? O2 O4 2.980(7) 2_544 ? O3 Cu2 1.964(5) 3_565 ? O3 O3 2.546(10) 3_565 ? O4 Cu1 1.995(5) 4_665 ? O4 Cu1 2.017(5) 2 ? O4 O4 2.690(8) 3_665 ? O4 H1 0.9575 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.84(18) . 3 ? O2 Cu1 O4 175.8(2) . 4_566 ? O2 Cu1 O4 97.55(18) 3 4_566 ? O2 Cu1 O4 96.65(18) . 2_545 ? O2 Cu1 O4 176.2(2) 3 2_545 ? O4 Cu1 O4 84.21(18) 4_566 2_545 ? O2 Cu1 O1' 93.6(2) . 4_566 ? O2 Cu1 O1' 90.1(2) 3 4_566 ? O4 Cu1 O1' 90.52(18) 4_566 4_566 ? O4 Cu1 O1' 86.5(2) 2_545 4_566 ? O2 Cu1 O1 97.10(19) . 2_545 ? O2 Cu1 O1 89.34(19) 3 2_545 ? O4 Cu1 O1 78.72(18) 4_566 2_545 ? O4 Cu1 O1 94.35(18) 2_545 2_545 ? O1' Cu1 O1 169.05(19) 4_566 2_545 ? O2 Cu1 Cu1 41.16(15) . 3 ? O2 Cu1 Cu1 40.68(13) 3 3 ? O4 Cu1 Cu1 138.08(16) 4_566 3 ? O4 Cu1 Cu1 137.71(15) 2_545 3 ? O1' Cu1 Cu1 92.43(14) 4_566 3 ? O1 Cu1 Cu1 94.23(14) 2_545 3 ? O2 Cu1 Cu1 138.33(16) . 3_556 ? O2 Cu1 Cu1 139.83(15) 3 3_556 ? O4 Cu1 Cu1 42.39(15) 4_566 3_556 ? O4 Cu1 Cu1 41.82(14) 2_545 3_556 ? O1' Cu1 Cu1 87.99(14) 4_566 3_556 ? O1 Cu1 Cu1 85.43(14) 2_545 3_556 ? Cu1 Cu1 Cu1 179.35(8) 3 3_556 ? O4 Cu2 O3 171.5(2) . 3_565 ? O4 Cu2 O1' 89.4(2) . 2_554 ? O3 Cu2 O1' 95.7(2) 3_565 2_554 ? O4 Cu2 O3 92.5(2) . . ? O3 Cu2 O3 79.5(2) 3_565 . ? O1' Cu2 O3 147.3(2) 2_554 . ? O4 Cu2 O1 91.3(2) . 2 ? O3 Cu2 O1 94.0(2) 3_565 2 ? O1' Cu2 O1 103.6(2) 2_554 2 ? O3 Cu2 O1 109.0(2) . 2 ? O4 Cu2 Cu2 131.57(15) . 3_565 ? O3 Cu2 Cu2 40.38(15) 3_565 3_565 ? O1' Cu2 Cu2 128.20(18) 2_554 3_565 ? O3 Cu2 Cu2 39.12(13) . 3_565 ? O1 Cu2 Cu2 105.01(15) 2 3_565 ? O1 As1 O1' 109.9(3) . . ? O1 As1 O3 108.9(3) . . ? O1' As1 O3 109.7(3) . . ? O1 As1 O2 112.0(3) . . ? O1' As1 O2 109.7(3) . . ? O3 As1 O2 106.7(2) . . ? As1 O1 Cu2 127.0(3) . 2_545 ? As1 O1 Cu1 111.7(3) . 2 ? Cu2 O1 Cu1 115.4(2) 2_545 2 ? As1 O1' Cu2 125.9(3) . 2_544 ? As1 O1' Cu1 114.8(3) . 4_665 ? Cu2 O1' Cu1 117.3(2) 2_544 4_665 ? As1 O2 Cu1 124.9(3) . . ? As1 O2 Cu1 127.1(3) . 3 ? Cu1 O2 Cu1 98.16(18) . 3 ? As1 O2 O2 153.7(4) . 3 ? Cu1 O2 O2 49.40(16) . 3 ? Cu1 O2 O2 48.76(18) 3 3 ? As1 O2 O4 86.4(2) . 2_545 ? Cu1 O2 O4 42.54(13) . 2_545 ? Cu1 O2 O4 140.6(2) 3 2_545 ? O2 O2 O4 91.9(3) 3 2_545 ? As1 O2 O4 89.4(2) . 2_544 ? Cu1 O2 O4 139.6(2) . 2_544 ? Cu1 O2 O4 41.56(14) 3 2_544 ? O2 O2 O4 90.3(3) 3 2_544 ? O4 O2 O4 174.4(3) 2_545 2_544 ? As1 O3 Cu2 127.9(3) . 3_565 ? As1 O3 Cu2 124.7(3) . . ? Cu2 O3 Cu2 100.5(2) 3_565 . ? As1 O3 O3 157.7(5) . 3_565 ? Cu2 O3 O3 51.16(16) 3_565 3_565 ? Cu2 O3 O3 49.34(17) . 3_565 ? Cu2 O4 Cu1 120.6(3) . 4_665 ? Cu2 O4 Cu1 127.7(3) . 2 ? Cu1 O4 Cu1 95.79(18) 4_665 2 ? Cu2 O4 O4 146.7(3) . 3_665 ? Cu1 O4 O4 48.24(16) 4_665 3_665 ? Cu1 O4 O4 47.55(17) 2 3_665 ? Cu2 O4 H1 103.8 . . ? Cu1 O4 H1 101.6 4_665 . ? Cu1 O4 H1 103.8 2 . ? O4 O4 H1 109.2 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.96 2.24 2.796(7) 116.4 3_665 O4 H1 O1' 0.96 2.56 3.005(7) 108.7 3_665 _refine_diff_density_max 1.438 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.266 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite 25C jof in P 21/n CELL .71073 8.2294 8.6120 5.9358 90.000 90.063 90.000 ZERR 4 .0010 .0009 .0007 .00 .010 .00 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z EQIV $6 -x+1/2, y-1/2, -z-1/2 BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O2 O4_$6 BIND O3 O3_$3 HTAB O4 O1_$5 HTAB O4 O1'_$5 L.S. 5 LIST 4 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 1 PLAN 25 WGHT 0.038000 1.164600 EXTI 0.004315 BASF 0.66315 FVAR 0.30034 CU1 3 -0.001013 0.000085 0.249317 11.00000 0.01969 0.02485 = 0.01465 0.00040 -0.00107 -0.00408 CU2 3 0.137286 0.618710 -0.024257 11.00000 0.01628 0.02255 = 0.02287 0.00254 0.00040 0.00039 AS1 4 0.237210 0.250347 0.011135 11.00000 0.01604 0.01952 = 0.01652 -0.00002 -0.00037 -0.00051 O1 2 0.370351 0.253404 0.219620 11.00000 0.02121 0.02724 = 0.01880 0.00142 -0.00436 -0.00048 O1' 2 0.332718 0.277714 -0.235550 11.00000 0.02530 0.02074 = 0.01838 0.00023 0.00571 -0.00155 O2 2 0.130979 0.080735 0.003274 11.00000 0.02124 0.02149 = 0.01757 0.00023 0.00374 -0.00651 O3 2 0.100272 0.393255 0.052063 11.00000 0.01683 0.02172 = 0.03640 -0.00081 0.00146 -0.00041 O4 2 0.372212 0.597327 -0.001750 11.00000 0.01800 0.02157 = 0.01651 0.00188 0.00075 0.00198 AFIX 3 H1 1 0.410762 0.702177 -0.006410 11.00000 -1.20000 AFIX 0 HKLF 4 REM olivenite 25C jof in P 21/n REM R1 = 0.0337 for 1156 Fo > 4sig(Fo) and 0.0361 for all 1236 data REM 75 parameters refined using 0 restraints END WGHT 0.0380 1.1646 REM Highest difference peak 1.438, deepest hole -1.304, 1-sigma level 0.266 Q1 1 0.2851 0.2130 -0.1209 11.00000 0.05 1.44 Q2 1 0.2861 0.2783 -0.1166 11.00000 0.05 1.39 Q3 1 0.1730 0.5993 -0.1555 11.00000 0.05 1.26 Q4 1 0.1258 0.6136 -0.1236 11.00000 0.05 1.26 Q5 1 0.0576 -0.0187 0.1299 11.00000 0.05 1.25 Q6 1 0.1686 0.2397 0.1228 11.00000 0.05 1.17 Q7 1 0.0878 0.6556 0.0940 11.00000 0.05 1.16 Q8 1 -0.0631 -0.0014 0.3750 11.00000 0.05 1.11 Q9 1 0.0158 0.1061 0.2267 11.00000 0.05 0.77 Q10 1 0.1533 0.7214 -0.0018 11.00000 0.05 0.75 Q11 1 0.4042 0.2635 0.1125 11.00000 0.05 0.71 Q12 1 0.2166 0.3602 0.0331 11.00000 0.05 0.63 Q13 1 0.1772 0.6178 0.0261 11.00000 0.05 0.60 Q14 1 0.1402 0.0658 0.0629 11.00000 0.05 0.60 Q15 1 0.1764 0.0799 -0.1055 11.00000 0.05 0.59 Q16 1 0.2251 0.1421 0.0060 11.00000 0.05 0.59 Q17 1 0.1485 0.4160 -0.0742 11.00000 0.05 0.56 Q18 1 0.0026 -0.1049 0.2573 11.00000 0.05 0.53 Q19 1 0.3115 0.0604 -0.0911 11.00000 0.05 0.53 Q20 1 0.4581 0.1289 -0.1572 11.00000 0.05 0.51 Q21 1 0.0210 0.3717 -0.1533 11.00000 0.05 0.51 Q22 1 0.4279 0.7493 0.1582 11.00000 0.05 0.49 Q23 1 0.0746 0.5294 -0.3807 11.00000 0.05 0.49 Q24 1 0.4005 0.8251 0.1247 11.00000 0.05 0.48 Q25 1 0.1799 0.2587 -0.0488 11.00000 0.05 0.48 ; _shelx_res_checksum 74608 _shelx_hkl_file ; 1 0 0 3.8 0.6 1 2 0 0 125.5 2.3 1 3 0 0 3.4 1.3 1 4 0 0 18.5 1.7 1 5 0 0 5.0 1.6 1 6 0 0 73.9 2.8 1 7 0 0 0.0 1.5 1 8 0 0 1504.0 12.2 1 9 0 0 -3.6 1.8 1 10 0 0 30.4 2.3 1 11 0 0 -1.0 1.5 1 0 1 0 5.9 0.6 1 1 1 0 563.1 3.6 1 -1 1 0 541.1 4.3 1 2 1 0 289.2 3.4 1 -2 1 0 280.5 3.4 1 3 1 0 1246.2 7.9 1 -3 1 0 1288.6 8.1 1 4 1 0 13.7 1.3 1 -4 1 0 12.9 1.4 1 5 1 0 646.6 6.9 1 -5 1 0 674.0 7.1 1 6 1 0 344.6 5.5 1 -6 1 0 369.2 5.7 1 7 1 0 61.0 2.8 1 -7 1 0 62.9 2.7 1 8 1 0 278.7 5.4 1 -8 1 0 293.5 5.6 1 9 1 0 74.7 3.2 1 -9 1 0 84.8 3.2 1 10 1 0 18.7 2.1 1 -10 1 0 17.5 1.8 1 11 1 0 89.7 3.5 1 -11 1 0 88.5 3.5 1 0 2 0 82.4 1.9 1 1 2 0 723.1 5.1 1 -1 2 0 773.9 5.6 1 2 2 0 3420.9 12.3 1 -2 2 0 3343.7 14.4 1 3 2 0 230.8 3.7 1 -3 2 0 229.6 4.2 1 4 2 0 4.2 1.4 1 -4 2 0 3.4 1.3 1 5 2 0 507.2 6.3 1 -5 2 0 530.2 6.4 1 6 2 0 940.3 8.9 1 -6 2 0 967.4 9.1 1 7 2 0 24.3 2.0 1 -7 2 0 23.9 1.9 1 8 2 0 0.7 1.6 1 -8 2 0 0.0 1.5 1 9 2 0 160.5 4.4 1 -9 2 0 161.7 4.3 1 10 2 0 222.6 5.4 1 -10 2 0 233.6 5.3 1 11 2 0 0.6 1.4 1 -11 2 0 -1.0 1.5 1 0 3 0 3.8 1.1 1 1 3 0 1394.5 8.3 1 -1 3 0 1489.7 8.8 1 2 3 0 19.9 1.4 1 -2 3 0 18.1 1.7 1 3 3 0 190.7 3.7 1 -3 3 0 173.3 4.1 1 4 3 0 92.0 2.9 1 -4 3 0 88.0 3.2 1 5 3 0 140.8 3.6 1 -5 3 0 147.5 3.9 1 6 3 0 58.5 2.7 1 -6 3 0 54.5 2.6 1 7 3 0 374.2 6.2 1 -7 3 0 353.9 6.0 1 8 3 0 10.2 1.5 1 -8 3 0 8.1 1.5 1 9 3 0 102.7 3.8 1 -9 3 0 97.7 3.5 1 10 3 0 92.8 3.8 1 -10 3 0 89.2 3.4 1 11 3 0 4.2 1.7 1 -11 3 0 5.2 1.5 1 0 4 0 660.3 6.3 1 1 4 0 123.3 2.9 1 -1 4 0 129.5 3.1 1 2 4 0 8.9 1.2 1 -2 4 0 11.4 1.4 1 3 4 0 9.5 1.4 1 -3 4 0 11.1 1.8 1 4 4 0 3178.7 15.9 1 -4 4 0 2899.7 17.5 1 5 4 0 77.2 2.9 1 -5 4 0 76.1 3.5 1 6 4 0 21.1 2.0 1 -6 4 0 17.6 1.9 1 7 4 0 1.3 1.6 1 -7 4 0 1.2 1.4 1 8 4 0 101.0 3.7 1 -8 4 0 100.1 3.5 1 9 4 0 7.5 1.8 1 -9 4 0 8.6 1.5 1 10 4 0 13.0 2.0 1 -10 4 0 13.9 1.7 1 0 5 0 1.0 1.3 1 1 5 0 990.0 8.4 1 -1 5 0 1018.3 8.7 1 2 5 0 103.4 3.1 1 -2 5 0 98.6 3.1 1 3 5 0 37.2 2.1 1 -3 5 0 37.6 2.2 1 4 5 0 77.9 3.0 1 -4 5 0 67.9 3.2 1 5 5 0 105.1 3.3 1 -5 5 0 88.6 3.7 1 6 5 0 -0.7 1.5 1 -6 5 0 0.4 1.8 1 7 5 0 282.0 5.6 1 -7 5 0 266.2 6.1 1 8 5 0 26.0 2.0 1 -8 5 0 26.5 2.2 1 9 5 0 49.9 2.8 1 -9 5 0 42.6 2.7 1 10 5 0 75.6 3.4 1 -10 5 0 64.9 3.1 1 0 6 0 446.6 6.1 1 1 6 0 235.0 4.6 1 -1 6 0 247.8 4.7 1 2 6 0 1352.1 10.7 1 -2 6 0 1351.9 11.0 1 3 6 0 57.8 2.7 1 -3 6 0 50.1 2.6 1 4 6 0 86.1 3.2 1 -4 6 0 82.6 3.3 1 5 6 0 163.9 4.2 1 -5 6 0 142.6 4.7 1 6 6 0 447.6 7.0 1 -6 6 0 384.4 7.5 1 7 6 0 -0.5 1.5 1 -7 6 0 0.5 1.8 1 8 6 0 36.2 2.3 1 -8 6 0 32.3 2.7 1 9 6 0 80.3 3.5 1 -9 6 0 66.9 3.3 1 10 6 0 158.1 4.8 1 -10 6 0 140.4 4.6 1 0 7 0 0.0 1.3 1 1 7 0 34.5 2.2 1 -1 7 0 32.7 2.1 1 2 7 0 41.4 2.3 1 -2 7 0 41.2 2.3 1 3 7 0 512.4 7.2 1 -3 7 0 501.0 7.3 1 4 7 0 0.7 1.6 1 -4 7 0 1.7 1.5 1 5 7 0 169.5 4.5 1 -5 7 0 174.4 4.8 1 6 7 0 149.9 4.3 1 -6 7 0 147.9 4.7 1 7 7 0 1.3 1.5 1 -7 7 0 1.4 1.7 1 8 7 0 102.0 3.8 1 -8 7 0 86.8 4.1 1 9 7 0 37.8 2.6 1 -9 7 0 31.4 2.9 1 0 8 0 1542.9 12.4 1 1 8 0 6.9 1.6 1 -1 8 0 13.1 1.4 1 2 8 0 22.3 2.1 1 -2 8 0 22.2 2.0 1 3 8 0 11.7 1.7 1 -3 8 0 10.1 1.6 1 4 8 0 129.8 3.9 1 -4 8 0 118.5 3.9 1 5 8 0 5.7 1.7 1 -5 8 0 6.3 1.7 1 6 8 0 0.5 1.6 1 -6 8 0 1.2 1.6 1 7 8 0 0.7 1.5 1 -7 8 0 0.7 1.8 1 8 8 0 343.0 6.8 1 -8 8 0 277.3 6.9 1 0 9 0 -3.9 1.8 1 1 9 0 15.5 1.7 1 -1 9 0 14.4 1.6 1 2 9 0 43.8 2.5 1 -2 9 0 42.8 2.6 1 3 9 0 189.7 4.9 1 -3 9 0 188.7 4.8 1 4 9 0 8.5 1.6 1 -4 9 0 7.2 1.4 1 5 9 0 108.4 3.8 1 -5 9 0 113.0 4.0 1 6 9 0 78.8 3.6 1 -6 9 0 76.6 3.6 1 7 9 0 4.6 1.7 1 -7 9 0 3.3 1.9 1 0 10 0 3.2 1.5 1 1 10 0 7.0 1.8 1 -1 10 0 4.8 1.9 1 2 10 0 291.0 5.9 1 -2 10 0 276.5 5.8 1 3 10 0 4.2 1.6 1 -3 10 0 3.3 1.6 1 4 10 0 39.9 2.6 1 -4 10 0 38.2 2.6 1 5 10 0 17.3 2.0 1 -5 10 0 17.6 2.0 1 6 10 0 159.1 4.8 1 -6 10 0 141.2 4.7 1 0 11 0 -1.5 1.6 1 1 11 0 56.5 3.1 1 -1 11 0 65.3 3.0 1 2 11 0 40.4 2.7 1 -2 11 0 35.8 2.4 1 3 11 0 12.6 1.8 1 -3 11 0 13.2 1.8 1 4 11 0 20.5 2.0 1 -4 11 0 21.9 2.1 1 0 12 0 77.2 3.6 1 1 12 0 7.3 1.7 1 -1 12 0 6.7 1.7 1 0 0 1 8.8 1.1 1 1 0 1 952.5 6.1 1 -1 0 1 768.2 5.6 1 2 0 1 5.9 1.4 1 -2 0 1 4.5 1.3 1 3 0 1 1041.9 7.7 1 -3 0 1 934.9 7.3 1 4 0 1 0.2 1.5 1 -4 0 1 3.7 1.2 1 5 0 1 20.1 1.8 1 -5 0 1 22.6 1.7 1 6 0 1 1.1 1.6 1 -6 0 1 0.4 1.4 1 7 0 1 31.3 2.2 1 -7 0 1 48.2 2.5 1 8 0 1 1.8 1.7 1 -8 0 1 1.3 1.4 1 9 0 1 106.5 3.6 1 -9 0 1 109.7 3.7 1 10 0 1 0.0 1.7 1 -10 0 1 2.6 1.3 1 11 0 1 175.7 4.8 1 -11 0 1 188.5 4.9 1 0 1 1 845.2 5.7 1 0 -1 1 982.2 6.1 1 1 1 1 502.0 4.5 1 -1 1 1 496.9 4.9 1 1 -1 1 490.7 4.9 1 -1 -1 1 585.7 4.7 1 2 1 1 18.2 1.5 1 -2 1 1 19.7 2.0 1 2 -1 1 19.3 1.9 1 -2 -1 1 17.8 1.4 1 3 1 1 1210.3 8.3 1 -3 1 1 1198.1 9.0 1 3 -1 1 1186.3 8.4 1 -3 -1 1 1219.2 8.2 1 4 1 1 388.6 5.2 1 -4 1 1 393.0 5.5 1 4 -1 1 389.7 5.3 1 -4 -1 1 409.6 5.3 1 5 1 1 1069.4 9.1 1 -5 1 1 1128.4 9.6 1 5 -1 1 1040.6 8.9 1 -5 -1 1 1170.8 9.5 1 6 1 1 17.2 1.8 1 -6 1 1 10.4 1.6 1 6 -1 1 17.1 1.7 1 -6 -1 1 13.2 1.7 1 7 1 1 189.2 4.5 1 -7 1 1 169.7 4.3 1 7 -1 1 180.2 4.5 1 -7 -1 1 181.2 4.3 1 8 1 1 62.8 2.8 1 -8 1 1 61.3 2.8 1 8 -1 1 62.0 3.0 1 -8 -1 1 64.2 2.7 1 9 1 1 9.7 1.6 1 -9 1 1 8.8 1.7 1 9 -1 1 9.0 1.8 1 -9 -1 1 4.9 1.6 1 10 1 1 10.5 1.7 1 -10 1 1 10.1 1.8 1 10 -1 1 10.8 1.8 1 -10 -1 1 6.8 1.7 1 11 1 1 26.8 2.5 1 -11 1 1 25.9 2.1 1 11 -1 1 30.8 2.4 1 -11 -1 1 28.8 2.3 1 0 2 1 34.5 1.8 1 0 -2 1 35.9 1.6 1 1 2 1 19.4 1.5 1 -1 2 1 25.7 1.7 1 1 -2 1 30.8 1.9 1 -1 -2 1 28.6 1.6 1 2 2 1 514.5 5.4 1 -2 2 1 339.4 5.1 1 2 -2 1 433.1 5.9 1 -2 -2 1 418.6 4.7 1 3 2 1 15.5 1.6 1 -3 2 1 19.4 2.1 1 3 -2 1 15.3 1.8 1 -3 -2 1 18.2 1.6 1 4 2 1 128.4 3.3 1 -4 2 1 87.3 3.1 1 4 -2 1 141.7 3.5 1 -4 -2 1 92.7 2.8 1 5 2 1 133.8 3.4 1 -5 2 1 96.5 3.3 1 5 -2 1 120.5 3.4 1 -5 -2 1 119.3 3.3 1 6 2 1 180.1 4.2 1 -6 2 1 162.8 4.1 1 6 -2 1 171.8 4.0 1 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2.5 1 -8 -3 1 46.0 2.5 1 9 3 1 306.8 6.1 1 -9 3 1 267.4 5.8 1 9 -3 1 303.0 5.9 1 -9 -3 1 295.9 5.8 1 10 3 1 13.4 1.9 1 -10 3 1 8.1 1.7 1 10 -3 1 13.3 1.7 1 -10 -3 1 9.8 1.7 1 11 3 1 36.9 2.7 1 -11 3 1 29.3 2.5 1 11 -3 1 37.4 2.5 1 -11 -3 1 36.0 2.5 1 0 4 1 19.2 1.6 1 0 -4 1 19.3 1.4 1 1 4 1 248.0 4.3 1 -1 4 1 308.9 5.0 1 1 -4 1 276.6 4.3 1 -1 -4 1 349.1 4.9 1 2 4 1 8.2 1.5 1 -2 4 1 12.2 1.5 1 2 -4 1 8.3 1.3 1 -2 -4 1 16.9 1.4 1 3 4 1 162.4 3.7 1 -3 4 1 130.1 3.8 1 3 -4 1 171.9 3.7 1 -3 -4 1 165.9 3.6 1 4 4 1 8.7 1.4 1 -4 4 1 1.9 1.9 1 4 -4 1 12.3 1.4 1 -4 -4 1 5.2 1.5 1 5 4 1 249.2 4.8 1 -5 4 1 242.2 5.8 1 5 -4 1 232.3 4.7 1 -5 -4 1 299.3 5.2 1 6 4 1 3.7 1.7 1 -6 4 1 2.8 2.0 1 6 -4 1 5.7 1.6 1 -6 -4 1 7.5 1.5 1 7 4 1 394.7 6.5 1 -7 4 1 283.1 6.1 1 7 -4 1 371.0 6.2 1 -7 -4 1 355.6 6.1 1 8 4 1 4.8 1.7 1 -8 4 1 2.6 1.7 1 8 -4 1 2.5 1.6 1 -8 -4 1 3.1 1.5 1 9 4 1 47.3 2.8 1 -9 4 1 31.1 2.4 1 9 -4 1 48.8 2.7 1 -9 -4 1 32.9 2.4 1 10 4 1 1.4 1.6 1 -10 4 1 2.1 1.5 1 10 -4 1 1.5 1.8 1 -10 -4 1 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325.6 6.1 1 -8 2 2 323.8 6.3 1 8 -2 2 315.5 5.9 1 -8 -2 2 361.7 6.4 1 9 2 2 155.6 4.7 1 -9 2 2 135.4 4.4 1 9 -2 2 132.8 4.2 1 -9 -2 2 152.8 4.4 1 10 2 2 4.7 1.8 1 -10 2 2 4.1 1.6 1 10 -2 2 2.6 1.8 1 -10 -2 2 2.8 1.5 1 11 2 2 -0.4 1.7 1 -11 2 2 4.4 1.6 1 11 -2 2 2.2 1.7 1 -11 -2 2 3.6 1.6 1 0 3 2 16.0 1.7 1 0 -3 2 17.3 1.5 1 1 3 2 196.6 4.2 1 -1 3 2 132.2 3.6 1 1 -3 2 223.9 4.3 1 -1 -3 2 171.9 3.7 1 2 3 2 262.8 4.7 1 -2 3 2 171.4 4.1 1 2 -3 2 312.2 5.6 1 -2 -3 2 227.5 4.1 1 3 3 2 1110.3 9.5 1 -3 3 2 906.4 9.7 1 3 -3 2 1178.2 11.1 1 -3 -3 2 1132.5 9.2 1 4 3 2 359.3 5.7 1 -4 3 2 156.1 4.6 1 4 -3 2 365.0 6.4 1 -4 -3 2 233.9 4.6 1 5 3 2 364.7 6.0 1 -5 3 2 394.9 7.0 1 5 -3 2 361.4 6.5 1 -5 -3 2 451.0 6.6 1 6 3 2 11.1 1.6 1 -6 3 2 6.7 2.1 1 6 -3 2 8.4 1.6 1 -6 -3 2 9.3 1.7 1 7 3 2 25.9 2.1 1 -7 3 2 21.5 2.3 1 7 -3 2 19.8 2.0 1 -7 -3 2 21.3 1.9 1 8 3 2 4.6 1.7 1 -8 3 2 4.4 1.8 1 8 -3 2 3.3 1.8 1 -8 -3 2 6.5 1.7 1 9 3 2 82.6 3.5 1 -9 3 2 59.7 3.3 1 9 -3 2 72.6 3.1 1 -9 -3 2 65.9 3.1 1 10 3 2 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2 24.0 2.0 1 6 9 2 68.7 3.2 1 -6 9 2 53.3 3.2 1 6 -9 2 84.8 3.4 1 -6 -9 2 82.0 3.5 1 7 9 2 95.6 3.8 1 -7 9 2 85.4 4.1 1 7 -9 2 122.8 4.1 1 -7 -9 2 144.6 4.5 1 0 10 2 112.9 4.1 1 0 -10 2 159.6 4.5 1 1 10 2 25.3 2.1 1 -1 10 2 20.1 2.3 1 1 -10 2 38.9 2.4 1 -1 -10 2 26.1 2.1 1 2 10 2 6.1 1.8 1 -2 10 2 4.0 2.1 1 2 -10 2 7.7 1.8 1 -2 -10 2 9.5 1.7 1 3 10 2 10.1 1.9 1 -3 10 2 4.3 2.4 1 3 -10 2 6.2 1.9 1 -3 -10 2 19.0 1.8 1 4 10 2 347.8 6.9 1 -4 10 2 333.8 7.1 1 4 -10 2 439.1 7.3 1 -4 -10 2 511.8 8.1 1 5 10 2 14.7 1.9 1 -5 10 2 14.3 2.1 1 5 -10 2 22.3 2.0 1 -5 -10 2 20.2 1.9 1 0 11 2 2.3 1.5 1 0 -11 2 1.6 1.6 1 1 11 2 10.1 1.7 1 -1 11 2 7.8 1.9 1 1 -11 2 12.6 1.7 1 -1 -11 2 13.1 1.8 1 2 11 2 39.3 2.6 1 -2 11 2 33.7 2.8 1 2 -11 2 55.1 2.9 1 -2 -11 2 48.8 2.8 1 3 11 2 80.3 3.7 1 -3 11 2 73.4 3.7 1 3 -11 2 111.9 4.0 1 -3 -11 2 113.3 4.1 1 4 11 2 31.9 2.5 1 -4 11 2 17.1 2.2 1 -4 -11 2 31.5 2.4 1 0 0 3 0.8 1.9 1 1 0 3 399.2 6.0 1 -1 0 3 359.6 5.9 1 2 0 3 0.5 1.7 1 -2 0 3 0.7 1.6 1 3 0 3 825.0 8.9 1 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2.5 1 3 0 4 1.6 1.9 1 -3 0 4 1.6 1.8 1 4 0 4 168.8 4.7 1 -4 0 4 138.2 4.3 1 5 0 4 -1.1 2.0 1 -5 0 4 -1.0 1.7 1 6 0 4 81.4 3.5 1 -6 0 4 47.7 2.9 1 7 0 4 -0.4 1.8 1 -7 0 4 0.3 1.6 1 8 0 4 651.0 9.5 1 -8 0 4 806.1 10.5 1 9 0 4 -1.0 1.8 1 -9 0 4 0.7 1.6 1 10 0 4 15.6 2.2 1 -10 0 4 17.3 2.4 1 0 1 4 159.9 4.4 1 0 -1 4 193.3 5.0 1 1 1 4 311.2 6.1 1 -1 1 4 187.6 4.9 1 1 -1 4 331.6 6.4 1 -1 -1 4 246.6 5.4 1 2 1 4 52.2 3.0 1 -2 1 4 126.9 4.2 1 2 -1 4 52.6 3.0 1 -2 -1 4 129.5 4.0 1 3 1 4 448.6 7.2 1 -3 1 4 388.0 6.9 1 3 -1 4 464.6 7.6 1 -3 -1 4 423.7 6.9 1 4 1 4 -0.9 2.0 1 -4 1 4 2.5 1.9 1 4 -1 4 2.6 2.0 1 -4 -1 4 1.2 1.6 1 5 1 4 197.1 5.0 1 -5 1 4 304.8 6.3 1 5 -1 4 210.6 5.3 1 -5 -1 4 284.4 6.0 1 6 1 4 147.3 4.5 1 -6 1 4 125.5 4.2 1 6 -1 4 144.6 4.5 1 -6 -1 4 127.2 4.2 1 7 1 4 49.6 2.9 1 -7 1 4 46.1 2.9 1 7 -1 4 46.5 3.0 1 -7 -1 4 47.4 2.8 1 8 1 4 170.8 5.1 1 -8 1 4 113.7 4.2 1 8 -1 4 166.6 4.9 1 -8 -1 4 112.7 4.2 1 9 1 4 94.1 3.8 1 -9 1 4 57.8 3.3 1 9 -1 4 83.7 3.6 1 -9 -1 4 65.0 3.3 1 10 1 4 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3.7 1 -7 -1 6 81.0 3.6 1 8 1 6 79.8 3.8 1 -8 1 6 49.4 3.2 1 8 -1 6 70.6 3.8 1 -8 -1 6 50.9 3.2 1 0 2 6 384.6 7.7 1 0 -2 6 489.6 8.4 1 1 2 6 124.8 4.4 1 -1 2 6 47.7 3.1 1 1 -2 6 150.7 4.8 1 -1 -2 6 72.4 3.4 1 2 2 6 1.7 2.1 1 -2 2 6 1.8 1.8 1 2 -2 6 3.4 1.9 1 -2 -2 6 1.0 1.9 1 3 2 6 37.3 2.7 1 -3 2 6 90.1 4.2 1 3 -2 6 35.7 3.1 1 -3 -2 6 102.9 4.0 1 4 2 6 431.3 7.9 1 -4 2 6 571.6 9.2 1 4 -2 6 442.5 8.6 1 -4 -2 6 616.8 9.1 1 5 2 6 56.6 3.5 1 -5 2 6 39.7 2.9 1 5 -2 6 61.5 3.8 1 -5 -2 6 43.3 2.9 1 6 2 6 4.0 2.0 1 -6 2 6 11.5 1.8 1 6 -2 6 6.7 2.0 1 -6 -2 6 13.6 2.1 1 7 2 6 14.7 2.3 1 -7 2 6 32.4 2.6 1 7 -2 6 14.3 2.3 1 -7 -2 6 35.0 2.6 1 0 3 6 1.4 2.0 1 0 -3 6 2.2 2.0 1 1 3 6 82.1 3.7 1 -1 3 6 45.1 3.4 1 1 -3 6 115.2 4.3 1 -1 -3 6 80.4 3.7 1 2 3 6 47.2 3.0 1 -2 3 6 17.9 2.6 1 2 -3 6 57.2 3.3 1 -2 -3 6 35.1 2.6 1 3 3 6 184.2 5.4 1 -3 3 6 145.5 5.1 1 3 -3 6 227.2 6.0 1 -3 -3 6 193.9 5.3 1 4 3 6 124.7 4.6 1 -4 3 6 70.9 3.5 1 4 -3 6 151.0 5.3 1 -4 -3 6 91.3 3.8 1 5 3 6 54.2 3.4 1 -5 3 6 110.5 4.3 1 5 -3 6 57.6 3.7 1 -5 -3 6 115.8 4.3 1 6 3 6 40.5 2.9 1 -6 3 6 27.2 2.6 1 6 -3 6 43.8 3.2 1 -6 -3 6 31.7 2.5 1 7 3 6 16.4 2.1 1 -7 3 6 19.7 2.1 1 7 -3 6 15.4 2.4 1 -7 -3 6 19.2 2.3 1 0 4 6 41.9 3.0 1 0 -4 6 67.7 3.4 1 1 4 6 7.1 1.8 1 -1 4 6 -1.6 2.3 1 1 -4 6 4.5 2.0 1 -1 -4 6 0.8 2.0 1 2 4 6 269.2 6.2 1 -2 4 6 419.4 8.3 1 2 -4 6 393.2 7.8 1 -2 -4 6 523.6 8.5 1 3 4 6 3.7 2.0 1 -3 4 6 3.8 2.4 1 3 -4 6 4.6 2.3 1 -3 -4 6 7.4 1.9 1 4 4 6 42.9 3.0 1 -4 4 6 86.8 4.0 1 4 -4 6 50.7 3.6 1 -4 -4 6 92.6 3.9 1 5 4 6 0.5 2.0 1 -5 4 6 -3.0 2.0 1 5 -4 6 6.1 2.3 1 -5 -4 6 1.2 1.9 1 6 4 6 295.5 6.6 1 -6 4 6 293.9 6.8 1 6 -4 6 319.5 7.7 1 -6 -4 6 331.9 7.2 1 7 4 6 1.3 1.8 1 -7 4 6 2.2 1.9 1 7 -4 6 0.8 2.2 1 -7 -4 6 4.9 1.7 1 0 5 6 5.3 1.9 1 0 -5 6 3.2 1.9 1 1 5 6 91.4 3.9 1 -1 5 6 57.8 3.5 1 1 -5 6 146.2 4.6 1 -1 -5 6 91.0 3.7 1 2 5 6 70.9 3.6 1 -2 5 6 29.0 2.8 1 2 -5 6 98.8 4.3 1 -2 -5 6 52.3 3.0 1 3 5 6 75.4 3.6 1 -3 5 6 46.0 3.3 1 3 -5 6 98.2 4.2 1 -3 -5 6 72.3 3.6 1 4 5 6 59.2 3.3 1 -4 5 6 24.6 2.8 1 4 -5 6 82.0 3.9 1 -4 -5 6 41.4 2.8 1 5 5 6 38.4 2.9 1 -5 5 6 86.4 4.1 1 5 -5 6 48.5 3.6 1 -5 -5 6 99.5 4.1 1 6 5 6 19.3 2.3 1 -6 5 6 16.8 2.3 1 6 -5 6 23.2 2.6 1 -6 -5 6 18.9 2.2 1 0 6 6 302.1 6.8 1 0 -6 6 440.9 8.2 1 1 6 6 28.8 2.6 1 -1 6 6 11.6 2.0 1 1 -6 6 36.7 2.8 1 -1 -6 6 18.6 2.1 1 2 6 6 4.2 1.9 1 -2 6 6 1.7 1.9 1 2 -6 6 5.0 1.9 1 -2 -6 6 0.5 1.9 1 3 6 6 11.5 2.0 1 -3 6 6 21.1 2.9 1 3 -6 6 18.7 2.3 1 -3 -6 6 31.1 2.6 1 4 6 6 143.2 4.8 1 -4 6 6 151.2 5.5 1 4 -6 6 216.0 6.3 1 -4 -6 6 209.3 5.7 1 5 6 6 21.9 2.3 1 -5 6 6 4.0 2.3 1 5 -6 6 27.0 2.8 1 -5 -6 6 14.0 2.1 1 0 7 6 76.5 3.8 1 0 -7 6 109.4 4.5 1 1 7 6 63.8 3.6 1 -1 7 6 77.8 3.7 1 1 -7 6 95.4 4.0 1 -1 -7 6 105.6 4.1 1 2 7 6 13.2 2.2 1 -2 7 6 9.7 2.2 1 2 -7 6 17.6 2.1 1 -2 -7 6 21.0 2.2 1 3 7 6 18.4 2.2 1 -3 7 6 23.0 2.6 1 3 -7 6 25.1 2.5 1 -3 -7 6 29.6 2.6 1 4 7 6 2.4 1.9 1 -4 7 6 9.6 2.2 1 4 -7 6 6.7 2.2 1 -4 -7 6 14.7 2.1 1 0 8 6 9.0 2.0 1 0 -8 6 16.6 2.1 1 1 8 6 10.0 2.0 1 -1 8 6 2.4 2.3 1 1 -8 6 11.0 2.0 1 -1 -8 6 10.1 1.8 1 2 8 6 209.5 5.8 1 -2 8 6 127.9 4.7 1 2 -8 6 273.3 6.7 1 -2 -8 6 208.3 5.9 1 0 0 7 -2.0 2.0 1 1 0 7 21.3 2.4 1 -1 0 7 9.5 2.1 1 2 0 7 2.8 2.2 1 -2 0 7 0.5 1.9 1 3 0 7 133.9 4.9 1 -3 0 7 77.3 3.7 1 4 0 7 -3.0 2.2 1 -4 0 7 1.9 1.8 1 5 0 7 77.3 3.8 1 -5 0 7 73.0 3.5 1 6 0 7 2.3 1.9 1 -6 0 7 0.0 1.8 1 0 1 7 3.9 2.1 1 0 -1 7 6.9 1.9 1 1 1 7 29.3 2.8 1 -1 1 7 65.7 3.7 1 1 -1 7 35.6 2.9 1 -1 -1 7 75.0 3.7 1 2 1 7 16.8 2.3 1 -2 1 7 21.4 2.5 1 2 -1 7 23.1 2.6 1 -2 -1 7 21.7 2.3 1 3 1 7 103.1 4.5 1 -3 1 7 196.5 5.6 1 3 -1 7 112.0 4.7 1 -3 -1 7 220.5 5.9 1 4 1 7 2.0 2.3 1 -4 1 7 8.3 2.1 1 4 -1 7 5.6 2.5 1 -4 -1 7 5.1 2.1 1 5 1 7 113.3 4.4 1 -5 1 7 127.8 4.5 1 5 -1 7 119.8 4.7 1 -5 -1 7 126.2 4.6 1 6 1 7 9.7 2.5 1 -6 1 7 10.0 1.8 1 6 -1 7 12.4 2.2 1 -6 -1 7 9.0 2.1 1 0 2 7 52.0 3.2 1 0 -2 7 64.0 3.5 1 1 2 7 44.5 3.0 1 -1 2 7 23.3 2.7 1 1 -2 7 53.6 3.2 1 -1 -2 7 32.9 2.7 1 2 2 7 9.6 2.3 1 -2 2 7 14.7 2.3 1 2 -2 7 12.4 2.2 1 -2 -2 7 16.1 2.2 1 3 2 7 40.5 2.8 1 -3 2 7 26.3 2.7 1 3 -2 7 50.7 3.4 1 -3 -2 7 27.8 2.4 1 4 2 7 28.0 2.7 1 -4 2 7 34.7 2.8 1 4 -2 7 35.9 3.2 1 -4 -2 7 33.9 2.5 1 5 2 7 18.7 2.4 1 -5 2 7 11.5 2.0 1 5 -2 7 19.8 2.6 1 -5 -2 7 14.0 2.2 1 6 2 7 6.7 2.1 1 -6 2 7 12.7 1.8 1 6 -2 7 9.3 2.2 1 -6 -2 7 14.0 1.9 1 0 3 7 6.8 2.1 1 0 -3 7 2.9 1.9 1 1 3 7 118.4 4.7 1 -1 3 7 68.7 3.9 1 1 -3 7 160.1 5.1 1 -1 -3 7 108.4 4.3 1 2 3 7 14.6 2.0 1 -2 3 7 10.2 2.4 1 2 -3 7 21.0 2.4 1 -2 -3 7 13.1 2.0 1 3 3 7 81.2 3.9 1 -3 3 7 45.3 3.1 1 3 -3 7 102.3 4.3 1 -3 -3 7 70.1 3.4 1 4 3 7 5.9 2.0 1 -4 3 7 11.0 2.1 1 4 -3 7 2.1 2.2 1 -4 -3 7 9.5 1.7 1 5 3 7 30.6 2.7 1 -5 3 7 70.7 3.8 1 5 -3 7 38.4 3.2 1 -5 -3 7 87.7 3.8 1 0 4 7 2.2 2.1 1 0 -4 7 2.2 1.9 1 1 4 7 71.5 3.7 1 -1 4 7 64.5 3.7 1 1 -4 7 96.3 4.1 1 -1 -4 7 90.2 4.0 1 2 4 7 2.5 1.8 1 -2 4 7 3.1 1.9 1 2 -4 7 4.6 2.2 1 -2 -4 7 0.9 1.7 1 3 4 7 4.5 2.1 1 -3 4 7 0.6 2.2 1 3 -4 7 9.7 2.2 1 -3 -4 7 3.9 1.9 1 4 4 7 3.0 1.7 1 -4 4 7 0.0 2.0 1 4 -4 7 1.4 2.0 1 -4 -4 7 1.2 1.8 1 5 4 7 5.4 2.1 1 -5 4 7 9.1 2.3 1 5 -4 7 1.8 2.5 1 -5 -4 7 10.5 1.8 1 0 5 7 3.2 2.2 1 0 -5 7 6.6 2.0 1 1 5 7 78.2 3.9 1 -1 5 7 54.4 3.5 1 1 -5 7 109.2 4.5 1 -1 -5 7 98.0 4.0 1 2 5 7 14.9 2.1 1 -2 5 7 7.7 2.2 1 2 -5 7 20.4 2.3 1 -2 -5 7 14.4 2.0 1 3 5 7 49.4 3.1 1 -3 5 7 35.6 3.0 1 3 -5 7 62.7 3.6 1 -3 -5 7 54.3 3.3 1 4 5 7 5.2 1.7 1 -4 5 7 7.4 2.2 1 4 -5 7 6.1 2.1 1 -4 -5 7 6.8 2.1 1 0 6 7 16.6 2.3 1 0 -6 7 23.7 2.3 1 1 6 7 17.4 2.4 1 -1 6 7 3.8 2.1 1 1 -6 7 17.1 2.3 1 -1 -6 7 13.1 1.9 1 2 6 7 4.8 2.0 1 -2 6 7 9.0 2.0 1 2 -6 7 9.3 1.9 1 -2 -6 7 11.8 1.8 1 0 0 8 430.9 8.6 1 1 0 8 6.2 2.0 1 -1 0 8 -1.5 1.9 1 2 0 8 17.5 2.2 1 -2 0 8 12.6 2.2 1 3 0 8 0.6 2.1 1 -3 0 8 1.7 1.7 1 0 1 8 66.9 3.9 1 0 -1 8 76.3 3.8 1 1 1 8 103.1 4.4 1 -1 1 8 62.6 3.6 1 1 -1 8 120.1 4.6 1 -1 -1 8 72.7 3.8 1 2 1 8 29.5 2.9 1 -2 1 8 29.5 2.8 1 2 -1 8 33.5 2.8 1 -2 -1 8 34.4 2.7 1 3 1 8 48.4 3.3 1 -3 1 8 40.4 2.9 1 3 -1 8 59.8 3.6 1 -3 -1 8 42.0 2.9 1 0 2 8 0.0 1.9 1 0 -2 8 1.2 1.9 1 1 2 8 28.6 2.7 1 -1 2 8 12.7 2.3 1 1 -2 8 27.6 2.5 1 -1 -2 8 16.8 2.4 1 2 2 8 181.9 5.8 1 -2 2 8 238.6 6.6 1 2 -2 8 230.2 6.4 1 -2 -2 8 258.0 6.4 1 0 3 8 4.5 2.0 1 0 -3 8 0.3 1.9 1 1 3 8 37.5 3.1 1 -1 3 8 72.1 3.9 1 1 -3 8 53.3 3.2 1 -1 -3 8 74.8 3.8 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 37172 #==END data_OLI_50C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2309(9) _cell_length_b 8.6149(8) _cell_length_c 5.9377(7) _cell_angle_alpha 90 _cell_angle_beta 90.053(10) _cell_angle_gamma 90 _cell_volume 421.03(8) _cell_formula_units_Z 4 _cell_measurement_temperature 323(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.465 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.807 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 323(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1749 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.364 _diffrn_reflns_theta_max 26.517 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 877 _reflns_number_gt 773 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.339(4) ref 1 0 0 0 1 0 0 0 1 2 0.661(4) pmt -1 0 0 0 -1 0 0 0 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 877 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.00071(18) 0.00059(17) 0.24946(16) 0.0199(3) Uani 1 1 d . . . . . Cu2 Cu 0.13680(12) 0.61878(11) -0.0232(2) 0.0218(3) Uani 1 1 d . . . . . As1 As 0.23758(9) 0.25010(8) 0.01027(17) 0.0178(2) Uani 1 1 d . . . . . O1 O 0.3687(9) 0.2534(7) 0.2231(11) 0.0226(16) Uani 1 1 d . . . . . O1' O 0.3340(10) 0.2768(8) -0.2366(12) 0.0251(16) Uani 1 1 d . . . . . O2 O 0.1324(7) 0.0804(6) 0.0027(13) 0.0210(11) Uani 1 1 d . . . . . O3 O 0.0998(7) 0.3943(7) 0.0495(12) 0.0251(15) Uani 1 1 d . . . . . O4 O 0.3730(7) 0.5962(6) -0.0002(13) 0.0186(10) Uani 1 1 d . . . . . H1 H 0.4198 0.6825 -0.0063 0.022 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0222(4) 0.0246(5) 0.0130(5) -0.0004(5) 0.0045(8) -0.0048(4) Cu2 0.0183(4) 0.0232(5) 0.0238(6) 0.0029(6) 0.0003(5) 0.0011(4) As1 0.0187(4) 0.0198(4) 0.0147(4) 0.0004(4) 0.0025(5) -0.0004(3) O1 0.026(4) 0.026(4) 0.016(3) 0.005(2) -0.011(3) -0.003(3) O1' 0.032(4) 0.023(3) 0.021(4) -0.003(3) 0.004(3) -0.005(3) O2 0.025(2) 0.021(2) 0.017(3) -0.001(3) 0.004(4) -0.002(2) O3 0.020(3) 0.023(3) 0.032(4) 0.003(3) -0.001(3) 0.000(2) O4 0.019(2) 0.022(2) 0.015(2) 0.000(3) 0.001(4) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.955(7) . ? Cu1 O2 1.975(7) 3 ? Cu1 O4 1.997(7) 4_566 ? Cu1 O4 2.000(7) 2_545 ? Cu1 O1' 2.353(7) 4_566 ? Cu1 O1 2.396(6) 2_545 ? Cu1 Cu1 2.9625(19) 3 ? Cu1 Cu1 2.975(2) 3_556 ? Cu2 O3 1.957(6) 3_565 ? Cu2 O4 1.958(6) . ? Cu2 O1' 1.987(7) 2_554 ? Cu2 O3 2.005(6) . ? Cu2 O1 2.127(6) 2 ? Cu2 Cu2 3.056(2) 3_565 ? As1 O1 1.662(7) . ? As1 O1' 1.683(7) . ? As1 O3 1.698(6) . ? As1 O2 1.699(5) . ? O1 Cu2 2.127(6) 2_545 ? O1 Cu1 2.396(6) 2 ? O1' Cu2 1.987(7) 2_544 ? O1' Cu1 2.353(7) 4_665 ? O2 Cu1 1.975(7) 3 ? O2 O2 2.583(11) 3 ? O2 O4 2.958(10) 2_545 ? O2 O4 2.987(10) 2_544 ? O3 Cu2 1.957(6) 3_565 ? O3 O3 2.521(12) 3_565 ? O4 Cu1 1.997(7) 4_665 ? O4 Cu1 2.000(7) 2 ? O4 O4 2.668(10) 3_665 ? O4 H1 0.8385 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 82.2(2) . 3 ? O2 Cu1 O4 175.6(2) . 4_566 ? O2 Cu1 O4 97.5(2) 3 4_566 ? O2 Cu1 O4 96.8(2) . 2_545 ? O2 Cu1 O4 176.3(2) 3 2_545 ? O4 Cu1 O4 83.8(2) 4_566 2_545 ? O2 Cu1 O1' 93.7(2) . 4_566 ? O2 Cu1 O1' 89.9(3) 3 4_566 ? O4 Cu1 O1' 90.7(2) 4_566 4_566 ? O4 Cu1 O1' 86.7(3) 2_545 4_566 ? O2 Cu1 O1 96.3(2) . 2_545 ? O2 Cu1 O1 89.2(2) 3 2_545 ? O4 Cu1 O1 79.3(2) 4_566 2_545 ? O4 Cu1 O1 94.4(2) 2_545 2_545 ? O1' Cu1 O1 169.8(3) 4_566 2_545 ? O2 Cu1 Cu1 41.3(2) . 3 ? O2 Cu1 Cu1 40.83(19) 3 3 ? O4 Cu1 Cu1 138.2(2) 4_566 3 ? O4 Cu1 Cu1 138.0(2) 2_545 3 ? O1' Cu1 Cu1 92.34(19) 4_566 3 ? O1 Cu1 Cu1 93.59(17) 2_545 3 ? O2 Cu1 Cu1 138.5(2) . 3_556 ? O2 Cu1 Cu1 139.3(2) 3 3_556 ? O4 Cu1 Cu1 41.9(2) 4_566 3_556 ? O4 Cu1 Cu1 41.86(18) 2_545 3_556 ? O1' Cu1 Cu1 88.24(19) 4_566 3_556 ? O1 Cu1 Cu1 85.86(17) 2_545 3_556 ? Cu1 Cu1 Cu1 179.40(12) 3 3_556 ? O3 Cu2 O4 171.0(2) 3_565 . ? O3 Cu2 O1' 95.9(3) 3_565 2_554 ? O4 Cu2 O1' 89.9(3) . 2_554 ? O3 Cu2 O3 79.1(3) 3_565 . ? O4 Cu2 O3 92.3(2) . . ? O1' Cu2 O3 146.5(3) 2_554 . ? O3 Cu2 O1 94.4(3) 3_565 2 ? O4 Cu2 O1 91.0(3) . 2 ? O1' Cu2 O1 103.3(3) 2_554 2 ? O3 Cu2 O1 110.0(3) . 2 ? O3 Cu2 Cu2 40.10(17) 3_565 3_565 ? O4 Cu2 Cu2 131.20(16) . 3_565 ? O1' Cu2 Cu2 127.8(2) 2_554 3_565 ? O3 Cu2 Cu2 38.95(17) . 3_565 ? O1 Cu2 Cu2 105.9(2) 2 3_565 ? O1 As1 O1' 110.7(3) . . ? O1 As1 O3 108.5(3) . . ? O1' As1 O3 109.6(4) . . ? O1 As1 O2 111.4(3) . . ? O1' As1 O2 109.6(3) . . ? O3 As1 O2 107.0(3) . . ? As1 O1 Cu2 127.9(4) . 2_545 ? As1 O1 Cu1 111.2(3) . 2 ? Cu2 O1 Cu1 116.0(3) 2_545 2 ? As1 O1' Cu2 126.1(4) . 2_544 ? As1 O1' Cu1 114.5(3) . 4_665 ? Cu2 O1' Cu1 117.6(3) 2_544 4_665 ? As1 O2 Cu1 124.6(4) . . ? As1 O2 Cu1 127.1(4) . 3 ? Cu1 O2 Cu1 97.8(2) . 3 ? As1 O2 O2 153.1(4) . 3 ? Cu1 O2 O2 49.2(2) . 3 ? Cu1 O2 O2 48.6(2) 3 3 ? As1 O2 O4 86.7(3) . 2_545 ? Cu1 O2 O4 42.17(18) . 2_545 ? Cu1 O2 O4 139.9(3) 3 2_545 ? O2 O2 O4 91.4(4) 3 2_545 ? As1 O2 O4 89.7(3) . 2_544 ? Cu1 O2 O4 139.2(3) . 2_544 ? Cu1 O2 O4 41.52(19) 3 2_544 ? O2 O2 O4 90.0(4) 3 2_544 ? O4 O2 O4 174.5(3) 2_545 2_544 ? As1 O3 Cu2 127.7(3) . 3_565 ? As1 O3 Cu2 125.1(3) . . ? Cu2 O3 Cu2 100.9(3) 3_565 . ? As1 O3 O3 158.6(6) . 3_565 ? Cu2 O3 O3 51.3(2) 3_565 3_565 ? Cu2 O3 O3 49.6(2) . 3_565 ? Cu2 O4 Cu1 120.5(4) . 4_665 ? Cu2 O4 Cu1 127.9(4) . 2 ? Cu1 O4 Cu1 96.2(2) 4_665 2 ? Cu2 O4 O4 147.1(3) . 3_665 ? Cu1 O4 O4 48.2(2) 4_665 3_665 ? Cu1 O4 O4 48.1(2) 2 3_665 ? Cu2 O4 H1 111.4 . . ? Cu1 O4 H1 95.7 4_665 . ? Cu1 O4 H1 99.0 2 . ? O4 O4 H1 101.0 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.84 2.24 2.821(9) 127.0 3_665 O4 H1 O1' 0.84 2.51 2.998(10) 118.0 3_665 _refine_diff_density_max 1.679 _refine_diff_density_min -1.749 _refine_diff_density_rms 0.289 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite joh 50C in P 21/n CELL .71073 8.2309 8.6149 5.9377 90.000 90.053 90.000 ZERR 4 .0009 .0008 .0007 .00 .010 .00 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z EQIV $6 -x+1/2, y-1/2, -z-1/2 BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O2 O4_$6 BIND O3 O3_$3 HTAB O4 O1_$5 HTAB O4 O1'_$5 L.S. 5 LIST 4 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 1 PLAN 25 WGHT 0.055800 BASF 0.66101 FVAR 0.31740 CU1 3 -0.000708 0.000586 0.249460 11.00000 0.02215 0.02457 = 0.01300 -0.00035 0.00450 -0.00478 CU2 3 0.136800 0.618780 -0.023213 11.00000 0.01828 0.02321 = 0.02384 0.00293 0.00030 0.00106 AS1 4 0.237579 0.250101 0.010266 11.00000 0.01872 0.01984 = 0.01473 0.00041 0.00252 -0.00039 O1 2 0.368703 0.253430 0.223146 11.00000 0.02630 0.02573 = 0.01575 0.00455 -0.01065 -0.00341 O1' 2 0.334007 0.276825 -0.236575 11.00000 0.03152 0.02266 = 0.02108 -0.00325 0.00416 -0.00475 O2 2 0.132414 0.080416 0.002699 11.00000 0.02457 0.02110 = 0.01730 -0.00086 0.00356 -0.00155 O3 2 0.099776 0.394313 0.049469 11.00000 0.01957 0.02345 = 0.03232 0.00324 -0.00097 0.00006 O4 2 0.372950 0.596182 -0.000225 11.00000 0.01861 0.02157 = 0.01548 0.00035 0.00066 -0.00039 AFIX 3 H1 1 0.419750 0.682532 -0.006315 11.00000 -1.20000 AFIX 0 HKLF 4 REM olivenite joh 50C in P 21/n REM R1 = 0.0374 for 773 Fo > 4sig(Fo) and 0.0455 for all 877 data REM 74 parameters refined using 0 restraints END WGHT 0.0558 0.0000 REM Highest difference peak 1.679, deepest hole -1.749, 1-sigma level 0.289 Q1 1 0.1784 0.6059 -0.1207 11.00000 0.05 1.68 Q2 1 0.1899 0.2449 0.0994 11.00000 0.05 1.66 Q3 1 0.1040 0.5685 0.0321 11.00000 0.05 1.06 Q4 1 0.3017 0.2585 -0.1777 11.00000 0.05 1.01 Q5 1 0.2286 0.1179 -0.0381 11.00000 0.05 0.87 Q6 1 0.1017 0.6993 0.0363 11.00000 0.05 0.83 Q7 1 0.1209 0.2489 -0.0256 11.00000 0.05 0.83 Q8 1 0.3271 0.5881 0.1217 11.00000 0.05 0.83 Q9 1 0.4669 0.3430 -0.1529 11.00000 0.05 0.78 Q10 1 0.4400 0.2729 0.1288 11.00000 0.05 0.76 Q11 1 -0.0198 0.3963 0.0800 11.00000 0.05 0.75 Q12 1 0.1718 0.0681 -0.0551 11.00000 0.05 0.75 Q13 1 0.2609 0.3695 -0.0224 11.00000 0.05 0.74 Q14 1 0.2583 0.5847 -0.0361 11.00000 0.05 0.71 Q15 1 0.2769 0.2361 -0.0545 11.00000 0.05 0.65 Q16 1 0.3075 0.4601 0.0299 11.00000 0.05 0.62 Q17 1 0.0746 0.3971 0.1448 11.00000 0.05 0.60 Q18 1 -0.0287 -0.1042 0.2942 11.00000 0.05 0.60 Q19 1 -0.0411 0.0150 0.3437 11.00000 0.05 0.60 Q20 1 0.2416 0.4360 0.3048 11.00000 0.05 0.58 Q21 1 0.1592 0.4835 0.1950 11.00000 0.05 0.58 Q22 1 0.4997 0.8226 0.0980 11.00000 0.05 0.58 Q23 1 0.3054 -0.0233 -0.0635 11.00000 0.05 0.56 Q24 1 0.0440 -0.0007 0.1345 11.00000 0.05 0.56 Q25 1 0.0670 0.1244 0.0340 11.00000 0.05 0.56 ; _shelx_res_checksum 27096 _shelx_hkl_file ; 1 0 0 -2.0 1.1 1 2 0 0 141.6 3.3 1 3 0 0 -4.0 3.2 1 4 0 0 21.7 3.4 1 5 0 0 4.8 3.7 1 6 0 0 72.4 4.3 1 7 0 0 12.2 4.5 1 8 0 0 1627.7 13.2 1 9 0 0 -5.9 4.0 1 10 0 0 33.5 3.4 1 0 1 0 2.7 0.9 1 1 1 0 609.9 4.0 1 -1 1 0 614.5 4.0 1 2 1 0 342.4 4.4 1 -2 1 0 311.2 4.1 1 3 1 0 1489.9 9.0 1 -3 1 0 1416.2 10.7 1 4 1 0 10.3 3.2 1 -4 1 0 22.7 4.6 1 5 1 0 717.7 7.9 1 -5 1 0 673.8 8.0 1 6 1 0 380.8 6.7 1 -6 1 0 356.7 6.8 1 7 1 0 66.6 4.6 1 -7 1 0 66.3 4.3 1 8 1 0 302.4 6.6 1 -8 1 0 279.3 6.3 1 9 1 0 75.6 4.4 1 -9 1 0 73.1 4.4 1 10 1 0 12.2 3.9 1 -10 1 0 17.7 3.5 1 0 2 0 87.4 2.4 1 1 2 0 785.9 5.8 1 -1 2 0 958.5 6.3 1 2 2 0 3768.6 13.1 1 -2 2 0 3663.2 13.0 1 3 2 0 242.9 4.4 1 -3 2 0 247.7 4.4 1 4 2 0 2.9 3.2 1 -4 2 0 7.3 3.0 1 5 2 0 577.7 7.4 1 -5 2 0 588.0 7.7 1 6 2 0 1057.4 10.2 1 -6 2 0 1048.7 12.6 1 7 2 0 24.8 3.5 1 -7 2 0 12.4 6.2 1 8 2 0 8.4 3.9 1 -8 2 0 6.4 4.7 1 9 2 0 169.3 5.5 1 -9 2 0 153.7 5.7 1 10 2 0 251.4 6.4 1 -10 2 0 208.4 6.3 1 0 3 0 18.6 2.1 1 1 3 0 1533.5 8.8 1 -1 3 0 1539.5 8.8 1 2 3 0 22.4 2.3 1 -2 3 0 17.9 1.9 1 3 3 0 214.0 4.6 1 -3 3 0 204.6 4.4 1 4 3 0 96.3 3.6 1 -4 3 0 99.5 3.7 1 5 3 0 158.7 4.8 1 -5 3 0 147.6 4.7 1 6 3 0 58.0 4.2 1 -6 3 0 51.3 4.6 1 7 3 0 421.8 7.3 1 -7 3 0 409.3 7.3 1 8 3 0 13.7 4.2 1 -8 3 0 8.6 4.2 1 9 3 0 115.6 5.0 1 -9 3 0 109.2 5.8 1 0 4 0 762.9 7.1 1 1 4 0 133.5 3.6 1 -1 4 0 143.7 3.5 1 2 4 0 13.4 2.5 1 -2 4 0 8.1 2.9 1 3 4 0 13.0 3.4 1 -3 4 0 7.9 3.2 1 4 4 0 3568.0 16.7 1 -4 4 0 3418.3 16.4 1 5 4 0 79.1 4.0 1 -5 4 0 83.6 4.1 1 6 4 0 21.5 4.4 1 -6 4 0 13.7 3.5 1 7 4 0 -4.9 4.2 1 -7 4 0 2.2 3.4 1 8 4 0 112.5 4.9 1 -8 4 0 103.6 4.5 1 9 4 0 6.5 4.2 1 -9 4 0 10.2 3.4 1 0 5 0 -1.7 3.3 1 1 5 0 1135.2 9.4 1 -1 5 0 1138.6 9.4 1 2 5 0 102.8 3.9 1 -2 5 0 109.8 3.7 1 3 5 0 41.1 3.5 1 -3 5 0 42.5 3.1 1 4 5 0 85.3 4.2 1 -4 5 0 83.4 3.8 1 5 5 0 119.2 4.5 1 -5 5 0 111.0 4.7 1 6 5 0 0.1 4.1 1 -6 5 0 -3.6 3.4 1 7 5 0 323.3 6.8 1 -7 5 0 315.9 6.6 1 8 5 0 28.3 3.5 1 -8 5 0 28.9 3.2 1 9 5 0 53.9 4.1 1 -9 5 0 51.3 4.1 1 0 6 0 542.9 7.3 1 1 6 0 283.6 5.6 1 -1 6 0 271.2 5.5 1 2 6 0 1615.7 12.1 1 -2 6 0 1543.4 11.7 1 3 6 0 68.9 3.8 1 -3 6 0 68.7 4.0 1 4 6 0 97.2 4.2 1 -4 6 0 97.9 4.5 1 5 6 0 185.9 5.3 1 -5 6 0 170.3 5.5 1 6 6 0 536.8 8.3 1 -6 6 0 518.3 7.9 1 7 6 0 1.4 4.0 1 -7 6 0 0.4 3.4 1 8 6 0 44.6 3.6 1 -8 6 0 40.5 3.3 1 0 7 0 4.9 4.2 1 1 7 0 42.5 3.4 1 -1 7 0 45.6 3.3 1 2 7 0 59.2 4.0 1 -2 7 0 49.9 3.5 1 3 7 0 588.9 8.4 1 -3 7 0 589.7 8.2 1 4 7 0 -8.5 4.1 1 -4 7 0 4.1 3.8 1 5 7 0 209.6 5.7 1 -5 7 0 195.8 5.4 1 6 7 0 206.7 6.0 1 -6 7 0 190.6 5.5 1 7 7 0 8.5 3.8 1 -7 7 0 4.0 3.2 1 0 8 0 1987.1 14.4 1 1 8 0 -1.9 4.0 1 -1 8 0 9.4 3.9 1 2 8 0 31.6 3.8 1 -2 8 0 25.8 2.9 1 3 8 0 15.4 3.9 1 -3 8 0 12.0 4.0 1 4 8 0 158.8 5.0 1 -4 8 0 145.5 5.0 1 5 8 0 10.8 3.9 1 -5 8 0 7.0 3.9 1 6 8 0 0.2 3.7 1 -6 8 0 0.3 3.3 1 0 9 0 -4.7 3.9 1 1 9 0 23.1 3.9 1 -1 9 0 15.5 2.7 1 2 9 0 62.0 4.0 1 -2 9 0 62.9 4.2 1 3 9 0 255.1 6.1 1 -3 9 0 227.4 6.0 1 4 9 0 6.0 3.7 1 -4 9 0 6.5 4.0 1 5 9 0 155.0 5.2 1 -5 9 0 159.1 5.4 1 0 10 0 3.9 3.6 1 1 10 0 5.4 3.6 1 -1 10 0 11.4 3.7 1 2 10 0 409.7 7.6 1 -2 10 0 383.9 7.5 1 3 10 0 2.8 3.7 1 -3 10 0 -4.1 3.9 1 0 0 1 6.8 3.0 1 1 0 1 976.8 7.5 1 -1 0 1 954.0 8.0 1 2 0 1 5.1 5.3 1 -2 0 1 3.5 5.7 1 3 0 1 1331.4 10.9 1 -3 0 1 984.5 9.6 1 4 0 1 1.9 4.7 1 -4 0 1 10.1 3.9 1 5 0 1 11.5 5.4 1 -5 0 1 23.8 3.5 1 6 0 1 4.8 5.9 1 -6 0 1 8.4 4.5 1 7 0 1 36.7 6.2 1 -7 0 1 46.8 4.1 1 8 0 1 -5.5 5.1 1 -8 0 1 -3.1 4.0 1 9 0 1 110.2 5.4 1 -9 0 1 94.2 4.6 1 10 0 1 1.5 4.3 1 -10 0 1 0.3 3.6 1 0 1 1 1035.8 7.1 1 0 -1 1 1213.4 7.6 1 1 1 1 720.1 6.5 1 -1 1 1 750.0 7.1 1 1 -1 1 608.3 7.0 1 -1 -1 1 688.6 6.2 1 2 1 1 8.1 4.2 1 -2 1 1 -5.2 4.9 1 2 -1 1 10.8 6.2 1 -2 -1 1 8.7 3.9 1 3 1 1 1385.2 10.1 1 -3 1 1 1464.5 12.1 1 3 -1 1 1283.7 11.9 1 -3 -1 1 1222.6 9.1 1 4 1 1 447.0 6.8 1 -4 1 1 451.1 9.1 1 4 -1 1 437.0 8.6 1 -4 -1 1 389.0 6.2 1 5 1 1 1230.8 11.0 1 -5 1 1 1242.2 14.0 1 5 -1 1 1227.0 13.2 1 -5 -1 1 1134.1 10.1 1 6 1 1 18.3 5.2 1 -6 1 1 12.8 6.4 1 6 -1 1 14.4 7.5 1 -6 -1 1 6.9 4.7 1 7 1 1 196.7 6.2 1 -7 1 1 165.5 6.1 1 7 -1 1 196.8 8.0 1 -7 -1 1 176.9 5.6 1 8 1 1 62.0 4.3 1 -8 1 1 56.8 3.9 1 8 -1 1 67.1 6.5 1 -8 -1 1 62.1 3.8 1 9 1 1 12.6 4.2 1 -9 1 1 -0.5 4.1 1 9 -1 1 7.2 5.2 1 -9 -1 1 5.9 3.8 1 10 1 1 12.0 4.3 1 -10 1 1 4.6 4.1 1 10 -1 1 11.0 5.2 1 -10 -1 1 8.5 3.7 1 0 2 1 15.4 3.0 1 0 -2 1 21.5 3.3 1 1 2 1 10.7 2.7 1 -1 2 1 14.6 3.2 1 1 -2 1 -10.7 3.6 1 -1 -2 1 -1.8 3.3 1 2 2 1 472.1 5.9 1 -2 2 1 457.2 6.5 1 2 -2 1 501.0 6.6 1 -2 -2 1 401.0 5.5 1 3 2 1 15.5 3.2 1 -3 2 1 22.2 3.9 1 3 -2 1 18.7 4.3 1 -3 -2 1 14.2 2.9 1 4 2 1 145.8 4.5 1 -4 2 1 99.7 5.6 1 4 -2 1 171.2 6.8 1 -4 -2 1 89.9 3.8 1 5 2 1 138.7 4.8 1 -5 2 1 123.9 6.7 1 5 -2 1 164.9 8.3 1 -5 -2 1 103.8 4.3 1 6 2 1 178.9 5.6 1 -6 2 1 179.5 7.9 1 6 -2 1 185.7 9.5 1 -6 -2 1 148.6 5.2 1 7 2 1 148.8 5.2 1 -7 2 1 91.2 7.9 1 7 -2 1 141.0 8.5 1 -7 -2 1 100.7 4.8 1 8 2 1 94.7 4.9 1 -8 2 1 58.7 6.5 1 8 -2 1 96.1 7.1 1 -8 -2 1 69.9 4.4 1 9 2 1 74.9 4.4 1 -9 2 1 40.3 4.7 1 9 -2 1 66.3 6.7 1 -9 -2 1 48.9 4.0 1 10 2 1 36.0 4.0 1 -10 2 1 33.7 4.9 1 10 -2 1 36.0 6.0 1 -10 -2 1 26.5 3.5 1 0 3 1 581.3 6.1 1 0 -3 1 540.9 6.1 1 1 3 1 2110.1 11.0 1 -1 3 1 1926.7 10.7 1 1 -3 1 2044.7 11.1 1 -1 -3 1 1780.0 10.2 1 2 3 1 6.1 3.1 1 -2 3 1 3.8 3.2 1 2 -3 1 -2.7 3.5 1 -2 -3 1 3.3 3.3 1 3 3 1 421.6 6.1 1 -3 3 1 379.1 6.1 1 3 -3 1 420.1 6.5 1 -3 -3 1 348.9 5.8 1 4 3 1 241.9 5.2 1 -4 3 1 218.6 5.4 1 4 -3 1 247.0 6.1 1 -4 -3 1 195.9 4.9 1 5 3 1 52.1 3.7 1 -5 3 1 80.7 4.7 1 5 -3 1 55.8 5.5 1 -5 -3 1 79.0 4.3 1 6 3 1 24.8 4.6 1 -6 3 1 31.7 5.6 1 6 -3 1 23.2 6.7 1 -6 -3 1 15.8 4.9 1 7 3 1 226.8 5.9 1 -7 3 1 261.6 7.7 1 7 -3 1 201.2 8.4 1 -7 -3 1 233.0 5.9 1 8 3 1 33.5 3.8 1 -8 3 1 42.3 5.3 1 8 -3 1 26.7 6.7 1 -8 -3 1 43.2 4.0 1 9 3 1 333.6 7.2 1 -9 3 1 268.9 8.7 1 9 -3 1 308.9 10.0 1 -9 -3 1 259.5 6.4 1 0 4 1 18.7 2.4 1 0 -4 1 16.7 2.5 1 1 4 1 286.6 5.1 1 -1 4 1 341.8 5.5 1 1 -4 1 283.0 5.3 1 -1 -4 1 335.7 5.7 1 2 4 1 10.5 3.6 1 -2 4 1 10.2 3.4 1 2 -4 1 10.6 3.6 1 -2 -4 1 11.7 3.9 1 3 4 1 177.3 4.6 1 -3 4 1 167.1 4.7 1 3 -4 1 179.2 5.0 1 -3 -4 1 145.5 4.5 1 4 4 1 14.5 3.8 1 -4 4 1 6.6 4.0 1 4 -4 1 17.4 4.2 1 -4 -4 1 3.1 4.5 1 5 4 1 265.3 6.2 1 -5 4 1 294.3 6.4 1 5 -4 1 259.4 6.8 1 -5 -4 1 255.9 6.0 1 6 4 1 4.0 4.4 1 -6 4 1 10.5 4.2 1 6 -4 1 -2.1 5.1 1 -6 -4 1 1.6 4.6 1 7 4 1 416.2 7.5 1 -7 4 1 336.3 7.0 1 7 -4 1 423.7 8.8 1 -7 -4 1 313.5 6.8 1 8 4 1 2.2 4.3 1 -8 4 1 2.2 4.0 1 8 -4 1 -1.7 5.1 1 -8 -4 1 8.6 4.1 1 9 4 1 57.2 4.1 1 -9 4 1 40.1 4.1 1 9 -4 1 48.3 5.5 1 -9 -4 1 27.8 3.9 1 0 5 1 490.4 6.9 1 0 -5 1 475.4 7.0 1 1 5 1 1296.6 10.4 1 -1 5 1 1200.5 10.0 1 1 -5 1 1229.8 10.3 1 -1 -5 1 1136.0 10.0 1 2 5 1 16.5 2.7 1 -2 5 1 12.7 3.9 1 2 -5 1 19.0 3.2 1 -2 -5 1 11.9 4.4 1 3 5 1 244.5 5.5 1 -3 5 1 216.6 5.6 1 3 -5 1 243.0 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-6 2 5 46.7 5.6 1 6 -2 5 30.0 5.6 1 -6 -2 5 42.7 5.7 1 7 2 5 110.6 6.5 1 -7 2 5 53.5 6.8 1 7 -2 5 93.2 6.6 1 -7 -2 5 33.2 5.5 1 0 3 5 69.7 5.6 1 0 -3 5 50.2 5.6 1 1 3 5 778.2 11.9 1 -1 3 5 558.1 10.4 1 1 -3 5 674.6 11.3 1 -1 -3 5 452.3 9.6 1 2 3 5 14.5 6.3 1 -2 3 5 7.9 6.2 1 2 -3 5 19.8 6.3 1 -2 -3 5 15.8 6.1 1 3 3 5 165.1 6.7 1 -3 3 5 87.6 6.0 1 3 -3 5 139.7 7.0 1 -3 -3 5 70.9 5.8 1 4 3 5 29.8 5.8 1 -4 3 5 38.8 6.3 1 4 -3 5 21.5 6.4 1 -4 -3 5 33.3 5.0 1 5 3 5 56.9 6.0 1 -5 3 5 88.3 6.4 1 5 -3 5 47.3 7.3 1 -5 -3 5 68.1 6.4 1 6 3 5 18.5 5.7 1 -6 3 5 17.3 6.8 1 6 -3 5 32.4 6.3 1 -6 -3 5 3.5 5.5 1 7 3 5 123.2 6.4 1 -7 3 5 191.8 7.9 1 7 -3 5 119.3 7.7 1 -7 -3 5 164.0 7.1 1 0 4 5 13.2 5.8 1 0 -4 5 -0.4 5.7 1 1 4 5 109.0 6.3 1 -1 4 5 179.6 6.6 1 1 -4 5 75.9 5.8 1 -1 -4 5 150.9 6.5 1 2 4 5 -2.9 5.6 1 -2 4 5 2.8 6.0 1 2 -4 5 -5.5 5.9 1 -2 -4 5 5.8 5.7 1 3 4 5 29.6 5.2 1 -3 4 5 28.9 4.4 1 3 -4 5 15.5 6.1 1 -3 -4 5 23.3 4.4 1 4 4 5 -7.4 5.4 1 -4 4 5 8.1 6.0 1 4 -4 5 12.1 5.8 1 -4 -4 5 9.4 5.5 1 5 4 5 52.6 4.7 1 -5 4 5 74.7 5.5 1 5 -4 5 51.7 5.4 1 -5 -4 5 62.6 5.5 1 6 4 5 2.1 4.9 1 -6 4 5 -1.8 6.2 1 6 -4 5 -5.2 6.2 1 -6 -4 5 -3.0 5.5 1 0 5 5 37.8 4.7 1 0 -5 5 36.0 5.4 1 1 5 5 467.1 9.0 1 -1 5 5 412.0 9.0 1 1 -5 5 379.8 9.0 1 -1 -5 5 324.7 8.5 1 2 5 5 37.5 5.4 1 -2 5 5 29.5 5.8 1 2 -5 5 27.8 5.2 1 -2 -5 5 20.2 5.0 1 3 5 5 95.7 4.9 1 -3 5 5 106.9 6.0 1 3 -5 5 82.0 5.7 1 -3 -5 5 64.9 6.3 1 4 5 5 26.7 4.2 1 -4 5 5 43.1 5.6 1 4 -5 5 13.3 5.8 1 -4 -5 5 45.1 5.0 1 5 5 5 24.0 4.4 1 -5 5 5 52.4 4.7 1 5 -5 5 23.1 5.6 1 -5 -5 5 43.8 4.6 1 -6 5 5 8.6 5.7 1 6 -5 5 27.8 6.2 1 -6 -5 5 7.4 5.1 1 0 6 5 74.5 4.6 1 0 -6 5 69.4 5.5 1 1 6 5 14.5 4.1 1 -1 6 5 13.4 5.2 1 1 -6 5 16.6 4.3 1 -1 -6 5 6.8 4.9 1 2 6 5 24.4 3.7 1 -2 6 5 31.3 3.9 1 2 -6 5 25.1 5.3 1 -2 -6 5 34.3 5.0 1 3 6 5 29.6 3.6 1 -3 6 5 7.8 5.4 1 3 -6 5 23.2 5.6 1 -3 -6 5 7.8 5.0 1 4 6 5 40.5 3.9 1 -4 6 5 29.9 4.2 1 4 -6 5 33.5 5.5 1 -4 -6 5 28.0 4.7 1 5 6 5 61.1 4.5 1 -5 6 5 19.7 5.0 1 5 -6 5 44.8 5.1 1 -5 -6 5 16.0 4.0 1 0 7 5 10.1 4.6 1 0 -7 5 11.8 4.8 1 1 7 5 61.6 4.3 1 -1 7 5 108.4 5.6 1 1 -7 5 47.4 5.6 1 -1 -7 5 89.2 5.0 1 2 7 5 14.2 3.4 1 -2 7 5 8.9 4.7 1 2 -7 5 9.0 5.1 1 -2 -7 5 12.6 4.8 1 3 7 5 155.8 5.9 1 -3 7 5 243.1 7.2 1 3 -7 5 116.4 6.3 1 -3 -7 5 192.1 6.7 1 0 8 5 6.6 4.4 1 0 -8 5 10.8 4.7 1 0 0 6 86.6 6.4 1 1 0 6 15.4 6.7 1 -1 0 6 -3.3 6.5 1 2 0 6 914.3 14.0 1 -2 0 6 625.5 11.7 1 3 0 6 37.5 7.8 1 -3 0 6 -1.1 6.3 1 4 0 6 53.5 6.9 1 -4 0 6 47.4 5.5 1 5 0 6 0.7 6.1 1 -5 0 6 8.2 5.7 1 6 0 6 290.0 9.4 1 -6 0 6 432.9 10.4 1 0 1 6 195.7 8.4 1 0 -1 6 176.2 7.3 1 1 1 6 174.9 7.7 1 -1 1 6 268.7 9.1 1 1 -1 6 176.5 7.4 1 -1 -1 6 255.6 8.1 1 2 1 6 72.6 7.1 1 -2 1 6 32.8 6.5 1 2 -1 6 48.3 6.9 1 -2 -1 6 30.5 6.1 1 3 1 6 99.1 6.1 1 -3 1 6 137.8 7.1 1 3 -1 6 88.4 7.1 1 -3 -1 6 114.0 6.9 1 4 1 6 16.0 6.5 1 -4 1 6 21.1 6.6 1 4 -1 6 15.1 6.0 1 -4 -1 6 19.2 4.5 1 5 1 6 185.7 7.7 1 -5 1 6 88.1 6.6 1 5 -1 6 179.6 8.4 1 -5 -1 6 67.9 6.0 1 6 1 6 52.7 5.5 1 -6 1 6 31.2 6.1 1 6 -1 6 57.3 6.8 1 -6 -1 6 29.4 5.3 1 0 2 6 530.3 11.0 1 0 -2 6 491.1 10.0 1 1 2 6 144.0 6.6 1 -1 2 6 67.9 6.6 1 1 -2 6 145.1 6.5 1 -1 -2 6 75.9 6.4 1 2 2 6 -1.0 6.0 1 -2 2 6 5.0 6.6 1 2 -2 6 14.4 6.0 1 -2 -2 6 -7.9 6.4 1 3 2 6 56.3 5.1 1 -3 2 6 108.3 7.2 1 3 -2 6 49.2 6.5 1 -3 -2 6 100.0 6.1 1 4 2 6 646.4 11.6 1 -4 2 6 703.3 12.8 1 4 -2 6 583.3 11.6 1 -4 -2 6 637.5 11.0 1 5 2 6 75.4 5.5 1 -5 2 6 46.1 6.2 1 5 -2 6 67.5 6.5 1 -5 -2 6 41.4 5.3 1 0 3 6 0.0 5.9 1 0 -3 6 4.5 5.7 1 1 3 6 143.0 6.6 1 -1 3 6 75.0 6.4 1 1 -3 6 109.6 5.8 1 -1 -3 6 77.8 5.9 1 2 3 6 61.0 6.1 1 -2 3 6 29.8 5.4 1 2 -3 6 64.0 5.5 1 -2 -3 6 30.5 5.7 1 3 3 6 260.5 8.0 1 -3 3 6 206.4 7.9 1 3 -3 6 240.9 8.0 1 -3 -3 6 185.9 7.4 1 4 3 6 169.0 6.8 1 -4 3 6 86.7 7.1 1 4 -3 6 146.0 6.8 1 -4 -3 6 81.6 6.2 1 5 3 6 93.7 5.6 1 -5 3 6 136.2 6.8 1 5 -3 6 89.3 7.2 1 -5 -3 6 107.5 5.8 1 0 4 6 62.1 5.1 1 0 -4 6 50.5 5.0 1 1 4 6 3.8 5.5 1 -1 4 6 -0.3 5.8 1 1 -4 6 4.1 5.3 1 -1 -4 6 -0.3 5.1 1 2 4 6 447.9 9.5 1 -2 4 6 619.1 11.2 1 2 -4 6 361.0 8.9 1 -2 -4 6 522.4 10.0 1 3 4 6 0.7 5.2 1 -3 4 6 13.7 5.7 1 3 -4 6 10.0 5.3 1 -3 -4 6 0.0 5.2 1 4 4 6 78.5 5.7 1 -4 4 6 118.8 6.5 1 4 -4 6 50.0 5.5 1 -4 -4 6 96.9 5.4 1 0 5 6 -5.7 5.2 1 0 -5 6 0.0 5.2 1 1 5 6 151.7 5.9 1 -1 5 6 101.4 5.4 1 1 -5 6 106.6 5.8 1 -1 -5 6 80.0 5.2 1 2 5 6 103.4 5.0 1 -2 5 6 54.7 4.9 1 2 -5 6 73.2 5.3 1 -2 -5 6 42.3 4.7 1 3 5 6 117.3 6.1 1 -3 5 6 93.8 6.3 1 3 -5 6 92.1 6.4 1 -3 -5 6 71.2 5.3 1 0 6 6 527.3 9.6 1 0 -6 6 410.9 9.0 1 1 6 6 40.9 4.1 1 -1 6 6 18.5 4.5 1 1 -6 6 32.9 5.3 1 -1 -6 6 14.1 5.0 1 2 6 6 1.1 4.5 1 -2 6 6 7.6 4.6 1 2 -6 6 11.0 4.8 1 -2 -6 6 -2.9 4.9 1 0 0 7 -3.2 5.8 1 1 0 7 7.1 6.2 1 -1 0 7 4.8 6.1 1 2 0 7 -6.8 5.9 1 -2 0 7 -8.2 5.9 1 3 0 7 171.3 7.2 1 -3 0 7 76.4 6.4 1 0 1 7 12.4 5.8 1 0 -1 7 11.6 5.4 1 1 1 7 44.3 5.6 1 -1 1 7 79.1 5.8 1 1 -1 7 42.6 5.6 1 -1 -1 7 74.7 5.2 1 2 1 7 22.8 4.6 1 -2 1 7 26.1 5.3 1 2 -1 7 20.4 6.1 1 -2 -1 7 12.3 5.8 1 3 1 7 150.5 7.5 1 -3 1 7 231.4 8.6 1 3 -1 7 159.8 7.4 1 -3 -1 7 215.9 7.8 1 0 2 7 60.2 5.3 1 0 -2 7 54.6 5.8 1 1 2 7 60.8 5.6 1 -1 2 7 28.7 5.7 1 1 -2 7 48.8 4.7 1 -1 -2 7 15.9 5.0 1 2 2 7 18.0 6.0 1 -2 2 7 26.9 6.0 1 2 -2 7 13.9 5.7 1 -2 -2 7 18.6 5.3 1 -3 2 7 28.3 7.0 1 -3 -2 7 29.4 4.8 1 0 3 7 4.6 5.6 1 0 -3 7 10.1 5.2 1 1 3 7 174.4 6.8 1 -1 3 7 109.2 6.4 1 1 -3 7 153.0 6.3 1 -1 -3 7 91.9 5.6 1 2 3 7 7.0 6.0 1 -2 3 7 15.0 5.9 1 2 -3 7 4.0 5.5 1 -2 -3 7 5.2 5.2 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 87852 #==END data_OLI_100C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2352(12) _cell_length_b 8.6266(11) _cell_length_c 5.9424(8) _cell_angle_alpha 90 _cell_angle_beta 90.040(11) _cell_angle_gamma 90 _cell_volume 422.16(10) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.453 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.759 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1753 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.361 _diffrn_reflns_theta_max 26.491 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 878 _reflns_number_gt 754 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.334(5) ref 1 0 0 0 1 0 0 0 1 2 0.666(5) pmt -1 0 0 0 -1 0 0 0 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.6260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 878 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.0005(2) 0.0006(2) 0.24943(17) 0.0216(3) Uani 1 1 d . . . . . Cu2 Cu 0.13681(13) 0.61895(12) -0.0210(3) 0.0242(3) Uani 1 1 d . . . . . As1 As 0.23740(9) 0.25009(9) 0.00932(18) 0.0189(2) Uani 1 1 d . . . . . O1 O 0.3669(10) 0.2541(8) 0.2222(12) 0.0281(19) Uani 1 1 d . . . . . O1' O 0.3370(10) 0.2760(9) -0.2348(12) 0.0248(17) Uani 1 1 d . . . . . O2 O 0.1316(7) 0.0801(6) 0.0022(14) 0.0224(12) Uani 1 1 d . . . . . O3 O 0.1005(7) 0.3940(7) 0.0437(14) 0.0270(17) Uani 1 1 d . . . . . O4 O 0.3720(7) 0.5954(6) 0.0026(15) 0.0195(11) Uani 1 1 d . . . . . H1 H 0.4141 0.6781 -0.0079 0.023 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0237(5) 0.0269(5) 0.0141(5) -0.0005(6) 0.0045(9) -0.0053(4) Cu2 0.0197(5) 0.0250(5) 0.0280(6) 0.0035(7) 0.0009(6) 0.0009(4) As1 0.0202(4) 0.0206(4) 0.0158(4) 0.0003(5) 0.0035(5) -0.0011(3) O1 0.033(4) 0.031(4) 0.021(4) 0.008(3) -0.015(3) -0.007(4) O1' 0.033(4) 0.025(4) 0.016(3) -0.005(3) 0.004(3) -0.008(3) O2 0.028(3) 0.023(3) 0.017(3) 0.001(3) 0.003(4) -0.005(2) O3 0.022(3) 0.020(3) 0.039(5) 0.001(3) 0.003(3) 0.001(2) O4 0.019(2) 0.023(3) 0.016(2) -0.002(4) 0.004(4) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.953(7) . ? Cu1 O2 1.970(8) 3 ? Cu1 O4 1.990(8) 2_545 ? Cu1 O4 2.014(7) 4_566 ? Cu1 O1' 2.348(8) 4_566 ? Cu1 O1 2.400(7) 2_545 ? Cu1 Cu1 2.965(2) 3 ? Cu1 Cu1 2.978(2) 3_556 ? Cu2 O4 1.952(6) . ? Cu2 O3 1.962(6) 3_565 ? Cu2 O1' 1.997(7) 2_554 ? Cu2 O3 2.001(6) . ? Cu2 O1 2.124(7) 2 ? Cu2 Cu2 3.058(2) 3_565 ? As1 O1 1.654(8) . ? As1 O1' 1.682(7) . ? As1 O3 1.690(6) . ? As1 O2 1.706(6) . ? O1 Cu2 2.124(7) 2_545 ? O1 Cu1 2.401(7) 2 ? O1' Cu2 1.997(7) 2_544 ? O1' Cu1 2.348(8) 4_665 ? O2 Cu1 1.970(8) 3 ? O2 O2 2.570(12) 3 ? O2 O4 2.946(11) 2_545 ? O2 O4 3.003(11) 2_544 ? O3 Cu2 1.962(6) 3_565 ? O3 O3 2.520(12) 3_565 ? O4 Cu1 1.989(8) 2 ? O4 Cu1 2.014(7) 4_665 ? O4 O4 2.675(11) 3_665 ? O4 H1 0.7954 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.9(3) . 3 ? O2 Cu1 O4 96.7(3) . 2_545 ? O2 Cu1 O4 176.4(2) 3 2_545 ? O2 Cu1 O4 176.0(2) . 4_566 ? O2 Cu1 O4 97.8(3) 3 4_566 ? O4 Cu1 O4 83.9(2) 2_545 4_566 ? O2 Cu1 O1' 93.4(2) . 4_566 ? O2 Cu1 O1' 90.5(3) 3 4_566 ? O4 Cu1 O1' 86.3(3) 2_545 4_566 ? O4 Cu1 O1' 90.6(2) 4_566 4_566 ? O2 Cu1 O1 96.2(3) . 2_545 ? O2 Cu1 O1 89.5(2) 3 2_545 ? O4 Cu1 O1 93.9(2) 2_545 2_545 ? O4 Cu1 O1 79.8(2) 4_566 2_545 ? O1' Cu1 O1 170.3(3) 4_566 2_545 ? O2 Cu1 Cu1 41.1(2) . 3 ? O2 Cu1 Cu1 40.71(19) 3 3 ? O4 Cu1 Cu1 137.7(2) 2_545 3 ? O4 Cu1 Cu1 138.4(2) 4_566 3 ? O1' Cu1 Cu1 92.57(19) 4_566 3 ? O1 Cu1 Cu1 93.75(19) 2_545 3 ? O2 Cu1 Cu1 138.8(2) . 3_556 ? O2 Cu1 Cu1 139.4(2) 3 3_556 ? O4 Cu1 Cu1 42.2(2) 2_545 3_556 ? O4 Cu1 Cu1 41.6(2) 4_566 3_556 ? O1' Cu1 Cu1 87.94(19) 4_566 3_556 ? O1 Cu1 Cu1 85.74(19) 2_545 3_556 ? Cu1 Cu1 Cu1 179.49(14) 3 3_556 ? O4 Cu2 O3 170.8(2) . 3_565 ? O4 Cu2 O1' 90.9(3) . 2_554 ? O3 Cu2 O1' 95.6(3) 3_565 2_554 ? O4 Cu2 O3 91.9(2) . . ? O3 Cu2 O3 79.0(3) 3_565 . ? O1' Cu2 O3 144.5(3) 2_554 . ? O4 Cu2 O1 90.7(3) . 2 ? O3 Cu2 O1 94.2(3) 3_565 2 ? O1' Cu2 O1 103.7(3) 2_554 2 ? O3 Cu2 O1 111.7(3) . 2 ? O4 Cu2 Cu2 130.95(17) . 3_565 ? O3 Cu2 Cu2 39.96(17) 3_565 3_565 ? O1' Cu2 Cu2 126.5(3) 2_554 3_565 ? O3 Cu2 Cu2 39.02(18) . 3_565 ? O1 Cu2 Cu2 106.8(2) 2 3_565 ? O1 As1 O1' 110.0(4) . . ? O1 As1 O3 108.8(4) . . ? O1' As1 O3 109.4(4) . . ? O1 As1 O2 111.5(4) . . ? O1' As1 O2 110.0(4) . . ? O3 As1 O2 107.1(3) . . ? As1 O1 Cu2 128.2(4) . 2_545 ? As1 O1 Cu1 111.5(3) . 2 ? Cu2 O1 Cu1 115.7(3) 2_545 2 ? As1 O1' Cu2 126.1(4) . 2_544 ? As1 O1' Cu1 115.0(4) . 4_665 ? Cu2 O1' Cu1 117.8(3) 2_544 4_665 ? As1 O2 Cu1 124.6(4) . . ? As1 O2 Cu1 127.0(4) . 3 ? Cu1 O2 Cu1 98.1(3) . 3 ? As1 O2 O2 153.2(4) . 3 ? Cu1 O2 O2 49.4(2) . 3 ? Cu1 O2 O2 48.8(3) 3 3 ? As1 O2 O4 86.7(3) . 2_545 ? Cu1 O2 O4 42.1(2) . 2_545 ? Cu1 O2 O4 140.2(3) 3 2_545 ? O2 O2 O4 91.4(4) 3 2_545 ? As1 O2 O4 89.5(3) . 2_544 ? Cu1 O2 O4 139.6(3) . 2_544 ? Cu1 O2 O4 41.63(19) 3 2_544 ? O2 O2 O4 90.3(4) 3 2_544 ? O4 O2 O4 174.8(3) 2_545 2_544 ? As1 O3 Cu2 127.9(3) . 3_565 ? As1 O3 Cu2 126.1(4) . . ? Cu2 O3 Cu2 101.0(3) 3_565 . ? As1 O3 O3 161.2(6) . 3_565 ? Cu2 O3 O3 51.2(2) 3_565 3_565 ? Cu2 O3 O3 49.8(2) . 3_565 ? Cu2 O4 Cu1 128.6(4) . 2 ? Cu2 O4 Cu1 120.4(4) . 4_665 ? Cu1 O4 Cu1 96.1(2) 2 4_665 ? Cu2 O4 O4 147.7(4) . 3_665 ? Cu1 O4 O4 48.4(3) 2 3_665 ? Cu1 O4 O4 47.7(2) 4_665 3_665 ? Cu2 O4 H1 109.5 . . ? Cu1 O4 H1 101.3 2 . ? Cu1 O4 H1 94.7 4_665 . ? O4 O4 H1 102.0 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.80 2.29 2.846(10) 128.1 3_665 O4 H1 O1' 0.80 2.54 2.979(11) 116.6 3_665 _refine_diff_density_max 1.695 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.288 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite joi 100C in P 21/n CELL .71073 8.2352 8.6266 5.9424 90.000 90.040 90.000 ZERR 4 .0012 .0011 .0008 .00 .011 .00 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z EQIV $6 -x+1/2, y-1/2, -z-1/2 BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O2 O4_$6 BIND O3 O3_$3 HTAB O4 O1_$5 HTAB O4 O1'_$5 L.S. 5 LIST 4 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 1 PLAN 25 HTAB WGHT 0.048900 0.626000 BASF 0.66641 FVAR 0.31621 CU1 3 -0.000521 0.000592 0.249432 11.00000 0.02366 0.02686 = 0.01415 -0.00050 0.00449 -0.00525 CU2 3 0.136815 0.618953 -0.021037 11.00000 0.01967 0.02503 = 0.02795 0.00346 0.00092 0.00089 AS1 4 0.237396 0.250087 0.009322 11.00000 0.02024 0.02057 = 0.01580 0.00031 0.00354 -0.00109 O1 2 0.366889 0.254055 0.222223 11.00000 0.03277 0.03055 = 0.02093 0.00840 -0.01463 -0.00708 O1' 2 0.336960 0.276047 -0.234768 11.00000 0.03315 0.02494 = 0.01627 -0.00459 0.00385 -0.00846 O2 2 0.131574 0.080092 0.002185 11.00000 0.02763 0.02303 = 0.01655 0.00096 0.00304 -0.00509 O3 2 0.100458 0.393973 0.043708 11.00000 0.02184 0.01985 = 0.03933 0.00103 0.00273 0.00057 O4 2 0.371993 0.595444 0.002645 11.00000 0.01924 0.02312 = 0.01623 -0.00244 0.00384 0.00024 AFIX 3 H1 1 0.414088 0.678112 -0.007867 11.00000 -1.20000 AFIX 0 HKLF 4 REM olivenite joi 100C in P 21/n REM R1 = 0.0382 for 754 Fo > 4sig(Fo) and 0.0482 for all 878 data REM 74 parameters refined using 0 restraints END WGHT 0.0489 0.6265 REM Instructions for potential hydrogen bonds HTAB O4 O1_$5 HTAB O4 O1'_$5 REM Highest difference peak 1.695, deepest hole -1.691, 1-sigma level 0.288 Q1 1 0.1769 0.6096 -0.1197 11.00000 0.05 1.70 Q2 1 0.1905 0.2447 0.1104 11.00000 0.05 1.61 Q3 1 0.0950 0.7248 0.0436 11.00000 0.05 0.94 Q4 1 0.0288 0.0007 0.1031 11.00000 0.05 0.88 Q5 1 -0.0314 0.1080 0.2936 11.00000 0.05 0.86 Q6 1 0.1872 0.1206 -0.0059 11.00000 0.05 0.85 Q7 1 0.3026 0.2566 -0.1574 11.00000 0.05 0.82 Q8 1 0.0608 0.1133 0.0798 11.00000 0.05 0.80 Q9 1 0.2742 0.0949 -0.1405 11.00000 0.05 0.79 Q10 1 -0.0001 -0.1094 0.2726 11.00000 0.05 0.79 Q11 1 0.5219 0.7231 -0.0831 11.00000 0.05 0.77 Q12 1 0.2377 0.3747 -0.0713 11.00000 0.05 0.76 Q13 1 0.2602 0.5965 -0.0278 11.00000 0.05 0.74 Q14 1 0.0797 0.3999 0.1376 11.00000 0.05 0.73 Q15 1 0.0970 0.5705 0.0376 11.00000 0.05 0.73 Q16 1 0.3114 0.6135 0.1365 11.00000 0.05 0.71 Q17 1 0.3603 0.2445 -0.3539 11.00000 0.05 0.63 Q18 1 0.2256 0.4176 -0.4049 11.00000 0.05 0.61 Q19 1 0.4497 0.2401 -0.0946 11.00000 0.05 0.61 Q20 1 0.1074 0.2393 0.0252 11.00000 0.05 0.58 Q21 1 0.1133 0.2795 -0.0013 11.00000 0.05 0.57 Q22 1 0.0318 0.2907 0.1826 11.00000 0.05 0.57 Q23 1 0.2941 0.0786 0.2215 11.00000 0.05 0.57 Q24 1 -0.0115 0.1377 -0.0341 11.00000 0.05 0.56 Q25 1 0.0180 0.4239 -0.1130 11.00000 0.05 0.56 ; _shelx_res_checksum 2280 _shelx_hkl_file ; 1 0 0 -1.7 1.1 1 2 0 0 132.2 3.2 1 3 0 0 -6.0 3.2 1 4 0 0 32.3 3.9 1 5 0 0 -1.6 3.8 1 6 0 0 80.7 4.3 1 7 0 0 7.5 4.4 1 8 0 0 1550.9 12.8 1 9 0 0 -13.7 3.9 1 10 0 0 31.0 3.4 1 0 1 0 2.2 0.9 1 1 1 0 611.1 4.0 1 -1 1 0 621.2 4.0 1 2 1 0 324.1 4.3 1 -2 1 0 311.8 4.2 1 3 1 0 1380.0 8.6 1 -3 1 0 1381.4 10.8 1 4 1 0 11.7 2.1 1 -4 1 0 12.6 3.5 1 5 1 0 711.2 7.8 1 -5 1 0 644.1 8.0 1 6 1 0 382.5 6.8 1 -6 1 0 351.5 6.7 1 7 1 0 64.8 4.7 1 -7 1 0 46.0 4.4 1 8 1 0 303.5 6.7 1 -8 1 0 276.9 6.2 1 9 1 0 74.0 4.5 1 -9 1 0 63.3 4.0 1 10 1 0 22.4 3.4 1 -10 1 0 12.4 3.9 1 0 2 0 84.5 2.2 1 1 2 0 802.1 5.8 1 -1 2 0 825.7 5.9 1 2 2 0 3729.5 13.0 1 -2 2 0 3683.9 13.1 1 3 2 0 243.2 4.3 1 -3 2 0 239.7 4.5 1 4 2 0 -7.3 3.3 1 -4 2 0 3.3 3.1 1 5 2 0 561.0 7.2 1 -5 2 0 571.6 7.6 1 6 2 0 1018.6 10.1 1 -6 2 0 995.0 12.4 1 7 2 0 24.9 3.6 1 -7 2 0 9.4 6.8 1 8 2 0 9.5 4.1 1 -8 2 0 7.4 4.6 1 9 2 0 168.7 5.4 1 -9 2 0 128.7 5.4 1 10 2 0 225.9 6.1 1 -10 2 0 181.3 6.0 1 0 3 0 15.1 1.8 1 1 3 0 1549.6 8.9 1 -1 3 0 1522.5 8.8 1 2 3 0 18.1 2.1 1 -2 3 0 18.4 2.0 1 3 3 0 213.4 4.5 1 -3 3 0 201.5 4.4 1 4 3 0 95.0 3.7 1 -4 3 0 92.3 3.4 1 5 3 0 147.2 4.7 1 -5 3 0 154.3 4.8 1 6 3 0 71.5 4.6 1 -6 3 0 72.9 4.3 1 7 3 0 379.4 7.1 1 -7 3 0 373.4 7.1 1 8 3 0 4.7 4.1 1 -8 3 0 11.2 3.8 1 9 3 0 107.3 4.8 1 -9 3 0 101.2 6.0 1 0 4 0 747.5 7.1 1 1 4 0 131.9 3.5 1 -1 4 0 146.8 3.7 1 2 4 0 13.6 2.3 1 -2 4 0 8.4 3.0 1 3 4 0 9.8 2.5 1 -3 4 0 7.0 3.1 1 4 4 0 3488.4 16.7 1 -4 4 0 3374.9 16.3 1 5 4 0 86.7 4.4 1 -5 4 0 85.3 4.0 1 6 4 0 14.7 4.0 1 -6 4 0 19.2 3.5 1 7 4 0 3.5 4.0 1 -7 4 0 5.1 3.3 1 8 4 0 117.0 5.0 1 -8 4 0 97.0 4.2 1 9 4 0 4.0 4.1 1 -9 4 0 3.9 3.5 1 0 5 0 3.5 3.3 1 1 5 0 1115.0 9.4 1 -1 5 0 1113.7 9.3 1 2 5 0 100.2 3.6 1 -2 5 0 103.5 3.9 1 3 5 0 37.4 3.1 1 -3 5 0 43.0 3.3 1 4 5 0 87.9 4.1 1 -4 5 0 84.3 3.9 1 5 5 0 116.6 4.6 1 -5 5 0 106.3 4.4 1 6 5 0 -2.0 4.0 1 -6 5 0 -5.1 3.5 1 7 5 0 312.2 6.7 1 -7 5 0 297.0 6.3 1 8 5 0 29.9 4.2 1 -8 5 0 28.7 3.5 1 9 5 0 51.4 4.2 1 -9 5 0 42.5 3.6 1 0 6 0 535.6 7.3 1 1 6 0 260.1 5.5 1 -1 6 0 254.8 5.4 1 2 6 0 1569.7 12.0 1 -2 6 0 1516.4 11.7 1 3 6 0 67.0 3.9 1 -3 6 0 73.8 4.1 1 4 6 0 99.1 4.3 1 -4 6 0 81.6 3.9 1 5 6 0 178.4 5.3 1 -5 6 0 174.0 5.2 1 6 6 0 501.1 8.1 1 -6 6 0 453.3 7.6 1 7 6 0 -0.8 4.0 1 -7 6 0 -3.0 3.4 1 8 6 0 40.3 4.0 1 -8 6 0 36.9 3.5 1 0 7 0 2.2 4.2 1 1 7 0 40.4 4.1 1 -1 7 0 38.6 3.4 1 2 7 0 45.3 4.3 1 -2 7 0 48.2 3.4 1 3 7 0 599.6 8.3 1 -3 7 0 561.3 8.1 1 4 7 0 -4.2 4.1 1 -4 7 0 0.8 3.7 1 5 7 0 193.3 5.4 1 -5 7 0 183.5 5.4 1 6 7 0 198.9 5.7 1 -6 7 0 181.2 5.5 1 7 7 0 6.9 3.8 1 -7 7 0 -2.0 3.4 1 0 8 0 1887.0 14.1 1 1 8 0 6.0 4.1 1 -1 8 0 7.5 4.0 1 2 8 0 28.5 3.0 1 -2 8 0 26.4 3.2 1 3 8 0 11.5 3.9 1 -3 8 0 7.6 4.1 1 4 8 0 138.9 4.9 1 -4 8 0 131.2 5.0 1 5 8 0 2.0 3.9 1 -5 8 0 3.9 3.8 1 6 8 0 -3.7 3.8 1 -6 8 0 -1.8 3.3 1 0 9 0 -5.0 3.9 1 1 9 0 11.9 4.1 1 -1 9 0 7.4 4.0 1 2 9 0 55.2 4.0 1 -2 9 0 58.1 3.7 1 3 9 0 225.6 5.9 1 -3 9 0 227.2 6.0 1 4 9 0 13.4 2.8 1 -4 9 0 13.5 3.8 1 5 9 0 140.1 5.1 1 -5 9 0 137.5 5.0 1 0 10 0 6.6 3.6 1 1 10 0 4.2 3.6 1 -1 10 0 10.6 3.6 1 2 10 0 365.2 7.2 1 -2 10 0 362.9 7.3 1 3 10 0 -3.5 3.6 1 -3 10 0 1.0 3.7 1 0 0 1 5.1 2.5 1 1 0 1 963.5 7.3 1 -1 0 1 940.0 8.0 1 2 0 1 9.0 5.2 1 -2 0 1 6.4 5.7 1 3 0 1 1177.9 10.6 1 -3 0 1 956.3 9.3 1 4 0 1 2.9 4.6 1 -4 0 1 6.3 3.9 1 5 0 1 9.9 5.4 1 -5 0 1 26.9 4.0 1 6 0 1 -15.2 6.0 1 -6 0 1 -1.0 4.5 1 7 0 1 19.4 4.8 1 -7 0 1 34.3 3.9 1 8 0 1 2.7 4.9 1 -8 0 1 -2.6 4.1 1 9 0 1 108.7 5.5 1 -9 0 1 96.4 4.9 1 10 0 1 6.4 4.3 1 -10 0 1 4.1 3.7 1 0 1 1 1075.9 7.2 1 0 -1 1 1012.0 7.0 1 1 1 1 603.8 6.1 1 -1 1 1 671.6 6.9 1 1 -1 1 696.3 7.4 1 -1 -1 1 593.8 5.8 1 2 1 1 11.3 4.2 1 -2 1 1 6.4 5.1 1 2 -1 1 -1.0 6.4 1 -2 -1 1 6.3 3.9 1 3 1 1 1343.8 9.9 1 -3 1 1 1384.1 11.7 1 3 -1 1 1294.2 12.1 1 -3 -1 1 1167.4 8.7 1 4 1 1 443.2 6.7 1 -4 1 1 418.5 9.1 1 4 -1 1 433.8 8.7 1 -4 -1 1 374.2 6.1 1 5 1 1 1203.4 10.8 1 -5 1 1 1131.6 13.3 1 5 -1 1 1189.2 13.1 1 -5 -1 1 1047.0 9.7 1 6 1 1 18.2 3.8 1 -6 1 1 11.1 6.1 1 6 -1 1 18.3 7.4 1 -6 -1 1 11.0 4.4 1 7 1 1 186.9 6.1 1 -7 1 1 153.8 6.4 1 7 -1 1 170.9 8.7 1 -7 -1 1 162.7 5.6 1 8 1 1 62.2 4.5 1 -8 1 1 55.7 4.4 1 8 -1 1 76.6 6.0 1 -8 -1 1 51.1 3.8 1 9 1 1 0.0 4.2 1 -9 1 1 4.8 4.0 1 9 -1 1 7.7 5.3 1 -9 -1 1 5.9 3.7 1 10 1 1 14.4 4.2 1 -10 1 1 9.0 3.8 1 10 -1 1 10.5 4.9 1 -10 -1 1 12.5 3.7 1 0 2 1 5.2 3.2 1 0 -2 1 10.1 3.3 1 1 2 1 4.8 3.0 1 -1 2 1 5.1 3.4 1 1 -2 1 9.9 4.0 1 -1 -2 1 14.8 2.9 1 2 2 1 456.1 5.8 1 -2 2 1 428.4 6.3 1 2 -2 1 479.9 6.5 1 -2 -2 1 389.1 5.4 1 3 2 1 13.9 3.3 1 -3 2 1 20.3 3.6 1 3 -2 1 11.9 4.3 1 -3 -2 1 16.3 2.8 1 4 2 1 146.2 4.5 1 -4 2 1 102.3 5.5 1 4 -2 1 162.4 7.2 1 -4 -2 1 78.1 3.6 1 5 2 1 144.8 5.1 1 -5 2 1 122.7 6.4 1 5 -2 1 131.6 8.1 1 -5 -2 1 102.0 4.3 1 6 2 1 183.4 5.7 1 -6 2 1 157.5 7.6 1 6 -2 1 183.5 9.0 1 -6 -2 1 145.9 5.1 1 7 2 1 139.1 5.8 1 -7 2 1 92.6 7.9 1 7 -2 1 128.1 8.3 1 -7 -2 1 96.6 4.7 1 8 2 1 87.7 4.9 1 -8 2 1 59.8 5.8 1 8 -2 1 93.9 7.1 1 -8 -2 1 71.1 4.0 1 9 2 1 68.9 4.8 1 -9 2 1 50.1 5.9 1 9 -2 1 62.8 6.5 1 -9 -2 1 48.0 4.1 1 10 2 1 26.3 3.4 1 -10 2 1 24.2 4.4 1 10 -2 1 24.6 5.7 1 -10 -2 1 28.1 4.0 1 0 3 1 577.0 6.2 1 0 -3 1 537.8 6.0 1 1 3 1 2133.5 11.1 1 -1 3 1 1929.8 10.7 1 1 -3 1 2018.8 11.0 1 -1 -3 1 1755.3 10.2 1 2 3 1 4.1 3.1 1 -2 3 1 10.4 3.0 1 2 -3 1 4.0 3.4 1 -2 -3 1 6.4 3.3 1 3 3 1 412.6 6.1 1 -3 3 1 390.0 6.1 1 3 -3 1 411.7 6.4 1 -3 -3 1 342.5 5.7 1 4 3 1 233.6 5.3 1 -4 3 1 213.5 5.4 1 4 -3 1 250.3 6.1 1 -4 -3 1 188.7 5.0 1 5 3 1 45.9 4.0 1 -5 3 1 65.2 4.2 1 5 -3 1 53.5 5.5 1 -5 -3 1 62.3 3.9 1 6 3 1 25.6 4.7 1 -6 3 1 17.6 5.9 1 6 -3 1 31.2 6.6 1 -6 -3 1 16.7 5.0 1 7 3 1 215.0 6.1 1 -7 3 1 225.5 7.1 1 7 -3 1 209.2 8.4 1 -7 -3 1 228.8 6.0 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4 5 12.0 5.2 1 -4 4 5 -4.2 6.1 1 4 -4 5 9.3 5.9 1 -4 -4 5 -5.9 5.5 1 5 4 5 64.0 4.9 1 -5 4 5 78.7 6.6 1 5 -4 5 65.3 6.3 1 -5 -4 5 59.8 5.1 1 6 4 5 7.7 4.7 1 -6 4 5 8.9 5.9 1 6 -4 5 1.6 6.1 1 -6 -4 5 6.7 5.0 1 0 5 5 39.1 4.2 1 0 -5 5 37.4 5.5 1 1 5 5 461.4 9.1 1 -1 5 5 382.1 8.6 1 1 -5 5 360.5 9.1 1 -1 -5 5 319.5 8.4 1 2 5 5 30.5 4.2 1 -2 5 5 30.2 5.0 1 2 -5 5 22.4 5.5 1 -2 -5 5 14.2 6.0 1 3 5 5 100.6 5.2 1 -3 5 5 86.5 5.6 1 3 -5 5 85.4 6.0 1 -3 -5 5 65.9 5.9 1 4 5 5 27.1 4.4 1 -4 5 5 40.3 5.2 1 4 -5 5 19.3 5.8 1 -4 -5 5 43.1 5.7 1 5 5 5 21.4 4.1 1 -5 5 5 38.5 4.7 1 5 -5 5 15.7 6.0 1 -5 -5 5 37.2 4.5 1 6 5 5 12.8 4.7 1 -6 5 5 9.7 5.7 1 6 -5 5 10.7 5.8 1 -6 -5 5 0.3 5.1 1 0 6 5 58.7 4.6 1 0 -6 5 46.0 5.4 1 1 6 5 15.6 3.4 1 -1 6 5 12.9 5.2 1 1 -6 5 13.6 4.9 1 -1 -6 5 13.3 5.2 1 2 6 5 22.3 4.1 1 -2 6 5 29.7 3.9 1 2 -6 5 14.2 4.4 1 -2 -6 5 24.1 5.3 1 3 6 5 21.0 3.6 1 -3 6 5 9.1 5.2 1 3 -6 5 22.6 5.1 1 -3 -6 5 6.3 5.0 1 4 6 5 36.7 4.1 1 -4 6 5 28.5 5.0 1 4 -6 5 29.1 5.3 1 -4 -6 5 15.3 5.1 1 5 6 5 52.2 4.5 1 -5 6 5 19.2 5.7 1 5 -6 5 35.4 5.1 1 -5 -6 5 17.3 4.9 1 0 7 5 10.6 4.7 1 0 -7 5 2.6 4.9 1 1 7 5 62.6 4.3 1 -1 7 5 99.6 4.8 1 1 -7 5 42.4 4.9 1 -1 -7 5 84.9 5.3 1 2 7 5 3.4 4.5 1 -2 7 5 4.1 4.8 1 2 -7 5 1.1 5.1 1 -2 -7 5 2.7 4.7 1 3 7 5 145.9 5.6 1 -3 7 5 222.3 7.0 1 3 -7 5 95.9 6.0 1 -3 -7 5 182.8 6.5 1 0 8 5 7.5 4.5 1 0 -8 5 6.2 4.6 1 0 0 6 99.8 6.8 1 1 0 6 -4.7 6.9 1 -1 0 6 -1.4 6.4 1 2 0 6 857.8 13.7 1 -2 0 6 632.6 11.5 1 3 0 6 5.5 7.1 1 -3 0 6 2.2 6.4 1 4 0 6 56.2 6.8 1 -4 0 6 50.9 6.0 1 5 0 6 15.5 6.4 1 -5 0 6 3.2 5.9 1 6 0 6 264.9 9.3 1 -6 0 6 371.0 9.6 1 0 1 6 160.8 8.1 1 0 -1 6 139.8 7.1 1 1 1 6 186.3 8.7 1 -1 1 6 254.3 8.6 1 1 -1 6 185.6 8.1 1 -1 -1 6 235.9 7.9 1 2 1 6 39.2 5.9 1 -2 1 6 23.5 4.7 1 2 -1 6 48.1 5.8 1 -2 -1 6 26.8 4.9 1 3 1 6 98.9 6.9 1 -3 1 6 116.0 7.3 1 3 -1 6 87.4 6.4 1 -3 -1 6 112.0 6.1 1 4 1 6 11.8 6.3 1 -4 1 6 11.8 6.8 1 4 -1 6 5.1 6.8 1 -4 -1 6 18.8 6.2 1 5 1 6 148.2 7.0 1 -5 1 6 80.2 6.2 1 5 -1 6 151.1 7.9 1 -5 -1 6 78.6 6.9 1 6 1 6 62.5 5.9 1 -6 1 6 25.0 5.9 1 6 -1 6 71.0 7.0 1 -6 -1 6 30.8 6.1 1 0 2 6 524.3 11.0 1 0 -2 6 463.1 9.8 1 1 2 6 148.3 6.8 1 -1 2 6 60.6 6.4 1 1 -2 6 126.7 6.3 1 -1 -2 6 62.7 6.0 1 2 2 6 1.7 6.4 1 -2 2 6 0.7 6.9 1 2 -2 6 9.6 6.2 1 -2 -2 6 2.9 5.9 1 3 2 6 41.8 6.1 1 -3 2 6 91.5 6.4 1 3 -2 6 34.9 6.8 1 -3 -2 6 81.8 5.5 1 4 2 6 625.0 11.5 1 -4 2 6 620.5 12.2 1 4 -2 6 556.7 11.3 1 -4 -2 6 604.7 11.1 1 5 2 6 76.4 5.4 1 -5 2 6 40.4 5.5 1 5 -2 6 65.7 6.1 1 -5 -2 6 47.9 5.4 1 0 3 6 1.2 6.0 1 0 -3 6 7.3 5.7 1 1 3 6 115.0 6.0 1 -1 3 6 66.0 5.5 1 1 -3 6 97.3 5.8 1 -1 -3 6 62.8 5.8 1 2 3 6 54.9 4.8 1 -2 3 6 14.7 6.8 1 2 -3 6 74.8 6.8 1 -2 -3 6 31.2 5.6 1 3 3 6 253.6 7.7 1 -3 3 6 210.4 8.0 1 3 -3 6 211.9 7.4 1 -3 -3 6 167.1 7.3 1 4 3 6 154.1 6.3 1 -4 3 6 67.1 6.3 1 4 -3 6 127.8 6.7 1 -4 -3 6 50.3 5.6 1 5 3 6 81.4 6.2 1 -5 3 6 130.7 6.9 1 5 -3 6 66.2 6.1 1 -5 -3 6 95.2 5.6 1 0 4 6 57.0 5.7 1 0 -4 6 68.3 5.9 1 1 4 6 -2.0 5.4 1 -1 4 6 5.1 5.4 1 1 -4 6 14.9 5.3 1 -1 -4 6 8.4 5.1 1 2 4 6 420.7 9.2 1 -2 4 6 547.9 10.4 1 2 -4 6 336.5 8.7 1 -2 -4 6 457.0 9.6 1 3 4 6 0.6 5.1 1 -3 4 6 6.1 6.1 1 3 -4 6 5.8 5.7 1 -3 -4 6 1.1 4.9 1 4 4 6 58.7 5.0 1 -4 4 6 106.0 6.3 1 4 -4 6 61.1 6.6 1 -4 -4 6 83.2 5.3 1 0 5 6 -0.1 5.0 1 0 -5 6 0.7 5.1 1 1 5 6 137.0 5.7 1 -1 5 6 86.1 5.1 1 1 -5 6 107.5 5.8 1 -1 -5 6 60.4 5.2 1 2 5 6 102.4 5.5 1 -2 5 6 45.4 4.9 1 2 -5 6 74.0 5.6 1 -2 -5 6 45.8 4.7 1 3 5 6 89.9 5.0 1 -3 5 6 75.0 5.5 1 3 -5 6 76.6 5.6 1 -3 -5 6 54.7 5.1 1 0 6 6 481.8 9.4 1 0 -6 6 373.7 9.0 1 1 6 6 28.5 3.9 1 -1 6 6 15.8 5.0 1 1 -6 6 21.2 4.7 1 -1 -6 6 14.3 5.1 1 2 6 6 3.3 4.7 1 -2 6 6 9.3 4.9 1 2 -6 6 8.1 5.1 1 -2 -6 6 10.3 4.6 1 0 0 7 3.0 5.4 1 1 0 7 21.6 6.3 1 -1 0 7 22.7 5.6 1 2 0 7 -13.3 5.9 1 -2 0 7 2.3 5.6 1 3 0 7 144.2 7.0 1 -3 0 7 59.3 5.6 1 0 1 7 0.7 6.2 1 0 -1 7 15.2 5.9 1 1 1 7 38.9 5.3 1 -1 1 7 67.9 6.0 1 1 -1 7 44.7 4.9 1 -1 -1 7 65.9 5.5 1 2 1 7 13.1 6.2 1 -2 1 7 20.0 5.5 1 2 -1 7 20.5 5.8 1 -2 -1 7 18.3 5.6 1 3 1 7 148.1 7.2 1 -3 1 7 201.3 7.8 1 3 -1 7 140.3 7.5 1 -3 -1 7 190.5 7.0 1 0 2 7 52.8 5.6 1 0 -2 7 38.0 4.6 1 1 2 7 48.0 5.3 1 -1 2 7 26.6 6.0 1 1 -2 7 38.6 5.1 1 -1 -2 7 27.4 5.0 1 2 2 7 13.8 5.8 1 -2 2 7 10.8 6.5 1 2 -2 7 3.3 5.6 1 -2 -2 7 15.9 5.5 1 3 2 7 44.2 5.0 1 -3 2 7 7.3 6.4 1 3 -2 7 42.1 4.6 1 -3 -2 7 17.8 4.6 1 0 3 7 1.9 5.7 1 0 -3 7 6.9 4.9 1 1 3 7 170.0 6.7 1 -1 3 7 113.2 6.3 1 1 -3 7 143.0 6.4 1 -1 -3 7 107.3 6.4 1 2 3 7 6.7 5.7 1 -2 3 7 2.5 5.9 1 2 -3 7 3.1 5.5 1 -2 -3 7 13.7 5.2 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 75181 #==END data_OLI_150C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2403(10) _cell_length_b 8.6442(9) _cell_length_c 5.9491(7) _cell_angle_alpha 90 _cell_angle_beta 90.059(10) _cell_angle_gamma 90 _cell_volume 423.76(8) _cell_formula_units_Z 4 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.436 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.692 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1762 _diffrn_reflns_av_unetI/netI 0.0511 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.356 _diffrn_reflns_theta_max 26.514 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 884 _reflns_number_gt 738 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.327(5) ref 1 0 0 0 1 0 0 0 1 2 0.673(5) pmt -1 0 0 0 -1 0 0 0 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+1.0016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 884 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.0004(2) 0.0008(2) 0.24953(17) 0.0233(3) Uani 1 1 d . . . . . Cu2 Cu 0.13686(12) 0.61911(12) -0.0173(3) 0.0269(3) Uani 1 1 d . . . . . As1 As 0.23719(9) 0.24983(9) 0.0075(2) 0.0197(2) Uani 1 1 d . . . . . O1 O 0.3644(12) 0.2562(9) 0.2233(12) 0.031(2) Uani 1 1 d . . . . . O1' O 0.3385(12) 0.2733(9) -0.2348(13) 0.0295(19) Uani 1 1 d . . . . . O2 O 0.1324(7) 0.0811(6) 0.0006(15) 0.0230(11) Uani 1 1 d . . . . . O3 O 0.0990(7) 0.3934(7) 0.0373(17) 0.033(2) Uani 1 1 d . . . . . O4 O 0.3726(7) 0.5956(6) 0.0002(16) 0.0207(11) Uani 1 1 d . . . . . H1 H 0.4094 0.6853 0.0016 0.025 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0249(5) 0.0294(5) 0.0157(5) 0.0001(6) 0.0043(9) -0.0059(4) Cu2 0.0198(4) 0.0269(5) 0.0339(7) 0.0029(8) 0.0018(7) 0.0002(4) As1 0.0203(4) 0.0213(4) 0.0176(4) -0.0001(6) 0.0031(6) -0.0009(3) O1 0.034(5) 0.041(5) 0.018(4) 0.011(3) -0.010(3) -0.005(4) O1' 0.040(5) 0.028(4) 0.021(4) -0.005(3) 0.005(4) -0.016(4) O2 0.028(3) 0.026(3) 0.015(2) 0.000(4) 0.001(4) -0.008(2) O3 0.022(3) 0.021(3) 0.056(6) 0.004(4) 0.001(4) 0.003(2) O4 0.023(2) 0.023(3) 0.016(2) 0.000(4) 0.003(4) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.969(7) . ? Cu1 O2 1.974(8) 3 ? Cu1 O4 1.998(9) 2_545 ? Cu1 O4 2.004(8) 4_566 ? Cu1 O1' 2.363(8) 4_566 ? Cu1 O1 2.399(9) 2_545 ? Cu1 Cu1 2.969(2) 3 ? Cu1 Cu1 2.980(2) 3_556 ? Cu2 O3 1.950(6) 3_565 ? Cu2 O4 1.956(6) . ? Cu2 O1' 1.998(8) 2_554 ? Cu2 O3 2.002(6) . ? Cu2 O1 2.113(8) 2 ? Cu2 Cu2 3.061(2) 3_565 ? As1 O1 1.657(8) . ? As1 O1' 1.679(8) . ? As1 O3 1.694(6) . ? As1 O2 1.696(5) . ? O1 Cu2 2.113(8) 2_545 ? O1 Cu1 2.399(9) 2 ? O1' Cu2 1.998(8) 2_544 ? O1' Cu1 2.363(8) 4_665 ? O2 Cu1 1.974(8) 3 ? O2 O2 2.594(11) 3 ? O2 O4 2.973(12) 2_545 ? O2 O4 2.982(12) 2_544 ? O3 Cu2 1.950(6) 3_565 ? O3 O3 2.500(12) 3_565 ? O4 Cu1 1.998(9) 2 ? O4 Cu1 2.004(8) 4_665 ? O4 O4 2.672(11) 3_665 ? O4 H1 0.8320 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 82.3(2) . 3 ? O2 Cu1 O4 97.1(3) . 2_545 ? O2 Cu1 O4 176.7(3) 3 2_545 ? O2 Cu1 O4 175.8(3) . 4_566 ? O2 Cu1 O4 97.1(3) 3 4_566 ? O4 Cu1 O4 83.8(2) 2_545 4_566 ? O2 Cu1 O1' 92.9(3) . 4_566 ? O2 Cu1 O1' 91.0(3) 3 4_566 ? O4 Cu1 O1' 85.8(3) 2_545 4_566 ? O4 Cu1 O1' 91.2(3) 4_566 4_566 ? O2 Cu1 O1 95.8(3) . 2_545 ? O2 Cu1 O1 89.5(3) 3 2_545 ? O4 Cu1 O1 93.7(2) 2_545 2_545 ? O4 Cu1 O1 80.1(3) 4_566 2_545 ? O1' Cu1 O1 171.2(3) 4_566 2_545 ? O2 Cu1 Cu1 41.2(2) . 3 ? O2 Cu1 Cu1 41.1(2) 3 3 ? O4 Cu1 Cu1 138.2(2) 2_545 3 ? O4 Cu1 Cu1 138.1(2) 4_566 3 ? O1' Cu1 Cu1 92.6(2) 4_566 3 ? O1 Cu1 Cu1 93.53(19) 2_545 3 ? O2 Cu1 Cu1 138.9(2) . 3_556 ? O2 Cu1 Cu1 138.9(2) 3 3_556 ? O4 Cu1 Cu1 41.9(2) 2_545 3_556 ? O4 Cu1 Cu1 41.8(2) 4_566 3_556 ? O1' Cu1 Cu1 88.0(2) 4_566 3_556 ? O1 Cu1 Cu1 85.86(19) 2_545 3_556 ? Cu1 Cu1 Cu1 179.38(16) 3 3_556 ? O3 Cu2 O4 170.8(2) 3_565 . ? O3 Cu2 O1' 95.4(4) 3_565 2_554 ? O4 Cu2 O1' 90.4(4) . 2_554 ? O3 Cu2 O3 78.5(3) 3_565 . ? O4 Cu2 O3 92.6(2) . . ? O1' Cu2 O3 141.8(4) 2_554 . ? O3 Cu2 O1 94.4(4) 3_565 2 ? O4 Cu2 O1 91.1(4) . 2 ? O1' Cu2 O1 103.7(3) 2_554 2 ? O3 Cu2 O1 114.3(4) . 2 ? O3 Cu2 Cu2 39.85(18) 3_565 3_565 ? O4 Cu2 Cu2 131.18(17) . 3_565 ? O1' Cu2 Cu2 125.0(3) 2_554 3_565 ? O3 Cu2 Cu2 38.61(17) . 3_565 ? O1 Cu2 Cu2 108.5(3) 2 3_565 ? O1 As1 O1' 110.3(3) . . ? O1 As1 O3 108.6(4) . . ? O1' As1 O3 109.6(5) . . ? O1 As1 O2 111.7(4) . . ? O1' As1 O2 109.7(4) . . ? O3 As1 O2 106.9(3) . . ? As1 O1 Cu2 128.2(5) . 2_545 ? As1 O1 Cu1 112.1(4) . 2 ? Cu2 O1 Cu1 116.2(3) 2_545 2 ? As1 O1' Cu2 127.2(4) . 2_544 ? As1 O1' Cu1 114.4(4) . 4_665 ? Cu2 O1' Cu1 117.7(4) 2_544 4_665 ? As1 O2 Cu1 124.6(4) . . ? As1 O2 Cu1 127.4(5) . 3 ? Cu1 O2 Cu1 97.7(2) . 3 ? As1 O2 O2 153.3(4) . 3 ? Cu1 O2 O2 48.9(2) . 3 ? Cu1 O2 O2 48.8(3) 3 3 ? As1 O2 O4 87.0(3) . 2_545 ? Cu1 O2 O4 41.8(2) . 2_545 ? Cu1 O2 O4 139.5(3) 3 2_545 ? O2 O2 O4 90.7(4) 3 2_545 ? As1 O2 O4 89.7(3) . 2_544 ? Cu1 O2 O4 139.4(3) . 2_544 ? Cu1 O2 O4 41.8(2) 3 2_544 ? O2 O2 O4 90.5(4) 3 2_544 ? O4 O2 O4 174.9(3) 2_545 2_544 ? As1 O3 Cu2 128.5(4) . 3_565 ? As1 O3 Cu2 126.3(4) . . ? Cu2 O3 Cu2 101.5(3) 3_565 . ? As1 O3 O3 163.8(8) . 3_565 ? Cu2 O3 O3 51.7(2) 3_565 3_565 ? Cu2 O3 O3 49.8(2) . 3_565 ? Cu2 O4 Cu1 127.2(4) . 2 ? Cu2 O4 Cu1 121.5(5) . 4_665 ? Cu1 O4 Cu1 96.2(2) 2 4_665 ? Cu2 O4 O4 147.6(4) . 3_665 ? Cu1 O4 O4 48.2(3) 2 3_665 ? Cu1 O4 O4 48.0(3) 4_665 3_665 ? Cu2 O4 H1 105.4 . . ? Cu1 O4 H1 100.5 2 . ? Cu1 O4 H1 101.8 4_665 . ? O4 O4 H1 106.9 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.83 2.35 2.848(10) 118.9 3_665 O4 H1 O1' 0.83 2.52 2.982(11) 115.9 3_665 _refine_diff_density_max 1.677 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.274 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite joj 150C in P 21/n CELL .71073 8.2403 8.6442 5.9491 90.000 90.059 90.000 ZERR 4 .0010 .0009 .0007 .00 .010 .00 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z EQIV $6 -x+1/2, y-1/2, -z-1/2 BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O2 O4_$6 BIND O3 O3_$3 HTAB O4 O1_$5 HTAB O4 O1'_$5 L.S. 5 LIST 4 FMAP 2 TWIN -1 0 0 0 -1 0 0 0 1 PLAN 25 WGHT 0.045900 1.001600 BASF 0.67252 FVAR 0.31283 CU1 3 -0.000433 0.000829 0.249531 11.00000 0.02492 0.02936 = 0.01566 0.00010 0.00431 -0.00585 CU2 3 0.136861 0.619114 -0.017338 11.00000 0.01983 0.02690 = 0.03390 0.00291 0.00180 0.00021 AS1 4 0.237187 0.249835 0.007550 11.00000 0.02030 0.02130 = 0.01763 -0.00006 0.00309 -0.00090 O1 2 0.364351 0.256225 0.223304 11.00000 0.03442 0.04053 = 0.01828 0.01055 -0.01034 -0.00533 O1' 2 0.338466 0.273279 -0.234790 11.00000 0.03964 0.02761 = 0.02115 -0.00506 0.00544 -0.01565 O2 2 0.132412 0.081088 0.000603 11.00000 0.02804 0.02581 = 0.01517 -0.00006 0.00110 -0.00812 O3 2 0.098968 0.393441 0.037286 11.00000 0.02188 0.02136 = 0.05554 0.00444 0.00071 0.00332 O4 2 0.372643 0.595626 0.000201 11.00000 0.02262 0.02319 = 0.01640 0.00025 0.00313 -0.00067 AFIX 3 H1 1 0.409403 0.685266 0.001591 11.00000 -1.20000 AFIX 0 HKLF 4 REM olivenite joj 150C in P 21/n REM R1 = 0.0371 for 738 Fo > 4sig(Fo) and 0.0488 for all 884 data REM 74 parameters refined using 0 restraints END WGHT 0.0460 1.0032 REM Highest difference peak 1.677, deepest hole -1.611, 1-sigma level 0.274 Q1 1 0.1949 0.2662 0.1074 11.00000 0.05 1.68 Q2 1 0.1784 0.5949 -0.1099 11.00000 0.05 1.51 Q3 1 0.2410 0.3751 -0.0203 11.00000 0.05 0.89 Q4 1 0.0836 0.6992 0.0453 11.00000 0.05 0.84 Q5 1 0.0732 0.3924 0.1405 11.00000 0.05 0.83 Q6 1 0.3294 0.5806 0.1040 11.00000 0.05 0.82 Q7 1 -0.0162 0.3600 0.0694 11.00000 0.05 0.80 Q8 1 0.0830 0.0778 0.0918 11.00000 0.05 0.78 Q9 1 0.2165 -0.0338 -0.1585 11.00000 0.05 0.77 Q10 1 0.2988 0.2707 -0.1691 11.00000 0.05 0.73 Q11 1 0.5236 0.6811 0.1020 11.00000 0.05 0.71 Q12 1 0.4528 0.2755 0.1090 11.00000 0.05 0.71 Q13 1 -0.0464 0.1068 0.3095 11.00000 0.05 0.70 Q14 1 0.2378 0.5448 -0.1748 11.00000 0.05 0.66 Q15 1 0.0179 0.3928 -0.1014 11.00000 0.05 0.66 Q16 1 0.4251 0.7950 0.0944 11.00000 0.05 0.65 Q17 1 0.1835 0.1308 -0.0274 11.00000 0.05 0.65 Q18 1 -0.1240 -0.0027 0.2574 11.00000 0.05 0.64 Q19 1 0.4244 0.1323 0.1428 11.00000 0.05 0.64 Q20 1 0.1630 0.0386 -0.0430 11.00000 0.05 0.64 Q21 1 0.1298 0.0419 -0.0727 11.00000 0.05 0.63 Q22 1 0.2697 0.1538 -0.0445 11.00000 0.05 0.63 Q23 1 0.0418 -0.0080 0.1150 11.00000 0.05 0.60 Q24 1 0.2973 0.3686 -0.1796 11.00000 0.05 0.60 Q25 1 0.3469 0.4930 -0.0335 11.00000 0.05 0.60 ; _shelx_res_checksum 67667 _shelx_hkl_file ; 1 0 0 -1.9 1.1 1 2 0 0 136.9 3.4 1 3 0 0 -5.0 3.2 1 4 0 0 19.9 3.4 1 5 0 0 -8.7 3.9 1 6 0 0 76.0 4.4 1 7 0 0 11.4 4.5 1 8 0 0 1479.6 12.6 1 9 0 0 -3.7 3.8 1 10 0 0 32.8 3.3 1 0 1 0 1.5 0.9 1 1 1 0 611.6 4.0 1 -1 1 0 603.3 4.0 1 2 1 0 307.6 4.2 1 -2 1 0 301.3 4.1 1 3 1 0 1356.3 8.6 1 -3 1 0 1364.9 10.9 1 4 1 0 10.1 2.9 1 -4 1 0 11.2 4.1 1 5 1 0 684.4 7.8 1 -5 1 0 638.2 7.8 1 6 1 0 364.7 6.6 1 -6 1 0 343.2 6.5 1 7 1 0 55.0 4.8 1 -7 1 0 45.0 4.3 1 8 1 0 309.8 6.6 1 -8 1 0 275.1 6.3 1 9 1 0 67.0 4.2 1 -9 1 0 58.6 4.0 1 10 1 0 19.1 3.4 1 -10 1 0 14.4 3.6 1 0 2 0 90.6 2.3 1 1 2 0 807.6 5.8 1 -1 2 0 800.1 5.8 1 2 2 0 3800.1 13.2 1 -2 2 0 3655.1 13.0 1 3 2 0 236.6 4.4 1 -3 2 0 227.5 4.4 1 4 2 0 7.3 3.1 1 -4 2 0 7.2 2.9 1 5 2 0 561.6 7.3 1 -5 2 0 548.8 7.3 1 6 2 0 952.1 9.7 1 -6 2 0 984.7 13.1 1 7 2 0 26.9 3.4 1 -7 2 0 13.0 6.1 1 8 2 0 3.6 4.0 1 -8 2 0 -4.7 4.7 1 9 2 0 157.9 5.7 1 -9 2 0 124.0 5.1 1 10 2 0 227.6 5.9 1 -10 2 0 179.4 5.9 1 0 3 0 6.8 2.8 1 1 3 0 1545.9 8.9 1 -1 3 0 1513.3 8.8 1 2 3 0 19.8 2.0 1 -2 3 0 17.4 2.0 1 3 3 0 203.7 4.3 1 -3 3 0 196.1 4.4 1 4 3 0 94.6 3.6 1 -4 3 0 93.8 3.7 1 5 3 0 146.4 4.6 1 -5 3 0 145.8 4.7 1 6 3 0 70.8 4.3 1 -6 3 0 70.2 4.4 1 7 3 0 363.2 6.9 1 -7 3 0 366.1 7.0 1 8 3 0 10.5 4.3 1 -8 3 0 11.4 3.8 1 9 3 0 94.9 4.9 1 -9 3 0 91.6 6.1 1 0 4 0 724.2 6.8 1 1 4 0 119.5 3.4 1 -1 4 0 134.7 3.6 1 2 4 0 11.1 2.0 1 -2 4 0 14.8 2.1 1 3 4 0 11.0 2.5 1 -3 4 0 7.6 3.1 1 4 4 0 3360.8 16.3 1 -4 4 0 3270.8 16.0 1 5 4 0 80.6 4.3 1 -5 4 0 79.1 3.8 1 6 4 0 16.2 3.0 1 -6 4 0 16.7 3.4 1 7 4 0 3.4 4.1 1 -7 4 0 2.9 3.3 1 8 4 0 109.2 4.5 1 -8 4 0 93.9 4.5 1 9 4 0 8.1 3.9 1 -9 4 0 8.0 3.5 1 0 5 0 -1.1 3.2 1 1 5 0 1074.1 9.2 1 -1 5 0 1079.2 9.2 1 2 5 0 96.0 3.7 1 -2 5 0 91.7 3.8 1 3 5 0 34.3 3.1 1 -3 5 0 38.0 3.2 1 4 5 0 87.4 4.0 1 -4 5 0 84.8 3.8 1 5 5 0 109.7 4.5 1 -5 5 0 109.8 4.6 1 6 5 0 2.6 4.0 1 -6 5 0 1.1 3.3 1 7 5 0 284.0 6.3 1 -7 5 0 272.9 6.2 1 8 5 0 40.6 3.9 1 -8 5 0 32.5 3.6 1 9 5 0 48.0 4.3 1 -9 5 0 33.4 3.5 1 0 6 0 505.6 7.0 1 1 6 0 248.6 5.3 1 -1 6 0 232.2 5.3 1 2 6 0 1490.5 11.6 1 -2 6 0 1453.5 11.4 1 3 6 0 67.0 3.8 1 -3 6 0 61.8 3.5 1 4 6 0 85.1 4.0 1 -4 6 0 82.9 4.5 1 5 6 0 158.1 4.9 1 -5 6 0 156.4 4.9 1 6 6 0 472.8 7.8 1 -6 6 0 427.6 7.4 1 7 6 0 1.6 3.9 1 -7 6 0 1.6 3.4 1 8 6 0 35.4 3.5 1 -8 6 0 31.8 3.6 1 0 7 0 6.9 4.0 1 1 7 0 35.9 3.4 1 -1 7 0 31.8 3.0 1 2 7 0 34.0 3.2 1 -2 7 0 39.6 3.3 1 3 7 0 541.3 8.0 1 -3 7 0 509.3 7.7 1 4 7 0 -4.0 3.9 1 -4 7 0 -3.9 3.9 1 5 7 0 179.9 5.4 1 -5 7 0 177.7 5.5 1 6 7 0 196.2 5.6 1 -6 7 0 179.3 5.4 1 7 7 0 -0.4 3.8 1 -7 7 0 1.8 3.3 1 0 8 0 1766.2 13.4 1 1 8 0 6.5 3.9 1 -1 8 0 9.1 3.8 1 2 8 0 32.7 3.3 1 -2 8 0 27.2 3.0 1 3 8 0 11.1 3.9 1 -3 8 0 7.4 3.9 1 4 8 0 133.3 4.7 1 -4 8 0 121.0 4.5 1 5 8 0 8.7 3.8 1 -5 8 0 4.3 3.9 1 6 8 0 1.4 3.4 1 -6 8 0 0.3 3.3 1 -7 8 0 0.9 3.3 1 0 9 0 -6.5 3.9 1 1 9 0 15.2 3.1 1 -1 9 0 12.0 3.2 1 2 9 0 54.8 3.6 1 -2 9 0 45.9 3.4 1 3 9 0 198.2 5.4 1 -3 9 0 185.8 5.4 1 4 9 0 12.0 3.8 1 -4 9 0 8.4 4.1 1 5 9 0 113.7 4.7 1 -5 9 0 111.4 4.6 1 0 10 0 -5.7 3.6 1 1 10 0 -2.8 3.6 1 -1 10 0 10.2 3.6 1 2 10 0 328.2 6.8 1 -2 10 0 326.9 6.9 1 3 10 0 0.2 3.4 1 -3 10 0 2.3 3.5 1 4 10 0 53.7 3.6 1 -4 10 0 47.8 3.8 1 0 0 1 3.7 2.9 1 1 0 1 954.3 7.3 1 -1 0 1 926.0 7.7 1 2 0 1 6.8 5.2 1 -2 0 1 11.0 5.6 1 3 0 1 1162.0 10.4 1 -3 0 1 929.4 9.2 1 4 0 1 0.9 4.5 1 -4 0 1 6.8 3.8 1 5 0 1 15.8 5.1 1 -5 0 1 16.9 3.6 1 6 0 1 2.3 5.6 1 -6 0 1 3.3 4.3 1 7 0 1 8.6 6.1 1 -7 0 1 29.1 4.2 1 8 0 1 12.9 5.0 1 -8 0 1 -5.1 4.0 1 9 0 1 100.2 5.1 1 -9 0 1 81.1 4.7 1 10 0 1 0.0 4.5 1 -10 0 1 -0.3 3.7 1 0 1 1 1030.7 7.0 1 0 -1 1 1003.2 7.0 1 1 1 1 586.0 5.9 1 -1 1 1 649.6 6.7 1 1 -1 1 698.9 7.3 1 -1 -1 1 590.8 5.8 1 2 1 1 8.0 4.0 1 -2 1 1 23.7 5.7 1 2 -1 1 -3.2 6.2 1 -2 -1 1 3.0 3.8 1 3 1 1 1321.3 9.6 1 -3 1 1 1307.9 11.3 1 3 -1 1 1210.3 11.5 1 -3 -1 1 1121.1 8.5 1 4 1 1 433.0 6.7 1 -4 1 1 401.3 8.5 1 4 -1 1 413.4 8.3 1 -4 -1 1 369.4 5.9 1 5 1 1 1170.9 10.5 1 -5 1 1 1136.5 13.3 1 5 -1 1 1160.2 13.0 1 -5 -1 1 1029.5 9.4 1 6 1 1 14.7 5.1 1 -6 1 1 14.2 6.3 1 6 -1 1 21.2 6.7 1 -6 -1 1 11.4 4.4 1 7 1 1 175.2 6.5 1 -7 1 1 146.6 5.8 1 7 -1 1 184.1 8.2 1 -7 -1 1 162.4 5.2 1 8 1 1 65.3 4.9 1 -8 1 1 49.0 4.0 1 8 -1 1 60.0 5.8 1 -8 -1 1 44.7 3.6 1 9 1 1 7.5 4.4 1 -9 1 1 3.4 4.0 1 9 -1 1 5.2 5.1 1 -9 -1 1 -0.1 3.6 1 10 1 1 12.8 4.3 1 -10 1 1 3.6 3.9 1 10 -1 1 15.7 5.0 1 -10 -1 1 10.0 3.7 1 0 2 1 10.0 2.8 1 0 -2 1 -1.5 3.2 1 1 2 1 10.2 3.5 1 -1 2 1 -4.1 3.3 1 1 -2 1 6.3 3.9 1 -1 -2 1 0.4 3.1 1 2 2 1 449.8 5.6 1 -2 2 1 424.5 6.0 1 2 -2 1 461.4 6.4 1 -2 -2 1 386.2 5.3 1 3 2 1 14.4 3.0 1 -3 2 1 10.8 3.6 1 3 -2 1 9.7 4.6 1 -3 -2 1 12.4 3.1 1 4 2 1 126.9 4.1 1 -4 2 1 88.7 5.4 1 4 -2 1 146.7 6.6 1 -4 -2 1 77.6 3.6 1 5 2 1 145.5 5.0 1 -5 2 1 112.1 6.8 1 5 -2 1 131.5 8.1 1 -5 -2 1 98.9 4.2 1 6 2 1 182.7 5.7 1 -6 2 1 152.3 7.3 1 6 -2 1 192.3 9.2 1 -6 -2 1 149.2 5.1 1 7 2 1 127.1 5.4 1 -7 2 1 91.5 7.3 1 7 -2 1 138.5 8.4 1 -7 -2 1 99.5 4.6 1 8 2 1 79.7 4.7 1 -8 2 1 69.5 7.1 1 8 -2 1 82.4 7.1 1 -8 -2 1 66.3 4.3 1 9 2 1 73.2 4.5 1 -9 2 1 46.9 4.9 1 9 -2 1 59.4 6.2 1 -9 -2 1 48.0 3.9 1 10 2 1 31.2 3.9 1 -10 2 1 29.6 4.0 1 10 -2 1 37.9 5.8 1 -10 -2 1 30.3 3.6 1 0 3 1 547.0 5.9 1 0 -3 1 515.1 5.9 1 1 3 1 2052.5 10.8 1 -1 3 1 1905.5 10.5 1 1 -3 1 1897.8 10.5 1 -1 -3 1 1683.5 9.8 1 2 3 1 7.3 3.0 1 -2 3 1 5.9 3.1 1 2 -3 1 0.7 3.3 1 -2 -3 1 6.6 3.1 1 3 3 1 412.1 6.0 1 -3 3 1 386.0 6.1 1 3 -3 1 387.4 6.1 1 -3 -3 1 344.9 5.6 1 4 3 1 245.6 5.5 1 -4 3 1 213.3 5.5 1 4 -3 1 242.7 6.0 1 -4 -3 1 187.2 4.8 1 5 3 1 45.6 3.8 1 -5 3 1 57.0 4.2 1 5 -3 1 40.0 5.4 1 -5 -3 1 56.1 3.8 1 6 3 1 15.5 4.0 1 -6 3 1 11.5 4.7 1 6 -3 1 22.6 7.0 1 -6 -3 1 12.9 4.8 1 7 3 1 209.9 5.9 1 -7 3 1 233.5 7.2 1 7 -3 1 199.1 8.5 1 -7 -3 1 206.4 6.0 1 8 3 1 37.9 4.0 1 -8 3 1 30.1 5.5 1 8 -3 1 32.2 6.9 1 -8 -3 1 30.7 3.4 1 9 3 1 287.4 7.0 1 -9 3 1 232.9 8.3 1 9 -3 1 271.1 9.7 1 -9 -3 1 241.3 6.1 1 0 4 1 7.2 2.8 1 0 -4 1 7.7 2.1 1 1 4 1 278.5 5.1 1 -1 4 1 329.9 5.4 1 1 -4 1 257.6 5.0 1 -1 -4 1 313.2 5.4 1 2 4 1 16.8 3.7 1 -2 4 1 14.7 2.4 1 2 -4 1 8.4 3.4 1 -2 -4 1 7.2 3.7 1 3 4 1 154.6 4.6 1 -3 4 1 151.9 4.4 1 3 -4 1 151.7 4.5 1 -3 -4 1 139.6 4.4 1 4 4 1 5.6 4.3 1 -4 4 1 10.8 3.3 1 4 -4 1 11.2 4.3 1 -4 -4 1 12.9 4.3 1 5 4 1 268.8 6.3 1 -5 4 1 268.5 6.3 1 5 -4 1 258.1 6.7 1 -5 -4 1 239.8 5.9 1 6 4 1 3.5 4.5 1 -6 4 1 5.8 4.4 1 6 -4 1 -1.8 5.4 1 -6 -4 1 -3.9 4.5 1 7 4 1 393.5 7.3 1 -7 4 1 324.1 7.1 1 7 -4 1 374.2 8.3 1 -7 -4 1 294.0 6.6 1 8 4 1 3.8 4.3 1 -8 4 1 6.2 4.1 1 8 -4 1 2.7 4.9 1 -8 -4 1 3.8 4.2 1 9 4 1 46.7 3.9 1 -9 4 1 33.2 4.5 1 9 -4 1 32.5 4.4 1 -9 -4 1 30.8 4.0 1 0 5 1 500.7 6.9 1 0 -5 1 438.5 6.6 1 1 5 1 1251.4 10.3 1 -1 5 1 1171.2 10.0 1 1 -5 1 1135.0 9.8 1 -1 -5 1 1065.4 9.7 1 2 5 1 5.0 4.1 1 -2 5 1 11.7 3.8 1 2 -5 1 9.9 3.0 1 -2 -5 1 9.9 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6 5 21.9 4.8 1 5 -6 5 17.8 4.6 1 -5 -6 5 7.6 5.0 1 0 7 5 8.6 4.8 1 0 -7 5 3.1 5.0 1 1 7 5 60.0 4.1 1 -1 7 5 88.2 4.8 1 1 -7 5 47.5 4.9 1 -1 -7 5 76.1 5.1 1 2 7 5 9.0 4.4 1 -2 7 5 6.1 4.6 1 2 -7 5 1.8 4.8 1 -2 -7 5 5.6 4.6 1 3 7 5 144.4 5.8 1 -3 7 5 184.5 6.5 1 3 -7 5 93.4 6.1 1 -3 -7 5 152.5 6.1 1 0 8 5 7.3 4.3 1 0 -8 5 -7.6 4.8 1 1 -8 5 5.3 4.8 1 -1 -8 5 -1.8 5.1 1 0 0 6 106.5 6.9 1 1 0 6 0.8 6.8 1 -1 0 6 0.0 6.7 1 2 0 6 768.3 13.0 1 -2 0 6 599.0 11.6 1 3 0 6 18.4 6.7 1 -3 0 6 2.3 6.0 1 4 0 6 53.5 6.1 1 -4 0 6 44.7 5.7 1 5 0 6 -5.5 6.3 1 -5 0 6 2.2 5.8 1 6 0 6 231.8 8.8 1 -6 0 6 328.5 9.2 1 0 1 6 91.7 6.6 1 0 -1 6 93.4 6.4 1 1 1 6 162.6 7.6 1 -1 1 6 236.9 8.7 1 1 -1 6 161.4 7.3 1 -1 -1 6 210.0 7.8 1 2 1 6 32.7 6.1 1 -2 1 6 13.9 6.8 1 2 -1 6 31.2 6.0 1 -2 -1 6 10.7 6.3 1 3 1 6 96.8 6.2 1 -3 1 6 109.2 6.7 1 3 -1 6 90.1 6.7 1 -3 -1 6 106.7 6.4 1 4 1 6 10.2 6.3 1 -4 1 6 10.0 6.5 1 4 -1 6 10.9 6.7 1 -4 -1 6 17.9 6.1 1 5 1 6 118.3 6.3 1 -5 1 6 62.8 6.0 1 5 -1 6 123.9 7.2 1 -5 -1 6 53.0 5.7 1 6 1 6 46.4 6.5 1 -6 1 6 29.0 5.3 1 6 -1 6 46.4 6.4 1 -6 -1 6 22.6 5.5 1 0 2 6 481.5 10.5 1 0 -2 6 446.4 9.5 1 1 2 6 111.3 6.1 1 -1 2 6 68.5 5.7 1 1 -2 6 90.8 5.7 1 -1 -2 6 56.0 5.2 1 2 2 6 2.7 6.1 1 -2 2 6 -1.3 6.5 1 2 -2 6 -0.9 6.1 1 -2 -2 6 2.8 5.7 1 3 2 6 41.6 6.1 1 -3 2 6 67.7 5.7 1 3 -2 6 33.7 5.7 1 -3 -2 6 64.4 5.1 1 4 2 6 569.5 10.8 1 -4 2 6 583.0 11.7 1 4 -2 6 547.1 11.1 1 -4 -2 6 524.7 10.4 1 5 2 6 62.3 4.9 1 -5 2 6 39.8 7.3 1 5 -2 6 59.0 6.4 1 -5 -2 6 44.0 6.1 1 0 3 6 -4.2 5.6 1 0 -3 6 7.1 5.6 1 1 3 6 95.5 5.8 1 -1 3 6 68.4 5.5 1 1 -3 6 87.8 5.5 1 -1 -3 6 56.1 5.1 1 2 3 6 37.4 4.4 1 -2 3 6 22.5 6.1 1 2 -3 6 35.4 4.8 1 -2 -3 6 31.3 6.0 1 3 3 6 239.5 7.6 1 -3 3 6 189.9 7.7 1 3 -3 6 202.1 7.7 1 -3 -3 6 167.7 6.8 1 4 3 6 112.2 6.2 1 -4 3 6 45.6 5.9 1 4 -3 6 80.9 5.7 1 -4 -3 6 45.4 5.3 1 5 3 6 77.0 5.6 1 -5 3 6 116.3 7.9 1 5 -3 6 68.0 5.7 1 -5 -3 6 93.3 5.8 1 0 4 6 65.1 5.1 1 0 -4 6 55.1 5.2 1 1 4 6 6.8 5.1 1 -1 4 6 1.8 5.2 1 1 -4 6 4.6 5.3 1 -1 -4 6 -0.8 5.2 1 2 4 6 396.1 8.9 1 -2 4 6 504.3 10.0 1 2 -4 6 323.9 8.5 1 -2 -4 6 385.1 8.7 1 3 4 6 -5.9 4.9 1 -3 4 6 13.8 5.6 1 3 -4 6 6.4 5.2 1 -3 -4 6 -2.2 4.8 1 4 4 6 74.6 5.7 1 -4 4 6 94.3 6.1 1 4 -4 6 66.6 6.0 1 -4 -4 6 74.7 5.2 1 0 5 6 -3.4 4.9 1 0 -5 6 7.8 4.5 1 1 5 6 106.8 5.1 1 -1 5 6 78.8 5.2 1 1 -5 6 75.8 5.1 1 -1 -5 6 56.1 5.0 1 2 5 6 90.6 5.4 1 -2 5 6 50.5 5.2 1 2 -5 6 61.4 4.9 1 -2 -5 6 34.9 4.9 1 3 5 6 100.8 5.2 1 -3 5 6 80.2 5.5 1 3 -5 6 73.3 5.8 1 -3 -5 6 58.2 4.8 1 0 6 6 450.6 9.0 1 0 -6 6 358.9 8.5 1 1 6 6 17.8 4.1 1 -1 6 6 13.2 4.7 1 1 -6 6 8.9 4.8 1 -1 -6 6 1.1 4.9 1 2 6 6 4.1 4.7 1 -2 6 6 -2.1 4.6 1 2 -6 6 5.3 4.9 1 -2 -6 6 4.6 4.6 1 0 0 7 0.7 5.7 1 1 0 7 31.6 5.7 1 -1 0 7 10.4 5.9 1 2 0 7 9.9 5.4 1 -2 0 7 -1.3 5.4 1 3 0 7 116.3 6.4 1 -3 0 7 55.6 5.7 1 0 1 7 0.2 6.1 1 0 -1 7 7.6 5.4 1 1 1 7 38.7 5.7 1 -1 1 7 63.6 5.6 1 1 -1 7 44.8 5.0 1 -1 -1 7 68.2 5.5 1 2 1 7 10.4 5.7 1 -2 1 7 7.2 6.0 1 2 -1 7 7.3 6.0 1 -2 -1 7 9.7 5.5 1 3 1 7 142.2 7.0 1 -3 1 7 201.1 7.9 1 3 -1 7 132.6 7.1 1 -3 -1 7 160.6 7.2 1 0 2 7 20.6 5.9 1 0 -2 7 18.5 5.6 1 1 2 7 30.5 4.9 1 -1 2 7 13.0 5.7 1 1 -2 7 29.0 4.2 1 -1 -2 7 14.8 5.3 1 2 2 7 8.2 5.6 1 -2 2 7 19.9 6.3 1 2 -2 7 3.6 5.7 1 -2 -2 7 23.4 5.0 1 3 2 7 34.5 4.9 1 -3 2 7 21.0 6.3 1 3 -2 7 29.5 4.7 1 -3 -2 7 18.2 5.1 1 0 3 7 1.3 5.6 1 0 -3 7 1.6 5.0 1 1 3 7 148.5 6.6 1 -1 3 7 110.4 6.4 1 1 -3 7 118.4 6.0 1 -1 -3 7 88.1 5.4 1 2 3 7 7.8 5.4 1 -2 3 7 8.4 5.6 1 2 -3 7 6.0 5.4 1 -2 -3 7 2.2 5.1 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 53071 #==END data_OLI_200C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 58 _space_group_name_H-M_alt 'P n n m' _space_group_name_Hall '-P 2 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.2448(8) _cell_length_b 8.6632(8) _cell_length_c 5.9553(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 425.37(8) _cell_formula_units_Z 4 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.419 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.625 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 473(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1648 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.411 _diffrn_reflns_theta_max 26.510 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 489 _reflns_number_gt 410 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.3504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 489 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.2494(2) 0.0251(3) Uani 1 2 d S T P . . Cu2 Cu 0.13737(13) 0.61925(13) 0.0000 0.0311(3) Uani 1 2 d S T P . . As1 As 0.23663(11) 0.24965(10) 0.0000 0.0211(3) Uani 1 2 d S T P . . O1 O 0.3511(6) 0.2650(5) 0.2265(8) 0.0353(12) Uani 1 1 d . . . . . O2 O 0.1315(8) 0.0817(6) 0.0000 0.0241(13) Uani 1 2 d S T P . . O3 O 0.0989(8) 0.3924(7) 0.0000 0.048(2) Uani 1 2 d S T P . . O4 O 0.3726(8) 0.5970(6) 0.0000 0.0228(12) Uani 1 2 d S T P . . H1 H 0.4270 0.6850 0.0000 0.027 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0277(6) 0.0317(6) 0.0159(5) 0.000 0.000 -0.0069(5) Cu2 0.0214(6) 0.0290(6) 0.0430(7) 0.000 0.000 0.0009(5) As1 0.0216(5) 0.0221(4) 0.0195(5) 0.000 0.000 -0.0015(3) O1 0.045(3) 0.036(2) 0.024(2) 0.0078(19) -0.012(2) -0.015(2) O2 0.029(3) 0.024(3) 0.019(3) 0.000 0.000 -0.005(2) O3 0.023(3) 0.018(3) 0.102(7) 0.000 0.000 0.000(3) O4 0.023(3) 0.027(3) 0.019(3) 0.000 0.000 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.970(4) 5 ? Cu1 O2 1.970(4) . ? Cu1 O4 2.009(4) 3_545 ? Cu1 O4 2.009(4) 7_566 ? Cu1 O1 2.382(4) 4_455 ? Cu1 O1 2.382(4) 3_545 ? Cu1 Cu1 2.970(2) 5 ? Cu1 Cu1 2.985(2) 5_556 ? Cu2 O4 1.949(6) . ? Cu2 O3 1.950(7) 5_565 ? Cu2 O3 1.991(6) . ? Cu2 O1 2.063(5) 3 ? Cu2 O1 2.063(5) 8_665 ? Cu2 Cu2 3.066(2) 5_565 ? As1 O1 1.651(5) . ? As1 O1 1.651(5) 6 ? As1 O3 1.679(6) . ? As1 O2 1.694(6) . ? O1 Cu2 2.063(5) 3_545 ? O1 Cu1 2.382(4) 3 ? O2 Cu1 1.970(4) 5 ? O2 O2 2.590(13) 5 ? O2 O4 2.9808(5) 3_545 ? O3 Cu2 1.950(7) 5_565 ? O3 O3 2.477(13) 5_565 ? O4 Cu1 2.009(4) 3 ? O4 Cu1 2.009(4) 7_665 ? O4 O4 2.690(12) 5_665 ? O4 H1 0.8837 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 82.2(3) 5 . ? O2 Cu1 O4 176.2(2) 5 3_545 ? O2 Cu1 O4 97.01(17) . 3_545 ? O2 Cu1 O4 97.01(17) 5 7_566 ? O2 Cu1 O4 176.2(2) . 7_566 ? O4 Cu1 O4 84.1(3) 3_545 7_566 ? O2 Cu1 O1 93.9(2) 5 4_455 ? O2 Cu1 O1 91.3(2) . 4_455 ? O4 Cu1 O1 82.4(2) 3_545 4_455 ? O4 Cu1 O1 92.5(2) 7_566 4_455 ? O2 Cu1 O1 91.3(2) 5 3_545 ? O2 Cu1 O1 93.9(2) . 3_545 ? O4 Cu1 O1 92.5(2) 3_545 3_545 ? O4 Cu1 O1 82.4(2) 7_566 3_545 ? O1 Cu1 O1 173.1(2) 4_455 3_545 ? O2 Cu1 Cu1 41.09(14) 5 5 ? O2 Cu1 Cu1 41.09(14) . 5 ? O4 Cu1 Cu1 137.97(13) 3_545 5 ? O4 Cu1 Cu1 137.97(13) 7_566 5 ? O1 Cu1 Cu1 93.46(12) 4_455 5 ? O1 Cu1 Cu1 93.46(12) 3_545 5 ? O2 Cu1 Cu1 138.91(14) 5 5_556 ? O2 Cu1 Cu1 138.91(14) . 5_556 ? O4 Cu1 Cu1 42.03(13) 3_545 5_556 ? O4 Cu1 Cu1 42.03(13) 7_566 5_556 ? O1 Cu1 Cu1 86.54(12) 4_455 5_556 ? O1 Cu1 Cu1 86.54(12) 3_545 5_556 ? Cu1 Cu1 Cu1 180.0 5 5_556 ? O4 Cu2 O3 171.4(2) . 5_565 ? O4 Cu2 O3 93.5(3) . . ? O3 Cu2 O3 77.9(3) 5_565 . ? O4 Cu2 O1 90.82(18) . 3 ? O3 Cu2 O1 94.46(19) 5_565 3 ? O3 Cu2 O1 127.70(14) . 3 ? O4 Cu2 O1 90.82(18) . 8_665 ? O3 Cu2 O1 94.46(19) 5_565 8_665 ? O3 Cu2 O1 127.70(14) . 8_665 ? O1 Cu2 O1 104.3(3) 3 8_665 ? O4 Cu2 Cu2 131.96(18) . 5_565 ? O3 Cu2 Cu2 39.41(18) 5_565 5_565 ? O3 Cu2 Cu2 38.46(19) . 5_565 ? O1 Cu2 Cu2 116.53(16) 3 5_565 ? O1 Cu2 Cu2 116.53(16) 8_665 5_565 ? O1 As1 O1 109.5(4) . 6 ? O1 As1 O3 109.1(2) . . ? O1 As1 O3 109.1(2) 6 . ? O1 As1 O2 111.19(18) . . ? O1 As1 O2 111.19(18) 6 . ? O3 As1 O2 106.7(3) . . ? As1 O1 Cu2 128.5(2) . 3_545 ? As1 O1 Cu1 114.4(2) . 3 ? Cu2 O1 Cu1 116.8(2) 3_545 3 ? As1 O2 Cu1 126.17(16) . . ? As1 O2 Cu1 126.17(16) . 5 ? Cu1 O2 Cu1 97.8(3) . 5 ? As1 O2 O2 153.9(5) . 5 ? Cu1 O2 O2 48.91(14) . 5 ? Cu1 O2 O2 48.92(14) 5 5 ? As1 O2 O4 88.14(16) . 3_545 ? Cu1 O2 O4 41.99(12) . 3_545 ? Cu1 O2 O4 139.7(3) 5 3_545 ? O2 O2 O4 90.84(18) 5 3_545 ? As1 O3 Cu2 129.6(4) . 5_565 ? As1 O3 Cu2 128.3(4) . . ? Cu2 O3 Cu2 102.1(3) 5_565 . ? As1 O3 O3 178.6(5) . 5_565 ? Cu2 O3 O3 51.8(2) 5_565 5_565 ? Cu2 O3 O3 50.3(2) . 5_565 ? Cu2 O4 Cu1 124.15(19) . 3 ? Cu2 O4 Cu1 124.15(19) . 7_665 ? Cu1 O4 Cu1 95.9(3) 3 7_665 ? Cu2 O4 O4 147.0(4) . 5_665 ? Cu1 O4 O4 47.97(13) 3 5_665 ? Cu1 O4 O4 47.97(13) 7_665 5_665 ? Cu2 O4 H1 114.8 . . ? Cu1 O4 H1 95.5 3 . ? Cu1 O4 H1 95.5 7_665 . ? O4 O4 H1 98.2 5_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.88 2.31 2.905(7) 124.2 5_665 _refine_diff_density_max 0.746 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.203 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite jok 200C in Pnnm CELL .71073 8.2448 8.6632 5.9553 90.000 90.000 90.000 ZERR 4 .0008 .0008 .0008 .00 .000 .00 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$3 HTAB O4 O1_$5 L.S. 5 LIST 4 FMAP 2 PLAN 25 WGHT 0.031000 1.350400 FVAR 0.31270 CU1 3 0.000000 0.000000 0.249380 10.50000 0.02766 0.03165 = 0.01594 0.00000 0.00000 -0.00687 CU2 3 0.137373 0.619254 0.000000 10.50000 0.02135 0.02900 = 0.04301 0.00000 0.00000 0.00086 AS1 4 0.236626 0.249654 0.000000 10.50000 0.02156 0.02212 = 0.01951 0.00000 0.00000 -0.00149 O1 2 0.351050 0.265002 0.226455 11.00000 0.04542 0.03594 = 0.02447 0.00777 -0.01213 -0.01528 O2 2 0.131531 0.081678 0.000000 10.50000 0.02870 0.02412 = 0.01942 0.00000 0.00000 -0.00523 O3 2 0.098878 0.392352 0.000000 10.50000 0.02326 0.01833 = 0.10189 0.00000 0.00000 -0.00014 O4 2 0.372633 0.597034 0.000000 10.50000 0.02259 0.02693 = 0.01897 0.00000 0.00000 0.00081 AFIX 3 H1 1 0.426951 0.684972 0.000000 10.50000 -1.20000 AFIX 0 HKLF 4 REM olivenite jok 200C in Pnnm REM R1 = 0.0331 for 410 Fo > 4sig(Fo) and 0.0423 for all 489 data REM 45 parameters refined using 0 restraints END WGHT 0.0314 1.3461 REM Highest difference peak 0.746, deepest hole -1.007, 1-sigma level 0.203 Q1 1 0.2412 0.1446 0.0000 10.50000 0.05 0.75 Q2 1 0.1137 0.2941 0.0000 10.50000 0.05 0.63 Q3 1 0.2246 0.3580 0.0000 10.50000 0.05 0.59 Q4 1 0.1506 0.1823 0.0568 11.00000 0.05 0.55 Q5 1 0.1294 0.7059 0.0000 10.50000 0.05 0.54 Q6 1 0.0042 -0.1072 0.2424 11.00000 0.05 0.54 Q7 1 0.0866 0.5931 0.1107 11.00000 0.05 0.51 Q8 1 0.2993 0.6067 0.1097 11.00000 0.05 0.48 Q9 1 0.1991 0.0227 0.1009 11.00000 0.05 0.47 Q10 1 0.3094 0.2458 0.1183 11.00000 0.05 0.46 Q11 1 0.0265 0.3934 0.0000 10.50000 0.05 0.46 Q12 1 0.0299 0.6690 0.0640 11.00000 0.05 0.46 Q13 1 0.5109 0.7331 -0.1119 11.00000 0.05 0.43 Q14 1 0.2493 0.4403 0.0946 11.00000 0.05 0.42 Q15 1 0.3724 0.2507 0.3980 11.00000 0.05 0.42 Q16 1 0.1935 0.5517 0.0754 11.00000 0.05 0.41 Q17 1 0.0983 0.4955 0.0000 10.50000 0.05 0.40 Q18 1 0.2338 0.5874 0.0000 10.50000 0.05 0.39 Q19 1 0.0298 0.1726 0.0000 10.50000 0.05 0.39 Q20 1 0.3102 0.0253 0.0000 10.50000 0.05 0.38 Q21 1 0.4438 0.6018 0.1352 11.00000 0.05 0.37 Q22 1 0.3764 0.1847 0.1685 11.00000 0.05 0.36 Q23 1 0.3363 0.4655 0.0000 10.50000 0.05 0.36 Q24 1 0.4315 0.3049 0.3888 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3 7 3 318.8 7.3 1 -3 7 3 294.4 7.1 1 3 -7 3 287.6 7.2 1 -3 -7 3 276.1 7.3 1 4 7 3 32.5 3.7 1 -4 7 3 18.9 4.5 1 4 -7 3 25.7 4.8 1 -4 -7 3 23.6 5.0 1 5 7 3 332.7 7.4 1 -5 7 3 305.7 7.4 1 5 -7 3 302.9 7.8 1 -5 -7 3 290.8 7.2 1 6 7 3 5.5 4.2 1 -6 7 3 -10.4 4.5 1 6 -7 3 2.5 5.1 1 -6 -7 3 6.1 4.3 1 0 8 3 6.3 4.3 1 0 -8 3 -2.9 4.6 1 1 8 3 47.9 4.5 1 -1 8 3 50.5 4.5 1 1 -8 3 42.4 4.7 1 -1 -8 3 35.7 5.1 1 2 8 3 4.8 4.2 1 -2 8 3 3.3 4.3 1 2 -8 3 1.6 4.7 1 -2 -8 3 3.6 4.4 1 3 8 3 91.0 4.5 1 -3 8 3 86.1 5.5 1 3 -8 3 83.5 5.5 1 -3 -8 3 80.2 5.2 1 4 8 3 -1.6 4.1 1 -4 8 3 1.2 4.4 1 4 -8 3 -5.4 4.6 1 -4 -8 3 -6.8 4.2 1 5 8 3 3.7 4.2 1 -5 8 3 -1.6 4.6 1 5 -8 3 7.2 4.8 1 -5 -8 3 -3.7 4.0 1 0 9 3 58.2 4.4 1 0 -9 3 51.0 4.3 1 1 9 3 59.3 3.7 1 -1 9 3 56.7 4.1 1 1 -9 3 50.1 4.4 1 -1 -9 3 47.8 4.2 1 2 9 3 -1.4 3.9 1 -2 9 3 2.7 4.2 1 2 -9 3 1.8 4.5 1 -2 -9 3 2.1 3.9 1 3 9 3 147.7 5.3 1 -3 9 3 137.2 5.2 1 3 -9 3 137.2 6.0 1 -3 -9 3 126.8 5.1 1 4 9 3 37.8 3.6 1 -4 9 3 44.8 4.3 1 4 -9 3 38.4 5.2 1 -4 -9 3 31.8 4.4 1 0 0 4 5352.8 26.8 1 1 0 4 16.4 6.9 1 -1 0 4 -5.5 7.0 1 2 0 4 38.3 6.7 1 -2 0 4 36.3 6.4 1 3 0 4 15.3 7.3 1 -3 0 4 -0.1 7.8 1 4 0 4 145.2 7.4 1 -4 0 4 133.9 7.5 1 5 0 4 -8.5 7.1 1 -5 0 4 -3.1 6.9 1 6 0 4 29.2 5.4 1 -6 0 4 22.5 6.8 1 7 0 4 0.5 6.3 1 -7 0 4 3.7 6.2 1 8 0 4 732.5 12.4 1 -8 0 4 546.2 11.2 1 0 1 4 11.7 7.2 1 0 -1 4 3.9 7.5 1 1 1 4 269.3 8.4 1 -1 1 4 267.7 8.3 1 1 -1 4 258.7 8.5 1 -1 -1 4 240.5 8.2 1 2 1 4 44.9 5.6 1 -2 1 4 45.1 5.7 1 2 -1 4 50.9 7.5 1 -2 -1 4 52.7 5.6 1 3 1 4 492.4 10.5 1 -3 1 4 485.1 10.6 1 3 -1 4 504.2 11.2 1 -3 -1 4 461.6 10.0 1 4 1 4 16.3 6.8 1 -4 1 4 12.3 7.6 1 4 -1 4 6.0 7.7 1 -4 -1 4 11.4 7.1 1 5 1 4 249.7 8.2 1 -5 1 4 223.4 8.2 1 5 -1 4 222.9 9.0 1 -5 -1 4 202.0 7.6 1 6 1 4 146.3 6.9 1 -6 1 4 127.8 7.1 1 6 -1 4 152.4 8.1 1 -6 -1 4 114.0 7.2 1 7 1 4 49.8 5.5 1 -7 1 4 39.7 5.6 1 7 -1 4 47.4 7.1 1 -7 -1 4 41.1 5.8 1 8 1 4 147.8 7.0 1 -8 1 4 108.5 7.2 1 8 -1 4 147.8 8.3 1 -8 -1 4 122.0 6.7 1 0 2 4 22.3 6.2 1 0 -2 4 18.8 7.0 1 1 2 4 202.4 7.2 1 -1 2 4 203.5 7.4 1 1 -2 4 178.3 7.4 1 -1 -2 4 181.4 7.4 1 2 2 4 1619.8 15.3 1 -2 2 4 1597.3 16.0 1 2 -2 4 1543.8 16.2 1 -2 -2 4 1423.1 14.8 1 3 2 4 63.9 5.2 1 -3 2 4 88.8 7.1 1 3 -2 4 67.8 7.8 1 -3 -2 4 70.6 6.8 1 4 2 4 5.5 6.3 1 -4 2 4 16.6 7.3 1 4 -2 4 2.9 7.7 1 -4 -2 4 7.1 6.3 1 5 2 4 166.5 7.0 1 -5 2 4 154.8 7.3 1 5 -2 4 157.6 8.1 1 -5 -2 4 130.7 6.7 1 6 2 4 531.8 10.0 1 -6 2 4 467.1 10.8 1 6 -2 4 509.4 11.4 1 -6 -2 4 374.7 8.9 1 7 2 4 18.7 5.7 1 -7 2 4 18.6 6.2 1 7 -2 4 21.3 7.1 1 -7 -2 4 8.4 5.7 1 8 2 4 -3.6 5.6 1 -8 2 4 0.0 5.8 1 8 -2 4 -8.2 6.9 1 -8 -2 4 1.7 5.3 1 0 3 4 2.5 6.3 1 0 -3 4 3.0 6.7 1 1 3 4 505.2 9.4 1 -1 3 4 509.7 9.8 1 1 -3 4 483.7 10.0 1 -1 -3 4 445.6 9.3 1 2 3 4 12.2 6.3 1 -2 3 4 19.2 6.9 1 2 -3 4 15.8 7.2 1 -2 -3 4 9.7 6.7 1 3 3 4 109.3 6.0 1 -3 3 4 103.0 7.1 1 3 -3 4 102.7 7.0 1 -3 -3 4 99.8 6.2 1 4 3 4 45.2 5.1 1 -4 3 4 30.0 5.5 1 4 -3 4 39.3 6.4 1 -4 -3 4 22.5 5.9 1 5 3 4 96.8 5.5 1 -5 3 4 83.6 5.8 1 5 -3 4 87.0 7.0 1 -5 -3 4 71.1 5.3 1 6 3 4 41.7 5.7 1 -6 3 4 38.9 6.0 1 6 -3 4 54.7 6.9 1 -6 -3 4 27.8 4.6 1 7 3 4 192.3 7.2 1 -7 3 4 148.8 7.6 1 7 -3 4 147.7 8.4 1 -7 -3 4 121.6 6.1 1 8 3 4 11.2 5.4 1 -8 3 4 14.7 6.4 1 8 -3 4 21.9 6.6 1 -8 -3 4 13.9 5.3 1 0 4 4 449.0 8.9 1 0 -4 4 401.4 9.1 1 1 4 4 16.7 5.5 1 -1 4 4 19.0 6.0 1 1 -4 4 37.3 6.2 1 -1 -4 4 27.6 7.0 1 2 4 4 14.0 6.0 1 -2 4 4 0.2 5.6 1 2 -4 4 2.4 6.6 1 -2 -4 4 6.2 6.1 1 3 4 4 -5.2 5.6 1 -3 4 4 -3.0 6.1 1 3 -4 4 1.3 6.5 1 -3 -4 4 0.0 5.9 1 4 4 4 1501.7 14.7 1 -4 4 4 1419.8 15.1 1 4 -4 4 1304.7 15.1 1 -4 -4 4 1199.5 13.5 1 5 4 4 32.6 4.0 1 -5 4 4 15.3 6.6 1 5 -4 4 51.3 7.2 1 -5 -4 4 16.2 5.5 1 6 4 4 10.6 5.3 1 -6 4 4 18.3 5.7 1 6 -4 4 18.3 6.6 1 -6 -4 4 9.9 5.0 1 7 4 4 3.9 4.8 1 -7 4 4 5.7 5.4 1 7 -4 4 5.3 6.5 1 -7 -4 4 -2.0 4.7 1 0 5 4 -2.2 5.7 1 0 -5 4 -1.3 6.0 1 1 5 4 348.2 8.0 1 -1 5 4 348.0 8.4 1 1 -5 4 286.6 8.1 1 -1 -5 4 298.9 8.1 1 2 5 4 53.3 5.2 1 -2 5 4 48.8 4.4 1 2 -5 4 36.1 5.0 1 -2 -5 4 39.2 4.5 1 3 5 4 38.7 4.4 1 -3 5 4 42.3 4.7 1 3 -5 4 32.3 5.1 1 -3 -5 4 34.7 4.9 1 4 5 4 53.7 4.9 1 -4 5 4 44.7 6.2 1 4 -5 4 45.5 6.0 1 -4 -5 4 37.2 5.7 1 5 5 4 81.6 5.0 1 -5 5 4 72.0 5.5 1 5 -5 4 68.7 6.4 1 -5 -5 4 51.7 4.8 1 6 5 4 -4.6 4.9 1 -6 5 4 5.5 5.2 1 6 -5 4 5.4 5.9 1 -6 -5 4 -2.0 4.8 1 7 5 4 127.6 5.5 1 -7 5 4 127.3 6.1 1 7 -5 4 100.8 7.2 1 -7 -5 4 81.8 5.4 1 0 6 4 131.0 5.7 1 0 -6 4 117.2 5.9 1 1 6 4 83.0 4.7 1 -1 6 4 81.6 5.1 1 1 -6 4 64.3 5.1 1 -1 -6 4 63.0 5.0 1 2 6 4 694.7 10.3 1 -2 6 4 683.3 10.5 1 2 -6 4 581.2 10.2 1 -2 -6 4 561.8 9.7 1 3 6 4 26.3 3.7 1 -3 6 4 28.1 4.1 1 3 -6 4 18.4 6.0 1 -3 -6 4 20.7 4.2 1 4 6 4 15.5 4.9 1 -4 6 4 16.3 5.3 1 4 -6 4 7.9 5.7 1 -4 -6 4 13.8 4.9 1 5 6 4 55.1 4.3 1 -5 6 4 56.5 4.6 1 5 -6 4 53.5 6.1 1 -5 -6 4 45.1 4.9 1 6 6 4 228.8 6.6 1 -6 6 4 232.2 7.4 1 6 -6 4 196.9 8.1 1 -6 -6 4 173.4 6.2 1 0 7 4 7.3 4.8 1 0 -7 4 6.6 5.2 1 1 7 4 22.3 3.9 1 -1 7 4 17.8 3.6 1 1 -7 4 14.3 5.3 1 -1 -7 4 21.3 4.9 1 2 7 4 10.5 4.6 1 -2 7 4 12.2 4.8 1 2 -7 4 3.4 5.1 1 -2 -7 4 3.6 4.9 1 3 7 4 228.7 6.6 1 -3 7 4 226.1 6.8 1 3 -7 4 207.7 7.2 1 -3 -7 4 196.1 6.6 1 4 7 4 -2.5 4.2 1 -4 7 4 0.8 4.7 1 4 -7 4 -3.3 5.2 1 -4 -7 4 -4.2 4.5 1 5 7 4 81.9 4.8 1 -5 7 4 83.9 5.7 1 5 -7 4 79.2 5.9 1 -5 -7 4 63.9 5.2 1 0 8 4 722.6 10.5 1 0 -8 4 606.2 10.2 1 1 8 4 -3.4 4.4 1 -1 8 4 7.7 4.3 1 1 -8 4 5.3 4.4 1 -1 -8 4 0.0 4.4 1 2 8 4 20.5 3.5 1 -2 8 4 7.4 5.0 1 2 -8 4 4.8 5.0 1 -2 -8 4 8.0 4.5 1 3 8 4 6.1 4.1 1 -3 8 4 1.1 4.5 1 3 -8 4 0.4 4.8 1 -3 -8 4 -2.4 4.5 1 4 8 4 109.2 5.0 1 -4 8 4 97.4 5.7 1 4 -8 4 94.9 5.9 1 -4 -8 4 85.1 4.9 1 0 9 4 -1.1 4.1 1 0 -9 4 -0.4 4.4 1 1 9 4 9.8 4.4 1 -1 9 4 13.7 4.5 1 1 -9 4 16.0 4.1 1 -1 -9 4 16.8 4.5 1 0 0 5 12.7 7.8 1 1 0 5 55.2 7.1 1 -1 0 5 71.7 7.8 1 2 0 5 5.7 7.4 1 -2 0 5 3.9 7.1 1 3 0 5 100.0 8.0 1 -3 0 5 105.5 6.5 1 4 0 5 -9.9 7.0 1 -4 0 5 0.6 6.4 1 5 0 5 33.8 7.0 1 -5 0 5 3.7 6.6 1 6 0 5 0.3 6.4 1 -6 0 5 -3.9 6.3 1 7 0 5 4.1 6.6 1 -7 0 5 8.1 6.0 1 0 1 5 83.8 8.5 1 0 -1 5 59.4 5.9 1 1 1 5 210.1 8.3 1 -1 1 5 228.5 8.5 1 1 -1 5 203.6 8.6 1 -1 -1 5 215.5 7.8 1 2 1 5 2.6 7.1 1 -2 1 5 0.7 7.4 1 2 -1 5 14.1 7.2 1 -2 -1 5 7.0 6.7 1 3 1 5 325.8 9.5 1 -3 1 5 326.1 9.4 1 3 -1 5 323.3 9.6 1 -3 -1 5 316.1 8.9 1 4 1 5 47.0 6.6 1 -4 1 5 50.9 6.0 1 4 -1 5 49.3 6.7 1 -4 -1 5 36.5 5.8 1 5 1 5 266.8 8.4 1 -5 1 5 251.7 8.9 1 5 -1 5 241.3 8.7 1 -5 -1 5 226.5 7.7 1 6 1 5 13.2 6.2 1 -6 1 5 4.3 6.5 1 6 -1 5 6.3 6.8 1 -6 -1 5 1.4 6.1 1 7 1 5 58.0 5.6 1 -7 1 5 57.3 5.8 1 7 -1 5 57.3 7.1 1 -7 -1 5 48.7 5.5 1 0 2 5 17.0 7.1 1 0 -2 5 7.9 7.0 1 1 2 5 1.2 6.9 1 -1 2 5 8.5 7.1 1 1 -2 5 2.1 7.1 1 -1 -2 5 1.0 6.8 1 2 2 5 81.1 5.9 1 -2 2 5 84.2 6.5 1 2 -2 5 81.4 6.1 1 -2 -2 5 82.6 6.0 1 3 2 5 -13.8 6.4 1 -3 2 5 -5.6 6.6 1 3 -2 5 2.5 6.7 1 -3 -2 5 4.4 6.1 1 4 2 5 19.0 6.3 1 -4 2 5 8.6 6.9 1 4 -2 5 10.7 7.0 1 -4 -2 5 17.3 5.8 1 5 2 5 54.5 6.5 1 -5 2 5 49.5 7.2 1 5 -2 5 32.8 6.3 1 -5 -2 5 36.2 6.1 1 6 2 5 35.6 4.7 1 -6 2 5 37.1 6.9 1 6 -2 5 34.8 6.0 1 -6 -2 5 14.1 5.9 1 7 2 5 64.0 5.4 1 -7 2 5 64.9 6.1 1 7 -2 5 55.6 6.8 1 -7 -2 5 44.4 5.5 1 0 3 5 66.4 5.2 1 0 -3 5 51.9 5.5 1 1 3 5 612.5 10.6 1 -1 3 5 563.1 10.5 1 1 -3 5 532.9 10.4 1 -1 -3 5 478.2 10.1 1 2 3 5 -5.1 6.0 1 -2 3 5 -8.3 6.4 1 2 -3 5 2.3 6.3 1 -2 -3 5 11.6 5.8 1 3 3 5 109.9 5.8 1 -3 3 5 93.7 5.8 1 3 -3 5 105.9 7.4 1 -3 -3 5 82.7 5.7 1 4 3 5 37.0 4.7 1 -4 3 5 35.9 7.3 1 4 -3 5 37.7 6.5 1 -4 -3 5 24.4 4.5 1 5 3 5 23.5 5.1 1 -5 3 5 16.9 6.7 1 5 -3 5 21.3 6.4 1 -5 -3 5 19.8 5.1 1 6 3 5 10.5 5.4 1 -6 3 5 7.9 6.7 1 6 -3 5 5.0 6.4 1 -6 -3 5 7.3 5.5 1 7 3 5 112.1 6.3 1 -7 3 5 94.5 6.8 1 7 -3 5 89.0 7.2 1 -7 -3 5 68.2 6.5 1 0 4 5 -8.4 5.7 1 0 -4 5 5.2 5.6 1 1 4 5 34.3 4.4 1 -1 4 5 40.3 4.9 1 1 -4 5 26.3 6.4 1 -1 -4 5 45.5 5.7 1 2 4 5 -4.3 5.3 1 -2 4 5 -18.7 5.9 1 2 -4 5 -10.7 6.2 1 -2 -4 5 2.1 5.2 1 3 4 5 23.4 4.9 1 -3 4 5 21.5 4.8 1 3 -4 5 12.0 6.4 1 -3 -4 5 41.8 6.0 1 4 4 5 -0.5 5.4 1 -4 4 5 -2.4 6.1 1 4 -4 5 4.3 6.0 1 -4 -4 5 -3.1 5.5 1 5 4 5 75.0 5.2 1 -5 4 5 65.3 5.5 1 5 -4 5 57.8 6.2 1 -5 -4 5 50.6 4.9 1 6 4 5 8.4 5.1 1 -6 4 5 -8.2 6.5 1 6 -4 5 -0.2 6.1 1 -6 -4 5 6.9 5.1 1 0 5 5 48.5 4.9 1 0 -5 5 39.9 4.6 1 1 5 5 413.5 9.2 1 -1 5 5 389.8 8.6 1 1 -5 5 313.4 8.3 1 -1 -5 5 326.4 8.6 1 2 5 5 10.8 5.3 1 -2 5 5 3.4 5.2 1 2 -5 5 2.1 5.6 1 -2 -5 5 7.3 5.5 1 3 5 5 84.9 5.2 1 -3 5 5 78.2 5.1 1 3 -5 5 70.2 5.8 1 -3 -5 5 64.0 5.7 1 4 5 5 23.3 3.9 1 -4 5 5 17.6 5.6 1 4 -5 5 11.2 6.2 1 -4 -5 5 23.6 4.4 1 5 5 5 11.4 5.2 1 -5 5 5 13.9 5.8 1 5 -5 5 19.7 6.0 1 -5 -5 5 16.8 5.1 1 6 5 5 0.1 4.6 1 -6 5 5 13.5 5.5 1 6 -5 5 2.4 5.7 1 -6 -5 5 0.0 4.8 1 0 6 5 5.0 5.2 1 0 -6 5 -1.1 5.4 1 1 6 5 -4.7 5.0 1 -1 6 5 6.5 5.0 1 1 -6 5 7.4 5.3 1 -1 -6 5 -0.4 5.1 1 2 6 5 16.1 5.0 1 -2 6 5 17.2 5.5 1 2 -6 5 16.7 4.7 1 -2 -6 5 14.1 4.6 1 3 6 5 13.6 4.6 1 -3 6 5 13.1 5.2 1 3 -6 5 10.9 5.2 1 -3 -6 5 9.3 4.9 1 4 6 5 5.8 4.4 1 -4 6 5 5.9 5.2 1 4 -6 5 13.3 5.4 1 -4 -6 5 -5.4 4.6 1 5 6 5 24.8 4.7 1 -5 6 5 10.3 5.6 1 5 -6 5 26.4 6.0 1 -5 -6 5 6.5 4.8 1 0 7 5 3.9 4.8 1 0 -7 5 9.0 4.9 1 1 7 5 67.3 4.5 1 -1 7 5 68.0 4.4 1 1 -7 5 46.1 5.1 1 -1 -7 5 63.5 5.5 1 2 7 5 2.8 4.2 1 -2 7 5 2.1 4.6 1 2 -7 5 1.7 5.1 1 -2 -7 5 -2.6 4.6 1 3 7 5 131.3 5.3 1 -3 7 5 131.5 6.0 1 3 -7 5 108.4 6.3 1 -3 -7 5 106.0 5.6 1 0 8 5 7.3 4.1 1 0 -8 5 0.7 4.5 1 1 8 5 12.6 4.5 1 -1 8 5 13.7 4.5 1 1 -8 5 10.4 4.9 1 -1 -8 5 1.9 4.8 1 0 0 6 115.0 6.9 1 1 0 6 -2.2 6.7 1 -1 0 6 0.0 6.6 1 2 0 6 688.0 12.3 1 -2 0 6 657.8 12.1 1 3 0 6 16.2 7.0 1 -3 0 6 -5.0 6.3 1 4 0 6 66.7 6.3 1 -4 0 6 42.9 5.4 1 5 0 6 9.7 6.4 1 -5 0 6 2.1 5.7 1 6 0 6 248.9 8.8 1 -6 0 6 223.3 8.7 1 0 1 6 17.9 6.9 1 0 -1 6 8.5 6.5 1 1 1 6 187.3 8.0 1 -1 1 6 188.3 7.8 1 1 -1 6 191.0 8.3 1 -1 -1 6 192.1 7.6 1 2 1 6 7.7 6.6 1 -2 1 6 0.3 6.8 1 2 -1 6 12.7 6.7 1 -2 -1 6 5.4 6.1 1 3 1 6 76.0 6.1 1 -3 1 6 80.5 6.6 1 3 -1 6 75.1 6.4 1 -3 -1 6 76.1 5.7 1 4 1 6 15.2 6.4 1 -4 1 6 13.2 6.5 1 4 -1 6 19.3 6.9 1 -4 -1 6 3.8 6.2 1 5 1 6 87.2 5.9 1 -5 1 6 73.6 6.6 1 5 -1 6 94.5 6.9 1 -5 -1 6 73.3 6.7 1 6 1 6 40.4 5.8 1 -6 1 6 45.9 6.5 1 6 -1 6 40.8 6.9 1 -6 -1 6 40.6 6.0 1 0 2 6 487.4 10.4 1 0 -2 6 445.2 9.9 1 1 2 6 72.8 5.8 1 -1 2 6 64.5 7.3 1 1 -2 6 64.5 5.3 1 -1 -2 6 66.4 6.0 1 2 2 6 13.3 6.0 1 -2 2 6 11.3 6.5 1 2 -2 6 -1.7 6.4 1 -2 -2 6 7.7 5.8 1 3 2 6 29.7 5.4 1 -3 2 6 30.9 5.6 1 3 -2 6 28.5 5.6 1 -3 -2 6 23.7 4.9 1 4 2 6 573.0 10.9 1 -4 2 6 558.1 11.5 1 4 -2 6 512.5 11.6 1 -4 -2 6 500.7 10.4 1 5 2 6 38.6 5.0 1 -5 2 6 68.9 7.3 1 5 -2 6 33.5 5.9 1 -5 -2 6 47.8 6.0 1 0 3 6 8.6 5.9 1 0 -3 6 3.5 5.6 1 1 3 6 75.8 5.5 1 -1 3 6 63.9 5.6 1 1 -3 6 65.2 6.4 1 -1 -3 6 62.5 5.6 1 2 3 6 20.3 6.0 1 -2 3 6 24.2 5.7 1 2 -3 6 19.0 6.2 1 -2 -3 6 16.8 5.8 1 3 3 6 214.4 7.3 1 -3 3 6 200.1 7.5 1 3 -3 6 180.3 7.2 1 -3 -3 6 173.2 7.0 1 4 3 6 43.5 4.8 1 -4 3 6 43.7 6.0 1 4 -3 6 46.1 5.6 1 -4 -3 6 24.0 5.6 1 5 3 6 89.1 5.7 1 -5 3 6 83.0 6.4 1 5 -3 6 70.2 6.0 1 -5 -3 6 66.3 5.2 1 0 4 6 57.3 4.8 1 0 -4 6 51.6 5.5 1 1 4 6 3.5 5.5 1 -1 4 6 0.1 5.3 1 1 -4 6 1.6 5.4 1 -1 -4 6 -6.1 5.2 1 2 4 6 435.0 9.4 1 -2 4 6 434.4 9.8 1 2 -4 6 348.3 8.9 1 -2 -4 6 348.6 8.7 1 3 4 6 -4.8 5.0 1 -3 4 6 4.9 5.7 1 3 -4 6 5.6 5.4 1 -3 -4 6 6.9 4.8 1 4 4 6 85.1 5.3 1 -4 4 6 80.9 6.4 1 4 -4 6 55.4 6.0 1 -4 -4 6 61.0 5.7 1 0 5 6 -4.5 5.1 1 0 -5 6 1.7 4.9 1 1 5 6 93.8 5.7 1 -1 5 6 78.2 4.8 1 1 -5 6 67.9 5.7 1 -1 -5 6 59.9 5.1 1 2 5 6 68.1 4.8 1 -2 5 6 62.5 5.3 1 2 -5 6 42.2 4.7 1 -2 -5 6 43.1 5.0 1 3 5 6 83.8 5.1 1 -3 5 6 89.6 5.8 1 3 -5 6 57.8 5.0 1 -3 -5 6 52.5 4.7 1 0 6 6 437.6 9.0 1 0 -6 6 352.0 8.6 1 1 6 6 9.2 4.7 1 -1 6 6 8.7 4.8 1 1 -6 6 13.6 4.8 1 -1 -6 6 5.5 5.0 1 2 6 6 12.5 4.6 1 -2 6 6 8.4 4.8 1 2 -6 6 6.4 4.9 1 -2 -6 6 2.2 4.7 1 0 0 7 -7.3 5.8 1 1 0 7 13.7 4.9 1 -1 0 7 17.8 4.5 1 2 0 7 -10.3 5.9 1 -2 0 7 -3.8 5.8 1 3 0 7 70.8 6.5 1 -3 0 7 64.3 6.2 1 0 1 7 13.8 5.9 1 0 -1 7 15.4 5.8 1 1 1 7 48.3 5.9 1 -1 1 7 44.7 5.4 1 1 -1 7 50.2 6.2 1 -1 -1 7 36.5 4.9 1 2 1 7 -2.9 5.9 1 -2 1 7 1.4 5.8 1 2 -1 7 -3.3 5.6 1 -2 -1 7 8.9 5.5 1 3 1 7 177.9 7.8 1 -3 1 7 149.0 7.3 1 3 -1 7 125.9 6.6 1 -3 -1 7 145.1 6.7 1 0 2 7 4.0 6.0 1 0 -2 7 3.6 5.4 1 1 2 7 10.8 5.6 1 -1 2 7 0.7 6.0 1 1 -2 7 9.0 5.5 1 -1 -2 7 10.0 5.5 1 2 2 7 16.8 5.7 1 -2 2 7 17.3 4.1 1 2 -2 7 12.2 5.6 1 -2 -2 7 4.0 5.5 1 3 2 7 16.4 5.6 1 -3 2 7 21.0 5.9 1 3 -2 7 15.4 6.1 1 -3 -2 7 10.6 5.4 1 0 3 7 8.9 5.7 1 0 -3 7 10.7 5.1 1 1 3 7 118.3 6.4 1 -1 3 7 108.4 5.8 1 1 -3 7 124.6 6.4 1 -1 -3 7 104.7 5.8 1 2 3 7 -0.8 5.4 1 -2 3 7 -2.2 5.6 1 2 -3 7 12.8 5.3 1 -2 -3 7 -8.3 5.3 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 17869 #==END data_OLI_250C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 58 _space_group_name_H-M_alt 'P n n m' _space_group_name_Hall '-P 2 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.2506(8) _cell_length_b 8.6723(8) _cell_length_c 5.9577(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 426.28(8) _cell_formula_units_Z 4 _cell_measurement_temperature 523(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.410 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.588 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 523(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1651 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.408 _diffrn_reflns_theta_max 26.482 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 489 _reflns_number_gt 413 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.8791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 489 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.24912(18) 0.0266(3) Uani 1 2 d S T P . . Cu2 Cu 0.13743(13) 0.61923(12) 0.0000 0.0332(3) Uani 1 2 d S T P . . As1 As 0.23653(10) 0.24953(9) 0.0000 0.0222(2) Uani 1 2 d S T P . . O1 O 0.3518(6) 0.2648(5) 0.2280(8) 0.0379(12) Uani 1 1 d . . . . . O2 O 0.1330(8) 0.0808(6) 0.0000 0.0254(12) Uani 1 2 d S T P . . O3 O 0.0992(8) 0.3917(7) 0.0000 0.048(2) Uani 1 2 d S T P . . O4 O 0.3728(7) 0.5967(6) 0.0000 0.0252(12) Uani 1 2 d S T P . . H1 H 0.4143 0.6841 0.0000 0.030 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0294(6) 0.0331(6) 0.0172(5) 0.000 0.000 -0.0082(4) Cu2 0.0230(5) 0.0304(5) 0.0462(7) 0.000 0.000 0.0007(5) As1 0.0220(4) 0.0235(4) 0.0211(4) 0.000 0.000 -0.0014(3) O1 0.051(3) 0.039(2) 0.024(2) 0.0084(19) -0.014(2) -0.016(2) O2 0.029(3) 0.025(3) 0.022(3) 0.000 0.000 -0.007(2) O3 0.024(3) 0.024(3) 0.096(6) 0.000 0.000 0.004(3) O4 0.023(3) 0.028(3) 0.025(3) 0.000 0.000 -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.974(4) 5 ? Cu1 O2 1.974(4) . ? Cu1 O4 2.009(4) 7_566 ? Cu1 O4 2.009(4) 3_545 ? Cu1 O1 2.382(4) 4_455 ? Cu1 O1 2.382(4) 3_545 ? Cu1 Cu1 2.968(2) 5 ? Cu1 Cu1 2.989(2) 5_556 ? Cu2 O4 1.952(6) . ? Cu2 O3 1.955(7) 5_565 ? Cu2 O3 1.999(6) . ? Cu2 O1 2.056(4) 3 ? Cu2 O1 2.056(4) 8_665 ? Cu2 Cu2 3.069(2) 5_565 ? As1 O1 1.663(4) . ? As1 O1 1.663(4) 6 ? As1 O3 1.674(6) . ? As1 O2 1.694(5) . ? O1 Cu2 2.056(4) 3_545 ? O1 Cu1 2.382(4) 3 ? O2 Cu1 1.974(4) 5 ? O2 O2 2.603(12) 5 ? O2 O4 2.9824(6) 3_545 ? O3 Cu2 1.955(7) 5_565 ? O3 O3 2.493(12) 5_565 ? O4 Cu1 2.009(4) 7_665 ? O4 Cu1 2.009(4) 3 ? O4 O4 2.686(11) 5_665 ? O4 H1 0.8317 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 82.5(3) 5 . ? O2 Cu1 O4 96.95(17) 5 7_566 ? O2 Cu1 O4 175.9(2) . 7_566 ? O2 Cu1 O4 175.9(2) 5 3_545 ? O2 Cu1 O4 96.95(17) . 3_545 ? O4 Cu1 O4 83.9(2) 7_566 3_545 ? O2 Cu1 O1 93.5(2) 5 4_455 ? O2 Cu1 O1 91.39(19) . 4_455 ? O4 Cu1 O1 92.68(18) 7_566 4_455 ? O4 Cu1 O1 82.42(19) 3_545 4_455 ? O2 Cu1 O1 91.39(19) 5 3_545 ? O2 Cu1 O1 93.5(2) . 3_545 ? O4 Cu1 O1 82.42(19) 7_566 3_545 ? O4 Cu1 O1 92.68(18) 3_545 3_545 ? O1 Cu1 O1 173.4(2) 4_455 3_545 ? O2 Cu1 Cu1 41.25(13) 5 5 ? O2 Cu1 Cu1 41.25(13) . 5 ? O4 Cu1 Cu1 138.06(12) 7_566 5 ? O4 Cu1 Cu1 138.06(12) 3_545 5 ? O1 Cu1 Cu1 93.28(11) 4_455 5 ? O1 Cu1 Cu1 93.28(11) 3_545 5 ? O2 Cu1 Cu1 138.75(13) 5 5_556 ? O2 Cu1 Cu1 138.75(13) . 5_556 ? O4 Cu1 Cu1 41.94(12) 7_566 5_556 ? O4 Cu1 Cu1 41.94(12) 3_545 5_556 ? O1 Cu1 Cu1 86.72(11) 4_455 5_556 ? O1 Cu1 Cu1 86.72(11) 3_545 5_556 ? Cu1 Cu1 Cu1 180.0 5 5_556 ? O4 Cu2 O3 171.5(2) . 5_565 ? O4 Cu2 O3 93.3(2) . . ? O3 Cu2 O3 78.2(3) 5_565 . ? O4 Cu2 O1 91.05(17) . 3 ? O3 Cu2 O1 94.18(18) 5_565 3 ? O3 Cu2 O1 127.82(13) . 3 ? O4 Cu2 O1 91.05(17) . 8_665 ? O3 Cu2 O1 94.18(18) 5_565 8_665 ? O3 Cu2 O1 127.82(13) . 8_665 ? O1 Cu2 O1 104.0(3) 3 8_665 ? O4 Cu2 Cu2 131.89(16) . 5_565 ? O3 Cu2 Cu2 39.59(17) 5_565 5_565 ? O3 Cu2 Cu2 38.57(18) . 5_565 ? O1 Cu2 Cu2 116.47(15) 3 5_565 ? O1 Cu2 Cu2 116.47(15) 8_665 5_565 ? O1 As1 O1 109.5(4) . 6 ? O1 As1 O3 109.2(2) . . ? O1 As1 O3 109.2(2) 6 . ? O1 As1 O2 110.92(17) . . ? O1 As1 O2 110.92(17) 6 . ? O3 As1 O2 107.1(3) . . ? As1 O1 Cu2 128.3(2) . 3_545 ? As1 O1 Cu1 114.1(2) . 3 ? Cu2 O1 Cu1 117.29(19) 3_545 3 ? As1 O2 Cu1 125.93(15) . 5 ? As1 O2 Cu1 125.93(15) . . ? Cu1 O2 Cu1 97.5(3) 5 . ? As1 O2 O2 152.9(4) . 5 ? Cu1 O2 O2 48.75(13) 5 5 ? Cu1 O2 O2 48.75(13) . 5 ? As1 O2 O4 88.18(15) . 3_545 ? Cu1 O2 O4 139.3(3) 5 3_545 ? Cu1 O2 O4 41.98(11) . 3_545 ? O2 O2 O4 90.65(17) 5 3_545 ? As1 O3 Cu2 129.8(3) . 5_565 ? As1 O3 Cu2 128.3(4) . . ? Cu2 O3 Cu2 101.8(3) 5_565 . ? As1 O3 O3 178.5(5) . 5_565 ? Cu2 O3 O3 51.7(2) 5_565 5_565 ? Cu2 O3 O3 50.1(2) . 5_565 ? Cu2 O4 Cu1 124.14(18) . 7_665 ? Cu2 O4 Cu1 124.14(18) . 3 ? Cu1 O4 Cu1 96.1(2) 7_665 3 ? Cu2 O4 O4 147.1(4) . 5_665 ? Cu1 O4 O4 48.06(12) 7_665 5_665 ? Cu1 O4 O4 48.06(12) 3 5_665 ? Cu2 O4 H1 108.5 . . ? Cu1 O4 H1 99.5 7_665 . ? Cu1 O4 H1 99.5 3 . ? O4 O4 H1 104.4 5_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.83 2.40 2.907(7) 119.9 5_665 _refine_diff_density_max 0.640 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.186 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite jol 250C in P nnm CELL .71073 8.2506 8.6723 5.9577 90.000 90.000 90.000 ZERR 4 .0008 .0008 .0008 .00 .000 .00 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$3 HTAB O4 O1_$5 L.S. 5 LIST 4 FMAP 2 PLAN 25 WGHT 0.029500 0.879100 FVAR 0.31248 CU1 3 0.000000 0.000000 0.249124 10.50000 0.02945 0.03311 = 0.01722 0.00000 0.00000 -0.00825 CU2 3 0.137429 0.619230 0.000000 10.50000 0.02304 0.03040 = 0.04622 0.00000 0.00000 0.00066 AS1 4 0.236529 0.249527 0.000000 10.50000 0.02201 0.02348 = 0.02112 0.00000 0.00000 -0.00142 O1 2 0.351771 0.264800 0.228013 11.00000 0.05083 0.03895 = 0.02378 0.00844 -0.01404 -0.01559 O2 2 0.132950 0.080823 0.000000 10.50000 0.02906 0.02500 = 0.02208 0.00000 0.00000 -0.00697 O3 2 0.099239 0.391659 0.000000 10.50000 0.02439 0.02386 = 0.09577 0.00000 0.00000 0.00357 O4 2 0.372848 0.596705 0.000000 10.50000 0.02322 0.02753 = 0.02497 0.00000 0.00000 -0.00153 AFIX 3 H1 1 0.414308 0.684125 0.000000 10.50000 -1.20000 AFIX 0 HKLF 4 REM olivenite jol 250C in P nnm REM R1 = 0.0328 for 413 Fo > 4sig(Fo) and 0.0431 for all 489 data REM 45 parameters refined using 0 restraints END WGHT 0.0299 0.8166 REM Highest difference peak 0.640, deepest hole -0.805, 1-sigma level 0.186 Q1 1 0.1180 0.2946 0.0000 10.50000 0.05 0.64 Q2 1 0.1623 0.5643 0.1012 11.00000 0.05 0.54 Q3 1 0.2197 0.1451 0.0000 10.50000 0.05 0.51 Q4 1 0.2420 0.3564 0.0000 10.50000 0.05 0.50 Q5 1 0.2830 0.2599 0.1458 11.00000 0.05 0.50 Q6 1 -0.0080 0.3258 -0.0741 11.00000 0.05 0.49 Q7 1 0.1137 0.7331 0.0852 11.00000 0.05 0.49 Q8 1 0.1508 0.5030 0.0281 11.00000 0.05 0.48 Q9 1 0.0281 -0.1041 0.2320 11.00000 0.05 0.47 Q10 1 0.2490 0.5798 0.0000 10.50000 0.05 0.45 Q11 1 0.1226 0.7028 0.0000 10.50000 0.05 0.43 Q12 1 0.3089 0.5829 0.1062 11.00000 0.05 0.42 Q13 1 0.1485 0.2332 0.0975 11.00000 0.05 0.41 Q14 1 0.2489 0.0549 0.1190 11.00000 0.05 0.40 Q15 1 0.4967 0.7114 0.1427 11.00000 0.05 0.40 Q16 1 0.3800 0.3259 0.1350 11.00000 0.05 0.39 Q17 1 0.2922 0.4556 0.0641 11.00000 0.05 0.38 Q18 1 0.5270 0.2529 0.3339 11.00000 0.05 0.36 Q19 1 0.4647 0.2771 0.1151 11.00000 0.05 0.36 Q20 1 0.1273 0.4182 0.0987 11.00000 0.05 0.35 Q21 1 0.1561 0.4007 0.1085 11.00000 0.05 0.33 Q22 1 0.1823 0.4577 0.2138 11.00000 0.05 0.33 Q23 1 0.0021 0.1548 0.0000 10.50000 0.05 0.32 Q24 1 0.4299 0.3166 0.3890 11.00000 0.05 0.31 Q25 1 0.3652 0.1815 0.1736 11.00000 0.05 0.31 ; _shelx_res_checksum 43577 _shelx_hkl_file ; 1 0 0 0.8 1.0 1 2 0 0 140.3 3.3 1 3 0 0 -7.2 3.2 1 4 0 0 21.6 3.2 1 5 0 0 1.8 3.7 1 6 0 0 65.5 4.3 1 7 0 0 11.6 4.4 1 8 0 0 1329.0 12.0 1 9 0 0 -4.4 3.9 1 10 0 0 36.6 3.8 1 0 1 0 1.5 0.9 1 1 1 0 604.5 4.0 1 -1 1 0 606.4 3.9 1 2 1 0 328.9 4.3 1 -2 1 0 297.8 4.0 1 3 1 0 1325.9 8.5 1 -3 1 0 1382.8 11.5 1 4 1 0 11.0 2.3 1 -4 1 0 6.8 3.9 1 5 1 0 639.8 7.5 1 -5 1 0 576.7 7.4 1 6 1 0 365.1 6.7 1 -6 1 0 341.2 6.5 1 7 1 0 53.1 4.6 1 -7 1 0 39.5 3.8 1 8 1 0 292.7 6.5 1 -8 1 0 274.1 6.2 1 9 1 0 58.8 4.1 1 -9 1 0 48.2 4.0 1 10 1 0 11.8 4.1 1 -10 1 0 11.3 3.9 1 0 2 0 104.8 2.4 1 1 2 0 801.2 5.7 1 -1 2 0 792.5 5.7 1 2 2 0 3699.7 12.9 1 -2 2 0 3678.3 13.0 1 3 2 0 214.3 4.2 1 -3 2 0 211.6 4.3 1 4 2 0 5.6 3.0 1 -4 2 0 5.8 3.0 1 5 2 0 539.4 7.1 1 -5 2 0 574.2 7.8 1 6 2 0 903.0 9.4 1 -6 2 0 891.1 12.7 1 7 2 0 28.4 4.0 1 -7 2 0 14.6 5.3 1 8 2 0 -7.5 3.9 1 -8 2 0 -2.8 4.5 1 9 2 0 136.4 5.1 1 -9 2 0 110.2 5.0 1 10 2 0 178.9 5.7 1 -10 2 0 145.7 5.4 1 0 3 0 5.5 2.2 1 1 3 0 1492.4 8.7 1 -1 3 0 1496.6 8.7 1 2 3 0 17.5 2.1 1 -2 3 0 13.0 2.4 1 3 3 0 188.9 4.2 1 -3 3 0 181.1 4.3 1 4 3 0 87.8 3.4 1 -4 3 0 89.0 3.5 1 5 3 0 136.2 4.5 1 -5 3 0 133.6 4.5 1 6 3 0 78.8 4.5 1 -6 3 0 76.3 4.7 1 7 3 0 319.0 6.6 1 -7 3 0 329.1 6.9 1 8 3 0 9.3 4.1 1 -8 3 0 7.5 4.1 1 9 3 0 84.0 4.5 1 -9 3 0 65.5 5.5 1 0 4 0 711.1 6.9 1 1 4 0 109.7 3.4 1 -1 4 0 118.9 3.4 1 2 4 0 24.5 2.8 1 -2 4 0 12.7 2.0 1 3 4 0 20.1 3.4 1 -3 4 0 9.8 3.0 1 4 4 0 3201.0 15.8 1 -4 4 0 3090.5 15.6 1 5 4 0 86.8 4.2 1 -5 4 0 86.5 3.8 1 6 4 0 9.6 4.2 1 -6 4 0 16.5 3.9 1 7 4 0 2.2 3.8 1 -7 4 0 2.9 3.4 1 8 4 0 90.1 4.4 1 -8 4 0 83.8 4.5 1 9 4 0 1.0 4.0 1 -9 4 0 3.5 3.5 1 0 5 0 3.7 3.2 1 1 5 0 1000.5 8.9 1 -1 5 0 1018.1 8.8 1 2 5 0 89.3 3.5 1 -2 5 0 84.2 3.6 1 3 5 0 35.6 3.1 1 -3 5 0 30.1 3.3 1 4 5 0 92.7 4.1 1 -4 5 0 91.7 4.4 1 5 5 0 86.9 4.2 1 -5 5 0 84.9 4.0 1 6 5 0 -4.3 4.0 1 -6 5 0 0.5 3.3 1 7 5 0 254.3 6.3 1 -7 5 0 227.1 5.8 1 8 5 0 32.5 3.6 1 -8 5 0 38.3 3.2 1 9 5 0 38.0 4.0 1 -9 5 0 29.1 3.2 1 0 6 0 510.5 7.2 1 1 6 0 245.8 5.3 1 -1 6 0 220.0 5.1 1 2 6 0 1398.3 11.3 1 -2 6 0 1405.5 11.2 1 3 6 0 72.6 4.0 1 -3 6 0 64.5 3.8 1 4 6 0 73.3 4.0 1 -4 6 0 63.4 3.6 1 5 6 0 146.0 4.8 1 -5 6 0 142.3 4.9 1 6 6 0 409.3 7.4 1 -6 6 0 395.4 7.0 1 7 6 0 0.7 4.0 1 -7 6 0 0.2 3.3 1 8 6 0 39.6 4.4 1 -8 6 0 32.6 3.3 1 0 7 0 2.8 4.2 1 1 7 0 29.3 4.0 1 -1 7 0 30.9 3.4 1 2 7 0 31.9 3.2 1 -2 7 0 31.1 3.1 1 3 7 0 470.3 7.4 1 -3 7 0 456.7 7.5 1 4 7 0 -0.4 4.0 1 -4 7 0 -1.2 3.7 1 5 7 0 158.0 5.3 1 -5 7 0 155.3 5.0 1 6 7 0 179.1 5.3 1 -6 7 0 165.8 5.2 1 7 7 0 -0.4 3.7 1 -7 7 0 3.9 3.3 1 0 8 0 1599.2 12.9 1 1 8 0 6.5 4.0 1 -1 8 0 13.0 3.9 1 2 8 0 25.0 3.4 1 -2 8 0 33.5 3.2 1 3 8 0 7.1 4.0 1 -3 8 0 10.1 3.8 1 4 8 0 122.1 4.7 1 -4 8 0 110.5 4.7 1 5 8 0 5.0 3.7 1 -5 8 0 -0.3 3.7 1 6 8 0 -2.2 3.6 1 -6 8 0 0.5 3.3 1 7 8 0 3.7 3.3 1 -7 8 0 5.4 3.3 1 0 9 0 -6.5 4.0 1 1 9 0 11.4 3.6 1 -1 9 0 17.5 4.1 1 2 9 0 43.6 3.3 1 -2 9 0 46.6 3.3 1 3 9 0 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5.9 1 -5 -3 4 71.2 5.6 1 6 3 4 47.3 5.0 1 -6 3 4 34.4 6.1 1 6 -3 4 37.2 6.0 1 -6 -3 4 34.8 5.3 1 7 3 4 156.2 6.0 1 -7 3 4 140.1 7.4 1 7 -3 4 149.3 8.1 1 -7 -3 4 113.4 6.5 1 8 3 4 17.9 5.4 1 -8 3 4 15.4 6.1 1 8 -3 4 15.5 6.9 1 -8 -3 4 9.0 5.6 1 0 4 4 455.6 9.1 1 0 -4 4 396.4 9.1 1 1 4 4 17.7 5.7 1 -1 4 4 18.5 4.1 1 1 -4 4 20.3 4.9 1 -1 -4 4 16.2 6.2 1 2 4 4 7.3 5.8 1 -2 4 4 6.4 6.1 1 2 -4 4 15.7 6.6 1 -2 -4 4 9.8 6.2 1 3 4 4 0.5 5.5 1 -3 4 4 3.1 6.1 1 3 -4 4 2.2 6.7 1 -3 -4 4 5.3 5.7 1 4 4 4 1425.4 13.9 1 -4 4 4 1355.5 14.6 1 4 -4 4 1258.1 14.8 1 -4 -4 4 1106.9 13.0 1 5 4 4 32.9 4.4 1 -5 4 4 26.7 5.1 1 5 -4 4 21.9 6.9 1 -5 -4 4 25.2 4.2 1 6 4 4 11.4 5.2 1 -6 4 4 13.9 6.1 1 6 -4 4 7.9 6.4 1 -6 -4 4 4.4 5.3 1 7 4 4 6.5 4.7 1 -7 4 4 -15.5 5.9 1 7 -4 4 -3.1 6.2 1 -7 -4 4 -5.9 5.1 1 0 5 4 -0.9 5.4 1 0 -5 4 6.4 5.7 1 1 5 4 329.0 7.9 1 -1 5 4 327.0 7.7 1 1 -5 4 255.1 8.2 1 -1 -5 4 268.3 7.5 1 2 5 4 41.7 4.2 1 -2 5 4 44.5 4.3 1 2 -5 4 28.6 5.5 1 -2 -5 4 47.1 5.3 1 3 5 4 41.6 4.9 1 -3 5 4 42.4 4.6 1 3 -5 4 31.9 5.5 1 -3 -5 4 31.9 4.3 1 4 5 4 47.2 5.1 1 -4 5 4 43.2 4.3 1 4 -5 4 31.1 5.9 1 -4 -5 4 43.2 5.6 1 5 5 4 64.0 4.5 1 -5 5 4 61.6 5.7 1 5 -5 4 57.8 6.2 1 -5 -5 4 55.5 4.8 1 6 5 4 8.6 4.6 1 -6 5 4 6.1 5.4 1 6 -5 4 2.8 6.0 1 -6 -5 4 -0.5 4.9 1 7 5 4 105.8 5.3 1 -7 5 4 104.8 6.3 1 7 -5 4 106.0 7.4 1 -7 -5 4 79.7 5.2 1 0 6 4 133.7 5.6 1 0 -6 4 114.0 6.1 1 1 6 4 84.2 5.4 1 -1 6 4 79.1 4.9 1 1 -6 4 61.1 6.0 1 -1 -6 4 64.0 5.2 1 2 6 4 664.1 10.1 1 -2 6 4 652.7 10.1 1 2 -6 4 560.7 10.2 1 -2 -6 4 540.3 9.6 1 3 6 4 26.0 4.7 1 -3 6 4 23.5 4.0 1 3 -6 4 25.9 4.6 1 -3 -6 4 23.2 4.7 1 4 6 4 13.0 4.6 1 -4 6 4 16.3 5.3 1 4 -6 4 11.1 5.5 1 -4 -6 4 18.2 4.5 1 5 6 4 47.2 4.1 1 -5 6 4 45.2 5.1 1 5 -6 4 53.4 6.1 1 -5 -6 4 36.0 4.2 1 6 6 4 228.8 6.9 1 -6 6 4 213.2 7.3 1 6 -6 4 181.9 7.7 1 -6 -6 4 175.8 6.5 1 0 7 4 -4.9 5.0 1 0 -7 4 -5.1 5.1 1 1 7 4 20.5 4.7 1 -1 7 4 26.2 4.7 1 1 -7 4 20.4 5.4 1 -1 -7 4 24.6 5.1 1 2 7 4 7.3 4.7 1 -2 7 4 9.1 4.8 1 2 -7 4 0.4 5.2 1 -2 -7 4 7.6 4.8 1 3 7 4 215.1 6.7 1 -3 7 4 211.4 6.7 1 3 -7 4 185.0 7.5 1 -3 -7 4 181.8 6.2 1 4 7 4 -5.3 4.2 1 -4 7 4 -14.6 5.1 1 4 -7 4 2.0 5.0 1 -4 -7 4 9.7 4.2 1 5 7 4 87.3 4.7 1 -5 7 4 72.2 4.9 1 5 -7 4 73.1 6.0 1 -5 -7 4 61.0 5.1 1 0 8 4 696.1 10.4 1 0 -8 4 570.2 9.8 1 1 8 4 0.2 4.5 1 -1 8 4 5.8 4.4 1 1 -8 4 -0.6 4.6 1 -1 -8 4 2.9 4.5 1 2 8 4 5.6 4.6 1 -2 8 4 21.0 4.4 1 2 -8 4 11.6 4.9 1 -2 -8 4 12.1 4.4 1 3 8 4 7.1 4.1 1 -3 8 4 -6.0 4.8 1 3 -8 4 -0.4 4.8 1 -3 -8 4 -1.1 4.5 1 4 8 4 113.6 5.5 1 -4 8 4 82.0 5.0 1 4 -8 4 80.9 5.8 1 -4 -8 4 68.5 4.8 1 0 9 4 1.9 4.3 1 0 -9 4 1.9 4.1 1 1 9 4 13.6 4.3 1 -1 9 4 15.5 4.5 1 1 -9 4 12.8 4.7 1 -1 -9 4 12.3 4.4 1 0 0 5 16.2 7.4 1 1 0 5 48.8 7.9 1 -1 0 5 47.4 7.2 1 2 0 5 -1.3 7.4 1 -2 0 5 3.6 6.9 1 3 0 5 101.2 6.9 1 -3 0 5 97.5 6.9 1 4 0 5 9.1 6.8 1 -4 0 5 -3.5 6.5 1 5 0 5 19.1 7.0 1 -5 0 5 19.9 6.4 1 6 0 5 -2.6 6.5 1 -6 0 5 0.3 6.1 1 7 0 5 6.7 6.4 1 -7 0 5 5.1 5.9 1 0 1 5 58.6 5.9 1 0 -1 5 52.1 7.5 1 1 1 5 218.4 8.5 1 -1 1 5 226.0 8.8 1 1 -1 5 206.4 8.0 1 -1 -1 5 203.3 8.6 1 2 1 5 -22.4 7.7 1 -2 1 5 0.7 7.3 1 2 -1 5 9.5 7.1 1 -2 -1 5 7.9 6.7 1 3 1 5 307.9 8.9 1 -3 1 5 291.3 8.9 1 3 -1 5 297.2 8.7 1 -3 -1 5 275.5 8.2 1 4 1 5 37.7 5.9 1 -4 1 5 37.5 6.0 1 4 -1 5 40.1 5.5 1 -4 -1 5 44.2 5.4 1 5 1 5 249.4 8.6 1 -5 1 5 220.3 7.9 1 5 -1 5 238.1 8.7 1 -5 -1 5 206.6 7.9 1 6 1 5 9.7 6.2 1 -6 1 5 4.8 6.4 1 6 -1 5 10.1 6.7 1 -6 -1 5 -5.4 5.9 1 7 1 5 70.2 6.0 1 -7 1 5 60.2 6.1 1 7 -1 5 58.8 6.0 1 -7 -1 5 44.3 5.3 1 0 2 5 8.4 7.0 1 0 -2 5 4.7 6.8 1 1 2 5 -3.0 7.0 1 -1 2 5 9.2 7.2 1 1 -2 5 7.5 6.9 1 -1 -2 5 10.9 6.7 1 2 2 5 72.1 5.9 1 -2 2 5 68.0 5.8 1 2 -2 5 67.6 5.6 1 -2 -2 5 74.0 6.0 1 3 2 5 -5.2 6.3 1 -3 2 5 3.8 6.9 1 3 -2 5 -9.3 6.5 1 -3 -2 5 -3.3 6.1 1 4 2 5 12.2 6.0 1 -4 2 5 14.9 6.8 1 4 -2 5 10.6 6.6 1 -4 -2 5 27.6 6.2 1 5 2 5 41.5 5.0 1 -5 2 5 32.4 7.0 1 5 -2 5 31.5 5.0 1 -5 -2 5 32.1 6.0 1 6 2 5 30.8 4.6 1 -6 2 5 27.9 5.6 1 6 -2 5 21.1 5.7 1 -6 -2 5 16.9 6.0 1 7 2 5 58.4 5.0 1 -7 2 5 57.0 6.8 1 7 -2 5 59.6 7.5 1 -7 -2 5 52.0 6.1 1 0 3 5 57.5 5.1 1 0 -3 5 52.8 6.3 1 1 3 5 562.2 10.4 1 -1 3 5 532.7 10.5 1 1 -3 5 478.3 10.0 1 -1 -3 5 463.4 10.2 1 2 3 5 2.7 5.6 1 -2 3 5 -5.0 6.4 1 2 -3 5 -4.4 6.3 1 -2 -3 5 -1.3 5.9 1 3 3 5 107.5 5.9 1 -3 3 5 104.8 6.4 1 3 -3 5 99.8 6.5 1 -3 -3 5 94.6 5.9 1 4 3 5 27.5 4.4 1 -4 3 5 36.0 5.2 1 4 -3 5 45.1 7.1 1 -4 -3 5 22.9 5.3 1 5 3 5 30.5 5.5 1 -5 3 5 41.1 6.1 1 5 -3 5 8.1 6.8 1 -5 -3 5 24.2 4.9 1 6 3 5 5.0 5.2 1 -6 3 5 -6.5 6.6 1 6 -3 5 9.2 6.4 1 -6 -3 5 8.7 5.4 1 7 3 5 89.8 5.8 1 -7 3 5 89.5 7.1 1 7 -3 5 87.0 7.1 1 -7 -3 5 63.8 5.4 1 0 4 5 -4.1 5.4 1 0 -4 5 6.8 5.7 1 1 4 5 24.7 4.8 1 -1 4 5 34.5 5.5 1 1 -4 5 25.3 4.9 1 -1 -4 5 36.6 6.1 1 2 4 5 1.0 5.2 1 -2 4 5 6.7 5.6 1 2 -4 5 9.2 5.9 1 -2 -4 5 0.0 5.6 1 3 4 5 23.5 4.0 1 -3 4 5 34.0 6.3 1 3 -4 5 17.2 6.2 1 -3 -4 5 21.9 5.9 1 4 4 5 -4.0 5.2 1 -4 4 5 7.8 5.6 1 4 -4 5 -0.7 6.1 1 -4 -4 5 -2.6 5.5 1 5 4 5 72.8 4.8 1 -5 4 5 52.8 5.3 1 5 -4 5 64.4 6.6 1 -5 -4 5 52.4 4.7 1 6 4 5 -6.3 4.9 1 -6 4 5 -6.8 6.3 1 6 -4 5 -5.2 6.0 1 -6 -4 5 7.2 5.0 1 0 5 5 47.4 4.7 1 0 -5 5 37.2 5.2 1 1 5 5 364.9 8.2 1 -1 5 5 372.4 8.5 1 1 -5 5 312.2 8.2 1 -1 -5 5 313.8 8.6 1 2 5 5 8.0 5.0 1 -2 5 5 7.5 5.4 1 2 -5 5 -5.1 5.8 1 -2 -5 5 8.1 5.3 1 3 5 5 73.7 5.3 1 -3 5 5 72.2 4.9 1 3 -5 5 64.8 5.8 1 -3 -5 5 64.9 5.3 1 4 5 5 20.7 3.6 1 -4 5 5 17.6 3.9 1 4 -5 5 13.2 5.9 1 -4 -5 5 6.9 5.4 1 5 5 5 19.3 4.0 1 -5 5 5 19.4 5.8 1 5 -5 5 11.9 6.1 1 -5 -5 5 9.5 5.4 1 6 5 5 -0.7 4.4 1 -6 5 5 5.3 5.6 1 6 -5 5 -1.4 6.1 1 -6 -5 5 1.4 4.9 1 0 6 5 9.6 4.6 1 0 -6 5 3.6 5.2 1 1 6 5 -0.5 4.6 1 -1 6 5 3.9 5.0 1 1 -6 5 -5.7 5.6 1 -1 -6 5 -1.7 5.4 1 2 6 5 30.6 4.3 1 -2 6 5 20.0 5.2 1 2 -6 5 26.4 5.2 1 -2 -6 5 10.3 5.4 1 3 6 5 8.0 4.7 1 -3 6 5 9.8 5.2 1 3 -6 5 12.4 5.3 1 -3 -6 5 4.0 4.8 1 4 6 5 -2.7 4.4 1 -4 6 5 5.1 5.1 1 4 -6 5 3.7 5.4 1 -4 -6 5 -10.0 5.0 1 5 6 5 13.3 4.5 1 -5 6 5 26.7 5.7 1 5 -6 5 6.3 5.8 1 -5 -6 5 17.0 4.4 1 0 7 5 7.5 4.8 1 0 -7 5 11.9 4.9 1 1 7 5 61.8 4.9 1 -1 7 5 60.0 4.2 1 1 -7 5 40.3 4.7 1 -1 -7 5 47.2 5.1 1 2 7 5 0.0 4.4 1 -2 7 5 -4.9 4.7 1 2 -7 5 -9.8 4.9 1 -2 -7 5 0.4 4.6 1 3 7 5 125.5 5.2 1 -3 7 5 125.9 6.0 1 3 -7 5 106.0 6.6 1 -3 -7 5 101.0 5.4 1 0 8 5 3.0 4.3 1 0 -8 5 8.9 4.5 1 1 8 5 11.1 4.4 1 -1 8 5 7.0 4.4 1 1 -8 5 6.1 4.8 1 -1 -8 5 13.7 4.5 1 0 0 6 97.3 6.9 1 1 0 6 13.4 6.4 1 -1 0 6 -8.7 6.7 1 2 0 6 620.6 11.8 1 -2 0 6 595.8 11.1 1 3 0 6 21.7 6.7 1 -3 0 6 0.3 6.1 1 4 0 6 43.0 5.3 1 -4 0 6 40.6 6.2 1 5 0 6 -5.8 6.5 1 -5 0 6 7.9 5.7 1 6 0 6 251.2 9.2 1 -6 0 6 209.3 8.1 1 0 1 6 7.4 6.8 1 0 -1 6 11.4 6.4 1 1 1 6 194.9 8.3 1 -1 1 6 192.6 8.1 1 1 -1 6 188.1 7.8 1 -1 -1 6 182.6 7.5 1 2 1 6 11.5 6.8 1 -2 1 6 6.5 6.8 1 2 -1 6 15.7 6.5 1 -2 -1 6 -1.2 6.2 1 3 1 6 76.3 6.2 1 -3 1 6 71.2 5.6 1 3 -1 6 65.4 6.0 1 -3 -1 6 72.3 6.3 1 4 1 6 12.9 6.4 1 -4 1 6 16.5 6.3 1 4 -1 6 11.8 6.6 1 -4 -1 6 10.4 6.1 1 5 1 6 72.1 6.5 1 -5 1 6 71.8 6.5 1 5 -1 6 64.3 6.1 1 -5 -1 6 65.2 6.0 1 6 1 6 41.6 6.0 1 -6 1 6 41.9 6.5 1 6 -1 6 36.5 6.2 1 -6 -1 6 37.7 5.3 1 0 2 6 470.2 10.4 1 0 -2 6 445.3 9.9 1 1 2 6 59.6 5.8 1 -1 2 6 71.9 6.7 1 1 -2 6 56.0 5.9 1 -1 -2 6 53.8 6.4 1 2 2 6 18.9 5.9 1 -2 2 6 10.2 6.5 1 2 -2 6 -1.0 6.3 1 -2 -2 6 1.9 6.1 1 3 2 6 26.1 5.0 1 -3 2 6 20.5 7.1 1 3 -2 6 20.9 5.8 1 -3 -2 6 17.8 4.4 1 4 2 6 540.8 10.8 1 -4 2 6 512.3 11.5 1 4 -2 6 510.9 11.0 1 -4 -2 6 451.7 9.9 1 5 2 6 44.9 4.7 1 -5 2 6 31.0 6.7 1 5 -2 6 37.4 6.1 1 -5 -2 6 29.8 5.6 1 0 3 6 -5.2 6.1 1 0 -3 6 6.3 5.7 1 1 3 6 71.6 6.3 1 -1 3 6 67.1 6.8 1 1 -3 6 59.1 6.5 1 -1 -3 6 55.6 6.6 1 2 3 6 20.8 5.8 1 -2 3 6 22.6 5.3 1 2 -3 6 26.2 5.6 1 -2 -3 6 38.4 5.9 1 3 3 6 207.9 7.4 1 -3 3 6 199.6 8.0 1 3 -3 6 180.2 7.6 1 -3 -3 6 165.1 7.2 1 4 3 6 43.1 5.4 1 -4 3 6 32.7 5.6 1 4 -3 6 30.6 6.2 1 -4 -3 6 27.4 5.4 1 5 3 6 85.8 5.8 1 -5 3 6 80.1 6.0 1 5 -3 6 78.6 6.9 1 -5 -3 6 67.5 5.6 1 0 4 6 57.3 5.1 1 0 -4 6 46.7 5.3 1 1 4 6 4.1 5.2 1 -1 4 6 2.3 5.5 1 1 -4 6 -2.4 5.4 1 -1 -4 6 8.4 5.1 1 2 4 6 417.4 9.0 1 -2 4 6 389.3 9.3 1 2 -4 6 331.7 8.6 1 -2 -4 6 323.4 8.5 1 3 4 6 4.7 4.7 1 -3 4 6 9.7 5.7 1 3 -4 6 18.3 5.3 1 -3 -4 6 -6.5 5.1 1 4 4 6 81.5 5.6 1 -4 4 6 77.2 6.1 1 4 -4 6 77.1 6.2 1 -4 -4 6 64.5 5.0 1 0 5 6 -4.4 5.0 1 0 -5 6 -11.7 5.0 1 1 5 6 77.7 4.9 1 -1 5 6 67.5 4.8 1 1 -5 6 53.2 4.8 1 -1 -5 6 60.5 5.0 1 2 5 6 58.8 5.3 1 -2 5 6 48.5 5.0 1 2 -5 6 41.5 4.4 1 -2 -5 6 39.7 4.7 1 3 5 6 73.4 4.6 1 -3 5 6 72.9 4.9 1 3 -5 6 60.2 5.5 1 -3 -5 6 54.2 5.0 1 0 6 6 373.7 8.6 1 0 -6 6 320.3 8.5 1 1 6 6 2.9 4.6 1 -1 6 6 3.4 4.7 1 1 -6 6 4.7 5.0 1 -1 -6 6 -3.5 5.0 1 2 6 6 4.5 4.3 1 -2 6 6 3.4 4.8 1 2 -6 6 5.2 4.6 1 -2 -6 6 9.8 4.9 1 0 0 7 -5.0 5.8 1 1 0 7 13.5 6.0 1 -1 0 7 10.1 5.9 1 2 0 7 5.6 5.4 1 -2 0 7 -4.7 5.7 1 3 0 7 63.5 6.5 1 -3 0 7 64.5 5.9 1 0 1 7 3.7 5.9 1 0 -1 7 11.3 5.6 1 1 1 7 39.3 5.6 1 -1 1 7 45.8 5.4 1 1 -1 7 50.2 6.0 1 -1 -1 7 51.4 5.7 1 2 1 7 -2.2 5.7 1 -2 1 7 0.5 5.8 1 2 -1 7 2.1 5.6 1 -2 -1 7 -6.9 5.6 1 3 1 7 141.4 6.8 1 -3 1 7 134.6 7.0 1 3 -1 7 132.4 6.9 1 -3 -1 7 121.1 6.4 1 0 2 7 16.5 5.7 1 0 -2 7 1.8 5.2 1 1 2 7 8.6 5.4 1 -1 2 7 13.5 5.7 1 1 -2 7 -1.9 5.1 1 -1 -2 7 8.3 5.1 1 2 2 7 11.4 5.6 1 -2 2 7 14.7 5.8 1 2 -2 7 7.3 5.7 1 -2 -2 7 9.9 5.3 1 3 2 7 17.9 5.7 1 -3 2 7 -2.6 6.1 1 3 -2 7 11.9 5.4 1 -3 -2 7 15.1 5.1 1 0 3 7 6.6 5.3 1 0 -3 7 13.0 4.9 1 1 3 7 107.6 5.9 1 -1 3 7 116.4 6.2 1 1 -3 7 91.8 6.1 1 -1 -3 7 91.0 5.4 1 2 3 7 -2.7 5.2 1 -2 3 7 -8.0 5.7 1 2 -3 7 0.0 5.3 1 -2 -3 7 1.9 4.6 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 8982 #==END data_OLI_300C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 58 _space_group_name_H-M_alt 'P n n m' _space_group_name_Hall '-P 2 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.2547(10) _cell_length_b 8.6792(10) _cell_length_c 5.9605(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 427.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 573(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.402 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.557 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 573(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1652 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.406 _diffrn_reflns_theta_max 26.531 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 490 _reflns_number_gt 405 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 490 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.24932(18) 0.0276(3) Uani 1 2 d S T P . . Cu2 Cu 0.13751(12) 0.61933(12) 0.0000 0.0345(3) Uani 1 2 d S T P . . As1 As 0.23630(9) 0.24950(8) 0.0000 0.0229(2) Uani 1 2 d S T P . . O1 O 0.3502(6) 0.2647(5) 0.2276(8) 0.0391(11) Uani 1 1 d . . . . . O2 O 0.1309(7) 0.0809(6) 0.0000 0.0276(12) Uani 1 2 d S T P . . O3 O 0.0996(7) 0.3929(6) 0.0000 0.048(2) Uani 1 2 d S T P . . O4 O 0.3723(7) 0.5965(5) 0.0000 0.0242(11) Uani 1 2 d S T P . . H1 H 0.4249 0.6803 0.0000 0.029 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0298(5) 0.0349(5) 0.0181(5) 0.000 0.000 -0.0084(4) Cu2 0.0232(5) 0.0321(5) 0.0482(6) 0.000 0.000 0.0016(4) As1 0.0227(4) 0.0238(4) 0.0222(4) 0.000 0.000 -0.0015(3) O1 0.050(3) 0.040(2) 0.028(2) 0.0098(18) -0.015(2) -0.0156(19) O2 0.038(3) 0.026(2) 0.019(3) 0.000 0.000 -0.010(2) O3 0.024(3) 0.021(3) 0.099(6) 0.000 0.000 0.002(2) O4 0.022(2) 0.029(3) 0.022(2) 0.000 0.000 -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.967(4) 5 ? Cu1 O2 1.967(4) . ? Cu1 O4 2.011(4) 7_566 ? Cu1 O4 2.011(4) 3_545 ? Cu1 O1 2.391(4) 4_455 ? Cu1 O1 2.391(4) 3_545 ? Cu1 Cu1 2.972(2) 5 ? Cu1 Cu1 2.988(2) 5_556 ? Cu2 O4 1.948(6) . ? Cu2 O3 1.960(6) 5_565 ? Cu2 O3 1.990(5) . ? Cu2 O1 2.059(4) 3 ? Cu2 O1 2.059(4) 8_665 ? Cu2 Cu2 3.073(2) 5_565 ? As1 O1 1.656(4) . ? As1 O1 1.656(4) 6 ? As1 O3 1.680(5) . ? As1 O2 1.702(5) . ? O1 Cu2 2.059(4) 3_545 ? O1 Cu1 2.391(4) 3 ? O2 Cu1 1.967(4) 5 ? O2 O2 2.578(11) 5 ? O2 O4 2.9834(5) 3_545 ? O3 Cu2 1.960(6) 5_565 ? O3 O3 2.483(11) 5_565 ? O4 Cu1 2.011(4) 3 ? O4 Cu1 2.011(4) 7_665 ? O4 O4 2.692(10) 5_665 ? O4 H1 0.8471 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.9(2) 5 . ? O2 Cu1 O4 97.16(15) 5 7_566 ? O2 Cu1 O4 176.2(2) . 7_566 ? O2 Cu1 O4 176.2(2) 5 3_545 ? O2 Cu1 O4 97.16(15) . 3_545 ? O4 Cu1 O4 84.0(2) 7_566 3_545 ? O2 Cu1 O1 93.7(2) 5 4_455 ? O2 Cu1 O1 91.30(19) . 4_455 ? O4 Cu1 O1 92.40(17) 7_566 4_455 ? O4 Cu1 O1 82.68(18) 3_545 4_455 ? O2 Cu1 O1 91.30(19) 5 3_545 ? O2 Cu1 O1 93.7(2) . 3_545 ? O4 Cu1 O1 82.68(18) 7_566 3_545 ? O4 Cu1 O1 92.40(17) 3_545 3_545 ? O1 Cu1 O1 173.4(2) 4_455 3_545 ? O2 Cu1 Cu1 40.94(12) 5 5 ? O2 Cu1 Cu1 40.94(12) . 5 ? O4 Cu1 Cu1 137.98(11) 7_566 5 ? O4 Cu1 Cu1 137.98(11) 3_545 5 ? O1 Cu1 Cu1 93.30(11) 4_455 5 ? O1 Cu1 Cu1 93.30(11) 3_545 5 ? O2 Cu1 Cu1 139.06(12) 5 5_556 ? O2 Cu1 Cu1 139.06(12) . 5_556 ? O4 Cu1 Cu1 42.02(11) 7_566 5_556 ? O4 Cu1 Cu1 42.02(11) 3_545 5_556 ? O1 Cu1 Cu1 86.70(11) 4_455 5_556 ? O1 Cu1 Cu1 86.70(11) 3_545 5_556 ? Cu1 Cu1 Cu1 180.0 5 5_556 ? O4 Cu2 O3 171.1(2) . 5_565 ? O4 Cu2 O3 93.2(2) . . ? O3 Cu2 O3 77.9(2) 5_565 . ? O4 Cu2 O1 90.78(16) . 3 ? O3 Cu2 O1 94.71(17) 5_565 3 ? O3 Cu2 O1 127.79(13) . 3 ? O4 Cu2 O1 90.78(16) . 8_665 ? O3 Cu2 O1 94.71(17) 5_565 8_665 ? O3 Cu2 O1 127.79(13) . 8_665 ? O1 Cu2 O1 104.1(3) 3 8_665 ? O4 Cu2 Cu2 131.78(15) . 5_565 ? O3 Cu2 Cu2 39.29(16) 5_565 5_565 ? O3 Cu2 Cu2 38.58(16) . 5_565 ? O1 Cu2 Cu2 116.70(14) 3 5_565 ? O1 Cu2 Cu2 116.70(14) 8_665 5_565 ? O1 As1 O1 110.0(3) . 6 ? O1 As1 O3 108.82(19) . . ? O1 As1 O3 108.82(19) 6 . ? O1 As1 O2 111.01(16) . . ? O1 As1 O2 111.01(16) 6 . ? O3 As1 O2 107.1(3) . . ? As1 O1 Cu2 128.7(2) . 3_545 ? As1 O1 Cu1 114.1(2) . 3 ? Cu2 O1 Cu1 116.90(19) 3_545 3 ? As1 O2 Cu1 125.98(15) . . ? As1 O2 Cu1 125.98(15) . 5 ? Cu1 O2 Cu1 98.1(2) . 5 ? As1 O2 O2 153.7(4) . 5 ? Cu1 O2 O2 49.06(12) . 5 ? Cu1 O2 O2 49.06(12) 5 5 ? As1 O2 O4 88.03(14) . 3_545 ? Cu1 O2 O4 41.98(10) . 3_545 ? Cu1 O2 O4 140.0(3) 5 3_545 ? O2 O2 O4 90.98(16) 5 3_545 ? As1 O3 Cu2 129.1(3) . 5_565 ? As1 O3 Cu2 128.8(3) . . ? Cu2 O3 Cu2 102.1(2) 5_565 . ? As1 O3 O3 179.3(4) . 5_565 ? Cu2 O3 O3 51.6(2) 5_565 5_565 ? Cu2 O3 O3 50.53(19) . 5_565 ? Cu2 O4 Cu1 124.32(16) . 3 ? Cu2 O4 Cu1 124.32(16) . 7_665 ? Cu1 O4 Cu1 96.0(2) 3 7_665 ? Cu2 O4 O4 147.4(3) . 5_665 ? Cu1 O4 O4 47.98(11) 3 5_665 ? Cu1 O4 O4 47.98(11) 7_665 5_665 ? Cu2 O4 H1 115.0 . . ? Cu1 O4 H1 95.1 3 . ? Cu1 O4 H1 95.1 7_665 . ? O4 O4 H1 97.6 5_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.85 2.35 2.922(6) 125.4 5_665 _refine_diff_density_max 0.640 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.183 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite jom 300C in P nnm CELL .71073 8.2547 8.6792 5.9605 90.000 90.00 90.000 ZERR 4 .0010 .0010 .0007 .00 .00 .00 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$3 HTAB O4 O1_$5 L.S. 5 LIST 4 FMAP 2 PLAN 25 WGHT 0.035800 FVAR 0.30668 CU1 3 0.000000 0.000000 0.249316 10.50000 0.02980 0.03490 = 0.01805 0.00000 0.00000 -0.00837 CU2 3 0.137507 0.619332 0.000000 10.50000 0.02316 0.03212 = 0.04818 0.00000 0.00000 0.00164 AS1 4 0.236303 0.249498 0.000000 10.50000 0.02274 0.02377 = 0.02217 0.00000 0.00000 -0.00154 O1 2 0.350240 0.264662 0.227583 11.00000 0.05009 0.03957 = 0.02757 0.00981 -0.01454 -0.01557 O2 2 0.130942 0.080895 0.000000 10.50000 0.03774 0.02583 = 0.01930 0.00000 0.00000 -0.00967 O3 2 0.099632 0.392857 0.000000 10.50000 0.02379 0.02141 = 0.09910 0.00000 0.00000 0.00214 O4 2 0.372296 0.596475 0.000000 10.50000 0.02196 0.02867 = 0.02195 0.00000 0.00000 -0.00063 AFIX 3 H1 1 0.424886 0.680285 0.000000 10.50000 -1.20000 AFIX 0 HKLF 4 REM olivenite jom 300C in P nnm REM R1 = 0.0312 for 405 Fo > 4sig(Fo) and 0.0438 for all 490 data REM 45 parameters refined using 0 restraints END WGHT 0.0358 0.0000 REM Highest difference peak 0.640, deepest hole -0.775, 1-sigma level 0.183 Q1 1 0.1290 0.5783 0.1208 11.00000 0.05 0.64 Q2 1 0.2095 0.1515 0.0000 10.50000 0.05 0.60 Q3 1 0.2253 0.3573 0.0000 10.50000 0.05 0.59 Q4 1 0.1006 0.2983 0.0000 10.50000 0.05 0.52 Q5 1 -0.0007 -0.1048 0.2555 11.00000 0.05 0.50 Q6 1 0.4018 0.2201 0.1387 11.00000 0.05 0.47 Q7 1 0.1556 0.5055 0.0000 10.50000 0.05 0.47 Q8 1 0.1559 0.2565 0.1050 11.00000 0.05 0.47 Q9 1 0.2526 0.5716 0.0000 10.50000 0.05 0.46 Q10 1 0.4298 0.3213 0.3561 11.00000 0.05 0.43 Q11 1 0.0425 0.6638 0.0000 10.50000 0.05 0.41 Q12 1 0.3513 0.5036 0.0000 10.50000 0.05 0.40 Q13 1 0.0045 0.1653 0.0000 10.50000 0.05 0.39 Q14 1 0.0657 0.3967 0.0663 11.00000 0.05 0.39 Q15 1 0.2615 0.2479 0.1753 11.00000 0.05 0.38 Q16 1 0.1198 0.7708 0.0000 10.50000 0.05 0.37 Q17 1 0.5000 0.5000 0.0000 10.25000 0.05 0.36 Q18 1 0.0766 -0.0056 0.1094 11.00000 0.05 0.33 Q19 1 0.1039 0.1095 0.1180 11.00000 0.05 0.32 Q20 1 0.3255 0.3290 0.1119 11.00000 0.05 0.31 Q21 1 0.3229 0.2690 0.1083 11.00000 0.05 0.31 Q22 1 0.2202 -0.0284 0.1191 11.00000 0.05 0.31 Q23 1 0.4279 0.7804 0.0000 10.50000 0.05 0.30 Q24 1 0.4894 0.7196 0.1435 11.00000 0.05 0.29 Q25 1 0.2765 0.6315 0.0861 11.00000 0.05 0.28 ; _shelx_res_checksum 8752 _shelx_hkl_file ; 1 0 0 -1.1 1.1 1 2 0 0 134.6 3.3 1 3 0 0 -5.2 3.2 1 4 0 0 15.6 2.9 1 5 0 0 -6.1 3.9 1 6 0 0 69.2 4.5 1 7 0 0 11.2 4.5 1 8 0 0 1272.5 11.7 1 9 0 0 -6.2 3.8 1 10 0 0 26.8 3.4 1 0 1 0 1.2 0.8 1 1 1 0 601.0 4.0 1 -1 1 0 587.5 3.9 1 2 1 0 308.5 4.2 1 -2 1 0 292.3 4.0 1 3 1 0 1330.6 8.5 1 -3 1 0 1330.2 11.0 1 4 1 0 9.4 3.1 1 -4 1 0 10.1 3.8 1 5 1 0 635.0 7.5 1 -5 1 0 569.6 7.3 1 6 1 0 350.4 6.6 1 -6 1 0 341.0 6.4 1 7 1 0 41.1 4.5 1 -7 1 0 37.7 4.3 1 8 1 0 291.0 6.8 1 -8 1 0 274.8 6.2 1 9 1 0 54.2 4.2 1 -9 1 0 52.8 4.1 1 10 1 0 16.9 2.9 1 -10 1 0 18.8 3.3 1 0 2 0 95.7 2.4 1 1 2 0 766.7 5.6 1 -1 2 0 781.7 5.6 1 2 2 0 3629.9 12.8 1 -2 2 0 3566.2 12.7 1 3 2 0 205.4 4.1 1 -3 2 0 205.7 4.2 1 4 2 0 4.6 3.0 1 -4 2 0 3.9 3.1 1 5 2 0 521.0 6.9 1 -5 2 0 540.3 7.4 1 6 2 0 830.9 9.0 1 -6 2 0 858.1 12.6 1 7 2 0 25.4 4.1 1 -7 2 0 19.7 4.8 1 8 2 0 -1.3 3.9 1 -8 2 0 0.6 4.3 1 9 2 0 119.3 5.1 1 -9 2 0 107.9 5.1 1 10 2 0 164.9 5.6 1 -10 2 0 146.5 5.5 1 0 3 0 7.9 2.7 1 1 3 0 1454.9 8.6 1 -1 3 0 1411.4 8.5 1 2 3 0 14.3 2.1 1 -2 3 0 18.5 1.9 1 3 3 0 187.0 4.3 1 -3 3 0 167.8 4.1 1 4 3 0 82.2 3.5 1 -4 3 0 79.8 3.5 1 5 3 0 129.7 4.3 1 -5 3 0 127.8 4.5 1 6 3 0 69.3 4.0 1 -6 3 0 68.7 4.4 1 7 3 0 308.0 6.5 1 -7 3 0 302.1 6.4 1 8 3 0 12.9 4.0 1 -8 3 0 8.4 4.0 1 9 3 0 68.3 4.1 1 -9 3 0 69.4 5.8 1 0 4 0 697.9 6.8 1 1 4 0 103.9 3.1 1 -1 4 0 116.9 3.2 1 2 4 0 16.8 2.4 1 -2 4 0 17.4 2.2 1 3 4 0 15.5 2.8 1 -3 4 0 6.8 3.0 1 4 4 0 3072.4 15.5 1 -4 4 0 2945.6 15.2 1 5 4 0 85.6 4.2 1 -5 4 0 79.0 3.9 1 6 4 0 19.3 3.2 1 -6 4 0 11.3 3.5 1 7 4 0 -1.5 3.9 1 -7 4 0 1.6 3.5 1 8 4 0 77.3 4.2 1 -8 4 0 68.5 3.8 1 9 4 0 1.9 3.9 1 -9 4 0 3.7 3.4 1 0 5 0 4.1 3.2 1 1 5 0 942.0 8.6 1 -1 5 0 961.8 8.7 1 2 5 0 85.3 3.6 1 -2 5 0 81.7 3.5 1 3 5 0 34.1 3.1 1 -3 5 0 34.0 3.3 1 4 5 0 84.9 3.9 1 -4 5 0 92.1 4.1 1 5 5 0 83.2 4.2 1 -5 5 0 82.9 4.3 1 6 5 0 0.4 3.8 1 -6 5 0 2.5 3.3 1 7 5 0 229.0 5.9 1 -7 5 0 224.0 5.8 1 8 5 0 31.3 3.4 1 -8 5 0 31.4 3.4 1 9 5 0 34.6 4.0 1 -9 5 0 33.1 3.5 1 0 6 0 495.4 6.9 1 1 6 0 204.2 4.9 1 -1 6 0 216.4 5.0 1 2 6 0 1350.6 11.0 1 -2 6 0 1314.3 10.8 1 3 6 0 64.4 3.8 1 -3 6 0 69.9 4.3 1 4 6 0 70.2 4.0 1 -4 6 0 63.8 4.0 1 5 6 0 136.3 4.8 1 -5 6 0 134.0 5.0 1 6 6 0 377.1 6.9 1 -6 6 0 353.2 6.7 1 7 6 0 7.0 3.9 1 -7 6 0 0.4 3.2 1 8 6 0 36.5 3.6 1 -8 6 0 35.1 3.6 1 0 7 0 -2.0 4.0 1 1 7 0 22.9 3.0 1 -1 7 0 32.3 3.5 1 2 7 0 23.6 4.0 1 -2 7 0 29.4 3.3 1 3 7 0 436.1 7.2 1 -3 7 0 428.3 7.2 1 4 7 0 0.7 3.8 1 -4 7 0 5.5 3.7 1 5 7 0 137.4 4.7 1 -5 7 0 135.0 4.9 1 6 7 0 177.3 5.4 1 -6 7 0 154.3 5.4 1 7 7 0 4.7 3.7 1 -7 7 0 -4.5 3.3 1 0 8 0 1498.3 12.5 1 1 8 0 5.8 3.8 1 -1 8 0 9.0 3.7 1 2 8 0 29.0 3.1 1 -2 8 0 32.2 3.2 1 3 8 0 9.4 3.7 1 -3 8 0 6.7 3.8 1 4 8 0 105.2 4.3 1 -4 8 0 108.2 4.5 1 5 8 0 6.8 3.6 1 -5 8 0 6.9 3.6 1 6 8 0 3.1 3.6 1 -6 8 0 -2.8 3.4 1 7 8 0 -2.4 3.5 1 -7 8 0 2.1 3.3 1 0 9 0 3.2 3.8 1 1 9 0 12.6 3.8 1 -1 9 0 10.9 3.7 1 2 9 0 42.5 3.8 1 -2 9 0 33.7 3.1 1 3 9 0 150.6 5.0 1 -3 9 0 146.7 5.1 1 4 9 0 17.0 3.3 1 -4 9 0 6.4 3.7 1 5 9 0 81.1 4.0 1 -5 9 0 86.4 4.4 1 0 10 0 4.0 3.5 1 1 10 0 0.5 3.4 1 -1 10 0 2.6 3.7 1 2 10 0 267.9 6.2 1 -2 10 0 260.4 6.3 1 3 10 0 -0.5 3.2 1 -3 10 0 1.1 3.5 1 4 10 0 43.8 3.4 1 -4 10 0 45.7 3.8 1 0 0 1 8.7 2.8 1 1 0 1 1014.9 7.4 1 -1 0 1 867.9 7.4 1 2 0 1 2.3 5.1 1 -2 0 1 2.2 5.3 1 3 0 1 1147.0 10.1 1 -3 0 1 876.6 8.9 1 4 0 1 -1.3 4.4 1 -4 0 1 -2.1 3.8 1 5 0 1 -11.5 5.0 1 -5 0 1 0.9 3.9 1 6 0 1 -3.0 5.6 1 -6 0 1 0.3 4.4 1 7 0 1 9.9 5.6 1 -7 0 1 11.6 4.4 1 8 0 1 2.0 4.9 1 -8 0 1 -0.4 3.6 1 9 0 1 86.0 5.1 1 -9 0 1 86.5 4.9 1 10 0 1 1.8 4.1 1 -10 0 1 2.4 3.7 1 0 1 1 1081.6 7.0 1 0 -1 1 909.9 6.5 1 1 1 1 618.1 5.9 1 -1 1 1 613.3 6.6 1 1 -1 1 691.5 7.1 1 -1 -1 1 545.5 5.5 1 2 1 1 2.8 3.3 1 -2 1 1 -0.6 5.4 1 2 -1 1 1.2 5.9 1 -2 -1 1 6.6 3.7 1 3 1 1 1283.7 9.5 1 -3 1 1 1141.6 10.8 1 3 -1 1 1248.3 11.6 1 -3 -1 1 992.7 8.1 1 4 1 1 420.3 6.5 1 -4 1 1 360.7 8.2 1 4 -1 1 430.2 8.3 1 -4 -1 1 343.8 5.7 1 5 1 1 1097.2 10.2 1 -5 1 1 947.1 11.8 1 5 -1 1 1138.6 12.8 1 -5 -1 1 911.6 9.0 1 6 1 1 14.5 4.8 1 -6 1 1 12.1 5.8 1 6 -1 1 21.1 7.1 1 -6 -1 1 12.7 4.5 1 7 1 1 156.3 6.0 1 -7 1 1 137.7 5.6 1 7 -1 1 174.7 7.7 1 -7 -1 1 136.7 5.2 1 8 1 1 58.0 5.0 1 -8 1 1 40.6 4.1 1 8 -1 1 50.5 5.9 1 -8 -1 1 51.1 4.1 1 9 1 1 -0.9 4.2 1 -9 1 1 2.8 3.9 1 9 -1 1 0.0 5.1 1 -9 -1 1 6.7 3.5 1 10 1 1 8.0 4.1 1 -10 1 1 4.3 3.9 1 10 -1 1 15.0 4.9 1 -10 -1 1 12.0 3.7 1 0 2 1 20.6 3.5 1 0 -2 1 21.9 3.6 1 1 2 1 10.6 3.4 1 -1 2 1 9.1 3.6 1 1 -2 1 -12.2 3.6 1 -1 -2 1 5.8 3.5 1 2 2 1 422.6 5.5 1 -2 2 1 395.4 5.9 1 2 -2 1 394.0 6.3 1 -2 -2 1 368.0 5.2 1 3 2 1 14.6 3.1 1 -3 2 1 15.8 3.5 1 3 -2 1 12.5 3.9 1 -3 -2 1 11.8 3.1 1 4 2 1 105.2 3.8 1 -4 2 1 103.2 5.3 1 4 -2 1 94.6 5.8 1 -4 -2 1 84.0 3.6 1 5 2 1 129.6 4.8 1 -5 2 1 116.9 6.4 1 5 -2 1 142.4 7.6 1 -5 -2 1 110.3 4.5 1 6 2 1 155.6 5.3 1 -6 2 1 135.1 7.5 1 6 -2 1 180.8 9.4 1 -6 -2 1 124.5 4.7 1 7 2 1 109.4 4.8 1 -7 2 1 111.0 7.1 1 7 -2 1 94.7 8.1 1 -7 -2 1 104.4 4.9 1 8 2 1 69.8 4.3 1 -8 2 1 55.7 5.8 1 8 -2 1 66.3 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7 4 0.9 4.7 1 4 -7 4 -11.4 5.1 1 -4 -7 4 4.3 4.1 1 5 7 4 76.3 4.5 1 -5 7 4 66.1 4.9 1 5 -7 4 67.4 5.6 1 -5 -7 4 45.2 4.7 1 0 8 4 633.0 9.9 1 0 -8 4 509.6 9.3 1 1 8 4 -3.3 4.4 1 -1 8 4 5.1 4.1 1 1 -8 4 -2.2 4.6 1 -1 -8 4 -1.1 4.4 1 2 8 4 4.4 4.5 1 -2 8 4 16.0 4.3 1 2 -8 4 15.7 4.1 1 -2 -8 4 6.6 4.4 1 3 8 4 -6.2 4.4 1 -3 8 4 4.9 4.5 1 3 -8 4 0.1 4.7 1 -3 -8 4 -5.1 4.2 1 4 8 4 91.6 4.7 1 -4 8 4 75.9 4.8 1 4 -8 4 74.3 5.3 1 -4 -8 4 64.6 4.6 1 0 9 4 0.8 3.9 1 0 -9 4 4.5 4.3 1 1 9 4 14.8 4.2 1 -1 9 4 12.9 4.2 1 1 -9 4 13.3 4.4 1 -1 -9 4 11.3 4.3 1 0 0 5 6.4 7.4 1 1 0 5 53.2 7.5 1 -1 0 5 50.9 5.5 1 2 0 5 11.5 7.3 1 -2 0 5 7.5 6.7 1 3 0 5 101.3 6.6 1 -3 0 5 81.5 6.8 1 4 0 5 3.2 6.9 1 -4 0 5 -5.9 6.2 1 5 0 5 13.1 6.8 1 -5 0 5 14.7 6.2 1 6 0 5 1.6 6.3 1 -6 0 5 5.7 5.8 1 7 0 5 -1.7 6.8 1 -7 0 5 0.3 6.1 1 0 1 5 50.5 7.3 1 0 -1 5 57.6 5.9 1 1 1 5 182.9 8.5 1 -1 1 5 201.0 8.0 1 1 -1 5 192.9 7.9 1 -1 -1 5 187.3 7.5 1 2 1 5 -5.5 7.2 1 -2 1 5 -2.0 7.1 1 2 -1 5 -0.8 7.2 1 -2 -1 5 5.8 6.6 1 3 1 5 293.7 8.6 1 -3 1 5 290.6 9.0 1 3 -1 5 277.5 9.1 1 -3 -1 5 266.2 8.3 1 4 1 5 37.1 6.2 1 -4 1 5 40.3 5.9 1 4 -1 5 36.9 5.3 1 -4 -1 5 40.4 5.1 1 5 1 5 226.8 7.7 1 -5 1 5 204.8 8.0 1 5 -1 5 242.7 8.6 1 -5 -1 5 199.7 7.7 1 6 1 5 6.9 5.7 1 -6 1 5 6.9 6.1 1 6 -1 5 8.4 6.4 1 -6 -1 5 -1.6 5.6 1 7 1 5 63.7 5.4 1 -7 1 5 54.5 6.2 1 7 -1 5 60.8 7.3 1 -7 -1 5 52.4 5.4 1 0 2 5 3.9 6.9 1 0 -2 5 -0.4 6.7 1 1 2 5 -1.3 6.7 1 -1 2 5 6.0 7.1 1 1 -2 5 -2.1 6.8 1 -1 -2 5 1.0 6.5 1 2 2 5 64.3 6.0 1 -2 2 5 73.5 5.9 1 2 -2 5 60.8 5.9 1 -2 -2 5 58.2 5.6 1 3 2 5 -2.1 6.0 1 -3 2 5 -6.1 6.7 1 3 -2 5 3.8 6.4 1 -3 -2 5 8.8 5.9 1 4 2 5 15.9 5.9 1 -4 2 5 5.6 6.7 1 4 -2 5 8.9 6.7 1 -4 -2 5 9.3 6.0 1 5 2 5 36.8 4.8 1 -5 2 5 30.5 5.1 1 5 -2 5 34.1 5.6 1 -5 -2 5 21.8 5.5 1 6 2 5 23.8 5.1 1 -6 2 5 24.2 7.1 1 6 -2 5 25.1 6.1 1 -6 -2 5 16.5 4.1 1 7 2 5 55.2 5.2 1 -7 2 5 49.4 5.5 1 7 -2 5 53.2 6.1 1 -7 -2 5 41.6 5.3 1 0 3 5 54.8 4.9 1 0 -3 5 44.2 5.6 1 1 3 5 488.9 9.6 1 -1 3 5 496.3 10.2 1 1 -3 5 441.0 9.9 1 -1 -3 5 419.6 9.1 1 2 3 5 -10.3 5.8 1 -2 3 5 -1.7 6.2 1 2 -3 5 1.8 5.9 1 -2 -3 5 -3.7 5.9 1 3 3 5 103.2 6.1 1 -3 3 5 97.1 6.3 1 3 -3 5 108.4 7.0 1 -3 -3 5 79.3 5.6 1 4 3 5 38.7 5.2 1 -4 3 5 37.0 6.4 1 4 -3 5 24.7 5.8 1 -4 -3 5 25.3 5.6 1 5 3 5 24.9 5.1 1 -5 3 5 20.2 6.6 1 5 -3 5 16.6 4.8 1 -5 -3 5 12.8 5.4 1 6 3 5 9.1 5.3 1 -6 3 5 7.2 6.7 1 6 -3 5 13.3 6.4 1 -6 -3 5 5.0 5.1 1 7 3 5 81.5 5.8 1 -7 3 5 75.1 6.9 1 7 -3 5 69.0 6.9 1 -7 -3 5 66.5 5.7 1 0 4 5 -6.9 5.5 1 0 -4 5 -4.1 5.5 1 1 4 5 21.2 3.7 1 -1 4 5 39.4 6.5 1 1 -4 5 35.6 5.4 1 -1 -4 5 20.7 4.8 1 2 4 5 2.9 5.2 1 -2 4 5 -4.5 5.6 1 2 -4 5 1.5 5.8 1 -2 -4 5 -1.3 5.5 1 3 4 5 23.1 5.0 1 -3 4 5 21.5 4.5 1 3 -4 5 18.5 5.7 1 -3 -4 5 12.3 5.7 1 4 4 5 8.3 5.0 1 -4 4 5 3.0 5.7 1 4 -4 5 -1.6 5.9 1 -4 -4 5 0.7 5.5 1 5 4 5 58.2 4.5 1 -5 4 5 58.5 5.2 1 5 -4 5 47.0 5.6 1 -5 -4 5 47.1 5.2 1 6 4 5 0.9 4.8 1 -6 4 5 4.9 6.1 1 6 -4 5 0.6 6.0 1 -6 -4 5 1.5 4.9 1 0 5 5 41.0 5.1 1 0 -5 5 35.5 5.9 1 1 5 5 343.1 8.0 1 -1 5 5 353.8 8.5 1 1 -5 5 293.2 8.1 1 -1 -5 5 289.3 7.8 1 2 5 5 -4.1 5.3 1 -2 5 5 -6.3 5.3 1 2 -5 5 10.0 5.3 1 -2 -5 5 -5.3 5.4 1 3 5 5 70.1 4.6 1 -3 5 5 73.4 4.8 1 3 -5 5 64.6 6.3 1 -3 -5 5 66.6 5.7 1 4 5 5 12.4 4.5 1 -4 5 5 15.4 5.4 1 4 -5 5 17.8 5.7 1 -4 -5 5 22.3 5.4 1 5 5 5 18.0 4.6 1 -5 5 5 15.0 5.6 1 5 -5 5 14.8 5.6 1 -5 -5 5 14.4 4.9 1 6 5 5 -3.7 4.5 1 -6 5 5 1.6 5.6 1 6 -5 5 -2.7 5.9 1 -6 -5 5 -0.7 4.6 1 0 6 5 13.7 4.8 1 0 -6 5 -1.6 5.1 1 1 6 5 -3.8 4.8 1 -1 6 5 0.8 5.0 1 1 -6 5 5.7 5.1 1 -1 -6 5 5.8 4.9 1 2 6 5 12.9 5.0 1 -2 6 5 17.5 3.8 1 2 -6 5 10.8 5.5 1 -2 -6 5 9.7 5.2 1 3 6 5 6.5 4.6 1 -3 6 5 2.4 5.2 1 3 -6 5 10.1 5.3 1 -3 -6 5 1.4 4.7 1 4 6 5 2.3 4.4 1 -4 6 5 2.2 5.1 1 4 -6 5 2.7 5.4 1 -4 -6 5 0.8 4.8 1 5 6 5 15.0 4.6 1 -5 6 5 7.8 5.7 1 5 -6 5 3.0 6.0 1 -5 -6 5 7.0 4.8 1 0 7 5 12.4 3.4 1 0 -7 5 13.0 4.7 1 1 7 5 52.2 4.0 1 -1 7 5 57.1 4.1 1 1 -7 5 44.7 5.2 1 -1 -7 5 44.6 5.0 1 2 7 5 -7.9 4.3 1 -2 7 5 10.7 4.4 1 2 -7 5 0.7 4.7 1 -2 -7 5 9.3 4.2 1 3 7 5 115.9 5.5 1 -3 7 5 123.0 5.8 1 3 -7 5 94.1 5.8 1 -3 -7 5 92.5 5.4 1 0 8 5 -2.1 4.3 1 0 -8 5 0.5 4.4 1 1 8 5 9.8 4.1 1 -1 8 5 0.6 4.4 1 1 -8 5 7.3 4.5 1 -1 -8 5 0.1 4.6 1 0 0 6 97.8 7.2 1 1 0 6 -7.1 6.6 1 -1 0 6 10.9 6.1 1 2 0 6 607.6 11.7 1 -2 0 6 595.1 11.4 1 3 0 6 13.9 6.6 1 -3 0 6 1.2 6.1 1 4 0 6 46.6 5.5 1 -4 0 6 36.8 5.7 1 5 0 6 4.4 5.9 1 -5 0 6 -9.9 6.0 1 6 0 6 213.8 8.4 1 -6 0 6 199.8 8.0 1 0 1 6 -8.0 7.1 1 0 -1 6 4.9 6.2 1 1 1 6 179.8 8.0 1 -1 1 6 166.7 7.4 1 1 -1 6 169.2 7.3 1 -1 -1 6 161.1 7.4 1 2 1 6 8.5 6.3 1 -2 1 6 22.1 6.7 1 2 -1 6 3.1 6.6 1 -2 -1 6 -2.8 5.9 1 3 1 6 80.5 6.5 1 -3 1 6 67.9 6.0 1 3 -1 6 74.8 5.8 1 -3 -1 6 62.6 5.4 1 4 1 6 17.8 6.1 1 -4 1 6 16.3 6.3 1 4 -1 6 4.5 6.5 1 -4 -1 6 14.8 5.9 1 5 1 6 65.2 6.2 1 -5 1 6 76.2 6.9 1 5 -1 6 73.1 6.5 1 -5 -1 6 68.8 6.1 1 6 1 6 32.0 5.1 1 -6 1 6 23.7 5.5 1 6 -1 6 35.2 6.0 1 -6 -1 6 30.8 4.7 1 0 2 6 441.6 10.0 1 0 -2 6 416.4 9.5 1 1 2 6 61.1 6.0 1 -1 2 6 53.8 5.5 1 1 -2 6 62.2 6.0 1 -1 -2 6 50.0 5.2 1 2 2 6 2.5 5.9 1 -2 2 6 7.8 6.3 1 2 -2 6 -2.4 6.1 1 -2 -2 6 5.5 5.6 1 3 2 6 17.2 6.4 1 -3 2 6 16.4 6.7 1 3 -2 6 19.8 6.4 1 -3 -2 6 20.1 5.2 1 4 2 6 517.4 10.5 1 -4 2 6 465.7 10.7 1 4 -2 6 468.3 10.6 1 -4 -2 6 422.2 9.4 1 5 2 6 32.9 5.5 1 -5 2 6 37.5 5.7 1 5 -2 6 30.7 6.6 1 -5 -2 6 32.6 4.8 1 0 3 6 -5.7 5.8 1 0 -3 6 5.3 5.4 1 1 3 6 60.2 5.6 1 -1 3 6 67.2 5.5 1 1 -3 6 46.9 6.3 1 -1 -3 6 57.6 5.5 1 2 3 6 16.0 4.8 1 -2 3 6 20.8 6.3 1 2 -3 6 16.6 5.9 1 -2 -3 6 13.5 5.8 1 3 3 6 181.9 6.8 1 -3 3 6 164.9 7.3 1 3 -3 6 156.0 6.8 1 -3 -3 6 147.5 6.1 1 4 3 6 36.6 4.8 1 -4 3 6 41.5 5.9 1 4 -3 6 40.4 6.4 1 -4 -3 6 34.5 4.8 1 5 3 6 67.0 5.5 1 -5 3 6 55.4 6.0 1 5 -3 6 63.2 5.5 1 -5 -3 6 52.0 5.0 1 0 4 6 50.5 5.0 1 0 -4 6 39.0 5.4 1 1 4 6 0.7 4.9 1 -1 4 6 0.9 5.4 1 1 -4 6 -5.5 5.4 1 -1 -4 6 3.7 5.2 1 2 4 6 368.7 8.5 1 -2 4 6 361.6 9.0 1 2 -4 6 315.3 8.3 1 -2 -4 6 285.3 8.1 1 3 4 6 -4.0 4.9 1 -3 4 6 11.8 5.6 1 3 -4 6 2.4 5.5 1 -3 -4 6 -0.1 5.0 1 4 4 6 68.8 5.0 1 -4 4 6 62.4 5.2 1 4 -4 6 60.2 5.8 1 -4 -4 6 54.8 5.5 1 0 5 6 -4.8 4.8 1 0 -5 6 3.9 4.7 1 1 5 6 75.6 4.9 1 -1 5 6 61.2 4.6 1 1 -5 6 62.7 5.6 1 -1 -5 6 45.1 4.7 1 2 5 6 49.5 4.6 1 -2 5 6 51.2 4.7 1 2 -5 6 40.1 4.5 1 -2 -5 6 43.2 5.4 1 3 5 6 66.4 5.0 1 -3 5 6 62.5 4.9 1 3 -5 6 53.7 5.7 1 -3 -5 6 46.8 4.7 1 4 -5 6 17.6 5.4 1 0 6 6 375.4 8.8 1 0 -6 6 294.4 8.1 1 1 6 6 9.7 4.6 1 -1 6 6 11.8 4.7 1 1 -6 6 5.5 4.9 1 -1 -6 6 4.3 4.7 1 2 6 6 11.2 4.6 1 -2 6 6 5.2 4.8 1 2 -6 6 5.4 4.8 1 -2 -6 6 8.5 4.5 1 0 0 7 -0.3 5.5 1 1 0 7 19.0 5.7 1 -1 0 7 13.3 5.5 1 2 0 7 0.8 5.4 1 -2 0 7 -8.5 5.5 1 3 0 7 52.9 5.0 1 -3 0 7 47.5 5.3 1 0 1 7 -3.6 5.9 1 0 -1 7 6.6 5.7 1 1 1 7 31.1 5.2 1 -1 1 7 40.2 6.0 1 1 -1 7 39.4 5.9 1 -1 -1 7 30.2 4.5 1 2 1 7 -0.7 5.5 1 -2 1 7 0.2 5.4 1 2 -1 7 3.1 5.2 1 -2 -1 7 4.8 5.1 1 3 1 7 142.0 7.0 1 -3 1 7 127.4 6.8 1 3 -1 7 117.8 6.4 1 -3 -1 7 120.3 6.3 1 0 2 7 -0.6 5.5 1 0 -2 7 -1.2 5.1 1 1 2 7 -2.7 5.8 1 -1 2 7 2.9 5.4 1 1 -2 7 1.4 5.4 1 -1 -2 7 3.4 5.2 1 2 2 7 19.1 5.4 1 -2 2 7 20.8 5.8 1 2 -2 7 10.2 5.5 1 -2 -2 7 15.3 4.9 1 3 2 7 11.8 5.7 1 -3 2 7 13.1 5.5 1 3 -2 7 16.1 5.6 1 -3 -2 7 10.7 5.2 1 0 3 7 9.7 5.5 1 0 -3 7 -2.2 4.8 1 1 3 7 111.3 6.2 1 -1 3 7 98.4 6.2 1 1 -3 7 95.4 6.2 1 -1 -3 7 82.3 5.4 1 2 3 7 -2.6 5.2 1 -2 3 7 4.4 5.2 1 2 -3 7 1.2 5.2 1 -2 -3 7 0.3 4.8 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 21257 #==END data_OLI_400C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 58 _space_group_name_H-M_alt 'P n n m' _space_group_name_Hall '-P 2 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.2628(10) _cell_length_b 8.6879(10) _cell_length_c 5.9674(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 428.38(9) _cell_formula_units_Z 4 _cell_measurement_temperature 673(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.389 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.501 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 673(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1657 _diffrn_reflns_av_unetI/netI 0.0394 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.403 _diffrn_reflns_theta_max 26.504 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 491 _reflns_number_gt 407 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.7196P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 491 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.24927(19) 0.0316(3) Uani 1 2 d S T P . . Cu2 Cu 0.13767(14) 0.61922(14) 0.0000 0.0389(4) Uani 1 2 d S T P . . As1 As 0.23611(10) 0.24958(10) 0.0000 0.0251(3) Uani 1 2 d S T P . . O1 O 0.3504(6) 0.2650(5) 0.2284(8) 0.0426(13) Uani 1 1 d . . . . . O2 O 0.1310(8) 0.0807(7) 0.0000 0.0301(14) Uani 1 2 d S T P . . O3 O 0.0981(8) 0.3926(7) 0.0000 0.054(2) Uani 1 2 d S T P . . O4 O 0.3718(8) 0.5962(6) 0.0000 0.0272(12) Uani 1 2 d S T P . . H1 H 0.3984 0.6970 0.0000 0.033 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0339(6) 0.0400(6) 0.0207(6) 0.000 0.000 -0.0104(5) Cu2 0.0257(6) 0.0369(6) 0.0540(8) 0.000 0.000 0.0020(5) As1 0.0243(5) 0.0268(5) 0.0243(5) 0.000 0.000 -0.0020(3) O1 0.053(3) 0.046(3) 0.029(2) 0.012(2) -0.017(2) -0.020(2) O2 0.036(3) 0.031(3) 0.023(3) 0.000 0.000 -0.012(3) O3 0.027(3) 0.028(4) 0.106(7) 0.000 0.000 0.001(3) O4 0.028(3) 0.029(3) 0.025(3) 0.000 0.000 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.969(4) 5 ? Cu1 O2 1.969(4) . ? Cu1 O4 2.015(4) 7_566 ? Cu1 O4 2.015(4) 3_545 ? Cu1 O1 2.391(4) 4_455 ? Cu1 O1 2.391(4) 3_545 ? Cu1 Cu1 2.975(2) 5 ? Cu1 Cu1 2.992(2) 5_556 ? Cu2 O4 1.945(7) . ? Cu2 O3 1.951(7) 5_565 ? Cu2 O3 1.996(6) . ? Cu2 O1 2.059(5) 3 ? Cu2 O1 2.059(5) 8_665 ? Cu2 Cu2 3.077(2) 5_565 ? As1 O1 1.663(5) 6 ? As1 O1 1.663(5) . ? As1 O3 1.686(7) . ? As1 O2 1.705(6) . ? O1 Cu2 2.059(5) 3_545 ? O1 Cu1 2.391(4) 3 ? O2 Cu1 1.969(4) 5 ? O2 O2 2.580(12) 5 ? O2 O4 2.9868(6) 3_545 ? O3 Cu2 1.951(7) 5_565 ? O3 O3 2.472(13) 5_565 ? O4 Cu1 2.015(4) 3 ? O4 Cu1 2.015(4) 7_665 ? O4 O4 2.699(12) 5_665 ? O4 H1 0.9024 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.9(3) 5 . ? O2 Cu1 O4 97.14(17) 5 7_566 ? O2 Cu1 O4 176.3(2) . 7_566 ? O2 Cu1 O4 176.3(2) 5 3_545 ? O2 Cu1 O4 97.14(17) . 3_545 ? O4 Cu1 O4 84.1(3) 7_566 3_545 ? O2 Cu1 O1 93.6(2) 5 4_455 ? O2 Cu1 O1 91.3(2) . 4_455 ? O4 Cu1 O1 92.35(19) 7_566 4_455 ? O4 Cu1 O1 82.9(2) 3_545 4_455 ? O2 Cu1 O1 91.3(2) 5 3_545 ? O2 Cu1 O1 93.6(2) . 3_545 ? O4 Cu1 O1 82.9(2) 7_566 3_545 ? O4 Cu1 O1 92.35(19) 3_545 3_545 ? O1 Cu1 O1 173.6(2) 4_455 3_545 ? O2 Cu1 Cu1 40.93(14) 5 5 ? O2 Cu1 Cu1 40.93(14) . 5 ? O4 Cu1 Cu1 137.95(13) 7_566 5 ? O4 Cu1 Cu1 137.95(13) 3_545 5 ? O1 Cu1 Cu1 93.20(12) 4_455 5 ? O1 Cu1 Cu1 93.20(12) 3_545 5 ? O2 Cu1 Cu1 139.07(14) 5 5_556 ? O2 Cu1 Cu1 139.07(14) . 5_556 ? O4 Cu1 Cu1 42.05(13) 7_566 5_556 ? O4 Cu1 Cu1 42.05(13) 3_545 5_556 ? O1 Cu1 Cu1 86.80(12) 4_455 5_556 ? O1 Cu1 Cu1 86.80(12) 3_545 5_556 ? Cu1 Cu1 Cu1 180.0 5 5_556 ? O4 Cu2 O3 171.1(3) . 5_565 ? O4 Cu2 O3 93.5(3) . . ? O3 Cu2 O3 77.6(3) 5_565 . ? O4 Cu2 O1 90.89(18) . 3 ? O3 Cu2 O1 94.6(2) 5_565 3 ? O3 Cu2 O1 127.91(15) . 3 ? O4 Cu2 O1 90.89(18) . 8_665 ? O3 Cu2 O1 94.6(2) 5_565 8_665 ? O3 Cu2 O1 127.91(15) . 8_665 ? O1 Cu2 O1 103.8(3) 3 8_665 ? O4 Cu2 Cu2 131.78(18) . 5_565 ? O3 Cu2 Cu2 39.31(19) 5_565 5_565 ? O3 Cu2 Cu2 38.25(19) . 5_565 ? O1 Cu2 Cu2 116.71(17) 3 5_565 ? O1 Cu2 Cu2 116.71(17) 8_665 5_565 ? O1 As1 O1 110.0(4) 6 . ? O1 As1 O3 108.9(2) 6 . ? O1 As1 O3 108.9(2) . . ? O1 As1 O2 111.00(19) 6 . ? O1 As1 O2 111.00(19) . . ? O3 As1 O2 106.8(3) . . ? As1 O1 Cu2 128.5(2) . 3_545 ? As1 O1 Cu1 114.1(2) . 3 ? Cu2 O1 Cu1 117.2(2) 3_545 3 ? As1 O2 Cu1 125.91(18) . 5 ? As1 O2 Cu1 125.91(18) . . ? Cu1 O2 Cu1 98.1(3) 5 . ? As1 O2 O2 153.6(5) . 5 ? Cu1 O2 O2 49.07(14) 5 5 ? Cu1 O2 O2 49.07(14) . 5 ? As1 O2 O4 88.00(16) . 3_545 ? Cu1 O2 O4 140.0(3) 5 3_545 ? Cu1 O2 O4 42.02(12) . 3_545 ? O2 O2 O4 91.03(18) 5 3_545 ? As1 O3 Cu2 129.5(4) . 5_565 ? As1 O3 Cu2 128.0(4) . . ? Cu2 O3 Cu2 102.4(3) 5_565 . ? As1 O3 O3 178.4(5) . 5_565 ? Cu2 O3 O3 52.0(2) 5_565 5_565 ? Cu2 O3 O3 50.4(2) . 5_565 ? Cu2 O4 Cu1 124.44(19) . 3 ? Cu2 O4 Cu1 124.44(19) . 7_665 ? Cu1 O4 Cu1 95.9(3) 3 7_665 ? Cu2 O4 O4 147.6(4) . 5_665 ? Cu1 O4 O4 47.95(13) 3 5_665 ? Cu1 O4 O4 47.95(13) 7_665 5_665 ? Cu2 O4 H1 98.2 . . ? Cu1 O4 H1 105.9 3 . ? Cu1 O4 H1 105.9 7_665 . ? O4 O4 H1 114.2 5_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.90 2.51 2.929(7) 109.2 5_665 _refine_diff_density_max 0.720 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.180 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite jon 400C in P nnm CELL .71073 8.2628 8.6879 5.9674 90.000 90.000 90.000 ZERR 4 .0010 .0010 .0008 .00 .000 .00 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$3 HTAB O4 O1_$5 L.S. 5 LIST 4 FMAP 2 PLAN 25 WGHT 0.043300 0.719600 FVAR 0.31224 CU1 3 0.000000 0.000000 0.249275 10.50000 0.03395 0.04004 = 0.02067 0.00000 0.00000 -0.01038 CU2 3 0.137673 0.619219 0.000000 10.50000 0.02574 0.03687 = 0.05402 0.00000 0.00000 0.00199 AS1 4 0.236113 0.249584 0.000000 10.50000 0.02427 0.02679 = 0.02426 0.00000 0.00000 -0.00197 O1 2 0.350381 0.264981 0.228359 11.00000 0.05333 0.04598 = 0.02851 0.01198 -0.01740 -0.01954 O2 2 0.131007 0.080716 0.000000 10.50000 0.03595 0.03101 = 0.02342 0.00000 0.00000 -0.01185 O3 2 0.098083 0.392561 0.000000 10.50000 0.02739 0.02813 = 0.10609 0.00000 0.00000 0.00070 O4 2 0.371806 0.596216 0.000000 10.50000 0.02774 0.02877 = 0.02497 0.00000 0.00000 0.00177 AFIX 3 H1 1 0.398366 0.696966 0.000000 10.50000 -1.20000 AFIX 0 HKLF 4 REM olivenite jon 400C in P nnm REM R1 = 0.0348 for 407 Fo > 4sig(Fo) and 0.0466 for all 491 data REM 45 parameters refined using 0 restraints END WGHT 0.0431 0.7378 REM Highest difference peak 0.720, deepest hole -0.734, 1-sigma level 0.180 Q1 1 0.0946 0.2835 0.0000 10.50000 0.05 0.72 Q2 1 0.2110 0.3581 0.0000 10.50000 0.05 0.72 Q3 1 0.1266 0.5774 0.1206 11.00000 0.05 0.72 Q4 1 0.1840 0.1537 0.0000 10.50000 0.05 0.70 Q5 1 0.0000 0.0000 0.4334 10.50000 0.05 0.59 Q6 1 0.0000 0.0000 0.0646 10.50000 0.05 0.58 Q7 1 0.1674 0.5019 0.0000 10.50000 0.05 0.49 Q8 1 0.1539 0.2554 0.1078 11.00000 0.05 0.48 Q9 1 0.2624 0.2529 0.1815 11.00000 0.05 0.47 Q10 1 0.0065 -0.1072 0.2397 11.00000 0.05 0.47 Q11 1 0.0201 0.6565 0.0839 11.00000 0.05 0.46 Q12 1 0.2286 0.0490 0.1171 11.00000 0.05 0.42 Q13 1 0.2607 0.6177 0.0910 11.00000 0.05 0.41 Q14 1 0.4653 0.2575 0.1083 11.00000 0.05 0.40 Q15 1 0.4308 0.8035 0.0000 10.50000 0.05 0.40 Q16 1 0.3776 0.2502 0.4250 11.00000 0.05 0.38 Q17 1 0.2397 -0.0542 0.1403 11.00000 0.05 0.38 Q18 1 0.3782 0.5030 0.0000 10.50000 0.05 0.38 Q19 1 0.2037 0.2439 0.3251 11.00000 0.05 0.38 Q20 1 0.1639 0.0243 0.0000 10.50000 0.05 0.36 Q21 1 0.1203 0.4249 0.1078 11.00000 0.05 0.36 Q22 1 0.1336 0.6867 0.0000 10.50000 0.05 0.36 Q23 1 0.4162 0.2432 0.1417 11.00000 0.05 0.35 Q24 1 0.3712 0.1318 0.1737 11.00000 0.05 0.34 Q25 1 0.3525 0.2685 0.0000 10.50000 0.05 0.34 ; _shelx_res_checksum 31565 _shelx_hkl_file ; 1 0 0 -1.3 1.1 1 2 0 0 156.0 3.6 1 3 0 0 -7.3 3.2 1 4 0 0 22.0 3.6 1 5 0 0 2.7 3.8 1 6 0 0 64.1 4.0 1 7 0 0 10.1 4.4 1 8 0 0 1191.8 11.5 1 9 0 0 -9.3 3.9 1 10 0 0 27.9 3.7 1 0 1 0 1.0 0.8 1 1 1 0 608.8 4.0 1 -1 1 0 621.1 4.0 1 2 1 0 286.2 4.3 1 -2 1 0 290.1 4.1 1 3 1 0 1332.3 8.5 1 -3 1 0 1401.9 11.8 1 4 1 0 9.9 3.1 1 -4 1 0 7.4 4.0 1 5 1 0 613.9 7.3 1 -5 1 0 586.5 7.4 1 6 1 0 348.9 6.7 1 -6 1 0 338.5 6.5 1 7 1 0 48.7 4.0 1 -7 1 0 40.6 4.3 1 8 1 0 301.1 6.8 1 -8 1 0 284.9 6.4 1 9 1 0 49.6 3.9 1 -9 1 0 42.4 3.6 1 10 1 0 13.8 3.9 1 -10 1 0 17.3 3.6 1 0 2 0 97.4 2.3 1 1 2 0 796.0 5.7 1 -1 2 0 807.2 5.8 1 2 2 0 3751.4 13.1 1 -2 2 0 3795.3 13.2 1 3 2 0 201.9 4.1 1 -3 2 0 213.8 4.4 1 4 2 0 4.2 3.1 1 -4 2 0 -1.3 3.1 1 5 2 0 522.2 7.0 1 -5 2 0 557.3 7.6 1 6 2 0 810.3 9.3 1 -6 2 0 868.9 13.4 1 7 2 0 24.7 4.0 1 -7 2 0 17.2 5.7 1 8 2 0 3.0 4.0 1 -8 2 0 0.7 4.5 1 9 2 0 118.7 5.1 1 -9 2 0 109.3 5.2 1 10 2 0 137.8 5.4 1 -10 2 0 123.5 5.3 1 0 3 0 14.3 1.9 1 1 3 0 1468.1 8.7 1 -1 3 0 1467.7 8.7 1 2 3 0 7.1 2.8 1 -2 3 0 13.4 2.3 1 3 3 0 164.5 4.0 1 -3 3 0 178.1 4.2 1 4 3 0 85.1 3.6 1 -4 3 0 86.6 3.6 1 5 3 0 130.1 4.6 1 -5 3 0 115.7 4.4 1 6 3 0 76.4 4.4 1 -6 3 0 75.7 4.5 1 7 3 0 282.4 6.5 1 -7 3 0 297.0 6.6 1 8 3 0 12.4 4.0 1 -8 3 0 10.3 4.1 1 9 3 0 59.5 4.3 1 -9 3 0 55.9 6.2 1 0 4 0 711.9 6.9 1 1 4 0 106.8 3.2 1 -1 4 0 111.3 3.5 1 2 4 0 18.1 2.3 1 -2 4 0 17.2 2.0 1 3 4 0 8.4 3.5 1 -3 4 0 8.8 2.9 1 4 4 0 3121.7 15.9 1 -4 4 0 2958.9 15.3 1 5 4 0 80.2 4.1 1 -5 4 0 82.0 4.3 1 6 4 0 21.7 4.0 1 -6 4 0 3.4 3.8 1 7 4 0 3.6 4.0 1 -7 4 0 1.1 3.3 1 8 4 0 70.0 4.2 1 -8 4 0 67.3 4.1 1 9 4 0 0.5 4.0 1 -9 4 0 7.4 3.5 1 0 5 0 0.5 3.5 1 1 5 0 958.4 8.8 1 -1 5 0 939.4 8.7 1 2 5 0 79.4 3.5 1 -2 5 0 82.4 3.7 1 3 5 0 29.9 3.0 1 -3 5 0 36.8 3.0 1 4 5 0 104.2 4.3 1 -4 5 0 97.5 4.1 1 5 5 0 78.6 4.2 1 -5 5 0 73.8 3.7 1 6 5 0 2.7 3.9 1 -6 5 0 -6.2 3.4 1 7 5 0 221.2 5.9 1 -7 5 0 197.2 5.7 1 8 5 0 41.4 4.4 1 -8 5 0 30.2 3.2 1 9 5 0 20.6 3.8 1 -9 5 0 40.4 3.9 1 0 6 0 496.2 7.1 1 1 6 0 211.0 5.2 1 -1 6 0 207.5 5.2 1 2 6 0 1325.1 11.2 1 -2 6 0 1281.8 11.0 1 3 6 0 64.0 3.7 1 -3 6 0 57.9 3.7 1 4 6 0 62.7 3.9 1 -4 6 0 54.4 3.7 1 5 6 0 117.2 4.5 1 -5 6 0 111.3 4.6 1 6 6 0 362.9 7.1 1 -6 6 0 328.8 6.5 1 7 6 0 4.7 4.0 1 -7 6 0 -1.0 3.3 1 8 6 0 36.7 3.9 1 -8 6 0 32.6 3.8 1 0 7 0 9.1 4.2 1 1 7 0 27.6 3.7 1 -1 7 0 21.9 3.9 1 2 7 0 17.6 3.9 1 -2 7 0 21.6 3.4 1 3 7 0 408.0 7.3 1 -3 7 0 386.0 7.2 1 4 7 0 0.7 3.9 1 -4 7 0 3.3 3.7 1 5 7 0 127.8 4.9 1 -5 7 0 112.2 4.6 1 6 7 0 160.4 5.3 1 -6 7 0 163.2 5.1 1 7 7 0 -1.9 3.7 1 -7 7 0 -3.9 3.3 1 0 8 0 1430.6 12.3 1 1 8 0 9.8 4.0 1 -1 8 0 7.9 3.9 1 2 8 0 34.6 3.2 1 -2 8 0 30.3 3.0 1 3 8 0 7.5 4.0 1 -3 8 0 11.0 3.8 1 4 8 0 95.3 4.2 1 -4 8 0 109.8 4.7 1 5 8 0 -2.1 3.9 1 -5 8 0 -4.2 3.7 1 6 8 0 -4.0 3.5 1 -6 8 0 3.0 3.3 1 7 8 0 2.8 3.5 1 -7 8 0 -0.4 3.5 1 0 9 0 0.0 3.8 1 1 9 0 13.0 3.8 1 -1 9 0 12.8 3.9 1 2 9 0 32.8 3.1 1 -2 9 0 35.8 3.9 1 3 9 0 126.2 4.5 1 -3 9 0 120.1 4.7 1 4 9 0 20.1 3.2 1 -4 9 0 13.9 4.0 1 5 9 0 72.3 4.1 1 -5 9 0 67.4 4.0 1 0 10 0 5.0 3.4 1 1 10 0 6.1 3.3 1 -1 10 0 5.8 3.6 1 2 10 0 223.8 6.0 1 -2 10 0 215.1 5.8 1 3 10 0 -2.1 3.3 1 -3 10 0 2.5 3.6 1 4 10 0 46.0 3.5 1 -4 10 0 41.4 3.6 1 0 0 1 -3.4 2.8 1 1 0 1 1008.6 7.5 1 -1 0 1 876.0 7.6 1 2 0 1 4.2 5.0 1 -2 0 1 11.1 5.5 1 3 0 1 1142.2 10.1 1 -3 0 1 922.0 9.3 1 4 0 1 -4.5 4.5 1 -4 0 1 5.7 3.9 1 5 0 1 6.0 5.0 1 -5 0 1 0.9 4.1 1 6 0 1 -0.3 5.5 1 -6 0 1 -5.0 4.5 1 7 0 1 15.8 5.5 1 -7 0 1 4.8 4.6 1 8 0 1 0.0 4.9 1 -8 0 1 -2.4 3.8 1 9 0 1 88.8 5.0 1 -9 0 1 82.3 4.4 1 10 0 1 2.8 4.3 1 -10 0 1 -2.7 3.7 1 0 1 1 1001.9 6.9 1 0 -1 1 1057.5 7.2 1 1 1 1 592.3 5.9 1 -1 1 1 610.6 6.6 1 1 -1 1 703.4 7.4 1 -1 -1 1 550.8 5.7 1 2 1 1 10.4 3.9 1 -2 1 1 -4.9 4.5 1 2 -1 1 4.4 6.1 1 -2 -1 1 9.6 3.7 1 3 1 1 1273.3 9.6 1 -3 1 1 1179.2 11.3 1 3 -1 1 1278.2 11.9 1 -3 -1 1 1021.5 8.4 1 4 1 1 409.2 6.4 1 -4 1 1 349.2 8.4 1 4 -1 1 436.4 8.6 1 -4 -1 1 334.5 5.7 1 5 1 1 1094.2 10.3 1 -5 1 1 933.6 12.2 1 5 -1 1 1092.7 12.7 1 -5 -1 1 906.1 9.1 1 6 1 1 13.7 5.0 1 -6 1 1 10.5 6.0 1 6 -1 1 12.4 7.2 1 -6 -1 1 10.8 4.5 1 7 1 1 156.7 6.1 1 -7 1 1 133.3 5.9 1 7 -1 1 146.3 8.1 1 -7 -1 1 130.1 4.9 1 8 1 1 42.7 4.3 1 -8 1 1 42.7 4.2 1 8 -1 1 45.9 5.3 1 -8 -1 1 39.0 4.0 1 9 1 1 -2.9 4.4 1 -9 1 1 -8.6 4.2 1 9 -1 1 2.5 5.1 1 -9 -1 1 5.9 3.6 1 10 1 1 5.9 3.9 1 -10 1 1 4.6 4.0 1 10 -1 1 7.3 4.8 1 -10 -1 1 5.9 3.8 1 0 2 1 33.8 3.4 1 0 -2 1 27.0 3.7 1 1 2 1 -4.8 3.0 1 -1 2 1 5.7 3.6 1 1 -2 1 3.6 3.9 1 -1 -2 1 10.8 3.5 1 2 2 1 402.2 5.4 1 -2 2 1 402.6 5.9 1 2 -2 1 415.6 6.2 1 -2 -2 1 366.3 5.2 1 3 2 1 11.6 3.0 1 -3 2 1 12.5 4.2 1 3 -2 1 15.5 4.8 1 -3 -2 1 9.4 3.1 1 4 2 1 94.3 3.8 1 -4 2 1 88.7 4.9 1 4 -2 1 95.6 6.1 1 -4 -2 1 83.2 3.7 1 5 2 1 128.1 4.7 1 -5 2 1 120.0 6.8 1 5 -2 1 128.8 7.8 1 -5 -2 1 115.0 4.3 1 6 2 1 150.2 5.2 1 -6 2 1 144.4 7.5 1 6 -2 1 154.7 9.4 1 -6 -2 1 128.1 5.2 1 7 2 1 103.5 5.0 1 -7 2 1 106.3 7.1 1 7 -2 1 100.2 8.1 1 -7 -2 1 86.9 5.3 1 8 2 1 67.2 4.8 1 -8 2 1 53.0 5.6 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10.1 1 -1 3 5 471.9 10.0 1 1 -3 5 430.0 10.2 1 -1 -3 5 399.9 9.1 1 2 3 5 5.7 5.9 1 -2 3 5 -3.3 6.4 1 2 -3 5 -2.1 6.1 1 -2 -3 5 -5.8 5.8 1 3 3 5 110.0 6.4 1 -3 3 5 98.1 6.0 1 3 -3 5 108.8 7.1 1 -3 -3 5 76.0 5.8 1 4 3 5 18.9 6.1 1 -4 3 5 23.2 4.7 1 4 -3 5 23.7 6.0 1 -4 -3 5 27.5 5.4 1 5 3 5 19.7 5.9 1 -5 3 5 18.6 6.7 1 5 -3 5 27.1 6.0 1 -5 -3 5 18.8 5.9 1 6 3 5 10.6 5.2 1 -6 3 5 6.4 6.6 1 6 -3 5 11.4 6.6 1 -6 -3 5 3.9 5.5 1 7 3 5 74.6 5.7 1 -7 3 5 55.7 6.9 1 7 -3 5 72.8 7.3 1 -7 -3 5 64.0 5.7 1 0 4 5 8.1 5.5 1 0 -4 5 -5.4 5.8 1 1 4 5 22.7 4.5 1 -1 4 5 24.2 4.7 1 1 -4 5 17.8 5.5 1 -1 -4 5 15.9 6.0 1 2 4 5 10.1 5.4 1 -2 4 5 3.9 5.8 1 2 -4 5 4.5 5.9 1 -2 -4 5 2.9 5.6 1 3 4 5 17.3 4.0 1 -3 4 5 17.4 5.9 1 3 -4 5 9.1 6.3 1 -3 -4 5 21.2 5.7 1 4 4 5 5.1 5.3 1 -4 4 5 8.8 5.9 1 4 -4 5 -8.5 6.1 1 -4 -4 5 4.2 5.3 1 5 4 5 58.8 5.6 1 -5 4 5 53.8 5.9 1 5 -4 5 55.0 6.7 1 -5 -4 5 46.8 4.7 1 6 4 5 4.9 5.1 1 -6 4 5 1.9 6.1 1 6 -4 5 -3.1 6.0 1 -6 -4 5 -3.2 5.1 1 0 5 5 33.1 4.1 1 0 -5 5 32.5 5.5 1 1 5 5 320.5 8.0 1 -1 5 5 331.5 8.5 1 1 -5 5 283.9 8.5 1 -1 -5 5 270.1 8.2 1 2 5 5 3.9 5.2 1 -2 5 5 5.2 5.3 1 2 -5 5 1.7 5.7 1 -2 -5 5 10.5 5.3 1 3 5 5 62.2 4.9 1 -3 5 5 55.9 4.9 1 3 -5 5 50.9 6.1 1 -3 -5 5 57.4 5.7 1 4 5 5 13.6 4.3 1 -4 5 5 16.1 5.5 1 4 -5 5 12.4 5.5 1 -4 -5 5 10.1 5.1 1 5 5 5 23.9 4.6 1 -5 5 5 24.5 5.6 1 5 -5 5 16.6 5.7 1 -5 -5 5 13.2 4.5 1 6 5 5 -1.2 4.3 1 -6 5 5 3.8 5.5 1 6 -5 5 2.4 5.8 1 -6 -5 5 0.7 4.8 1 0 6 5 -2.4 5.1 1 0 -6 5 3.2 5.0 1 1 6 5 -0.8 4.8 1 -1 6 5 5.6 4.9 1 1 -6 5 9.8 5.3 1 -1 -6 5 -0.3 5.0 1 2 6 5 10.4 4.2 1 -2 6 5 17.6 5.2 1 2 -6 5 13.8 5.5 1 -2 -6 5 17.2 4.9 1 3 6 5 3.1 4.7 1 -3 6 5 -6.0 5.3 1 3 -6 5 -5.3 5.6 1 -3 -6 5 2.9 4.8 1 4 6 5 -0.8 4.5 1 -4 6 5 5.8 5.2 1 4 -6 5 -0.4 5.6 1 -4 -6 5 5.0 4.3 1 5 6 5 8.6 4.6 1 -5 6 5 13.5 5.5 1 5 -6 5 17.0 5.7 1 -5 -6 5 9.3 4.6 1 0 7 5 5.1 4.5 1 0 -7 5 4.9 4.8 1 1 7 5 60.5 4.4 1 -1 7 5 54.0 4.4 1 1 -7 5 36.1 5.5 1 -1 -7 5 53.6 5.3 1 2 7 5 -4.5 4.2 1 -2 7 5 1.2 4.6 1 2 -7 5 0.0 4.8 1 -2 -7 5 -4.5 4.4 1 3 7 5 106.0 5.2 1 -3 7 5 94.5 5.4 1 3 -7 5 88.6 6.1 1 -3 -7 5 72.6 5.0 1 0 8 5 6.6 4.2 1 0 -8 5 4.4 4.7 1 1 8 5 1.3 4.6 1 -1 8 5 4.6 4.5 1 1 -8 5 4.1 4.7 1 -1 -8 5 8.9 4.7 1 0 0 6 88.3 7.3 1 1 0 6 8.4 6.4 1 -1 0 6 -14.5 6.6 1 2 0 6 557.9 11.7 1 -2 0 6 528.8 11.1 1 3 0 6 18.1 6.6 1 -3 0 6 -0.3 6.0 1 4 0 6 59.7 6.6 1 -4 0 6 37.3 6.1 1 5 0 6 -0.5 6.3 1 -5 0 6 0.5 5.9 1 6 0 6 208.0 9.1 1 -6 0 6 166.8 7.8 1 0 1 6 5.2 6.8 1 0 -1 6 -3.5 6.4 1 1 1 6 151.2 7.3 1 -1 1 6 148.4 7.4 1 1 -1 6 156.4 7.4 1 -1 -1 6 154.1 7.4 1 2 1 6 7.0 6.7 1 -2 1 6 1.9 6.7 1 2 -1 6 10.6 6.4 1 -2 -1 6 16.4 6.1 1 3 1 6 68.9 5.8 1 -3 1 6 60.8 6.6 1 3 -1 6 67.3 7.2 1 -3 -1 6 66.7 6.0 1 4 1 6 15.1 6.4 1 -4 1 6 4.9 6.4 1 4 -1 6 20.5 6.1 1 -4 -1 6 5.9 6.2 1 5 1 6 67.3 5.7 1 -5 1 6 65.1 6.7 1 5 -1 6 61.1 5.8 1 -5 -1 6 55.6 5.5 1 6 1 6 33.6 4.7 1 -6 1 6 29.2 6.4 1 6 -1 6 39.1 6.6 1 -6 -1 6 20.2 6.3 1 0 2 6 436.2 10.3 1 0 -2 6 416.3 10.1 1 1 2 6 43.7 5.2 1 -1 2 6 44.3 5.2 1 1 -2 6 42.3 6.7 1 -1 -2 6 42.0 6.4 1 2 2 6 9.3 6.2 1 -2 2 6 -6.3 6.6 1 2 -2 6 0.8 6.4 1 -2 -2 6 -6.5 5.9 1 3 2 6 16.2 6.1 1 -3 2 6 12.5 7.1 1 3 -2 6 19.6 5.9 1 -3 -2 6 11.9 6.0 1 4 2 6 457.5 10.0 1 -4 2 6 417.4 10.5 1 4 -2 6 421.4 10.5 1 -4 -2 6 377.5 9.2 1 5 2 6 29.8 4.4 1 -5 2 6 34.4 5.3 1 5 -2 6 23.9 7.2 1 -5 -2 6 32.2 5.2 1 0 3 6 -7.7 6.2 1 0 -3 6 1.4 5.6 1 1 3 6 69.7 5.8 1 -1 3 6 53.9 5.2 1 1 -3 6 47.8 5.9 1 -1 -3 6 51.5 6.0 1 2 3 6 15.5 5.8 1 -2 3 6 13.8 6.4 1 2 -3 6 10.9 6.0 1 -2 -3 6 13.5 5.7 1 3 3 6 162.0 6.9 1 -3 3 6 145.8 7.2 1 3 -3 6 150.1 7.5 1 -3 -3 6 132.4 6.5 1 4 3 6 29.7 4.4 1 -4 3 6 37.2 6.9 1 4 -3 6 36.0 5.3 1 -4 -3 6 38.2 5.4 1 5 3 6 65.2 5.9 1 -5 3 6 60.7 7.4 1 5 -3 6 53.7 5.5 1 -5 -3 6 50.0 4.9 1 0 4 6 39.4 5.0 1 0 -4 6 30.2 5.8 1 1 4 6 4.1 5.2 1 -1 4 6 -1.2 5.5 1 1 -4 6 -2.4 5.5 1 -1 -4 6 3.8 5.0 1 2 4 6 336.6 8.3 1 -2 4 6 321.9 8.7 1 2 -4 6 267.4 8.2 1 -2 -4 6 277.5 8.2 1 3 4 6 5.3 5.0 1 -3 4 6 -2.6 5.9 1 3 -4 6 12.2 5.4 1 -3 -4 6 5.9 5.2 1 4 4 6 67.8 5.6 1 -4 4 6 51.0 5.6 1 4 -4 6 50.2 5.0 1 -4 -4 6 45.7 4.7 1 0 5 6 -3.4 5.1 1 0 -5 6 -5.1 5.2 1 1 5 6 70.7 5.3 1 -1 5 6 58.9 4.7 1 1 -5 6 50.5 5.4 1 -1 -5 6 53.1 4.8 1 2 5 6 50.7 4.2 1 -2 5 6 41.8 4.8 1 2 -5 6 34.7 4.8 1 -2 -5 6 41.7 4.8 1 3 5 6 56.3 4.6 1 -3 5 6 54.1 4.8 1 3 -5 6 45.4 5.7 1 -3 -5 6 45.2 5.1 1 4 5 6 21.8 4.1 1 -4 5 6 14.3 5.1 1 4 -5 6 7.0 5.5 1 -4 -5 6 15.3 5.1 1 0 6 6 330.9 8.3 1 0 -6 6 257.0 7.7 1 1 6 6 4.2 4.6 1 -1 6 6 -2.6 4.7 1 1 -6 6 -0.1 5.0 1 -1 -6 6 -3.6 4.7 1 2 6 6 11.8 4.4 1 -2 6 6 8.1 4.8 1 2 -6 6 9.8 4.9 1 -2 -6 6 -4.3 4.9 1 0 0 7 -8.8 5.8 1 1 0 7 15.3 6.0 1 -1 0 7 16.3 5.9 1 2 0 7 1.9 5.4 1 -2 0 7 6.8 5.3 1 3 0 7 44.4 5.3 1 -3 0 7 43.5 5.3 1 0 1 7 4.2 5.7 1 0 -1 7 2.1 5.7 1 1 1 7 46.8 5.4 1 -1 1 7 37.1 5.2 1 1 -1 7 43.9 5.7 1 -1 -1 7 35.6 5.3 1 2 1 7 -6.9 5.9 1 -2 1 7 -4.2 5.6 1 2 -1 7 0.7 5.7 1 -2 -1 7 0.8 5.1 1 3 1 7 115.0 6.4 1 -3 1 7 100.6 6.3 1 3 -1 7 96.2 5.9 1 -3 -1 7 112.7 6.3 1 0 2 7 -0.7 5.5 1 0 -2 7 2.4 5.2 1 1 2 7 10.0 5.4 1 -1 2 7 4.4 5.9 1 1 -2 7 -1.0 5.3 1 -1 -2 7 -0.9 5.1 1 2 2 7 8.3 5.5 1 -2 2 7 8.0 5.6 1 2 -2 7 7.3 5.7 1 -2 -2 7 12.0 5.3 1 3 2 7 9.1 5.7 1 -3 2 7 5.2 5.9 1 3 -2 7 -0.5 6.0 1 -3 -2 7 9.1 5.2 1 0 3 7 6.6 5.5 1 0 -3 7 5.2 5.2 1 1 3 7 89.1 5.9 1 -1 3 7 89.2 6.2 1 1 -3 7 80.9 6.0 1 -1 -3 7 81.7 5.7 1 2 3 7 3.6 5.0 1 -2 3 7 2.2 5.8 1 2 -3 7 -4.2 5.2 1 -2 -3 7 -2.7 5.1 1 0 0 0 0.0 0.0 1 0 0 0 0.0 0.0 1 ; _shelx_hkl_checksum 27713 #==END data_OLI_500C _publ_contact_author ; Zema Michele ; _publ_contact_author_email ; michele.zema@unipv.it ; loop_ _publ_author_name _publ_author_address 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' _publ_section_title ; ?? ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_mineral ; OLIVENITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As Cu2 H O5' _chemical_formula_sum 'As Cu2 H O5' _chemical_formula_weight 283.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 58 _space_group_name_H-M_alt 'P n n m' _space_group_name_Hall '-P 2 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.2696(8) _cell_length_b 8.6978(8) _cell_length_c 5.9731(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 429.63(8) _cell_formula_units_Z 4 _cell_measurement_temperature 773(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.376 _exptl_crystal_F_000 528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 17.450 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.095 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 773(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1658 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.399 _diffrn_reflns_theta_max 26.510 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 492 _reflns_number_gt 390 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+2.1995P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 492 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.2505(3) 0.0365(4) Uani 1 2 d S T P . . Cu2 Cu 0.13776(19) 0.61915(19) 0.0000 0.0444(5) Uani 1 2 d S T P . . As1 As 0.23560(14) 0.24942(14) 0.0000 0.0292(4) Uani 1 2 d S T P . . O1 O 0.3502(9) 0.2648(7) 0.2271(12) 0.0499(19) Uani 1 1 d . . . . . O2 O 0.1303(11) 0.0815(9) 0.0000 0.0334(19) Uani 1 2 d S T P . . O3 O 0.0987(11) 0.3911(10) 0.0000 0.057(3) Uani 1 2 d S T P . . O4 O 0.3711(10) 0.5959(9) 0.0000 0.0333(18) Uani 1 2 d S T P . . H1 H 0.4214 0.6779 0.0000 0.040 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0385(8) 0.0472(9) 0.0240(7) 0.000 0.000 -0.0111(7) Cu2 0.0298(8) 0.0435(9) 0.0598(11) 0.000 0.000 0.0018(7) As1 0.0269(6) 0.0315(6) 0.0293(6) 0.000 0.000 -0.0021(5) O1 0.057(4) 0.053(4) 0.040(4) 0.014(3) -0.023(4) -0.020(3) O2 0.039(5) 0.034(4) 0.028(4) 0.000 0.000 -0.013(4) O3 0.025(4) 0.030(5) 0.116(10) 0.000 0.000 0.002(4) O4 0.027(4) 0.040(5) 0.033(4) 0.000 0.000 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.975(6) 5 ? Cu1 O2 1.975(6) . ? Cu1 O4 2.013(6) 7_566 ? Cu1 O4 2.013(6) 3_545 ? Cu1 O1 2.396(6) 4_455 ? Cu1 O1 2.396(6) 3_545 ? Cu1 Cu1 2.981(3) 5_556 ? Cu1 Cu1 2.992(3) 5 ? Cu2 O4 1.940(9) . ? Cu2 O3 1.958(9) 5_565 ? Cu2 O3 2.010(9) . ? Cu2 O1 2.067(7) 3 ? Cu2 O1 2.067(7) 8_665 ? Cu2 Cu2 3.080(3) 5_565 ? As1 O1 1.660(7) 6 ? As1 O1 1.660(7) . ? As1 O3 1.673(9) . ? As1 O2 1.701(8) . ? O1 Cu2 2.067(7) 3_545 ? O1 Cu1 2.396(6) 3 ? O2 Cu1 1.975(6) 5 ? O2 O2 2.579(17) 5 ? O2 O4 2.9892(6) 3_545 ? O3 Cu2 1.958(9) 5_565 ? O3 O3 2.501(17) 5_565 ? O4 Cu1 2.013(6) 3 ? O4 Cu1 2.013(6) 7_665 ? O4 O4 2.707(16) 5_665 ? O4 H1 0.8254 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 81.5(4) 5 . ? O2 Cu1 O4 97.1(2) 5 7_566 ? O2 Cu1 O4 176.6(3) . 7_566 ? O2 Cu1 O4 176.6(3) 5 3_545 ? O2 Cu1 O4 97.1(2) . 3_545 ? O4 Cu1 O4 84.5(3) 7_566 3_545 ? O2 Cu1 O1 93.8(3) 5 4_455 ? O2 Cu1 O1 91.0(3) . 4_455 ? O4 Cu1 O1 92.2(3) 7_566 4_455 ? O4 Cu1 O1 83.0(3) 3_545 4_455 ? O2 Cu1 O1 91.0(3) 5 3_545 ? O2 Cu1 O1 93.8(3) . 3_545 ? O4 Cu1 O1 83.0(3) 7_566 3_545 ? O4 Cu1 O1 92.2(3) 3_545 3_545 ? O1 Cu1 O1 173.6(4) 4_455 3_545 ? O2 Cu1 Cu1 139.24(18) 5 5_556 ? O2 Cu1 Cu1 139.24(18) . 5_556 ? O4 Cu1 Cu1 42.24(17) 7_566 5_556 ? O4 Cu1 Cu1 42.24(17) 3_545 5_556 ? O1 Cu1 Cu1 86.79(18) 4_455 5_556 ? O1 Cu1 Cu1 86.79(18) 3_545 5_556 ? O2 Cu1 Cu1 40.76(18) 5 5 ? O2 Cu1 Cu1 40.76(18) . 5 ? O4 Cu1 Cu1 137.76(17) 7_566 5 ? O4 Cu1 Cu1 137.76(17) 3_545 5 ? O1 Cu1 Cu1 93.21(18) 4_455 5 ? O1 Cu1 Cu1 93.21(18) 3_545 5 ? Cu1 Cu1 Cu1 180.0 5_556 5 ? O4 Cu2 O3 171.4(4) . 5_565 ? O4 Cu2 O3 93.3(4) . . ? O3 Cu2 O3 78.1(4) 5_565 . ? O4 Cu2 O1 90.9(3) . 3 ? O3 Cu2 O1 94.4(3) 5_565 3 ? O3 Cu2 O1 127.8(2) . 3 ? O4 Cu2 O1 90.9(3) . 8_665 ? O3 Cu2 O1 94.4(3) 5_565 8_665 ? O3 Cu2 O1 127.8(2) . 8_665 ? O1 Cu2 O1 104.1(4) 3 8_665 ? O4 Cu2 Cu2 131.7(3) . 5_565 ? O3 Cu2 Cu2 39.7(3) 5_565 5_565 ? O3 Cu2 Cu2 38.5(3) . 5_565 ? O1 Cu2 Cu2 116.6(2) 3 5_565 ? O1 Cu2 Cu2 116.6(2) 8_665 5_565 ? O1 As1 O1 109.6(5) 6 . ? O1 As1 O3 109.1(3) 6 . ? O1 As1 O3 109.1(3) . . ? O1 As1 O2 111.2(3) 6 . ? O1 As1 O2 111.2(3) . . ? O3 As1 O2 106.6(4) . . ? As1 O1 Cu2 128.5(3) . 3_545 ? As1 O1 Cu1 114.2(3) . 3 ? Cu2 O1 Cu1 117.0(3) 3_545 3 ? As1 O2 Cu1 126.0(2) . 5 ? As1 O2 Cu1 126.0(2) . . ? Cu1 O2 Cu1 98.5(4) 5 . ? As1 O2 O2 154.2(7) . 5 ? Cu1 O2 O2 49.24(18) 5 5 ? Cu1 O2 O2 49.24(18) . 5 ? As1 O2 O4 88.0(2) . 3_545 ? Cu1 O2 O4 140.3(4) 5 3_545 ? Cu1 O2 O4 41.94(16) . 3_545 ? O2 O2 O4 91.1(2) 5 3_545 ? As1 O3 Cu2 130.0(5) . 5_565 ? As1 O3 Cu2 128.2(5) . . ? Cu2 O3 Cu2 101.9(4) 5_565 . ? As1 O3 O3 178.2(7) . 5_565 ? Cu2 O3 O3 51.9(3) 5_565 5_565 ? Cu2 O3 O3 50.0(3) . 5_565 ? Cu2 O4 Cu1 124.7(3) . 3 ? Cu2 O4 Cu1 124.7(3) . 7_665 ? Cu1 O4 Cu1 95.5(3) 3 7_665 ? Cu2 O4 O4 147.9(6) . 5_665 ? Cu1 O4 O4 47.76(17) 3 5_665 ? Cu1 O4 O4 47.76(17) 7_665 5_665 ? Cu2 O4 H1 114.3 . . ? Cu1 O4 H1 95.2 3 . ? Cu1 O4 H1 95.2 7_665 . ? O4 O4 H1 97.8 5_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O1 0.83 2.38 2.936(10) 125.6 5_665 _refine_diff_density_max 1.283 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.229 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL olivenite joo 500C in P nnm CELL .71073 8.2696 8.6978 5.9731 90.000 90.000 90.000 ZERR 4 .0008 .0008 .0007 .00 .000 .00 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC H O CU AS UNIT 4 20 8 4 MERG 2 ACTA BOND $H SIZE 0.41 0.27 0.25 EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x, -y+1, -z EQIV $4 -x+1/2, y-1/2, -z+1/2 EQIV $5 -x+1, -y+1, -z BIND CU2 CU2_$3 BIND O4 O4_$5 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$3 HTAB O4 O1_$5 L.S. 5 LIST 4 FMAP 2 PLAN 25 WGHT 0.056700 2.199500 FVAR 0.31219 CU1 3 0.000000 0.000000 0.250458 10.50000 0.03848 0.04716 = 0.02395 0.00000 0.00000 -0.01111 CU2 3 0.137759 0.619151 0.000000 10.50000 0.02976 0.04350 = 0.05981 0.00000 0.00000 0.00177 AS1 4 0.235603 0.249422 0.000000 10.50000 0.02686 0.03150 = 0.02931 0.00000 0.00000 -0.00208 O1 2 0.350188 0.264764 0.227055 11.00000 0.05663 0.05300 = 0.04018 0.01402 -0.02278 -0.02017 O2 2 0.130264 0.081489 0.000000 10.50000 0.03859 0.03403 = 0.02760 0.00000 0.00000 -0.01333 O3 2 0.098710 0.391087 0.000000 10.50000 0.02476 0.02986 = 0.11637 0.00000 0.00000 0.00216 O4 2 0.371117 0.595891 0.000000 10.50000 0.02693 0.03970 = 0.03316 0.00000 0.00000 0.00171 AFIX 3 H1 1 0.421427 0.677851 0.000000 10.50000 -1.20000 AFIX 0 HKLF 4 REM olivenite joo 500C in P nnm REM R1 = 0.0446 for 390 Fo > 4sig(Fo) and 0.0601 for all 492 data REM 45 parameters refined using 0 restraints END WGHT 0.0558 2.2418 REM Highest difference peak 1.283, deepest hole -0.672, 1-sigma level 0.229 Q1 1 0.2253 0.3593 0.0000 10.50000 0.05 1.28 Q2 1 0.4093 0.7919 0.0000 10.50000 0.05 1.19 Q3 1 0.2839 0.1589 0.0000 10.50000 0.05 1.04 Q4 1 0.1255 0.2896 0.0000 10.50000 0.05 1.00 Q5 1 0.0043 -0.1021 0.2503 11.00000 0.05 0.84 Q6 1 0.1319 0.7037 0.0000 10.50000 0.05 0.76 Q7 1 0.0192 0.6623 0.0000 10.50000 0.05 0.71 Q8 1 0.2940 0.0336 0.0000 10.50000 0.05 0.57 Q9 1 0.1179 0.5985 0.1324 11.00000 0.05 0.55 Q10 1 0.2540 0.5665 0.0000 10.50000 0.05 0.53 Q11 1 0.0366 0.5608 0.0000 10.50000 0.05 0.52 Q12 1 0.1716 0.5407 0.0721 11.00000 0.05 0.52 Q13 1 0.1137 0.4994 0.0000 10.50000 0.05 0.50 Q14 1 -0.0171 0.1428 0.0000 10.50000 0.05 0.49 Q15 1 0.3827 0.4758 0.0000 10.50000 0.05 0.48 Q16 1 0.4690 0.6365 0.0000 10.50000 0.05 0.47 Q17 1 0.1315 -0.0198 0.2516 11.00000 0.05 0.45 Q18 1 0.1429 0.0398 0.0000 10.50000 0.05 0.42 Q19 1 0.2519 0.2547 0.1462 11.00000 0.05 0.40 Q20 1 0.4605 0.2895 0.1041 11.00000 0.05 0.39 Q21 1 0.4655 0.7166 0.1855 11.00000 0.05 0.38 Q22 1 0.5550 0.8367 0.0000 10.50000 0.05 0.35 Q23 1 0.0764 0.4060 0.0684 11.00000 0.05 0.35 Q24 1 0.2933 0.4322 0.0746 11.00000 0.05 0.34 Q25 1 0.4788 0.2576 0.2745 11.00000 0.05 0.33 ; _shelx_res_checksum 65433 _shelx_hkl_file ; 1 0 0 -1.1 1.1 1 2 0 0 135.8 3.3 1 3 0 0 -1.8 3.2 1 4 0 0 18.0 3.5 1 5 0 0 -2.2 3.8 1 6 0 0 52.8 3.7 1 7 0 0 5.0 4.5 1 8 0 0 1030.7 11.0 1 9 0 0 -3.1 3.9 1 10 0 0 25.9 3.8 1 0 1 0 2.0 0.8 1 1 1 0 568.1 3.8 1 -1 1 0 573.5 3.9 1 2 1 0 259.1 4.1 1 -2 1 0 279.9 4.1 1 3 1 0 1251.7 8.2 1 -3 1 0 1422.5 12.6 1 4 1 0 6.3 3.1 1 -4 1 0 4.4 4.2 1 5 1 0 567.7 7.1 1 -5 1 0 528.6 7.2 1 6 1 0 320.2 6.4 1 -6 1 0 297.8 6.3 1 7 1 0 37.4 4.7 1 -7 1 0 28.4 3.9 1 8 1 0 270.1 6.7 1 -8 1 0 270.2 6.3 1 9 1 0 31.8 4.5 1 -9 1 0 34.6 3.4 1 10 1 0 10.5 4.1 1 -10 1 0 19.2 4.0 1 0 2 0 104.6 2.5 1 1 2 0 725.8 5.5 1 -1 2 0 732.4 5.6 1 2 2 0 3476.7 12.6 1 -2 2 0 3567.2 12.8 1 3 2 0 189.4 3.9 1 -3 2 0 177.1 4.0 1 4 2 0 5.5 3.0 1 -4 2 0 7.8 3.2 1 5 2 0 472.6 6.7 1 -5 2 0 555.9 8.0 1 6 2 0 713.3 8.7 1 -6 2 0 809.6 13.6 1 7 2 0 18.6 3.7 1 -7 2 0 22.0 7.4 1 8 2 0 0.0 4.1 1 -8 2 0 -6.8 4.9 1 9 2 0 105.3 5.3 1 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