data_ada_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As H O5 Zn2' _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5312(3) _cell_length_b 8.3149(3) _cell_length_c 6.0590(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 429.80(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 6453 _cell_measurement_theta_min 2 _cell_measurement_theta_max 38 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.709 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.064 _exptl_absorpt_correction_T_max 0.118 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 10139 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0223 _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 3.42 _diffrn_reflns_theta_max 38.54 _reflns_number_total 1271 _reflns_number_gt 1215 _reflns_threshold_expression >2\s(I) _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-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.6566P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refXYZ _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0221(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1271 _refine_ls_number_parameters 48 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.25263(4) 0.01028(7) Uani 1 2 d S . . Zn2 Zn 0.13574(3) 0.63481(3) 0.0000 0.00672(7) Uani 1 2 d S . . As1 As 0.24403(2) 0.25057(2) 0.0000 0.00422(6) Uani 1 2 d S . . O1 O 0.36121(14) 0.27024(15) 0.2226(2) 0.00975(19) Uani 1 1 d . . . O2 O 0.14450(19) 0.07477(19) 0.0000 0.0075(2) Uani 1 2 d S . . O3 O 0.1062(2) 0.3950(2) 0.0000 0.0125(3) Uani 1 2 d S . . O4 O 0.37206(19) 0.6077(2) 0.0000 0.0074(2) Uani 1 2 d SD . . H1 H 0.418(4) 0.712(2) 0.0000 0.009 Uiso 1 2 d SD . . 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 Zn1 0.01260(13) 0.01501(13) 0.00324(11) 0.000 0.000 -0.00578(8) Zn2 0.00783(11) 0.00646(11) 0.00587(11) 0.000 0.000 0.00014(7) As1 0.00564(10) 0.00382(10) 0.00320(10) 0.000 0.000 -0.00060(5) O1 0.0133(5) 0.0112(4) 0.0048(4) 0.0024(3) -0.0036(3) -0.0045(4) O2 0.0115(7) 0.0056(5) 0.0055(6) 0.000 0.000 -0.0037(4) O3 0.0070(6) 0.0057(6) 0.0248(9) 0.000 0.000 0.0008(5) O4 0.0076(6) 0.0082(6) 0.0064(6) 0.000 0.000 0.0000(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O4 2.0590(11) 3_545 ? Zn1 O4 2.0590(11) 7_566 ? Zn1 O2 2.0613(11) 5 ? Zn1 O2 2.0613(11) . ? Zn1 O1 2.2526(12) 3_545 ? Zn1 O1 2.2526(12) 4_455 ? Zn1 Zn1 2.9977(5) 5_556 ? Zn2 O3 2.0100(17) . ? Zn2 O1 2.0233(12) 3 ? Zn2 O1 2.0233(12) 8_665 ? Zn2 O4 2.0287(17) . ? Zn2 O3 2.0788(18) 5_565 ? Zn2 Zn2 3.2234(5) 5_565 ? As1 O3 1.6807(17) . ? As1 O1 1.6868(11) . ? As1 O1 1.6868(11) 6 ? As1 O2 1.6905(15) . ? O1 Zn2 2.0233(12) 3_545 ? O1 Zn1 2.2526(12) 3 ? O2 Zn1 2.0613(11) 5 ? O2 O2 2.761(3) 5 ? O2 O4 3.0451(3) 3_544 ? O3 Zn2 2.0788(18) 5_565 ? O3 O3 2.517(3) 5_565 ? O4 Zn1 2.0590(11) 7_665 ? O4 Zn1 2.0590(11) 3 ? O4 O4 2.823(3) 5_665 ? O4 H1 0.956(10) . ? 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 O4 Zn1 O4 86.57(7) 3_545 7_566 ? O4 Zn1 O2 171.38(7) 3_545 5 ? O4 Zn1 O2 95.30(5) 7_566 5 ? O4 Zn1 O2 95.30(5) 3_545 . ? O4 Zn1 O2 171.38(7) 7_566 . ? O2 Zn1 O2 84.10(6) 5 . ? O4 Zn1 O1 92.39(5) 3_545 3_545 ? O4 Zn1 O1 82.03(6) 7_566 3_545 ? O2 Zn1 O1 96.20(5) 5 3_545 ? O2 Zn1 O1 89.48(6) . 3_545 ? O4 Zn1 O1 82.03(6) 3_545 4_455 ? O4 Zn1 O1 92.39(5) 7_566 4_455 ? O2 Zn1 O1 89.48(6) 5 4_455 ? O2 Zn1 O1 96.20(5) . 4_455 ? O1 Zn1 O1 172.36(6) 3_545 4_455 ? O4 Zn1 Zn1 43.29(3) 3_545 5_556 ? O4 Zn1 Zn1 43.29(3) 7_566 5_556 ? O2 Zn1 Zn1 137.95(3) 5 5_556 ? O2 Zn1 Zn1 137.95(3) . 5_556 ? O1 Zn1 Zn1 86.18(3) 3_545 5_556 ? O1 Zn1 Zn1 86.18(3) 4_455 5_556 ? O3 Zn2 O1 123.63(4) . 3 ? O3 Zn2 O1 123.63(4) . 8_665 ? O1 Zn2 O1 112.35(7) 3 8_665 ? O3 Zn2 O4 90.82(7) . . ? O1 Zn2 O4 92.81(4) 3 . ? O1 Zn2 O4 92.81(4) 8_665 . ? O3 Zn2 O3 75.95(8) . 5_565 ? O1 Zn2 O3 94.54(4) 3 5_565 ? O1 Zn2 O3 94.54(4) 8_665 5_565 ? O4 Zn2 O3 166.77(7) . 5_565 ? O3 Zn2 Zn2 38.73(5) . 5_565 ? O1 Zn2 Zn2 113.35(4) 3 5_565 ? O1 Zn2 Zn2 113.35(4) 8_665 5_565 ? O4 Zn2 Zn2 129.55(5) . 5_565 ? O3 Zn2 Zn2 37.22(5) 5_565 5_565 ? O3 As1 O1 110.21(5) . . ? O3 As1 O1 110.21(5) . 6 ? O1 As1 O1 106.18(8) . 6 ? O3 As1 O2 105.45(8) . . ? O1 As1 O2 112.43(5) . . ? O1 As1 O2 112.43(5) 6 . ? As1 O1 Zn2 128.16(7) . 3_545 ? As1 O1 Zn1 116.55(6) . 3 ? Zn2 O1 Zn1 114.20(5) 3_545 3 ? As1 O2 Zn1 124.14(5) . 5 ? As1 O2 Zn1 124.14(5) . . ? Zn1 O2 Zn1 95.90(6) 5 . ? As1 O2 O2 146.91(12) . 5 ? Zn1 O2 O2 47.95(3) 5 5 ? Zn1 O2 O2 47.95(3) . 5 ? As1 O2 O4 86.88(4) . 3_544 ? Zn1 O2 O4 42.32(3) 5 3_544 ? Zn1 O2 O4 137.57(7) . 3_544 ? O2 O2 O4 89.95(4) 5 3_544 ? As1 O3 Zn2 128.40(10) . . ? As1 O3 Zn2 127.55(9) . 5_565 ? Zn2 O3 Zn2 104.05(8) . 5_565 ? As1 O3 O3 178.35(14) . 5_565 ? Zn2 O3 O3 53.26(6) . 5_565 ? Zn2 O3 O3 50.79(6) 5_565 5_565 ? Zn2 O4 Zn1 125.11(5) . 7_665 ? Zn2 O4 Zn1 125.11(5) . 3 ? Zn1 O4 Zn1 93.43(7) 7_665 3 ? Zn2 O4 O4 147.02(11) . 5_665 ? Zn1 O4 O4 46.71(3) 7_665 5_665 ? Zn1 O4 O4 46.71(3) 3 5_665 ? Zn2 O4 H1 108(2) . . ? Zn1 O4 H1 100.2(17) 7_665 . ? Zn1 O4 H1 100.2(17) 3 . ? O4 O4 H1 105(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 0.956(10) 2.32(3) 2.8333(18) 113(2) 5_665 O4 H1 O1 0.956(10) 2.32(3) 2.8333(18) 113(2) 2_665 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 38.54 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.473 _refine_diff_density_min -1.315 _refine_diff_density_rms 0.205 _iucr_refine_instructions_details ; TITL ADA_25C_ccd Pnnm ba-c CELL 0.71073 8.5312 8.3149 6.0590 90.000 90.000 90.000 ZERR 4 0.0003 0.0003 0.0002 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA dfix 0.96 0.01 O4 H1 BOND $H EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 L.S. 4 LIST 4 FMAP 2 PLAN 25 WGHT 0.020100 0.656600 EXTI 0.022101 FVAR 0.40487 ZN1 4 0.000000 0.000000 0.252628 10.50000 0.01260 0.01501 = 0.00324 0.00000 0.00000 -0.00578 ZN2 4 0.135738 0.634813 0.000000 10.50000 0.00783 0.00646 = 0.00587 0.00000 0.00000 0.00014 AS1 2 0.244029 0.250570 0.000000 10.50000 0.00564 0.00382 = 0.00320 0.00000 0.00000 -0.00060 O1 3 0.361210 0.270237 0.222598 11.00000 0.01334 0.01117 = 0.00475 0.00241 -0.00355 -0.00450 O2 3 0.144498 0.074770 0.000000 10.50000 0.01152 0.00556 = 0.00552 0.00000 0.00000 -0.00366 O3 3 0.106193 0.394985 0.000000 10.50000 0.00697 0.00570 = 0.02476 0.00000 0.00000 0.00080 O4 3 0.372061 0.607682 0.000000 10.50000 0.00756 0.00824 = 0.00641 0.00000 0.00000 0.00003 H1 1 0.418381 0.712313 0.000000 10.50000 -1.20000 HKLF 4 REM ADA_25C_ccd Pnnm ba-c REM R1 = 0.0207 for 1215 Fo > 4sig(Fo) and 0.0217 for all 1271 data REM 48 parameters refined using 1 restraints END ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 1.72 0.28 0 1 0 1.87 0.29 0 -2 0 390.55 18.07 0 2 0 363.18 18.75 0 2 0 331.34 17.98 0 3 0 0.45 0.39 0 -3 0 1.07 0.37 0 -3 0 0.16 0.36 0 -4 0 1208.07 59.08 0 4 0 1249.25 61.38 0 4 0 1093.22 58.83 0 -4 0 1219.35 56.90 0 -5 0 -0.12 0.48 0 -5 0 0.07 0.38 0 5 0 0.29 0.66 0 5 0 -0.28 0.48 0 6 0 214.38 11.65 0 -6 0 206.97 10.63 0 -6 0 201.02 10.46 0 6 0 199.03 11.06 0 7 0 0.31 0.89 0 7 0 -0.35 0.64 0 -7 0 4.25 0.99 0 -7 0 -0.50 0.45 0 -8 0 4514.04 225.74 0 -8 0 4403.09 217.00 0 8 0 4854.20 234.11 0 8 0 4643.63 224.41 0 9 0 0.29 0.93 0 9 0 0.55 1.27 0 -9 0 -0.34 0.96 0 10 0 230.91 13.21 0 10 0 214.95 11.98 0 -10 0 206.89 11.51 0 11 0 0.04 1.49 0 -11 0 0.41 1.30 0 -12 0 326.25 16.71 0 12 0 305.69 18.51 0 -13 0 -0.36 1.46 0 13 0 -0.17 1.58 0 -14 0 -0.73 1.65 1 0 0 2.68 0.30 1 0 0 1.60 0.20 1 1 0 985.80 49.98 -1 1 0 1015.57 50.08 1 -1 0 896.42 46.37 -1 1 0 1023.13 47.98 1 1 0 963.17 47.93 -1 -2 0 1012.72 52.94 -1 2 0 1098.80 52.70 -1 2 0 1098.39 54.77 1 2 0 1030.83 52.51 1 -2 0 1101.55 50.92 1 -2 0 1094.10 53.03 1 2 0 1106.37 54.86 -1 3 0 2550.59 125.02 1 3 0 2557.17 125.14 1 -3 0 2317.78 116.15 -1 -3 0 2470.64 116.15 1 3 0 2533.07 119.98 -1 -3 0 2284.06 120.88 1 -3 0 2426.73 120.97 -1 3 0 2548.83 120.14 -1 4 0 23.92 2.05 1 4 0 24.18 1.88 -1 -4 0 23.72 1.80 -1 -4 0 26.22 1.67 1 -4 0 26.35 1.82 -1 4 0 26.76 2.01 1 4 0 23.53 2.05 1 -4 0 24.86 1.72 -1 5 0 1639.89 82.12 -1 -5 0 1584.31 82.30 -1 -5 0 1641.27 79.32 1 -5 0 1729.83 79.28 1 5 0 1685.41 81.92 1 5 0 1664.68 85.54 1 -5 0 1726.82 82.42 -1 5 0 1700.89 85.37 1 -6 0 740.08 32.23 1 6 0 664.76 34.99 -1 6 0 624.63 33.49 -1 -6 0 631.87 32.18 -1 -6 0 629.14 33.11 -1 6 0 719.74 34.91 1 6 0 645.82 33.22 1 -6 0 679.11 33.25 1 -7 0 1.59 0.86 -1 -7 0 0.55 0.57 -1 7 0 0.89 0.94 -1 7 0 0.73 0.93 -1 -7 0 2.93 1.00 1 7 0 1.02 1.09 1 7 0 1.02 0.73 1 -7 0 0.70 0.66 -1 8 0 115.23 7.23 1 -8 0 112.93 6.42 -1 -8 0 105.23 6.43 -1 -8 0 116.76 6.26 1 8 0 113.91 7.52 -1 8 0 116.17 7.12 1 -8 0 113.96 6.38 1 8 0 108.62 6.57 -1 -9 0 202.19 11.63 1 -9 0 234.26 11.81 -1 9 0 222.95 13.00 1 9 0 224.62 11.92 1 -9 0 216.19 11.66 1 9 0 233.98 13.39 -1 9 0 218.84 12.46 1 -10 0 19.01 2.27 -1 10 0 19.09 2.63 1 10 0 16.76 2.05 1 10 0 20.87 3.07 -1 10 0 21.58 2.86 -1 -10 0 14.49 2.16 -1 11 0 374.41 20.31 -1 11 0 344.35 19.05 -1 -11 0 336.12 18.28 1 11 0 355.60 20.58 1 -11 0 370.37 18.32 -1 -12 0 21.45 2.81 -1 12 0 22.38 3.25 1 12 0 20.91 3.37 1 -12 0 20.95 2.78 1 -13 0 113.63 7.21 1 13 0 104.49 8.48 -1 -13 0 112.45 7.36 1 -14 0 62.56 5.16 1 14 0 58.91 6.11 -1 -14 0 70.00 5.54 2 0 0 190.46 9.38 2 0 0 184.66 8.69 2 0 0 170.57 9.12 2 0 0 176.80 8.98 -2 1 0 830.38 44.08 2 -1 0 840.09 40.98 2 1 0 910.05 41.08 2 1 0 872.71 44.26 2 1 0 948.70 42.38 2 1 0 800.10 42.78 2 -1 0 881.46 42.87 2 -2 0 4570.82 223.00 -2 -2 0 4036.06 223.64 -2 2 0 4924.15 221.26 -2 2 0 4712.90 231.03 2 2 0 4709.35 215.11 2 2 0 4295.15 221.51 2 3 0 238.31 12.49 -2 3 0 236.59 12.21 2 -3 0 225.57 11.89 -2 -3 0 227.48 11.69 -2 3 0 242.72 12.06 2 -3 0 230.14 11.35 2 3 0 230.29 11.61 2 4 0 8.14 1.20 2 4 0 8.20 0.95 -2 -4 0 6.90 0.82 -2 4 0 10.73 1.16 2 -4 0 5.82 0.86 -2 -4 0 7.74 1.02 -2 4 0 8.08 1.20 2 -4 0 7.59 0.92 2 5 0 444.90 23.46 2 -5 0 455.52 21.50 -2 -5 0 427.28 22.01 -2 -5 0 432.03 21.51 -2 5 0 482.70 23.15 2 5 0 384.89 21.92 2 -5 0 441.85 22.25 -2 5 0 465.94 22.59 -2 -6 0 2793.55 137.27 -2 6 0 3060.85 147.65 2 -6 0 2912.81 142.77 2 6 0 2718.24 141.42 -2 6 0 2955.79 142.09 -2 -6 0 2748.30 142.56 2 6 0 3007.35 148.10 2 -6 0 3032.48 137.24 2 7 0 2.77 0.81 2 -7 0 3.66 0.91 -2 -7 0 3.52 1.12 -2 7 0 2.29 1.15 2 -7 0 2.80 0.94 2 7 0 2.86 1.34 -2 7 0 6.03 1.31 -2 8 0 89.94 6.01 -2 8 0 93.37 6.24 2 8 0 92.86 6.59 2 8 0 89.95 5.42 -2 -8 0 87.46 5.59 2 -8 0 95.81 5.54 2 -8 0 92.54 5.47 -2 -9 0 543.90 28.87 -2 9 0 578.00 30.34 -2 9 0 587.05 31.26 2 -9 0 634.88 28.92 2 9 0 575.84 29.48 2 9 0 591.79 31.92 2 -9 0 595.59 29.75 2 -10 0 1330.63 65.64 -2 10 0 1336.84 66.08 -2 -10 0 1248.41 63.44 2 10 0 1294.20 69.12 2 -10 0 1401.00 63.46 -2 10 0 1308.54 68.45 -2 -11 0 1.59 1.49 2 -11 0 2.10 1.41 2 11 0 1.28 1.94 -2 11 0 2.93 1.56 -2 11 0 4.33 1.82 -2 -12 0 41.59 4.02 2 12 0 43.57 5.16 2 -12 0 47.36 4.11 2 13 0 194.01 13.66 2 -13 0 231.02 12.02 -2 -13 0 204.92 12.02 -2 -14 0 308.45 16.59 2 14 0 295.14 18.58 3 0 0 0.87 0.37 3 0 0 0.37 0.28 3 0 0 0.76 0.33 3 0 0 0.20 0.25 3 1 0 2002.20 90.13 3 1 0 2007.36 97.10 3 -1 0 1864.27 94.00 3 1 0 1739.90 93.90 -3 1 0 1830.93 96.80 3 1 0 1986.20 93.01 3 -1 0 1930.16 90.17 3 2 0 382.43 18.38 3 -2 0 362.62 18.18 -3 2 0 395.13 19.55 3 2 0 374.34 19.90 3 2 0 390.97 18.82 3 -2 0 384.92 19.26 -3 -3 0 221.35 11.28 3 -3 0 219.53 11.50 -3 3 0 232.32 11.63 3 -3 0 207.14 10.76 -3 3 0 220.27 11.54 3 3 0 215.33 11.07 -3 -5 0 237.84 12.62 -3 5 0 258.08 13.36 3 -5 0 250.25 13.00 3 5 0 242.64 12.60 -3 -5 0 254.94 12.59 -3 5 0 250.19 13.29 3 -5 0 245.08 12.44 -3 -6 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6.14 -3 1 -10 60.98 6.86 -3 2 -10 49.06 6.05 -3 -2 -10 46.28 5.63 3 2 10 43.72 4.79 -3 -2 10 49.05 5.46 -3 -3 10 340.64 19.08 3 3 10 291.54 18.02 -3 -3 -10 311.77 19.33 -4 0 10 152.31 10.18 -4 0 -10 142.67 11.11 -4 -1 -10 -0.45 2.09 -4 -1 10 -0.98 1.82 4 1 10 -0.45 1.39 -4 1 -10 0.33 2.47 4 2 10 517.11 29.30 -4 -2 -10 518.99 30.93 -4 -2 10 590.98 30.07 4 -3 -10 9.03 2.35 0 0 0 0.00 0.00 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5234(5) _cell_length_b 8.3080(5) _cell_length_c 6.0555(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 428.81(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.752 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_T_max 0.118 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 1321 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 30.04 _reflns_number_total 686 _reflns_number_gt 612 _reflns_threshold_expression >2\s(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.7335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 686 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_restrained_S_all 1.275 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.25275(14) 0.0205(4) Uani 1 2 d S . . Zn2 Zn 0.13567(11) 0.63484(12) 0.0000 0.0166(4) Uani 1 2 d S . . As1 As 0.24394(8) 0.25061(10) 0.0000 0.0144(3) Uani 1 2 d S . . O1 O 0.3614(5) 0.2717(6) 0.2235(6) 0.0220(10) Uani 1 1 d . . . O2 O 0.1443(7) 0.0746(9) 0.0000 0.0178(12) Uani 1 2 d S . . O3 O 0.1070(7) 0.3947(9) 0.0000 0.0223(13) Uani 1 2 d S . . O4 O 0.3725(7) 0.6076(8) 0.0000 0.0178(12) Uani 1 2 d S . . H1 H 0.4141 0.6980 0.0000 0.021 Uiso 1 2 d SR . . 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 Zn1 0.0245(6) 0.0272(7) 0.0099(5) 0.000 0.000 -0.0064(4) Zn2 0.0194(5) 0.0179(6) 0.0124(5) 0.000 0.000 0.0003(4) As1 0.0173(5) 0.0163(6) 0.0096(4) 0.000 0.000 -0.0007(3) O1 0.029(2) 0.028(3) 0.0095(17) 0.0047(15) -0.0047(14) -0.0044(18) O2 0.023(3) 0.020(3) 0.011(2) 0.000 0.000 -0.003(2) O3 0.017(3) 0.018(3) 0.032(3) 0.000 0.000 -0.003(2) O4 0.022(3) 0.018(3) 0.013(2) 0.000 0.000 0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O4 2.055(4) 3_545 ? Zn1 O4 2.055(4) 7_566 ? Zn1 O2 2.059(4) 5 ? Zn1 O2 2.059(4) . ? Zn1 O1 2.239(5) 4_455 ? Zn1 O1 2.239(5) 3_545 ? Zn1 Zn1 2.9945(17) 5_556 ? Zn2 O3 2.010(7) . ? Zn2 O1 2.024(4) 3 ? Zn2 O1 2.024(4) 8_665 ? Zn2 O4 2.031(6) . ? Zn2 O3 2.083(6) 5_565 ? Zn2 Zn2 3.2201(19) 5_565 ? As1 O3 1.672(7) . ? As1 O2 1.691(7) . ? As1 O1 1.693(4) . ? As1 O1 1.693(4) 6 ? O1 Zn2 2.024(4) 3_545 ? O1 Zn1 2.239(5) 3 ? O2 Zn1 2.059(4) 5 ? O2 O2 2.754(12) 5 ? O2 O4 3.0435(10) 3_544 ? O3 Zn2 2.083(6) 5_565 ? O3 O3 2.527(14) 5_565 ? O4 Zn1 2.055(4) 3 ? O4 Zn1 2.055(4) 7_665 ? O4 O4 2.815(13) 5_665 ? O4 H1 0.8304 . ? 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 O4 Zn1 O4 86.5(3) 3_545 7_566 ? O4 Zn1 O2 171.3(3) 3_545 5 ? O4 Zn1 O2 95.43(17) 7_566 5 ? O4 Zn1 O2 95.43(17) 3_545 . ? O4 Zn1 O2 171.3(3) 7_566 . ? O2 Zn1 O2 84.0(2) 5 . ? O4 Zn1 O1 82.2(2) 3_545 4_455 ? O4 Zn1 O1 92.4(2) 7_566 4_455 ? O2 Zn1 O1 89.3(2) 5 4_455 ? O2 Zn1 O1 96.2(2) . 4_455 ? O4 Zn1 O1 92.4(2) 3_545 3_545 ? O4 Zn1 O1 82.2(2) 7_566 3_545 ? O2 Zn1 O1 96.2(2) 5 3_545 ? O2 Zn1 O1 89.3(2) . 3_545 ? O1 Zn1 O1 172.6(2) 4_455 3_545 ? O4 Zn1 Zn1 43.23(13) 3_545 5_556 ? O4 Zn1 Zn1 43.23(13) 7_566 5_556 ? O2 Zn1 Zn1 138.02(12) 5 5_556 ? O2 Zn1 Zn1 138.02(12) . 5_556 ? O1 Zn1 Zn1 86.32(10) 4_455 5_556 ? O1 Zn1 Zn1 86.32(10) 3_545 5_556 ? O3 Zn2 O1 123.99(15) . 3 ? O3 Zn2 O1 123.99(15) . 8_665 ? O1 Zn2 O1 111.6(3) 3 8_665 ? O3 Zn2 O4 90.6(3) . . ? O1 Zn2 O4 92.88(16) 3 . ? O1 Zn2 O4 92.88(16) 8_665 . ? O3 Zn2 O3 76.2(3) . 5_565 ? O1 Zn2 O3 94.50(17) 3 5_565 ? O1 Zn2 O3 94.50(17) 8_665 5_565 ? O4 Zn2 O3 166.8(3) . 5_565 ? O3 Zn2 Zn2 38.92(19) . 5_565 ? O1 Zn2 Zn2 113.56(14) 3 5_565 ? O1 Zn2 Zn2 113.56(14) 8_665 5_565 ? O4 Zn2 Zn2 129.5(2) . 5_565 ? O3 Zn2 Zn2 37.3(2) 5_565 5_565 ? O3 As1 O2 105.6(3) . . ? O3 As1 O1 109.8(2) . . ? O2 As1 O1 112.7(2) . . ? O3 As1 O1 109.8(2) . 6 ? O2 As1 O1 112.7(2) . 6 ? O1 As1 O1 106.2(3) . 6 ? As1 O1 Zn2 127.6(3) . 3_545 ? As1 O1 Zn1 116.8(2) . 3 ? Zn2 O1 Zn1 114.60(18) 3_545 3 ? As1 O2 Zn1 124.1(2) . 5 ? As1 O2 Zn1 124.1(2) . . ? Zn1 O2 Zn1 96.0(2) 5 . ? As1 O2 O2 146.9(5) . 5 ? Zn1 O2 O2 48.02(12) 5 5 ? Zn1 O2 O2 48.02(12) . 5 ? As1 O2 O4 86.88(18) . 3_544 ? Zn1 O2 O4 42.23(12) 5 3_544 ? Zn1 O2 O4 137.6(3) . 3_544 ? O2 O2 O4 89.93(17) 5 3_544 ? As1 O3 Zn2 128.7(4) . . ? As1 O3 Zn2 127.5(4) . 5_565 ? Zn2 O3 Zn2 103.8(3) . 5_565 ? As1 O3 O3 178.1(5) . 5_565 ? Zn2 O3 O3 53.2(3) . 5_565 ? Zn2 O3 O3 50.6(2) 5_565 5_565 ? Zn2 O4 Zn1 125.04(19) . 3 ? Zn2 O4 Zn1 125.04(19) . 7_665 ? Zn1 O4 Zn1 93.5(3) 3 7_665 ? Zn2 O4 O4 147.0(4) . 5_665 ? Zn1 O4 O4 46.77(13) 3 5_665 ? Zn1 O4 O4 46.77(13) 7_665 5_665 ? Zn2 O4 H1 108.9 . . ? Zn1 O4 H1 99.6 3 . ? Zn1 O4 H1 99.6 7_665 . ? O4 O4 H1 104.1 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 2.36 2.825(7) 116.3 5_665 O4 H1 O1 0.83 2.36 2.825(7) 116.3 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.890 _refine_diff_density_min -1.795 _refine_diff_density_rms 0.362 _iucr_refine_instructions_details ; TITL ADA_25C Pnnm ba-c CELL 0.71073 8.5234 8.3080 6.0555 90.000 90.000 90.000 ZERR 4 0.0005 0.0005 0.0004 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 HTAB BOND $H HTAB L.S. 4 LIST 4 FMAP 2 PLAN 25 WGHT 0.063100 1.733500 EXTI 0.017807 FVAR 0.38004 ZN1 4 0.000000 0.000000 0.252748 10.50000 0.02448 0.02720 = 0.00995 0.00000 0.00000 -0.00635 ZN2 4 0.135671 0.634841 0.000000 10.50000 0.01942 0.01793 = 0.01239 0.00000 0.00000 0.00031 AS1 2 0.243938 0.250613 0.000000 10.50000 0.01726 0.01626 = 0.00957 0.00000 0.00000 -0.00066 O1 3 0.361403 0.271716 0.223496 11.00000 0.02863 0.02788 = 0.00947 0.00469 -0.00470 -0.00436 O2 3 0.144288 0.074579 0.000000 10.50000 0.02257 0.02021 = 0.01077 0.00000 0.00000 -0.00334 O3 3 0.106992 0.394742 0.000000 10.50000 0.01691 0.01846 = 0.03150 0.00000 0.00000 -0.00273 O4 3 0.372452 0.607616 0.000000 10.50000 0.02215 0.01825 = 0.01306 0.00000 0.00000 0.00110 AFIX 3 H1 1 0.414065 0.697995 0.000000 10.50000 -1.20000 HKLF 4 REM jog 25c Pnnm ba-c REM R1 = 0.0419 for 612 Fo > 4sig(Fo) and 0.0456 for all 686 data REM 46 parameters refined using 0 restraints END WGHT 0.0627 1.8375 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 3.6 1.0 0 2 0 260.2 4.0 0 3 0 2.3 2.0 0 4 0 702.1 8.2 0 5 0 0.4 1.9 0 6 0 99.8 3.8 0 7 0 -0.7 2.0 0 8 0 1835.4 15.4 0 9 0 1.2 1.8 0 10 0 75.0 3.6 0 11 0 0.1 1.9 1 0 0 2.0 0.7 1 1 0 692.6 5.4 1 -1 0 1075.5 6.5 1 2 0 720.8 6.8 1 -2 0 1138.8 8.5 1 3 0 1614.4 11.5 1 -3 0 2906.3 15.3 1 4 0 15.3 1.7 1 -4 0 23.8 2.0 1 5 0 828.8 9.4 1 -5 0 1450.6 12.4 1 6 0 277.0 5.8 1 -6 0 508.4 7.8 1 7 0 0.5 2.0 1 -7 0 1.9 1.9 1 8 0 44.2 2.8 1 -8 0 70.9 3.4 1 9 0 81.4 3.7 1 -9 0 130.8 4.5 1 10 0 3.8 2.2 1 -10 0 11.8 2.2 1 11 0 94.7 4.1 1 -11 0 182.8 5.4 2 0 0 149.5 2.9 2 1 0 625.1 6.3 2 -1 0 805.7 6.2 2 2 0 3344.3 15.8 2 -2 0 4930.1 18.8 2 3 0 145.6 3.7 2 -3 0 240.9 4.9 2 4 0 4.8 2.0 2 -4 0 9.4 1.6 2 5 0 229.7 5.2 2 -5 0 396.5 6.8 2 6 0 1355.4 12.5 2 -6 0 2365.5 16.5 2 7 0 1.6 1.9 2 -7 0 2.2 2.1 2 8 0 33.9 2.4 2 -8 0 66.2 3.3 2 9 0 184.6 5.3 2 -9 0 372.2 7.4 2 10 0 387.8 7.7 2 -10 0 750.9 10.5 2 11 0 1.1 1.8 2 -11 0 1.8 1.9 3 0 0 -0.6 1.7 3 1 0 1362.2 10.5 3 -1 0 1653.1 9.1 3 2 0 236.4 4.8 3 -2 0 343.4 5.3 3 3 0 128.8 3.8 3 -3 0 214.4 4.8 3 4 0 4.5 1.9 3 -4 0 4.7 1.9 3 5 0 134.5 4.1 3 -5 0 227.2 5.3 3 6 0 107.1 3.9 3 -6 0 210.7 5.3 3 7 0 836.9 10.4 3 -7 0 1581.0 14.1 3 8 0 10.8 1.8 3 -8 0 18.8 2.1 3 9 0 72.9 3.5 3 -9 0 138.8 4.7 3 10 0 5.2 2.0 3 -10 0 7.2 2.2 3 11 0 0.1 1.8 3 -11 0 -1.5 2.0 4 0 0 34.7 2.3 4 1 0 31.1 2.0 4 -1 0 32.6 1.5 4 2 0 31.2 2.3 4 -2 0 39.5 2.1 4 3 0 14.8 1.7 4 -3 0 13.8 1.7 4 4 0 3346.6 19.6 4 -4 0 6001.8 26.3 4 5 0 66.9 3.1 4 -5 0 134.3 4.3 4 6 0 7.1 2.1 4 -6 0 6.7 2.1 4 7 0 1.7 1.9 4 -7 0 3.6 2.2 4 8 0 143.4 4.7 4 -8 0 273.9 6.3 4 9 0 0.8 1.9 4 -9 0 0.5 1.9 4 10 0 -0.3 1.9 4 -10 0 3.3 2.1 4 11 0 4.0 1.9 4 -11 0 8.3 1.7 5 0 0 2.6 1.5 5 1 0 908.8 10.2 5 -1 0 970.1 8.7 5 2 0 630.6 8.7 5 -2 0 751.1 8.1 5 3 0 181.2 4.9 5 -3 0 254.3 5.4 5 4 0 10.8 1.7 5 -4 0 20.0 2.1 5 5 0 110.3 4.0 5 -5 0 193.4 5.2 5 6 0 195.4 5.2 5 -6 0 347.4 7.0 5 7 0 290.6 6.4 5 -7 0 536.9 8.8 5 8 0 38.9 2.7 5 -8 0 75.7 3.6 5 9 0 65.3 3.3 5 -9 0 117.8 4.4 5 10 0 18.1 2.2 5 -10 0 35.0 2.6 6 0 0 98.6 3.6 6 1 0 420.1 7.4 6 -1 0 408.3 6.7 6 2 0 1242.2 12.7 6 -2 0 1375.4 10.7 6 3 0 66.0 3.2 6 -3 0 95.4 3.4 6 4 0 52.0 3.0 6 -4 0 71.2 3.3 6 5 0 42.9 2.7 6 -5 0 80.7 3.6 6 6 0 704.9 9.8 6 -6 0 1222.2 13.2 6 7 0 43.0 2.8 6 -7 0 73.7 3.6 6 8 0 0.8 1.8 6 -8 0 3.1 2.0 6 9 0 126.5 4.9 6 -9 0 242.2 6.0 6 10 0 141.2 4.9 6 -10 0 262.1 6.4 7 0 0 2.7 1.3 7 1 0 107.1 4.2 7 -1 0 101.6 3.5 7 2 0 29.3 2.5 7 -2 0 26.6 1.7 7 3 0 578.7 9.3 7 -3 0 728.1 9.0 7 4 0 -0.3 1.8 7 -4 0 0.4 1.8 7 5 0 265.0 6.3 7 -5 0 443.4 8.0 7 6 0 2.3 2.1 7 -6 0 10.1 1.8 7 7 0 20.5 2.1 7 -7 0 34.0 2.7 7 8 0 15.0 1.8 7 -8 0 19.5 2.2 7 9 0 49.4 3.1 7 -9 0 87.2 3.8 8 0 0 1859.2 15.1 8 1 0 197.3 5.4 8 -1 0 189.4 4.9 8 2 0 34.1 2.6 8 -2 0 41.5 2.0 8 3 0 4.9 1.8 8 -3 0 6.3 1.6 8 4 0 208.8 5.6 8 -4 0 273.9 6.1 8 5 0 0.0 1.7 8 -5 0 1.3 1.7 8 6 0 18.5 2.1 8 -6 0 32.7 2.7 8 7 0 29.9 2.4 8 -7 0 50.5 3.1 8 8 0 557.1 9.4 8 -8 0 1012.2 12.4 9 0 0 6.8 1.7 9 1 0 63.5 3.3 9 -1 0 68.4 3.2 9 2 0 189.5 5.5 9 -2 0 164.5 4.1 9 3 0 142.0 4.8 9 -3 0 161.0 4.3 9 4 0 -0.3 1.7 9 -4 0 1.5 1.5 9 5 0 83.3 3.8 9 -5 0 125.1 4.8 9 6 0 131.7 4.6 9 -6 0 239.2 6.4 9 7 0 38.0 2.7 9 -7 0 66.1 3.6 10 0 0 118.1 4.2 10 1 0 3.5 1.8 10 -1 0 2.9 1.6 10 2 0 442.3 8.7 10 -2 0 433.2 7.0 10 3 0 28.6 2.4 10 -3 0 33.4 2.1 10 4 0 0.9 1.5 10 -4 0 0.5 1.2 10 5 0 47.9 2.9 10 -5 0 64.2 3.4 10 6 0 199.6 5.7 10 -6 0 335.6 7.6 11 0 0 0.6 1.4 11 1 0 107.6 4.5 11 -1 0 100.4 3.8 11 2 0 2.2 1.7 11 -2 0 0.6 1.3 11 3 0 0.5 1.7 11 -3 0 2.7 1.2 11 4 0 5.0 1.7 11 -4 0 5.7 1.4 12 0 0 46.9 2.8 0 0 -1 9.5 0.7 0 1 -1 1330.7 6.1 0 -1 -1 1348.4 7.1 0 2 -1 12.3 1.2 0 -2 -1 13.3 1.6 0 3 -1 1215.1 8.7 0 -3 -1 1462.9 10.5 0 4 -1 2.2 1.7 0 -4 -1 2.2 2.0 0 5 -1 252.7 5.3 0 -5 -1 304.9 6.2 0 6 -1 5.8 2.1 0 -6 -1 6.8 2.4 0 7 -1 331.8 6.6 0 -7 -1 474.1 8.1 0 8 -1 0.2 2.0 0 -8 -1 3.3 2.1 0 9 -1 74.6 3.4 0 -9 -1 101.0 4.1 0 10 -1 0.9 1.8 0 -10 -1 2.2 1.9 0 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1281.0 13.7 0 9 -4 0.5 1.8 0 -9 -4 3.6 1.9 0 10 -4 58.5 3.2 0 -10 -4 55.7 3.5 1 0 -4 0.4 1.3 1 1 -4 387.2 5.5 1 -1 -4 365.8 5.5 1 2 -4 514.7 6.3 1 -2 -4 461.5 6.4 1 3 -4 1317.4 10.3 1 -3 -4 1196.6 10.7 1 4 -4 4.3 1.4 1 -4 -4 3.1 1.6 1 5 -4 654.8 8.0 1 -5 -4 624.5 8.5 1 6 -4 223.6 5.1 1 -6 -4 199.3 5.3 1 7 -4 1.4 1.8 1 -7 -4 1.9 1.8 1 8 -4 29.6 2.3 1 -8 -4 26.4 2.3 1 9 -4 55.7 3.1 1 -9 -4 62.1 3.4 1 10 -4 6.4 2.0 1 -10 -4 8.7 2.2 2 0 -4 64.7 2.4 2 1 -4 299.4 4.8 2 -1 -4 279.3 4.9 2 2 -4 3214.9 15.8 2 -2 -4 2934.2 15.8 2 3 -4 1.8 1.5 2 -3 -4 2.0 1.6 2 4 -4 8.8 1.4 2 -4 -4 6.1 1.3 2 5 -4 239.5 4.9 2 -5 -4 216.4 5.1 2 6 -4 1222.4 11.4 2 -6 -4 1111.1 11.8 2 7 -4 1.0 1.8 2 -7 -4 2.3 1.8 2 8 -4 36.3 2.4 2 -8 -4 26.1 2.3 2 9 -4 152.5 4.8 2 -9 -4 146.6 5.2 2 10 -4 380.1 7.6 2 -10 -4 407.5 8.4 3 0 -4 0.8 1.2 3 1 -4 1062.2 9.1 3 -1 -4 951.9 8.7 3 2 -4 163.5 3.8 3 -2 -4 161.5 4.0 3 3 -4 64.5 2.5 3 -3 -4 74.6 2.9 3 4 -4 4.9 1.5 3 -4 -4 3.7 1.7 3 5 -4 122.9 3.7 3 -5 -4 107.8 3.6 3 6 -4 82.4 3.2 3 -6 -4 88.7 3.5 3 7 -4 727.8 9.3 3 -7 -4 673.2 9.8 3 8 -4 7.0 1.9 3 -8 -4 6.9 2.2 3 9 -4 66.3 3.3 3 -9 -4 72.4 3.9 4 0 -4 130.2 3.4 4 1 -4 6.5 1.1 4 -1 -4 4.1 1.5 4 2 -4 3.9 1.3 4 -2 -4 4.1 1.5 4 3 -4 13.2 1.4 4 -3 -4 13.1 1.5 4 4 -4 3359.9 17.9 4 -4 -4 2888.6 17.7 4 5 -4 70.0 2.9 4 -5 -4 56.2 2.8 4 6 -4 14.9 1.6 4 -6 -4 13.5 1.7 4 7 -4 0.7 1.8 4 -7 -4 4.0 2.0 4 8 -4 143.7 4.7 4 -8 -4 134.4 4.7 4 9 -4 -0.1 1.6 4 -9 -4 1.8 1.9 5 0 -4 -0.2 1.3 5 1 -4 618.2 7.4 5 -1 -4 627.3 7.5 5 2 -4 416.3 6.1 5 -2 -4 412.7 6.2 5 3 -4 127.2 3.6 5 -3 -4 152.8 4.1 5 4 -4 6.5 1.8 5 -4 -4 2.5 1.7 5 5 -4 95.1 3.4 5 -5 -4 98.1 3.8 5 6 -4 137.7 4.3 5 -6 -4 144.5 4.4 5 7 -4 237.9 5.9 5 -7 -4 246.1 6.0 5 8 -4 27.7 2.4 5 -8 -4 28.0 2.2 5 9 -4 52.3 3.0 5 -9 -4 52.2 3.2 6 0 -4 40.9 2.2 6 1 -4 266.7 5.0 6 -1 -4 232.7 4.8 6 2 -4 1067.1 10.0 6 -2 -4 1033.0 10.0 6 3 -4 26.5 1.9 6 -3 -4 30.3 2.1 6 4 -4 59.2 2.7 6 -4 -4 52.6 2.6 6 5 -4 44.1 2.4 6 -5 -4 45.9 2.5 6 6 -4 652.3 9.2 6 -6 -4 688.3 9.4 6 7 -4 38.4 2.7 6 -7 -4 34.5 2.5 6 8 -4 1.3 1.8 6 -8 -4 2.6 1.9 7 0 -4 0.9 1.2 7 1 -4 77.7 2.9 7 -1 -4 77.4 3.0 7 2 -4 17.3 1.6 7 -2 -4 19.5 1.6 7 3 -4 499.7 7.5 7 -3 -4 493.3 7.2 7 4 -4 0.8 1.5 7 -4 -4 0.2 1.5 7 5 -4 221.5 5.3 7 -5 -4 233.6 5.6 7 6 -4 2.8 1.8 7 -6 -4 3.5 1.8 7 7 -4 14.1 1.8 7 -7 -4 18.5 1.9 8 0 -4 1987.7 14.3 8 1 -4 145.2 4.0 8 -1 -4 146.2 3.9 8 2 -4 29.7 2.0 8 -2 -4 24.0 1.8 8 3 -4 6.7 1.5 8 -3 -4 5.8 1.6 8 4 -4 187.3 5.1 8 -4 -4 174.3 4.6 8 5 -4 0.2 1.5 8 -5 -4 1.7 1.7 8 6 -4 14.1 2.0 8 -6 -4 13.7 1.7 9 0 -4 0.3 1.3 9 1 -4 60.3 2.8 9 -1 -4 69.2 2.9 9 2 -4 167.1 4.4 9 -2 -4 144.6 4.0 9 3 -4 136.1 4.3 9 -3 -4 130.6 4.0 9 4 -4 -0.2 1.5 9 -4 -4 0.7 1.6 9 5 -4 81.0 3.5 9 -5 -4 77.1 3.2 10 0 -4 124.4 3.8 10 1 -4 0.4 1.4 10 -1 -4 2.7 1.3 10 2 -4 473.1 7.6 10 -2 -4 431.6 6.9 10 3 -4 38.0 2.6 10 -3 -4 36.5 2.3 0 0 -5 -0.2 1.4 0 1 -5 361.4 5.7 0 -1 -5 384.4 6.0 0 2 -5 1.3 1.3 0 -2 -5 7.2 1.3 0 3 -5 448.4 6.4 0 -3 -5 371.5 6.5 0 4 -5 1.8 1.4 0 -4 -5 0.8 1.7 0 5 -5 37.4 2.3 0 -5 -5 38.3 2.4 0 6 -5 2.8 1.6 0 -6 -5 -0.2 1.7 0 7 -5 163.6 4.5 0 -7 -5 134.2 4.4 0 8 -5 0.0 1.7 0 -8 -5 -0.7 1.9 0 9 -5 81.3 3.7 0 -9 -5 53.9 3.1 1 0 -5 150.0 3.7 1 1 -5 335.2 5.4 1 -1 -5 313.8 5.4 1 2 -5 3.1 1.5 1 -2 -5 1.7 1.7 1 3 -5 1162.5 10.2 1 -3 -5 1033.9 10.3 1 4 -5 236.4 4.9 1 -4 -5 210.2 5.0 1 5 -5 1179.5 11.0 1 -5 -5 1163.5 11.6 1 6 -5 1.8 1.8 1 -6 -5 3.8 1.9 1 7 -5 198.7 5.0 1 -7 -5 162.6 4.8 1 8 -5 17.1 1.9 1 -8 -5 15.2 2.0 1 9 -5 22.3 2.2 1 -9 -5 19.7 2.1 2 0 -5 5.0 1.5 2 1 -5 1.9 1.4 2 -1 -5 3.0 1.4 2 2 -5 346.9 5.6 2 -2 -5 333.3 5.7 2 3 -5 16.8 1.6 2 -3 -5 16.9 1.7 2 4 -5 29.2 1.9 2 -4 -5 32.2 2.1 2 5 -5 2.5 1.6 2 -5 -5 2.7 1.8 2 6 -5 62.8 2.9 2 -6 -5 54.7 2.9 2 7 -5 0.8 1.7 2 -7 -5 -0.6 2.0 2 8 -5 24.0 2.1 2 -8 -5 18.1 2.3 2 9 -5 -0.9 1.8 2 -9 -5 0.6 1.8 3 0 -5 344.9 5.7 3 1 -5 821.4 8.4 3 -1 -5 763.4 8.4 3 2 -5 5.5 1.2 3 -2 -5 8.8 1.5 3 3 -5 228.2 4.7 3 -3 -5 229.4 5.2 3 4 -5 140.1 3.9 3 -4 -5 149.1 4.2 3 5 -5 120.3 3.7 3 -5 -5 72.5 3.2 3 6 -5 13.9 1.6 3 -6 -5 15.1 1.7 3 7 -5 244.3 5.8 3 -7 -5 232.5 6.0 3 8 -5 53.6 3.0 3 -8 -5 42.7 2.8 3 9 -5 288.2 6.7 3 -9 -5 233.5 6.2 4 0 -5 -1.0 1.3 4 1 -5 149.7 3.8 4 -1 -5 135.0 3.7 4 2 -5 45.3 2.2 4 -2 -5 52.5 2.5 4 3 -5 307.3 5.7 4 -3 -5 322.1 5.9 4 4 -5 3.9 1.6 4 -4 -5 -0.1 1.7 4 5 -5 67.8 3.0 4 -5 -5 59.4 3.0 4 6 -5 8.2 1.4 4 -6 -5 13.4 1.7 4 7 -5 88.7 3.5 4 -7 -5 84.0 3.6 4 8 -5 1.3 1.8 4 -8 -5 1.9 1.7 5 0 -5 15.5 1.5 5 1 -5 742.6 8.4 5 -1 -5 674.7 8.2 5 2 -5 36.3 2.2 5 -2 -5 32.0 2.0 5 3 -5 74.1 2.9 5 -3 -5 76.2 3.1 5 4 -5 86.5 3.2 5 -4 -5 96.3 3.6 5 5 -5 3.1 1.6 5 -5 -5 2.6 1.6 5 6 -5 34.4 2.4 5 -6 -5 30.3 2.3 5 7 -5 252.8 5.8 5 -7 -5 219.0 5.6 5 8 -5 5.0 1.8 5 -8 -5 2.2 1.6 6 0 -5 2.6 1.2 6 1 -5 12.2 1.4 6 -1 -5 8.7 1.3 6 2 -5 127.4 3.7 6 -2 -5 130.1 3.8 6 3 -5 11.7 1.5 6 -3 -5 14.7 1.6 6 4 -5 17.2 1.7 6 -4 -5 16.5 1.7 6 5 -5 2.4 1.6 6 -5 -5 1.5 1.6 6 6 -5 26.3 2.1 6 -6 -5 27.9 2.1 6 7 -5 24.1 2.3 6 -7 -5 24.2 2.1 7 0 -5 24.6 1.9 7 1 -5 187.1 4.6 7 -1 -5 175.7 4.4 7 2 -5 23.2 1.8 7 -2 -5 22.6 1.8 7 3 -5 275.5 5.7 7 -3 -5 300.0 5.9 7 4 -5 265.0 5.7 7 -4 -5 273.2 5.8 7 5 -5 274.5 5.9 7 -5 -5 263.5 5.8 7 6 -5 40.4 2.7 7 -6 -5 41.8 2.6 8 0 -5 0.0 1.4 8 1 -5 79.0 3.1 8 -1 -5 67.6 3.0 8 2 -5 68.1 3.0 8 -2 -5 62.5 2.8 8 3 -5 68.7 3.0 8 -3 -5 69.3 3.0 8 4 -5 6.3 1.6 8 -4 -5 1.8 1.5 8 5 -5 10.9 1.7 8 -5 -5 12.2 1.7 9 0 -5 20.8 1.8 9 1 -5 42.4 2.4 9 -1 -5 38.2 2.3 9 2 -5 24.8 1.9 9 -2 -5 23.0 1.8 9 3 -5 313.2 6.3 9 -3 -5 315.8 6.3 0 0 -6 629.7 7.9 0 1 -6 1.8 1.5 0 -1 -6 -1.5 1.7 0 2 -6 1280.0 11.1 0 -2 -6 1166.6 11.1 0 3 -6 1.0 1.4 0 -3 -6 -0.3 1.7 0 4 -6 336.4 5.9 0 -4 -6 260.5 5.6 0 5 -6 -0.5 1.5 0 -5 -6 -0.6 1.7 0 6 -6 628.9 8.6 0 -6 -6 568.9 8.8 0 7 -6 0.1 1.7 0 -7 -6 0.5 1.8 0 8 -6 153.8 4.7 0 -8 -6 125.7 4.4 1 0 -6 -1.2 1.4 1 1 -6 583.1 7.5 1 -1 -6 555.2 7.5 1 2 -6 265.2 5.3 1 -2 -6 251.1 5.2 1 3 -6 51.7 2.5 1 -3 -6 51.3 2.6 1 4 -6 3.4 1.5 1 -4 -6 1.9 1.8 1 5 -6 131.9 3.9 1 -5 -6 110.9 4.0 1 6 -6 51.0 2.6 1 -6 -6 45.9 2.8 1 7 -6 280.1 6.0 1 -7 -6 265.4 6.3 1 8 -6 0.2 1.9 1 -8 -6 4.0 2.0 2 0 -6 1398.2 11.6 2 1 -6 18.9 1.7 2 -1 -6 20.0 1.8 2 2 -6 10.3 1.4 2 -2 -6 8.3 1.6 2 3 -6 39.4 2.2 2 -3 -6 37.9 2.4 2 4 -6 898.6 9.7 2 -4 -6 852.3 10.0 2 5 -6 231.1 5.2 2 -5 -6 222.1 5.3 2 6 -6 9.8 1.4 2 -6 -6 9.5 1.7 2 7 -6 -0.6 1.7 2 -7 -6 0.9 1.9 2 8 -6 443.0 7.7 2 -8 -6 406.2 7.7 3 0 -6 0.0 1.4 3 1 -6 99.1 3.3 3 -1 -6 96.8 3.4 3 2 -6 102.8 3.3 3 -2 -6 89.4 3.3 3 3 -6 667.5 8.2 3 -3 -6 646.2 8.5 3 4 -6 1.5 1.6 3 -4 -6 2.5 1.7 3 5 -6 198.2 4.8 3 -5 -6 180.6 4.9 3 6 -6 19.1 1.9 3 -6 -6 16.3 1.8 3 7 -6 3.1 1.7 3 -7 -6 -0.1 1.8 4 0 -6 212.1 4.8 4 1 -6 -1.2 1.4 4 -1 -6 3.8 1.6 4 2 -6 1209.8 11.0 4 -2 -6 1099.2 10.8 4 3 -6 31.2 2.1 4 -3 -6 31.4 2.2 4 4 -6 398.4 6.6 4 -4 -6 402.4 7.0 4 5 -6 30.2 2.2 4 -5 -6 28.6 2.3 4 6 -6 643.2 8.9 4 -6 -6 603.9 9.1 4 7 -6 3.0 1.7 4 -7 -6 5.3 1.8 5 0 -6 -0.5 1.3 5 1 -6 103.1 3.5 5 -1 -6 93.2 3.3 5 2 -6 248.0 5.1 5 -2 -6 206.0 4.9 5 3 -6 298.7 5.7 5 -3 -6 292.6 5.8 5 4 -6 8.6 1.4 5 -4 -6 7.1 1.7 5 5 -6 152.2 4.3 5 -5 -6 153.1 4.6 5 6 -6 65.3 3.0 5 -6 -6 60.9 3.0 6 0 -6 534.5 7.6 6 1 -6 68.0 2.8 6 -1 -6 67.7 2.8 6 2 -6 16.0 1.6 6 -2 -6 15.9 1.7 6 3 -6 1.9 1.4 6 -3 -6 0.1 1.5 6 4 -6 786.3 9.5 6 -4 -6 797.4 9.7 6 5 -6 29.1 2.2 6 -5 -6 26.7 2.1 7 0 -6 -0.6 1.4 7 1 -6 229.8 5.2 7 -1 -6 216.1 5.1 7 2 -6 7.1 1.3 7 -2 -6 5.4 1.4 7 3 -6 4.6 1.4 7 -3 -6 1.1 1.5 7 4 -6 3.3 1.6 7 -4 -6 3.7 1.6 8 0 -6 158.1 4.4 8 1 -6 36.4 2.2 8 -1 -6 30.7 2.2 8 2 -6 408.2 7.2 8 -2 -6 366.1 6.6 0 0 -7 1.9 1.6 0 1 -7 54.9 2.6 0 -1 -7 54.4 2.7 0 2 -7 2.0 1.4 0 -2 -7 4.7 1.6 0 3 -7 182.5 4.6 0 -3 -7 146.7 4.3 0 4 -7 -0.4 1.6 0 -4 -7 0.0 1.6 0 5 -7 95.9 3.6 0 -5 -7 76.0 3.3 0 6 -7 -0.2 1.6 0 -6 -7 0.0 1.6 1 0 -7 217.9 5.0 1 1 -7 44.6 2.4 1 -1 -7 42.5 2.5 1 2 -7 3.8 1.7 1 -2 -7 3.4 1.7 1 3 -7 343.6 6.2 1 -3 -7 303.7 6.3 1 4 -7 15.8 1.7 1 -4 -7 11.5 1.6 1 5 -7 460.7 7.4 1 -5 -7 392.6 7.4 1 6 -7 3.2 1.7 1 -6 -7 1.0 1.7 2 0 -7 1.3 1.5 2 1 -7 6.2 1.6 2 -1 -7 3.6 1.8 2 2 -7 104.0 3.5 2 -2 -7 99.1 3.5 2 3 -7 0.0 1.3 2 -3 -7 -1.7 1.6 2 4 -7 1.2 1.6 2 -4 -7 -1.5 1.9 2 5 -7 1.5 1.4 2 -5 -7 3.1 1.7 2 6 -7 82.2 3.4 2 -6 -7 60.4 3.1 3 0 -7 212.2 5.0 3 1 -7 516.2 7.6 3 -1 -7 495.3 7.5 3 2 -7 49.7 2.5 3 -2 -7 41.5 2.4 3 3 -7 202.9 4.9 3 -3 -7 171.4 4.7 3 4 -7 40.1 2.3 3 -4 -7 38.6 2.5 3 5 -7 83.3 3.3 3 -5 -7 69.0 3.1 3 6 -7 4.4 1.7 3 -6 -7 3.2 1.7 4 0 -7 -0.6 1.6 4 1 -7 80.5 3.2 4 -1 -7 72.5 3.0 4 2 -7 15.9 1.7 4 -2 -7 14.1 1.7 4 3 -7 64.6 3.0 4 -3 -7 56.6 2.8 4 4 -7 0.1 1.5 4 -4 -7 3.0 1.7 4 5 -7 37.3 2.5 4 -5 -7 37.7 2.4 5 0 -7 4.6 1.5 5 1 -7 584.4 8.3 5 -1 -7 538.0 7.9 5 2 -7 -0.2 1.4 5 -2 -7 -0.3 1.5 5 3 -7 125.9 4.0 5 -3 -7 106.1 3.7 5 4 -7 46.0 2.5 5 -4 -7 46.2 2.6 6 0 -7 -0.1 1.4 6 1 -7 0.2 1.4 6 -1 -7 0.1 1.4 6 2 -7 54.3 2.7 6 -2 -7 49.6 2.7 6 3 -7 15.2 1.6 6 -3 -7 12.7 1.7 0 0 -8 1584.8 13.8 0 1 -8 -0.9 1.6 0 -1 -8 2.4 1.6 0 2 -8 9.2 1.5 0 -2 -8 8.5 1.7 0 3 -8 0.3 1.4 0 -3 -8 -0.5 1.7 0 4 -8 129.9 4.1 0 -4 -8 119.1 4.1 1 0 -8 0.0 1.7 1 1 -8 72.6 3.2 1 -1 -8 65.1 3.0 1 2 -8 88.6 3.5 1 -2 -8 79.4 3.5 1 3 -8 272.3 5.8 1 -3 -8 232.0 5.9 2 0 -8 15.9 1.8 2 1 -8 28.0 2.1 2 -1 -8 27.0 2.1 2 2 -8 606.7 8.6 2 -2 -8 561.1 8.6 2 3 -8 5.6 1.8 2 -3 -8 7.0 1.8 3 0 -8 1.1 1.5 3 1 -8 198.2 5.0 3 -1 -8 192.1 5.1 3 2 -8 37.2 2.3 3 -2 -8 32.2 2.4 4 0 -8 73.1 3.4 4 1 -8 0.6 1.4 4 -1 -8 2.5 1.5 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5286(5) _cell_length_b 8.3203(5) _cell_length_c 6.0570(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 429.81(4) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.709 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_T_max 0.118 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 946 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.49 _reflns_number_total 491 _reflns_number_gt 427 _reflns_threshold_expression >2\s(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+2.2763P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.023(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 491 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.368 _refine_ls_restrained_S_all 1.368 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.2525(2) 0.0280(5) Uani 1 2 d S . . Zn2 Zn 0.13608(13) 0.63474(15) 0.0000 0.0232(5) Uani 1 2 d S . . As1 As 0.24360(11) 0.25075(13) 0.0000 0.0200(4) Uani 1 2 d S . . O1 O 0.3597(6) 0.2695(6) 0.2230(9) 0.0269(12) Uani 1 1 d . . . O2 O 0.1441(9) 0.0749(10) 0.0000 0.0254(17) Uani 1 2 d S . . O3 O 0.1058(9) 0.3947(10) 0.0000 0.0308(18) Uani 1 2 d S . . O4 O 0.3715(9) 0.6081(10) 0.0000 0.0245(15) Uani 1 2 d S . . H1 H 0.4405 0.6684 0.0000 0.029 Uiso 1 2 d SR . . 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 Zn1 0.0295(7) 0.0325(10) 0.0221(7) 0.000 0.000 -0.0076(5) Zn2 0.0247(7) 0.0197(8) 0.0251(6) 0.000 0.000 0.0008(5) As1 0.0207(6) 0.0177(7) 0.0215(6) 0.000 0.000 -0.0006(4) O1 0.035(3) 0.022(3) 0.024(2) 0.006(2) -0.008(2) -0.006(2) O2 0.030(4) 0.022(4) 0.024(3) 0.000 0.000 -0.006(3) O3 0.027(4) 0.018(4) 0.048(5) 0.000 0.000 -0.003(3) O4 0.029(4) 0.021(4) 0.023(3) 0.000 0.000 -0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O2 2.058(5) 5 ? Zn1 O2 2.058(5) . ? Zn1 O4 2.063(5) 3_545 ? Zn1 O4 2.063(5) 7_566 ? Zn1 O1 2.265(5) 4_455 ? Zn1 O1 2.265(5) 3_545 ? Zn1 Zn1 2.998(2) 5_556 ? Zn2 O3 2.014(8) . ? Zn2 O1 2.018(5) 3 ? Zn2 O1 2.018(5) 8_665 ? Zn2 O4 2.020(8) . ? Zn2 O3 2.077(8) 5_565 ? Zn2 Zn2 3.227(2) 5_565 ? As1 O3 1.678(8) . ? As1 O1 1.682(5) . ? As1 O1 1.682(5) 6 ? As1 O2 1.692(8) . ? O1 Zn2 2.018(5) 3_545 ? O1 Zn1 2.265(5) 3 ? O2 Zn1 2.058(5) 5 ? O2 O2 2.755(15) 5 ? O2 O4 3.0440(12) 3_544 ? O3 Zn2 2.077(8) 5_565 ? O3 O3 2.516(16) 5_565 ? O4 Zn1 2.063(5) 3 ? O4 Zn1 2.063(5) 7_665 ? O4 O4 2.835(15) 5_665 ? O4 H1 0.7734 . ? 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 Zn1 O2 84.0(3) 5 . ? O2 Zn1 O4 171.4(3) 5 3_545 ? O2 Zn1 O4 95.2(2) . 3_545 ? O2 Zn1 O4 95.2(2) 5 7_566 ? O2 Zn1 O4 171.4(3) . 7_566 ? O4 Zn1 O4 86.8(3) 3_545 7_566 ? O2 Zn1 O1 89.4(3) 5 4_455 ? O2 Zn1 O1 96.2(3) . 4_455 ? O4 Zn1 O1 82.2(3) 3_545 4_455 ? O4 Zn1 O1 92.3(2) 7_566 4_455 ? O2 Zn1 O1 96.2(3) 5 3_545 ? O2 Zn1 O1 89.4(3) . 3_545 ? O4 Zn1 O1 92.3(2) 3_545 3_545 ? O4 Zn1 O1 82.2(3) 7_566 3_545 ? O1 Zn1 O1 172.5(3) 4_455 3_545 ? O2 Zn1 Zn1 137.99(15) 5 5_556 ? O2 Zn1 Zn1 137.99(15) . 5_556 ? O4 Zn1 Zn1 43.40(16) 3_545 5_556 ? O4 Zn1 Zn1 43.40(16) 7_566 5_556 ? O1 Zn1 Zn1 86.24(14) 4_455 5_556 ? O1 Zn1 Zn1 86.24(14) 3_545 5_556 ? O3 Zn2 O1 123.59(16) . 3 ? O3 Zn2 O1 123.59(16) . 8_665 ? O1 Zn2 O1 112.5(3) 3 8_665 ? O3 Zn2 O4 91.1(3) . . ? O1 Zn2 O4 92.5(2) 3 . ? O1 Zn2 O4 92.5(2) 8_665 . ? O3 Zn2 O3 75.9(4) . 5_565 ? O1 Zn2 O3 94.8(2) 3 5_565 ? O1 Zn2 O3 94.8(2) 8_665 5_565 ? O4 Zn2 O3 166.9(3) . 5_565 ? O3 Zn2 Zn2 38.6(2) . 5_565 ? O1 Zn2 Zn2 113.50(16) 3 5_565 ? O1 Zn2 Zn2 113.50(16) 8_665 5_565 ? O4 Zn2 Zn2 129.7(2) . 5_565 ? O3 Zn2 Zn2 37.2(2) 5_565 5_565 ? O3 As1 O1 110.3(2) . . ? O3 As1 O1 110.3(2) . 6 ? O1 As1 O1 106.8(4) . 6 ? O3 As1 O2 105.4(4) . . ? O1 As1 O2 112.1(2) . . ? O1 As1 O2 112.1(2) 6 . ? As1 O1 Zn2 128.8(3) . 3_545 ? As1 O1 Zn1 116.2(3) . 3 ? Zn2 O1 Zn1 114.0(2) 3_545 3 ? As1 O2 Zn1 124.1(3) . 5 ? As1 O2 Zn1 124.1(3) . . ? Zn1 O2 Zn1 96.0(3) 5 . ? As1 O2 O2 147.0(6) . 5 ? Zn1 O2 O2 47.99(15) 5 5 ? Zn1 O2 O2 47.99(15) . 5 ? As1 O2 O4 86.8(2) . 3_544 ? Zn1 O2 O4 42.45(14) 5 3_544 ? Zn1 O2 O4 137.8(3) . 3_544 ? O2 O2 O4 90.1(2) 5 3_544 ? As1 O3 Zn2 128.2(4) . . ? As1 O3 Zn2 127.7(4) . 5_565 ? Zn2 O3 Zn2 104.1(4) . 5_565 ? As1 O3 O3 178.6(6) . 5_565 ? Zn2 O3 O3 53.2(3) . 5_565 ? Zn2 O3 O3 50.9(3) 5_565 5_565 ? Zn2 O4 Zn1 125.2(2) . 3 ? Zn2 O4 Zn1 125.2(2) . 7_665 ? Zn1 O4 Zn1 93.2(3) 3 7_665 ? Zn2 O4 O4 146.9(5) . 5_665 ? Zn1 O4 O4 46.60(15) 3 5_665 ? Zn1 O4 O4 46.60(15) 7_665 5_665 ? Zn2 O4 H1 133.2 . . ? Zn1 O4 H1 83.1 3 . ? Zn1 O4 H1 83.1 7_665 . ? O4 O4 H1 79.9 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 0.77 2.23 2.849(8) 136.9 5_665 O4 H1 O1 0.77 2.23 2.849(8) 136.9 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.027 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.238 _iucr_refine_instructions_details ; TITL ADA_100C Pnnm ba-c CELL 0.71073 8.5286 8.3203 6.0570 90.000 90.000 90.000 ZERR 4 0.0005 0.0005 0.0003 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 BOND $H L.S. 4 LIST 4 FMAP 2 PLAN 35 WGHT 0.032800 2.276300 EXTI 0.023371 FVAR 0.43214 ZN1 4 0.000000 0.000000 0.252505 10.50000 0.02945 0.03253 = 0.02213 0.00000 0.00000 -0.00759 ZN2 4 0.136084 0.634738 0.000000 10.50000 0.02470 0.01971 = 0.02513 0.00000 0.00000 0.00084 AS1 2 0.243600 0.250745 0.000000 10.50000 0.02069 0.01772 = 0.02153 0.00000 0.00000 -0.00063 O1 3 0.359720 0.269495 0.222997 11.00000 0.03471 0.02203 = 0.02394 0.00636 -0.00763 -0.00629 O2 3 0.144065 0.074879 0.000000 10.50000 0.03021 0.02194 = 0.02399 0.00000 0.00000 -0.00601 O3 3 0.105793 0.394677 0.000000 10.50000 0.02653 0.01752 = 0.04822 0.00000 0.00000 -0.00307 O4 3 0.371524 0.608078 0.000000 10.50000 0.02896 0.02149 = 0.02312 0.00000 0.00000 -0.00278 AFIX 3 H1 1 0.440499 0.668426 0.000000 10.50000 -1.20000 REM jog 25c Pnnm ba-c REM R1 = 0.0419 for 612 Fo > 4sig(Fo) and 0.0456 for all 686 data REM 47 parameters refined using 0 restraints HKLF 4 REM ADA_100C Pnnm ba-c REM R1 = 0.0370 for 427 Fo > 4sig(Fo) and 0.0424 for all 491 data REM 46 parameters refined using 0 restraints END WGHT 0.0319 2.2968 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 4.2 0.9 0 -1 0 3.0 1.4 0 2 0 474.2 5.6 0 -2 0 475.9 5.4 0 3 0 -3.0 3.8 0 -3 0 -7.0 3.5 0 4 0 1222.5 10.9 0 -4 0 1351.3 11.3 0 5 0 -1.0 4.7 0 -5 0 -3.4 4.6 0 6 0 173.3 5.4 0 -6 0 228.2 5.8 0 7 0 1.4 4.9 0 -7 0 -2.2 5.0 0 8 0 2690.2 18.6 0 -8 0 3270.4 20.2 0 9 0 -1.0 4.2 0 -9 0 -14.3 4.6 0 10 0 121.8 4.7 0 -10 0 153.7 5.2 1 0 0 0.9 1.0 1 1 0 1184.2 5.8 1 -1 0 1047.7 5.8 1 2 0 1296.8 8.3 1 -2 0 1169.2 8.2 1 3 0 2750.3 13.8 1 -3 0 2623.0 14.0 1 4 0 24.0 2.9 1 -4 0 29.0 3.0 1 5 0 1442.8 12.6 1 -5 0 1603.6 13.2 1 6 0 476.2 8.1 1 -6 0 584.0 8.6 1 7 0 15.3 5.3 1 -7 0 6.0 5.1 1 8 0 55.2 4.1 1 -8 0 83.2 4.3 1 9 0 94.2 4.4 1 -9 0 118.9 4.9 1 10 0 8.4 3.8 1 -10 0 14.0 3.9 2 0 0 217.1 3.0 2 1 0 993.6 6.5 2 -1 0 881.7 6.4 2 2 0 5406.0 16.7 2 -2 0 4333.4 16.0 2 3 0 215.6 4.3 2 -3 0 221.9 4.6 2 4 0 14.1 3.6 2 -4 0 22.3 3.1 2 5 0 364.3 6.7 2 -5 0 418.1 7.3 2 6 0 2171.3 16.0 2 -6 0 2448.5 17.2 2 7 0 11.2 5.0 2 -7 0 -2.5 5.3 2 8 0 63.0 4.2 2 -8 0 90.5 4.6 2 9 0 282.5 6.7 2 -9 0 372.6 7.6 2 10 0 531.3 9.1 2 -10 0 717.5 10.4 3 0 0 -6.1 2.6 3 1 0 2848.5 12.3 3 -1 0 1883.3 10.1 3 2 0 387.2 5.1 3 -2 0 342.4 5.2 3 3 0 205.0 4.3 3 -3 0 192.1 4.5 3 4 0 9.1 4.3 3 -4 0 18.9 4.7 3 5 0 189.3 5.5 3 -5 0 179.5 5.5 3 6 0 171.0 5.6 3 -6 0 190.0 5.9 3 7 0 1258.9 13.0 3 -7 0 1470.9 14.2 3 8 0 15.1 4.9 3 -8 0 17.1 3.6 3 9 0 99.7 4.5 3 -9 0 139.1 5.1 3 10 0 10.2 3.8 3 -10 0 11.7 3.9 4 0 0 84.3 3.3 4 1 0 49.0 2.5 4 -1 0 44.9 2.4 4 2 0 37.1 2.5 4 -2 0 38.8 2.6 4 3 0 19.8 2.6 4 -3 0 20.6 2.6 4 4 0 5387.7 21.8 4 -4 0 4523.4 21.3 4 5 0 128.0 4.8 4 -5 0 122.2 4.9 4 6 0 13.9 5.0 4 -6 0 6.3 4.7 4 7 0 -3.5 4.9 4 -7 0 9.0 4.9 4 8 0 175.3 5.7 4 -8 0 229.2 6.4 4 9 0 -3.3 3.9 4 -9 0 -1.8 4.0 5 0 0 0.5 3.0 5 1 0 1398.9 10.5 5 -1 0 1247.4 9.7 5 2 0 1002.6 9.2 5 -2 0 931.1 9.1 5 3 0 266.1 5.4 5 -3 0 256.7 5.5 5 4 0 24.1 3.2 5 -4 0 24.5 3.5 5 5 0 168.1 5.2 5 -5 0 149.6 5.3 5 6 0 281.2 6.4 5 -6 0 293.5 6.9 5 7 0 393.2 7.6 5 -7 0 422.7 8.3 5 8 0 64.0 4.4 5 -8 0 73.9 4.5 5 9 0 76.3 4.2 5 -9 0 104.3 4.8 6 0 0 129.5 3.8 6 1 0 635.4 7.6 6 -1 0 583.3 7.2 6 2 0 2043.1 13.8 6 -2 0 1748.1 12.8 6 3 0 118.1 4.3 6 -3 0 117.0 4.5 6 4 0 85.3 4.1 6 -4 0 87.9 4.2 6 5 0 71.0 3.8 6 -5 0 76.3 4.2 6 6 0 1144.8 11.9 6 -6 0 1006.8 11.8 6 7 0 78.4 4.3 6 -7 0 81.4 4.6 6 8 0 1.2 4.5 6 -8 0 -1.3 4.6 7 0 0 1.0 3.8 7 1 0 170.5 4.8 7 -1 0 161.3 4.6 7 2 0 41.5 3.3 7 -2 0 38.0 3.4 7 3 0 880.5 9.9 7 -3 0 771.4 9.4 7 4 0 12.1 4.2 7 -4 0 -0.2 4.3 7 5 0 398.5 7.1 7 -5 0 380.3 7.3 7 6 0 10.4 4.2 7 -6 0 4.7 4.5 7 7 0 31.1 3.6 7 -7 0 29.3 3.5 8 0 0 3074.8 17.0 8 1 0 326.6 6.0 8 -1 0 309.3 5.9 8 2 0 66.1 3.5 8 -2 0 61.8 3.4 8 3 0 10.2 2.6 8 -3 0 12.1 3.9 8 4 0 284.9 6.1 8 -4 0 248.7 5.9 8 5 0 4.5 3.8 8 -5 0 -1.9 4.2 8 6 0 34.1 3.3 8 -6 0 32.4 3.6 9 0 0 -4.8 3.7 9 1 0 107.8 4.0 9 -1 0 93.4 3.8 9 2 0 269.8 5.7 9 -2 0 237.4 5.4 9 3 0 207.8 5.2 9 -3 0 168.5 4.8 9 4 0 -2.8 3.6 9 -4 0 0.9 3.6 9 5 0 108.5 4.3 9 -5 0 103.9 4.4 10 0 0 191.9 4.9 10 1 0 9.2 3.4 10 -1 0 3.9 3.6 10 2 0 702.7 8.9 10 -2 0 636.7 8.6 10 3 0 57.6 3.5 10 -3 0 44.9 3.3 0 0 -1 28.7 1.3 0 1 -1 1524.8 7.3 0 -1 -1 1571.5 7.0 0 2 -1 17.1 3.3 0 -2 -1 13.0 2.7 0 3 -1 1789.8 11.6 0 -3 -1 1757.4 10.7 0 4 -1 13.9 4.4 0 -4 -1 5.6 3.8 0 5 -1 340.7 6.7 0 -5 -1 330.0 6.3 0 6 -1 5.4 5.3 0 -6 -1 3.6 4.7 0 7 -1 415.9 8.1 0 -7 -1 479.9 8.1 0 8 -1 -8.5 4.9 0 -8 -1 2.2 4.3 0 9 -1 95.6 4.6 0 -9 -1 127.1 4.8 0 10 -1 7.6 3.7 0 -10 -1 5.3 3.6 1 0 -1 1272.6 6.1 1 1 -1 855.1 6.3 1 -1 -1 850.2 5.9 1 2 -1 19.9 3.5 1 -2 -1 23.8 3.0 1 3 -1 2530.4 14.2 1 -3 -1 2493.0 13.6 1 4 -1 553.7 7.7 1 -4 -1 595.1 7.7 1 5 -1 2781.3 17.3 1 -5 -1 3114.7 18.0 1 6 -1 2.7 5.4 1 -6 -1 8.0 5.2 1 7 -1 333.3 7.3 1 -7 -1 425.5 7.8 1 8 -1 75.7 4.4 1 -8 -1 92.6 4.5 1 9 -1 33.7 3.7 1 -9 -1 33.6 4.0 1 10 -1 21.4 3.5 1 -10 -1 22.8 3.0 2 0 -1 -0.4 3.6 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83.6 4.2 3 -3 -4 71.0 3.6 3 4 -4 -1.9 4.8 3 -4 -4 -4.2 4.4 3 5 -4 123.5 5.1 3 -5 -4 102.1 4.4 3 6 -4 102.3 5.0 3 -6 -4 80.1 4.2 3 7 -4 723.3 11.2 3 -7 -4 630.1 9.5 3 8 -4 10.1 4.6 3 -8 -4 1.2 4.5 4 0 -4 155.4 4.3 4 1 -4 5.5 4.1 4 -1 -4 13.1 4.0 4 2 -4 -2.4 4.3 4 -2 -4 4.3 4.2 4 3 -4 9.5 4.5 4 -3 -4 14.5 3.1 4 4 -4 3074.8 19.0 4 -4 -4 2661.6 17.2 4 5 -4 67.9 4.1 4 -5 -4 68.8 4.0 4 6 -4 33.7 3.6 4 -6 -4 13.2 4.6 4 7 -4 1.1 4.4 4 -7 -4 4.5 4.4 5 0 -4 3.3 3.8 5 1 -4 549.0 7.6 5 -1 -4 518.6 7.4 5 2 -4 432.1 7.0 5 -2 -4 382.3 6.8 5 3 -4 154.7 5.1 5 -3 -4 119.4 4.5 5 4 -4 2.4 5.1 5 -4 -4 5.8 4.4 5 5 -4 83.2 4.7 5 -5 -4 88.1 4.5 5 6 -4 124.4 5.2 5 -6 -4 138.9 5.2 5 7 -4 199.0 6.2 5 -7 -4 241.2 6.5 6 0 -4 35.8 2.8 6 1 -4 249.2 5.4 6 -1 -4 222.2 5.4 6 2 -4 1051.1 11.6 6 -2 -4 943.3 10.9 6 3 -4 28.7 4.7 6 -3 -4 29.4 4.1 6 4 -4 51.2 4.8 6 -4 -4 64.3 4.1 6 5 -4 39.7 4.2 6 -5 -4 44.7 3.7 6 6 -4 545.2 9.4 6 -6 -4 645.6 10.0 7 0 -4 -8.6 3.3 7 1 -4 65.0 3.9 7 -1 -4 66.9 3.8 7 2 -4 15.5 5.1 7 -2 -4 24.5 3.5 7 3 -4 394.2 8.4 7 -3 -4 428.3 8.5 7 4 -4 1.1 4.6 7 -4 -4 -3.3 4.5 7 5 -4 175.9 6.0 7 -5 -4 219.7 6.4 8 0 -4 1589.3 13.7 8 1 -4 145.6 5.5 8 -1 -4 154.6 5.9 8 2 -4 22.6 3.7 8 -2 -4 31.1 3.8 8 3 -4 4.7 4.4 8 -3 -4 -2.3 5.0 8 4 -4 139.5 5.4 8 -4 -4 184.5 6.3 9 0 -4 1.6 3.1 9 1 -4 52.2 3.4 9 -1 -4 49.9 3.7 0 0 -5 8.8 3.9 0 1 -5 318.3 5.9 0 -1 -5 311.8 5.9 0 2 -5 4.5 3.9 0 -2 -5 11.4 3.7 0 3 -5 339.9 6.3 0 -3 -5 329.1 6.2 0 4 -5 3.3 4.0 0 -4 -5 -0.5 3.7 0 5 -5 47.5 3.5 0 -5 -5 41.1 3.3 0 6 -5 -5.1 4.0 0 -6 -5 5.4 3.7 0 7 -5 187.1 5.6 0 -7 -5 146.2 4.9 1 0 -5 127.0 4.2 1 1 -5 286.5 5.6 1 -1 -5 282.4 5.6 1 2 -5 6.2 3.8 1 -2 -5 4.9 3.8 1 3 -5 1028.8 10.3 1 -3 -5 1004.6 10.3 1 4 -5 241.6 5.8 1 -4 -5 198.8 5.1 1 5 -5 1423.4 13.2 1 -5 -5 1072.5 11.3 1 6 -5 4.1 4.2 1 -6 -5 4.9 3.8 1 7 -5 223.2 6.1 1 -7 -5 175.1 5.4 2 0 -5 -2.6 3.7 2 1 -5 3.0 4.0 2 -1 -5 1.9 3.9 2 2 -5 281.8 5.6 2 -2 -5 284.6 5.8 2 3 -5 14.7 4.4 2 -3 -5 12.1 3.6 2 4 -5 41.5 3.4 2 -4 -5 22.6 2.9 2 5 -5 4.5 4.4 2 -5 -5 3.2 4.0 2 6 -5 64.3 4.1 2 -6 -5 55.0 3.6 2 7 -5 2.4 4.3 2 -7 -5 0.2 4.0 3 0 -5 281.7 5.5 3 1 -5 652.1 8.0 3 -1 -5 640.6 7.9 3 2 -5 8.5 3.6 3 -2 -5 5.9 3.8 3 3 -5 221.1 5.2 3 -3 -5 193.3 5.0 3 4 -5 150.4 4.9 3 -4 -5 136.3 4.6 3 5 -5 100.7 4.3 3 -5 -5 72.2 3.7 3 6 -5 1.3 4.4 3 -6 -5 19.3 3.1 3 7 -5 270.7 6.7 3 -7 -5 227.4 6.0 4 0 -5 -5.6 3.7 4 1 -5 119.7 4.1 4 -1 -5 115.1 4.0 4 2 -5 40.3 3.0 4 -2 -5 38.1 3.1 4 3 -5 316.4 6.2 4 -3 -5 249.0 5.6 4 4 -5 -0.2 4.1 4 -4 -5 -2.1 3.9 4 5 -5 69.4 3.9 4 -5 -5 54.6 3.5 4 6 -5 10.9 4.4 4 -6 -5 2.3 4.1 5 0 -5 5.5 3.6 5 1 -5 613.5 8.0 5 -1 -5 598.2 8.0 5 2 -5 40.8 3.0 5 -2 -5 31.5 3.0 5 3 -5 83.0 4.0 5 -3 -5 78.7 3.9 5 4 -5 102.5 4.4 5 -4 -5 82.2 4.0 5 5 -5 1.6 4.2 5 -5 -5 6.0 4.0 5 6 -5 32.2 3.7 5 -6 -5 45.3 3.8 6 0 -5 -2.8 3.0 6 1 -5 3.2 3.3 6 -1 -5 7.3 3.3 6 2 -5 126.6 4.3 6 -2 -5 100.9 4.0 6 3 -5 12.7 2.6 6 -3 -5 1.4 3.8 6 4 -5 13.1 4.0 6 -4 -5 7.7 3.8 6 5 -5 -7.7 4.1 6 -5 -5 3.6 3.9 7 0 -5 17.2 2.4 7 1 -5 162.6 4.6 7 -1 -5 146.3 4.4 7 2 -5 26.1 2.9 7 -2 -5 19.0 2.7 7 3 -5 284.0 6.5 7 -3 -5 244.4 5.9 8 0 -5 2.2 3.0 8 1 -5 68.6 3.5 8 -1 -5 55.6 3.3 0 0 -6 488.5 7.2 0 1 -6 -0.2 3.6 0 -1 -6 -4.3 3.6 0 2 -6 969.5 10.2 0 -2 -6 1015.3 10.6 0 3 -6 2.7 3.6 0 -3 -6 3.6 3.5 0 4 -6 269.7 5.9 0 -4 -6 234.3 5.5 0 5 -6 0.8 3.6 0 -5 -6 -1.4 3.7 0 6 -6 681.2 9.7 0 -6 -6 567.2 8.8 1 0 -6 3.6 3.7 1 1 -6 444.1 7.1 1 -1 -6 456.3 7.1 1 2 -6 204.9 5.1 1 -2 -6 199.6 5.1 1 3 -6 47.1 3.3 1 -3 -6 41.0 3.1 1 4 -6 0.6 3.7 1 -4 -6 5.1 3.5 1 5 -6 117.4 4.5 1 -5 -6 106.8 4.3 1 6 -6 57.4 3.9 1 -6 -6 44.6 3.5 2 0 -6 1198.2 11.1 2 1 -6 26.1 2.7 2 -1 -6 12.3 3.7 2 2 -6 9.3 3.6 2 -2 -6 8.7 3.5 2 3 -6 35.9 2.9 2 -3 -6 30.9 2.8 2 4 -6 833.9 9.8 2 -4 -6 696.0 8.9 2 5 -6 242.1 5.8 2 -5 -6 198.1 5.3 2 6 -6 25.7 3.1 2 -6 -6 12.9 3.8 3 0 -6 2.6 3.4 3 1 -6 83.8 3.6 3 -1 -6 78.3 3.6 3 2 -6 82.3 3.7 3 -2 -6 75.5 3.5 3 3 -6 533.5 7.7 3 -3 -6 515.5 7.7 3 4 -6 0.1 3.7 3 -4 -6 -4.4 3.7 3 5 -6 196.9 5.4 3 -5 -6 133.8 4.5 4 0 -6 160.2 4.6 4 1 -6 2.5 3.5 4 -1 -6 0.6 3.6 4 2 -6 898.3 9.9 4 -2 -6 894.8 10.1 4 3 -6 32.0 2.9 4 -3 -6 26.6 2.8 4 4 -6 408.4 7.4 4 -4 -6 326.4 6.4 4 5 -6 38.3 3.6 4 -5 -6 20.1 3.0 5 0 -6 -5.8 3.1 5 1 -6 77.7 3.4 5 -1 -6 74.6 3.4 5 2 -6 169.8 4.6 5 -2 -6 168.8 4.7 5 3 -6 250.3 5.6 5 -3 -6 193.1 5.1 5 4 -6 9.2 3.7 5 -4 -6 2.7 3.6 6 0 -6 387.2 6.7 6 1 -6 54.0 3.1 6 -1 -6 57.7 3.1 6 2 -6 11.0 3.4 6 -2 -6 18.2 2.4 0 0 -7 1.1 3.4 0 1 -7 44.1 3.2 0 -1 -7 48.2 3.4 0 2 -7 -3.9 3.3 0 -2 -7 4.4 3.3 0 3 -7 119.3 4.3 0 -3 -7 115.6 4.3 0 4 -7 1.7 3.5 0 -4 -7 5.9 3.0 1 0 -7 147.0 4.5 1 1 -7 31.3 2.9 1 -1 -7 32.9 2.7 1 2 -7 3.5 3.3 1 -2 -7 -0.8 3.3 1 3 -7 246.1 5.6 1 -3 -7 236.5 5.5 2 0 -7 0.6 3.3 2 1 -7 1.6 3.4 2 -1 -7 0.3 3.4 2 2 -7 80.9 3.6 2 -2 -7 73.1 3.5 2 3 -7 -6.2 3.5 2 -3 -7 5.2 3.3 3 0 -7 155.7 4.6 3 1 -7 353.4 6.5 3 -1 -7 368.4 6.5 3 2 -7 34.1 3.0 3 -2 -7 32.6 3.0 4 0 -7 3.8 3.0 4 1 -7 53.7 3.5 4 -1 -7 60.7 3.3 0 0 0 0.0 0.0 0 0 0 0.0 0.0 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5369(4) _cell_length_b 8.3356(4) _cell_length_c 6.0589(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 431.15(4) _cell_formula_units_Z 4 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.651 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_T_max 0.114 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 951 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.53 _reflns_number_total 494 _reflns_number_gt 424 _reflns_threshold_expression >2\s(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.1260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.022(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 494 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.25284(19) 0.0324(4) Uani 1 2 d S . . Zn2 Zn 0.13629(12) 0.63429(15) 0.0000 0.0259(4) Uani 1 2 d S . . As1 As 0.24302(10) 0.25063(12) 0.0000 0.0214(4) Uani 1 2 d S . . O1 O 0.3585(6) 0.2686(6) 0.2236(8) 0.0297(11) Uani 1 1 d . . . O2 O 0.1438(8) 0.0767(9) 0.0000 0.0267(16) Uani 1 2 d S . . O3 O 0.1054(8) 0.3935(9) 0.0000 0.0330(17) Uani 1 2 d S . . O4 O 0.3723(8) 0.6076(9) 0.0000 0.0263(14) Uani 1 2 d S . . H1 H 0.4588 0.6487 0.0000 0.032 Uiso 1 2 d SR . . 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 Zn1 0.0341(6) 0.0395(9) 0.0236(6) 0.000 0.000 -0.0101(5) Zn2 0.0267(6) 0.0233(7) 0.0278(6) 0.000 0.000 0.0007(5) As1 0.0216(5) 0.0191(7) 0.0235(5) 0.000 0.000 -0.0009(3) O1 0.039(2) 0.023(3) 0.027(2) 0.005(2) -0.008(2) -0.006(2) O2 0.033(4) 0.023(4) 0.024(3) 0.000 0.000 -0.006(3) O3 0.028(3) 0.019(4) 0.052(4) 0.000 0.000 -0.001(3) O4 0.029(3) 0.025(4) 0.025(3) 0.000 0.000 0.000(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O4 2.058(5) 3_545 ? Zn1 O4 2.058(5) 7_566 ? Zn1 O2 2.065(5) 5 ? Zn1 O2 2.065(5) . ? Zn1 O1 2.280(5) 4_455 ? Zn1 O1 2.280(5) 3_545 ? Zn1 Zn1 2.995(2) 5_556 ? Zn2 O1 2.015(5) 3 ? Zn2 O1 2.015(5) 8_665 ? Zn2 O3 2.025(8) . ? Zn2 O4 2.027(7) . ? Zn2 O3 2.076(7) 5_565 ? Zn2 Zn2 3.229(2) 5_565 ? As1 O3 1.673(8) . ? As1 O2 1.679(7) . ? As1 O1 1.682(5) . ? As1 O1 1.682(5) 6 ? O1 Zn2 2.015(5) 3_545 ? O1 Zn1 2.280(5) 3 ? O2 Zn1 2.065(5) 5 ? O2 O2 2.769(14) 5 ? O2 O4 3.0435(11) 3_544 ? O3 Zn2 2.076(7) 5_565 ? O3 O3 2.529(15) 5_565 ? O4 Zn1 2.058(5) 3 ? O4 Zn1 2.058(5) 7_665 ? O4 O4 2.823(14) 5_665 ? O4 H1 0.8136 . ? 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 O4 Zn1 O4 86.6(3) 3_545 7_566 ? O4 Zn1 O2 171.8(3) 3_545 5 ? O4 Zn1 O2 95.16(19) 7_566 5 ? O4 Zn1 O2 95.16(19) 3_545 . ? O4 Zn1 O2 171.8(3) 7_566 . ? O2 Zn1 O2 84.2(3) 5 . ? O4 Zn1 O1 82.3(2) 3_545 4_455 ? O4 Zn1 O1 92.4(2) 7_566 4_455 ? O2 Zn1 O1 89.6(2) 5 4_455 ? O2 Zn1 O1 95.7(2) . 4_455 ? O4 Zn1 O1 92.4(2) 3_545 3_545 ? O4 Zn1 O1 82.3(2) 7_566 3_545 ? O2 Zn1 O1 95.7(2) 5 3_545 ? O2 Zn1 O1 89.6(2) . 3_545 ? O1 Zn1 O1 172.8(3) 4_455 3_545 ? O4 Zn1 Zn1 43.31(14) 3_545 5_556 ? O4 Zn1 Zn1 43.31(14) 7_566 5_556 ? O2 Zn1 Zn1 137.90(14) 5 5_556 ? O2 Zn1 Zn1 137.90(14) . 5_556 ? O1 Zn1 Zn1 86.42(13) 4_455 5_556 ? O1 Zn1 Zn1 86.42(13) 3_545 5_556 ? O1 Zn2 O1 112.4(3) 3 8_665 ? O1 Zn2 O3 123.63(15) 3 . ? O1 Zn2 O3 123.63(15) 8_665 . ? O1 Zn2 O4 92.23(19) 3 . ? O1 Zn2 O4 92.23(19) 8_665 . ? O3 Zn2 O4 91.2(3) . . ? O1 Zn2 O3 94.82(19) 3 5_565 ? O1 Zn2 O3 94.82(19) 8_665 5_565 ? O3 Zn2 O3 76.1(3) . 5_565 ? O4 Zn2 O3 167.3(3) . 5_565 ? O1 Zn2 Zn2 113.66(15) 3 5_565 ? O1 Zn2 Zn2 113.66(15) 8_665 5_565 ? O3 Zn2 Zn2 38.6(2) . 5_565 ? O4 Zn2 Zn2 129.8(2) . 5_565 ? O3 Zn2 Zn2 37.5(2) 5_565 5_565 ? O3 As1 O2 105.1(3) . . ? O3 As1 O1 110.4(2) . . ? O2 As1 O1 111.9(2) . . ? O3 As1 O1 110.4(2) . 6 ? O2 As1 O1 111.9(2) . 6 ? O1 As1 O1 107.3(3) . 6 ? As1 O1 Zn2 129.3(3) . 3_545 ? As1 O1 Zn1 115.9(2) . 3 ? Zn2 O1 Zn1 114.0(2) 3_545 3 ? As1 O2 Zn1 124.6(2) . 5 ? As1 O2 Zn1 124.6(2) . . ? Zn1 O2 Zn1 95.8(3) 5 . ? As1 O2 O2 147.8(6) . 5 ? Zn1 O2 O2 47.90(14) 5 5 ? Zn1 O2 O2 47.90(14) . 5 ? As1 O2 O4 87.1(2) . 3_544 ? Zn1 O2 O4 42.33(13) 5 3_544 ? Zn1 O2 O4 137.5(3) . 3_544 ? O2 O2 O4 89.9(2) 5 3_544 ? As1 O3 Zn2 127.9(4) . . ? As1 O3 Zn2 128.2(4) . 5_565 ? Zn2 O3 Zn2 103.9(3) . 5_565 ? As1 O3 O3 179.2(6) . 5_565 ? Zn2 O3 O3 52.9(3) . 5_565 ? Zn2 O3 O3 51.0(2) 5_565 5_565 ? Zn2 O4 Zn1 125.1(2) . 3 ? Zn2 O4 Zn1 125.1(2) . 7_665 ? Zn1 O4 Zn1 93.4(3) 3 7_665 ? Zn2 O4 O4 146.9(5) . 5_665 ? Zn1 O4 O4 46.69(14) 3 5_665 ? Zn1 O4 O4 46.69(14) 7_665 5_665 ? Zn2 O4 H1 148.8 . . ? Zn1 O4 H1 72.7 3 . ? Zn1 O4 H1 72.7 7_665 . ? O4 O4 H1 64.3 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 0.81 2.18 2.861(8) 141.5 5_665 O4 H1 O1 0.81 2.18 2.861(8) 141.5 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.53 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.734 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.196 _iucr_refine_instructions_details ; TITL ADA_200C Pnnm ba-c CELL 0.71073 8.5369 8.3356 6.0589 90.000 90.000 90.000 ZERR 4 0.0004 0.0004 0.0003 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 BOND $H L.S. 4 LIST 4 FMAP 2 PLAN 35 WGHT 0.027700 2.126000 EXTI 0.022398 FVAR 0.42718 ZN1 4 0.000000 0.000000 0.252840 10.50000 0.03413 0.03947 = 0.02356 0.00000 0.00000 -0.01007 ZN2 4 0.136293 0.634293 0.000000 10.50000 0.02672 0.02330 = 0.02776 0.00000 0.00000 0.00067 AS1 2 0.243023 0.250628 0.000000 10.50000 0.02161 0.01911 = 0.02348 0.00000 0.00000 -0.00089 O1 3 0.358474 0.268603 0.223631 11.00000 0.03890 0.02328 = 0.02692 0.00501 -0.00819 -0.00639 O2 3 0.143803 0.076739 0.000000 10.50000 0.03320 0.02308 = 0.02378 0.00000 0.00000 -0.00589 O3 3 0.105414 0.393472 0.000000 10.50000 0.02838 0.01866 = 0.05205 0.00000 0.00000 -0.00138 O4 3 0.372306 0.607600 0.000000 10.50000 0.02855 0.02522 = 0.02525 0.00000 0.00000 0.00021 AFIX 3 H1 1 0.458760 0.648680 0.000000 10.50000 -1.20000 HKLF 4 REM ADA_200C Pnnm ba-c REM R1 = 0.0352 for 424 Fo > 4sig(Fo) and 0.0410 for all 494 data REM 46 parameters refined using 0 restraints END WGHT 0.0253 2.2970 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 4.0 1.5 0 -1 0 3.7 1.5 0 2 0 476.6 5.5 0 -2 0 484.2 5.5 0 3 0 0.7 3.8 0 -3 0 -7.6 3.6 0 4 0 1161.5 10.6 0 -4 0 1263.8 10.8 0 5 0 -7.1 4.8 0 -5 0 -3.8 4.6 0 6 0 207.7 5.7 0 -6 0 257.7 6.1 0 7 0 4.0 5.0 0 -7 0 -0.4 5.0 0 8 0 2454.3 17.6 0 -8 0 2977.9 19.3 0 9 0 -2.4 4.4 0 -9 0 -6.1 4.4 0 10 0 121.6 4.8 0 -10 0 158.8 5.2 1 0 0 2.5 1.0 1 1 0 1197.0 5.7 1 -1 0 1076.0 5.9 1 2 0 1729.5 9.3 1 -2 0 1151.6 8.2 1 3 0 2705.8 13.6 1 -3 0 2499.4 13.7 1 4 0 28.5 4.0 1 -4 0 30.3 3.1 1 5 0 1296.1 12.0 1 -5 0 1483.6 12.9 1 6 0 441.8 7.6 1 -6 0 551.5 8.5 1 7 0 2.1 5.1 1 -7 0 0.9 5.2 1 8 0 44.3 4.0 1 -8 0 57.0 4.1 1 9 0 61.8 4.0 1 -9 0 79.6 4.3 1 10 0 11.2 3.7 1 -10 0 9.8 3.9 2 0 0 217.2 3.0 2 1 0 942.3 6.2 2 -1 0 838.2 6.1 2 2 0 5210.4 16.2 2 -2 0 4433.9 16.2 2 3 0 182.4 4.0 2 -3 0 183.0 4.3 2 4 0 21.8 2.7 2 -4 0 37.0 3.2 2 5 0 326.8 6.4 2 -5 0 374.8 7.1 2 6 0 1983.0 15.4 2 -6 0 2295.3 16.9 2 7 0 2.1 5.0 2 -7 0 5.9 5.1 2 8 0 73.6 4.1 2 -8 0 100.8 4.7 2 9 0 244.0 6.4 2 -9 0 321.3 7.0 2 10 0 430.6 8.2 2 -10 0 569.8 9.6 3 0 0 -1.9 2.4 3 1 0 2087.2 10.5 3 -1 0 1849.2 9.9 3 2 0 358.9 4.8 3 -2 0 331.4 5.0 3 3 0 180.9 4.1 3 -3 0 167.0 4.3 3 4 0 14.2 3.4 3 -4 0 12.0 4.6 3 5 0 152.5 4.9 3 -5 0 155.5 5.3 3 6 0 171.5 5.5 3 -6 0 177.5 5.8 3 7 0 1035.9 11.9 3 -7 0 1292.7 13.5 3 8 0 4.2 4.6 3 -8 0 5.9 4.8 3 9 0 74.3 4.1 3 -9 0 102.5 4.6 3 10 0 2.3 3.7 3 -10 0 7.1 3.8 4 0 0 78.4 3.1 4 1 0 48.0 2.4 4 -1 0 38.1 2.2 4 2 0 26.3 2.3 4 -2 0 26.4 2.3 4 3 0 18.2 2.4 4 -3 0 16.7 2.7 4 4 0 4893.6 20.5 4 -4 0 4267.2 20.6 4 5 0 135.5 4.7 4 -5 0 137.2 5.1 4 6 0 15.8 5.0 4 -6 0 4.6 5.6 4 7 0 1.7 4.5 4 -7 0 9.7 5.0 4 8 0 147.2 5.6 4 -8 0 183.2 6.0 4 9 0 1.8 3.9 4 -9 0 -4.2 4.2 5 0 0 5.0 2.8 5 1 0 1255.8 9.8 5 -1 0 1187.1 9.4 5 2 0 950.9 8.8 5 -2 0 871.7 8.7 5 3 0 234.6 5.0 5 -3 0 221.7 5.3 5 4 0 29.1 3.3 5 -4 0 26.4 3.5 5 5 0 131.3 4.6 5 -5 0 124.6 5.0 5 6 0 242.9 5.9 5 -6 0 248.1 6.5 5 7 0 313.0 7.0 5 -7 0 353.5 7.6 5 8 0 52.8 3.9 5 -8 0 64.2 4.2 5 9 0 56.5 3.9 5 -9 0 69.4 4.2 6 0 0 111.9 3.6 6 1 0 586.4 7.2 6 -1 0 547.8 6.8 6 2 0 1878.3 12.9 6 -2 0 1671.8 12.4 6 3 0 122.8 4.3 6 -3 0 115.8 4.5 6 4 0 97.9 4.1 6 -4 0 98.8 4.3 6 5 0 60.9 3.7 6 -5 0 63.2 4.0 6 6 0 915.2 10.7 6 -6 0 871.7 10.9 6 7 0 82.3 4.4 6 -7 0 80.9 4.6 6 8 0 18.2 4.3 6 -8 0 8.5 4.7 7 0 0 3.0 3.8 7 1 0 124.0 4.2 7 -1 0 130.4 4.1 7 2 0 37.0 4.0 7 -2 0 39.1 3.3 7 3 0 756.5 9.0 7 -3 0 662.1 8.6 7 4 0 9.1 4.1 7 -4 0 7.1 4.2 7 5 0 333.6 6.5 7 -5 0 314.6 6.7 7 6 0 -3.8 4.1 7 -6 0 -1.7 4.6 7 7 0 32.5 4.2 7 -7 0 31.1 3.6 8 0 0 2895.8 16.6 8 1 0 328.6 5.9 8 -1 0 328.5 6.0 8 2 0 60.1 3.5 8 -2 0 53.0 3.4 8 3 0 10.8 3.6 8 -3 0 8.2 3.9 8 4 0 240.4 5.7 8 -4 0 220.5 5.5 8 5 0 -1.0 4.0 8 -5 0 11.4 4.1 8 6 0 48.4 3.6 8 -6 0 46.1 4.2 9 0 0 -8.8 3.9 9 1 0 80.2 3.7 9 -1 0 80.7 3.7 9 2 0 228.0 5.5 9 -2 0 204.1 5.2 9 3 0 162.7 4.8 9 -3 0 134.7 4.4 9 4 0 0.7 3.6 9 -4 0 -3.5 3.8 9 5 0 78.1 4.1 9 -5 0 74.0 4.0 10 0 0 190.2 5.0 10 1 0 4.9 3.2 10 -1 0 3.7 3.5 10 2 0 589.5 8.3 10 -2 0 547.1 8.0 10 3 0 61.0 3.6 10 -3 0 49.5 3.3 0 0 -1 29.0 1.3 0 1 -1 1520.9 7.2 0 -1 -1 1521.2 6.8 0 2 -1 20.5 3.1 0 -2 -1 20.3 2.3 0 3 -1 1695.9 11.2 0 -3 -1 1671.4 10.4 0 4 -1 5.0 4.5 0 -4 -1 0.9 3.8 0 5 -1 355.6 6.9 0 -5 -1 327.3 6.4 0 6 -1 3.6 5.2 0 -6 -1 5.6 4.8 0 7 -1 393.2 7.9 0 -7 -1 443.2 7.7 0 8 -1 6.2 4.7 0 -8 -1 -5.5 4.6 0 9 -1 83.3 4.4 0 -9 -1 106.2 4.6 0 10 -1 -4.3 3.9 0 -10 -1 4.8 3.5 1 0 -1 1279.5 6.1 1 1 -1 840.5 6.3 1 -1 -1 836.1 5.8 1 2 -1 28.7 3.4 1 -2 -1 10.6 3.3 1 3 -1 2532.8 14.3 1 -3 -1 2518.9 13.7 1 4 -1 540.5 7.8 1 -4 -1 578.9 7.6 1 5 -1 2681.2 16.9 1 -5 -1 2965.1 17.5 1 6 -1 -3.9 5.3 1 -6 -1 2.9 5.2 1 7 -1 308.7 6.9 1 -7 -1 400.3 7.5 1 8 -1 58.7 4.2 1 -8 -1 86.8 4.3 1 9 -1 29.9 3.4 1 -9 -1 43.9 3.7 1 10 -1 9.2 4.0 1 -10 -1 20.6 3.2 2 0 -1 0.7 3.4 2 1 -1 42.7 4.6 2 -1 -1 41.1 4.2 2 2 -1 832.5 8.5 2 -2 -1 865.1 8.6 2 3 -1 39.3 4.0 2 -3 -1 47.8 4.0 2 4 -1 50.5 3.7 2 -4 -1 60.2 3.7 2 5 -1 -6.8 5.1 2 -5 -1 8.3 5.0 2 6 -1 187.5 5.8 2 -6 -1 225.8 6.0 2 7 -1 5.7 5.0 2 -7 -1 8.7 5.0 2 8 -1 71.5 4.3 2 -8 -1 92.7 4.5 2 9 -1 -1.6 4.2 2 -9 -1 1.0 4.2 2 10 -1 32.4 3.5 2 -10 -1 43.5 3.4 3 0 -1 1684.0 9.3 3 1 -1 2325.1 11.8 3 -1 -1 2126.7 12.4 3 2 -1 34.4 3.4 3 -2 -1 25.1 3.4 3 3 -1 836.7 9.0 3 -3 -1 821.4 9.2 3 4 -1 406.3 7.0 3 -4 -1 464.8 7.6 3 5 -1 201.3 5.9 3 -5 -1 255.9 6.4 3 6 -1 7.2 5.3 3 -6 -1 6.6 5.5 3 7 -1 535.6 8.9 3 -7 -1 653.8 9.5 3 8 -1 115.4 4.9 3 -8 -1 144.3 5.3 3 9 -1 473.4 8.7 3 -9 -1 639.6 9.6 4 0 -1 0.1 3.1 4 1 -1 699.8 7.1 4 -1 -1 635.1 7.1 4 2 -1 198.4 4.4 4 -2 -1 203.9 4.9 4 3 -1 788.3 8.7 4 -3 -1 769.2 9.1 4 4 -1 11.9 4.5 4 -4 -1 11.2 5.3 4 5 -1 207.1 6.1 4 -5 -1 252.7 6.7 4 6 -1 31.0 4.0 4 -6 -1 33.7 4.2 4 7 -1 235.6 6.4 4 -7 -1 306.0 7.1 4 8 -1 -10.4 4.7 4 -8 -1 11.6 4.5 4 9 -1 35.6 4.2 4 -9 -1 54.6 3.8 5 0 -1 60.9 2.9 5 1 -1 2185.7 13.1 5 -1 -1 1990.2 12.5 5 2 -1 58.4 3.1 5 -2 -1 71.4 3.7 5 3 -1 240.7 5.2 5 -3 -1 246.1 5.8 5 4 -1 287.2 6.2 5 -4 -1 271.5 6.5 5 5 -1 20.6 3.6 5 -5 -1 18.4 6.0 5 6 -1 30.9 3.6 5 -6 -1 35.6 4.1 5 7 -1 494.9 9.0 5 -7 -1 608.6 9.6 5 8 -1 4.1 4.6 5 -8 -1 1.3 4.7 5 9 -1 482.6 8.6 5 -9 -1 669.6 10.2 6 0 -1 0.7 3.5 6 1 -1 7.8 4.0 6 -1 -1 5.3 3.9 6 2 -1 290.8 5.6 6 -2 -1 259.8 5.7 6 3 -1 40.5 3.4 6 -3 -1 43.5 3.7 6 4 -1 23.2 3.4 6 -4 -1 21.8 4.8 6 5 -1 -0.7 4.4 6 -5 -1 -3.3 5.1 6 6 -1 72.1 4.3 6 -6 -1 76.6 4.6 6 7 -1 35.9 3.8 6 -7 -1 49.6 4.2 6 8 -1 24.2 4.3 6 -8 -1 28.1 3.9 7 0 -1 137.4 4.2 7 1 -1 369.4 6.3 7 -1 -1 366.2 6.3 7 2 -1 45.9 3.3 7 -2 -1 44.5 3.3 7 3 -1 504.5 7.5 7 -3 -1 429.0 7.3 7 4 -1 441.4 7.3 7 -4 -1 374.8 6.9 7 5 -1 432.1 7.7 7 -5 -1 380.5 7.4 7 6 -1 68.3 4.1 7 -6 -1 72.3 4.2 7 7 -1 176.2 5.8 7 -7 -1 183.5 5.8 8 0 -1 1.6 3.5 8 1 -1 140.0 4.3 8 -1 -1 137.5 4.3 8 2 -1 148.7 4.6 8 -2 -1 132.0 4.2 8 3 -1 137.7 4.5 8 -3 -1 118.6 4.5 8 4 -1 -1.0 4.1 8 -4 -1 -0.5 4.2 8 5 -1 46.6 3.4 8 -5 -1 40.1 3.5 8 6 -1 27.6 3.5 8 -6 -1 30.7 4.1 9 0 -1 76.2 3.6 9 1 -1 32.0 2.9 9 -1 -1 37.3 2.9 9 2 -1 46.2 3.3 9 -2 -1 41.2 3.3 9 3 -1 496.9 7.7 9 -3 -1 411.3 7.0 9 4 -1 10.9 2.9 9 -4 -1 2.8 4.3 9 5 -1 524.4 8.4 9 -5 -1 455.2 7.9 10 0 -1 -0.8 3.0 10 1 -1 10.6 3.1 10 -1 -1 2.5 3.5 10 2 -1 37.7 3.0 10 -2 -1 35.8 2.8 10 3 -1 28.3 2.9 10 -3 -1 28.4 3.0 0 0 -2 2617.2 10.7 0 1 -2 -4.3 2.4 0 -1 -2 -3.4 2.4 0 2 -2 2966.4 13.4 0 -2 -2 2856.5 12.6 0 3 -2 -3.8 3.3 0 -3 -2 -1.1 2.9 0 4 -2 2068.0 13.9 0 -4 -2 2023.9 12.8 0 5 -2 1.8 4.9 0 -5 -2 -3.1 4.1 0 6 -2 1569.2 14.3 0 -6 -2 1557.9 13.2 0 7 -2 0.2 5.2 0 -7 -2 -12.1 4.6 0 8 -2 361.7 7.8 0 -8 -2 384.9 7.4 0 9 -2 -3.8 4.2 0 -9 -2 -5.0 4.1 0 10 -2 462.4 8.6 0 -10 -2 537.2 8.8 1 0 -2 1.2 2.5 1 1 -2 2424.2 11.2 1 -1 -2 2400.2 11.1 1 2 -2 1483.3 10.1 1 -2 -2 1338.4 9.0 1 3 -2 136.6 4.0 1 -3 -2 136.2 3.7 1 4 -2 14.3 4.6 1 -4 -2 12.3 4.0 1 5 -2 393.9 7.5 1 -5 -2 379.2 6.8 1 6 -2 124.8 5.3 1 -6 -2 126.1 4.9 1 7 -2 587.6 9.5 1 -7 -2 610.5 9.1 1 8 -2 4.6 4.7 1 -8 -2 1.4 4.6 1 9 -2 168.5 5.9 1 -9 -2 192.2 5.6 1 10 -2 43.2 3.7 1 -10 -2 66.1 3.8 2 0 -2 4331.7 59.0 2 1 -2 62.2 2.6 2 -1 -2 57.1 2.4 2 2 -2 51.1 3.6 2 -2 -2 36.9 3.1 2 3 -2 184.8 4.8 2 -3 -2 191.6 4.4 2 4 -2 2554.8 16.7 2 -4 -2 2526.4 15.7 2 5 -2 996.0 11.7 2 -5 -2 990.2 10.6 2 6 -2 27.1 4.1 2 -6 -2 35.6 4.7 2 7 -2 25.0 4.9 2 -7 -2 12.2 4.8 2 8 -2 807.2 11.0 2 -8 -2 1005.8 11.9 2 9 -2 92.5 4.6 2 -9 -2 124.2 4.8 3 0 -2 6.2 3.3 3 1 -2 444.9 6.6 3 -1 -2 411.3 5.8 3 2 -2 458.4 7.1 3 -2 -2 436.7 6.5 3 3 -2 2389.8 16.1 3 -3 -2 2332.6 15.2 3 4 -2 -7.6 5.2 3 -4 -2 4.2 4.9 3 5 -2 427.0 8.0 3 -5 -2 497.5 8.1 3 6 -2 25.4 3.7 3 -6 -2 42.9 4.1 3 7 -2 2.5 4.9 3 -7 -2 7.6 4.5 3 8 -2 11.1 4.8 3 -8 -2 14.4 4.5 3 9 -2 -1.9 4.4 3 -9 -2 12.3 4.1 4 0 -2 969.5 9.7 4 1 -2 0.0 5.3 4 -1 -2 5.2 5.5 4 2 -2 3835.4 20.6 4 -2 -2 4026.6 21.1 4 3 -2 179.2 5.6 4 -3 -2 212.8 5.9 4 4 -2 1544.9 14.1 4 -4 -2 1785.6 15.0 4 5 -2 101.7 5.2 4 -5 -2 127.3 5.2 4 6 -2 1376.5 13.7 4 -6 -2 1758.1 15.1 4 7 -2 11.9 4.8 4 -7 -2 14.7 5.0 4 8 -2 5.7 4.5 4 -8 -2 13.2 3.1 4 9 -2 1.0 4.3 4 -9 -2 9.1 4.0 5 0 -2 2.0 3.5 5 1 -2 290.3 5.6 5 -1 -2 296.4 6.4 5 2 -2 758.8 9.1 5 -2 -2 760.0 9.8 5 3 -2 772.9 10.0 5 -3 -2 805.6 10.6 5 4 -2 28.0 3.8 5 -4 -2 35.4 4.2 5 5 -2 335.0 7.2 5 -5 -2 446.9 8.4 5 6 -2 155.0 5.6 5 -6 -2 212.4 6.1 5 7 -2 26.6 4.5 5 -7 -2 29.4 3.7 5 8 -2 0.7 4.6 5 -8 -2 5.2 4.6 6 0 -2 1550.9 11.5 6 1 -2 135.3 4.3 6 -1 -2 115.5 4.3 6 2 -2 69.2 3.8 6 -2 -2 54.5 3.9 6 3 -2 10.7 5.0 6 -3 -2 11.5 5.4 6 4 -2 1842.5 15.2 6 -4 -2 1689.4 15.2 6 5 -2 72.0 4.6 6 -5 -2 81.0 4.6 6 6 -2 63.0 4.3 6 -6 -2 82.6 4.7 6 7 -2 1.9 4.6 6 -7 -2 0.0 4.7 6 8 -2 314.8 7.3 6 -8 -2 394.8 8.0 7 0 -2 -0.7 3.7 7 1 -2 590.8 7.8 7 -1 -2 542.8 7.6 7 2 -2 5.2 4.2 7 -2 -2 8.8 4.1 7 3 -2 -1.6 4.2 7 -3 -2 -3.9 4.4 7 4 -2 10.2 3.0 7 -4 -2 3.6 5.0 7 5 -2 97.6 4.7 7 -5 -2 85.9 4.7 7 6 -2 29.8 3.6 7 -6 -2 35.2 3.8 7 7 -2 258.7 6.7 7 -7 -2 334.8 7.5 8 0 -2 392.6 6.5 8 1 -2 92.1 3.8 8 -1 -2 95.7 4.0 8 2 -2 700.9 8.8 8 -2 -2 610.5 8.3 8 3 -2 6.8 3.8 8 -3 -2 6.8 4.2 8 4 -2 126.6 4.6 8 -4 -2 109.0 4.6 8 5 -2 23.8 3.4 8 -5 -2 21.0 3.3 8 6 -2 320.4 7.3 8 -6 -2 317.6 7.2 9 0 -2 -1.6 3.1 9 1 -2 167.7 4.7 9 -1 -2 153.9 4.6 9 2 -2 273.6 5.8 9 -2 -2 238.5 5.5 9 3 -2 68.2 3.6 9 -3 -2 50.9 3.3 9 4 -2 1.5 3.5 9 -4 -2 -4.4 3.8 9 -5 -2 37.7 3.8 10 0 -2 656.0 8.7 10 1 -2 11.1 2.5 10 -1 -2 11.0 3.1 10 2 -2 0.8 3.2 10 -2 -2 10.0 3.0 0 0 -3 2.7 2.6 0 1 -3 559.8 6.1 0 -1 -3 575.0 6.3 0 2 -3 0.9 3.1 0 -2 -3 3.2 2.9 0 3 -3 918.8 8.9 0 -3 -3 829.5 8.4 0 4 -3 1.3 4.3 0 -4 -3 -0.5 3.9 0 5 -3 367.1 6.9 0 -5 -3 293.1 6.0 0 6 -3 10.7 4.8 0 -6 -3 6.5 4.3 0 7 -3 362.0 7.6 0 -7 -3 303.2 6.5 0 8 -3 5.1 4.6 0 -8 -3 3.4 4.0 0 9 -3 32.4 3.7 0 -9 -3 31.5 3.1 1 0 -3 1116.6 8.5 1 1 -3 190.6 3.8 1 -1 -3 194.2 3.9 1 2 -3 26.2 3.0 1 -2 -3 20.1 2.9 1 3 -3 1482.1 11.6 1 -3 -3 1279.6 10.3 1 4 -3 174.9 5.1 1 -4 -3 150.9 4.5 1 5 -3 1797.2 14.5 1 -5 -3 1564.5 12.7 1 6 -3 -13.7 5.3 1 -6 -3 4.7 4.5 1 7 -3 205.3 6.2 1 -7 -3 190.8 5.5 1 8 -3 83.4 4.6 1 -8 -3 85.3 4.5 1 9 -3 25.1 3.5 1 -9 -3 21.4 3.3 2 0 -3 19.2 1.9 2 1 -3 13.9 2.6 2 -1 -3 18.3 2.8 2 2 -3 535.3 6.9 2 -2 -3 457.1 6.1 2 3 -3 7.1 4.1 2 -3 -3 7.0 3.4 2 4 -3 16.4 4.3 2 -4 -3 10.3 4.3 2 5 -3 9.8 5.2 2 -5 -3 1.4 4.6 2 6 -3 196.0 6.1 2 -6 -3 196.7 5.6 2 7 -3 7.5 5.2 2 -7 -3 0.0 4.8 2 8 -3 79.3 4.5 2 -8 -3 80.7 4.2 2 9 -3 -9.5 4.2 2 -9 -3 1.0 3.8 3 0 -3 1153.0 9.3 3 1 -3 1867.0 12.0 3 -1 -3 1820.7 12.0 3 2 -3 122.9 4.2 3 -2 -3 92.5 3.5 3 3 -3 703.9 8.9 3 -3 -3 611.0 7.8 3 4 -3 172.7 5.6 3 -4 -3 172.3 5.1 3 5 -3 214.3 6.4 3 -5 -3 211.7 5.8 3 6 -3 -0.3 5.3 3 -6 -3 3.0 4.7 3 7 -3 435.0 8.5 3 -7 -3 470.2 8.4 3 8 -3 79.1 4.7 3 -8 -3 103.1 5.0 3 9 -3 379.0 8.4 3 -9 -3 478.5 8.7 4 0 -3 7.1 3.8 4 1 -3 428.1 6.7 4 -1 -3 389.1 6.1 4 2 -3 102.5 4.6 4 -2 -3 86.3 3.9 4 3 -3 363.6 7.3 4 -3 -3 351.0 6.7 4 4 -3 7.0 5.7 4 -4 -3 11.1 5.1 4 5 -3 134.6 5.7 4 -5 -3 148.9 5.4 4 6 -3 21.9 3.5 4 -6 -3 27.7 3.7 4 7 -3 217.0 6.4 4 -7 -3 271.5 6.7 4 8 -3 -3.1 4.6 4 -8 -3 3.2 4.3 5 0 -3 32.9 2.9 5 1 -3 1734.7 13.8 5 -1 -3 1670.6 13.3 5 2 -3 15.5 5.9 5 -2 -3 4.0 5.5 5 3 -3 265.8 7.0 5 -3 -3 283.4 6.7 5 4 -3 147.7 5.8 5 -4 -3 172.0 5.8 5 5 -3 33.5 3.9 5 -5 -3 41.3 4.1 5 6 -3 18.9 5.1 5 -6 -3 12.9 5.0 5 7 -3 387.2 8.1 5 -7 -3 527.2 8.9 5 8 -3 -3.1 4.2 5 -8 -3 6.5 4.5 6 0 -3 6.5 4.6 6 1 -3 -4.7 5.9 6 -1 -3 4.6 6.2 6 2 -3 164.0 6.1 6 -2 -3 188.9 6.4 6 3 -3 35.5 4.2 6 -3 -3 31.1 4.1 6 4 -3 7.0 5.5 6 -4 -3 13.2 5.2 6 5 -3 -6.0 5.2 6 -5 -3 10.2 4.8 6 6 -3 61.6 4.3 6 -6 -3 83.8 4.6 6 7 -3 22.8 3.8 6 -7 -3 42.6 3.8 7 0 -3 163.8 4.5 7 1 -3 234.6 5.5 7 -1 -3 199.0 5.5 7 2 -3 11.6 4.1 7 -2 -3 17.2 5.3 7 3 -3 331.3 7.2 7 -3 -3 341.7 7.7 7 4 -3 203.3 6.2 7 -4 -3 235.6 6.6 7 5 -3 270.3 7.2 7 -5 -3 340.9 7.8 7 6 -3 33.0 3.9 7 -6 -3 50.3 4.1 8 0 -3 -0.2 3.2 8 1 -3 66.9 3.4 8 -1 -3 61.9 3.5 8 2 -3 82.6 3.8 8 -2 -3 74.5 3.9 8 3 -3 90.8 4.3 8 -3 -3 81.3 4.4 8 4 -3 0.9 4.0 8 -4 -3 4.3 4.2 8 5 -3 44.8 4.4 8 -5 -3 40.3 3.9 9 0 -3 70.3 3.3 9 1 -3 8.3 3.3 9 -1 -3 9.7 3.4 9 2 -3 33.4 3.0 9 -2 -3 27.0 2.9 9 3 -3 282.8 6.3 9 -3 -3 237.5 6.0 0 0 -4 7647.0 93.1 0 1 -4 3.5 3.5 0 -1 -4 7.7 3.4 0 2 -4 69.3 3.3 0 -2 -4 73.3 3.4 0 3 -4 -0.6 4.0 0 -3 -4 1.7 3.7 0 4 -4 583.4 8.0 0 -4 -4 505.7 7.3 0 5 -4 4.6 4.3 0 -5 -4 -3.6 4.1 0 6 -4 77.7 4.0 0 -6 -4 65.6 3.7 0 7 -4 2.7 4.3 0 -7 -4 0.8 4.0 0 8 -4 1599.5 15.3 0 -8 -4 1257.0 13.3 1 0 -4 2.1 3.1 1 1 -4 341.9 5.5 1 -1 -4 335.5 5.6 1 2 -4 397.2 6.1 1 -2 -4 412.2 6.3 1 3 -4 1216.5 10.9 1 -3 -4 1057.2 9.9 1 4 -4 12.1 4.5 1 -4 -4 -4.2 4.1 1 5 -4 614.6 8.7 1 -5 -4 489.8 7.6 1 6 -4 233.0 5.9 1 -6 -4 188.3 5.2 1 7 -4 -0.1 4.5 1 -7 -4 -1.5 4.2 1 8 -4 22.5 3.4 1 -8 -4 12.8 4.6 2 0 -4 59.7 3.0 2 1 -4 226.1 4.7 2 -1 -4 225.8 4.8 2 2 -4 2554.7 15.0 2 -2 -4 2388.4 14.4 2 3 -4 1.6 4.4 2 -3 -4 5.7 4.0 2 4 -4 12.7 4.8 2 -4 -4 15.4 3.6 2 5 -4 234.9 6.1 2 -5 -4 191.9 5.2 2 6 -4 1250.7 13.2 2 -6 -4 974.0 11.0 2 7 -4 -0.4 4.6 2 -7 -4 2.9 4.2 2 8 -4 45.9 4.0 2 -8 -4 46.9 3.8 3 0 -4 1.9 3.6 3 1 -4 885.0 8.9 3 -1 -4 867.9 9.1 3 2 -4 150.0 4.4 3 -2 -4 131.2 4.2 3 3 -4 87.1 4.8 3 -3 -4 63.9 3.5 3 4 -4 7.6 4.8 3 -4 -4 4.5 4.2 3 5 -4 95.1 4.6 3 -5 -4 79.7 4.0 3 6 -4 92.8 4.7 3 -6 -4 74.1 4.1 3 7 -4 611.9 10.1 3 -7 -4 518.7 8.8 3 8 -4 0.9 4.4 3 -8 -4 5.0 4.2 4 0 -4 132.1 4.2 4 1 -4 7.2 4.0 4 -1 -4 6.6 4.1 4 2 -4 9.2 4.1 4 -2 -4 7.8 4.2 4 3 -4 7.8 4.6 4 -3 -4 13.1 2.9 4 4 -4 2876.5 18.2 4 -4 -4 2422.5 16.4 4 5 -4 81.7 4.4 4 -5 -4 71.7 4.0 4 6 -4 34.1 3.7 4 -6 -4 12.7 4.5 4 7 -4 0.1 4.5 4 -7 -4 -3.3 4.4 4 8 -4 98.0 4.8 4 -8 -4 123.3 5.1 5 0 -4 -3.3 3.8 5 1 -4 493.3 7.2 5 -1 -4 449.9 6.9 5 2 -4 415.6 6.9 5 -2 -4 360.6 6.5 5 3 -4 125.1 4.7 5 -3 -4 95.8 4.4 5 4 -4 7.5 5.0 5 -4 -4 12.9 4.5 5 5 -4 71.1 4.3 5 -5 -4 75.9 4.3 5 6 -4 105.6 4.9 5 -6 -4 118.7 4.9 5 7 -4 157.7 5.7 5 -7 -4 195.7 6.1 6 0 -4 27.7 2.7 6 1 -4 219.2 5.3 6 -1 -4 212.9 5.3 6 2 -4 936.9 11.0 6 -2 -4 840.4 10.4 6 3 -4 33.5 3.8 6 -3 -4 30.6 3.4 6 4 -4 67.7 5.3 6 -4 -4 59.4 4.1 6 5 -4 32.3 4.0 6 -5 -4 35.1 4.1 6 6 -4 440.2 8.5 6 -6 -4 591.1 9.7 7 0 -4 6.6 3.1 7 1 -4 51.7 3.8 7 -1 -4 59.5 3.5 7 2 -4 16.8 3.5 7 -2 -4 18.4 3.3 7 3 -4 325.8 7.8 7 -3 -4 355.7 7.6 7 4 -4 -0.4 4.6 7 -4 -4 -0.9 4.5 7 5 -4 142.1 5.5 7 -5 -4 181.8 6.0 8 0 -4 1389.8 13.1 8 1 -4 144.7 5.3 8 -1 -4 146.0 5.8 8 2 -4 20.8 3.6 8 -2 -4 30.7 3.8 8 3 -4 -2.3 4.7 8 -3 -4 7.6 4.6 8 4 -4 115.6 5.3 8 -4 -4 149.4 5.7 9 0 -4 -4.6 3.2 9 1 -4 44.9 3.2 9 -1 -4 32.8 3.3 0 0 -5 9.5 3.7 0 1 -5 279.4 5.5 0 -1 -5 278.6 5.5 0 2 -5 4.8 3.8 0 -2 -5 1.3 3.7 0 3 -5 312.9 6.0 0 -3 -5 285.5 5.6 0 4 -5 2.6 4.0 0 -4 -5 -7.7 3.7 0 5 -5 43.6 3.5 0 -5 -5 33.7 3.2 0 6 -5 -4.0 4.1 0 -6 -5 0.4 3.7 0 7 -5 153.8 5.0 0 -7 -5 138.6 4.8 1 0 -5 110.3 3.9 1 1 -5 270.0 5.4 1 -1 -5 270.5 5.4 1 2 -5 -4.6 4.0 1 -2 -5 0.6 3.9 1 3 -5 955.8 9.9 1 -3 -5 885.1 9.4 1 4 -5 209.9 5.4 1 -4 -5 164.7 4.8 1 5 -5 1266.5 12.6 1 -5 -5 959.2 10.5 1 6 -5 7.4 4.0 1 -6 -5 0.4 4.0 1 7 -5 197.6 5.7 1 -7 -5 144.3 5.0 2 0 -5 0.9 3.7 2 1 -5 3.4 3.7 2 -1 -5 2.8 3.8 2 2 -5 265.2 5.5 2 -2 -5 258.2 5.5 2 3 -5 13.4 2.8 2 -3 -5 13.7 2.6 2 4 -5 24.3 3.1 2 -4 -5 20.1 2.8 2 5 -5 0.2 4.3 2 -5 -5 11.4 3.9 2 6 -5 61.6 4.5 2 -6 -5 51.1 3.5 2 7 -5 -1.5 4.3 2 -7 -5 -3.1 4.0 3 0 -5 284.3 5.5 3 1 -5 608.4 7.7 3 -1 -5 602.2 7.8 3 2 -5 2.5 3.7 3 -2 -5 7.9 3.7 3 3 -5 203.1 5.1 3 -3 -5 194.9 5.1 3 4 -5 145.4 4.7 3 -4 -5 107.2 4.2 3 5 -5 84.9 4.1 3 -5 -5 62.6 3.7 3 6 -5 13.3 4.3 3 -6 -5 11.4 2.6 3 7 -5 253.1 6.4 3 -7 -5 195.9 5.8 4 0 -5 -2.7 3.7 4 1 -5 104.6 4.0 4 -1 -5 100.6 4.0 4 2 -5 38.3 3.0 4 -2 -5 36.7 2.9 4 3 -5 272.2 5.9 4 -3 -5 228.5 5.5 4 4 -5 -5.0 4.1 4 -4 -5 0.5 3.9 4 5 -5 57.5 3.7 4 -5 -5 46.4 3.4 4 6 -5 9.6 4.2 4 -6 -5 3.9 4.1 5 0 -5 5.9 3.7 5 1 -5 571.4 7.8 5 -1 -5 554.4 7.8 5 2 -5 41.2 3.8 5 -2 -5 30.8 3.1 5 3 -5 72.8 3.7 5 -3 -5 71.1 3.7 5 4 -5 88.2 4.1 5 -4 -5 68.8 3.9 5 5 -5 3.1 4.1 5 -5 -5 -0.9 4.2 5 6 -5 32.6 4.4 5 -6 -5 36.3 4.2 6 0 -5 -1.8 3.1 6 1 -5 8.8 3.3 6 -1 -5 9.4 3.3 6 2 -5 109.6 4.0 6 -2 -5 99.8 3.9 6 3 -5 7.8 3.6 6 -3 -5 6.6 3.6 6 4 -5 13.2 3.3 6 -4 -5 4.6 4.0 6 5 -5 0.4 3.9 6 -5 -5 3.1 4.1 7 0 -5 4.6 3.2 7 1 -5 133.5 4.3 7 -1 -5 133.9 4.4 7 2 -5 29.6 2.9 7 -2 -5 21.0 2.8 7 3 -5 240.9 6.1 7 -3 -5 210.7 5.7 8 0 -5 7.9 2.9 8 1 -5 53.4 3.4 8 -1 -5 45.8 3.2 0 0 -6 438.4 6.9 0 1 -6 7.4 3.4 0 -1 -6 4.0 3.5 0 2 -6 876.4 9.6 0 -2 -6 931.5 9.9 0 3 -6 -2.0 3.6 0 -3 -6 0.5 3.4 0 4 -6 210.5 5.5 0 -4 -6 197.8 5.3 0 5 -6 -8.7 3.8 0 -5 -6 -3.8 3.5 0 6 -6 607.2 9.1 0 -6 -6 447.5 7.8 1 0 -6 -1.9 3.5 1 1 -6 398.2 6.7 1 -1 -6 401.4 6.7 1 2 -6 176.8 4.8 1 -2 -6 174.0 4.7 1 3 -6 42.7 3.2 1 -3 -6 39.2 3.1 1 4 -6 3.2 3.6 1 -4 -6 0.5 3.5 1 5 -6 111.3 4.4 1 -5 -6 91.8 4.0 1 6 -6 44.5 3.6 1 -6 -6 36.7 3.2 2 0 -6 1113.1 10.7 2 1 -6 18.5 2.6 2 -1 -6 11.9 2.7 2 2 -6 16.8 3.7 2 -2 -6 9.5 3.5 2 3 -6 28.8 2.9 2 -3 -6 27.0 2.8 2 4 -6 739.7 9.4 2 -4 -6 611.5 8.5 2 5 -6 216.4 5.5 2 -5 -6 168.9 5.0 2 6 -6 33.9 3.4 2 -6 -6 12.8 3.8 3 0 -6 -5.5 3.6 3 1 -6 83.1 3.7 3 -1 -6 75.7 3.5 3 2 -6 75.9 3.5 3 -2 -6 75.7 3.7 3 3 -6 484.9 7.4 3 -3 -6 454.8 7.3 3 4 -6 1.1 3.6 3 -4 -6 -0.5 3.6 3 5 -6 158.5 5.1 3 -5 -6 107.2 4.3 4 0 -6 135.1 4.3 4 1 -6 -0.2 3.5 4 -1 -6 10.9 3.3 4 2 -6 813.9 9.5 4 -2 -6 819.4 9.7 4 3 -6 33.8 2.9 4 -3 -6 30.0 2.9 4 4 -6 351.2 6.7 4 -4 -6 277.2 6.2 4 5 -6 31.3 3.2 4 -5 -6 23.4 2.9 5 0 -6 -5.8 3.0 5 1 -6 65.1 3.3 5 -1 -6 72.8 3.5 5 2 -6 145.1 4.5 5 -2 -6 129.4 4.3 5 3 -6 202.9 5.2 5 -3 -6 168.2 4.9 5 4 -6 7.3 3.6 5 -4 -6 2.7 3.6 6 0 -6 343.4 6.3 6 1 -6 51.7 3.1 6 -1 -6 48.7 3.0 6 2 -6 21.6 2.6 6 -2 -6 19.1 2.5 0 0 -7 -2.5 3.4 0 1 -7 33.4 3.0 0 -1 -7 34.6 2.9 0 2 -7 -1.4 3.4 0 -2 -7 2.8 3.3 0 3 -7 102.6 4.1 0 -3 -7 94.4 3.8 0 4 -7 3.0 3.4 0 -4 -7 -5.2 3.2 1 0 -7 122.8 4.2 1 1 -7 30.9 2.7 1 -1 -7 34.0 2.8 1 2 -7 -0.1 3.4 1 -2 -7 2.7 3.3 1 3 -7 230.6 5.6 1 -3 -7 211.2 5.3 1 4 -7 6.5 3.6 1 -4 -7 12.2 3.6 2 0 -7 -3.0 3.3 2 1 -7 5.0 3.5 2 -1 -7 -4.2 3.5 2 2 -7 65.6 3.5 2 -2 -7 68.9 3.5 2 3 -7 0.2 3.5 2 -3 -7 -0.4 3.5 3 0 -7 129.9 4.3 3 1 -7 315.0 6.2 3 -1 -7 318.0 6.2 3 2 -7 27.5 2.8 3 -2 -7 28.5 2.9 4 0 -7 -1.7 3.2 4 1 -7 47.8 3.1 4 -1 -7 48.8 3.3 0 0 0 0.0 0.0 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5469(5) _cell_length_b 8.3535(5) _cell_length_c 6.0609(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 432.73(4) _cell_formula_units_Z 4 _cell_measurement_temperature 573(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.583 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.112 _exptl_absorpt_correction_T_max 0.194 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 953 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.52 _reflns_number_total 495 _reflns_number_gt 422 _reflns_threshold_expression >2\s(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+2.5767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0183(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 495 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.351 _refine_ls_restrained_S_all 1.351 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.2527(2) 0.0365(5) Uani 1 2 d S . . Zn2 Zn 0.13663(14) 0.63394(16) 0.0000 0.0286(4) Uani 1 2 d S . . As1 As 0.24248(11) 0.25052(13) 0.0000 0.0229(4) Uani 1 2 d S . . O1 O 0.3576(6) 0.2686(7) 0.2232(9) 0.0329(13) Uani 1 1 d . . . O2 O 0.1425(9) 0.0764(10) 0.0000 0.0297(17) Uani 1 2 d S . . O3 O 0.1066(9) 0.3943(10) 0.0000 0.039(2) Uani 1 2 d S . . O4 O 0.3734(8) 0.6081(10) 0.0000 0.0295(16) Uani 1 2 d S . . H1 H 0.4598 0.6999 0.0000 0.035 Uiso 1 2 d SR . . 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 Zn1 0.0381(7) 0.0462(10) 0.0252(7) 0.000 0.000 -0.0124(6) Zn2 0.0290(6) 0.0259(8) 0.0308(6) 0.000 0.000 0.0007(5) As1 0.0227(5) 0.0208(7) 0.0251(6) 0.000 0.000 -0.0008(4) O1 0.042(3) 0.028(3) 0.029(2) 0.007(2) -0.008(2) -0.007(2) O2 0.034(4) 0.027(4) 0.028(3) 0.000 0.000 -0.008(3) O3 0.029(4) 0.025(4) 0.062(5) 0.000 0.000 -0.004(3) O4 0.032(3) 0.027(4) 0.029(3) 0.000 0.000 0.001(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O4 2.057(5) 3_545 ? Zn1 O4 2.057(5) 7_566 ? Zn1 O2 2.058(5) 5 ? Zn1 O2 2.058(5) . ? Zn1 O1 2.288(5) 4_455 ? Zn1 O1 2.288(5) 3_545 ? Zn1 Zn1 2.997(3) 5_556 ? Zn2 O3 2.018(9) . ? Zn2 O1 2.021(5) 3 ? Zn2 O1 2.021(5) 8_665 ? Zn2 O4 2.035(8) . ? Zn2 O3 2.092(8) 5_565 ? Zn2 Zn2 3.235(3) 5_565 ? As1 O3 1.671(9) . ? As1 O1 1.680(5) . ? As1 O1 1.680(5) 6 ? As1 O2 1.687(8) . ? O1 Zn2 2.021(5) 3_545 ? O1 Zn1 2.288(5) 3 ? O2 Zn1 2.058(5) 5 ? O2 O2 2.750(15) 5 ? O2 O4 3.0450(12) 3_544 ? O3 Zn2 2.092(8) 5_565 ? O3 O3 2.537(17) 5_565 ? O4 Zn1 2.057(5) 3 ? O4 Zn1 2.057(5) 7_665 ? O4 O4 2.819(15) 5_665 ? O4 H1 1.0650 . ? 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 O4 Zn1 O4 86.5(3) 3_545 7_566 ? O4 Zn1 O2 171.7(3) 3_545 5 ? O4 Zn1 O2 95.4(2) 7_566 5 ? O4 Zn1 O2 95.4(2) 3_545 . ? O4 Zn1 O2 171.7(3) 7_566 . ? O2 Zn1 O2 83.8(3) 5 . ? O4 Zn1 O1 82.1(3) 3_545 4_455 ? O4 Zn1 O1 92.5(2) 7_566 4_455 ? O2 Zn1 O1 89.7(3) 5 4_455 ? O2 Zn1 O1 95.7(3) . 4_455 ? O4 Zn1 O1 92.5(2) 3_545 3_545 ? O4 Zn1 O1 82.1(3) 7_566 3_545 ? O2 Zn1 O1 95.7(3) 5 3_545 ? O2 Zn1 O1 89.7(3) . 3_545 ? O1 Zn1 O1 172.7(3) 4_455 3_545 ? O4 Zn1 Zn1 43.24(16) 3_545 5_556 ? O4 Zn1 Zn1 43.24(16) 7_566 5_556 ? O2 Zn1 Zn1 138.08(16) 5 5_556 ? O2 Zn1 Zn1 138.08(16) . 5_556 ? O1 Zn1 Zn1 86.34(14) 4_455 5_556 ? O1 Zn1 Zn1 86.34(14) 3_545 5_556 ? O3 Zn2 O1 123.74(17) . 3 ? O3 Zn2 O1 123.74(17) . 8_665 ? O1 Zn2 O1 112.3(3) 3 8_665 ? O3 Zn2 O4 91.2(3) . . ? O1 Zn2 O4 92.0(2) 3 . ? O1 Zn2 O4 92.0(2) 8_665 . ? O3 Zn2 O3 76.2(4) . 5_565 ? O1 Zn2 O3 95.0(2) 3 5_565 ? O1 Zn2 O3 95.0(2) 8_665 5_565 ? O4 Zn2 O3 167.4(3) . 5_565 ? O3 Zn2 Zn2 38.9(2) . 5_565 ? O1 Zn2 Zn2 113.75(17) 3 5_565 ? O1 Zn2 Zn2 113.75(17) 8_665 5_565 ? O4 Zn2 Zn2 130.1(3) . 5_565 ? O3 Zn2 Zn2 37.3(2) 5_565 5_565 ? O3 As1 O1 110.0(2) . . ? O3 As1 O1 110.0(2) . 6 ? O1 As1 O1 107.3(4) . 6 ? O3 As1 O2 105.5(4) . . ? O1 As1 O2 112.0(2) . . ? O1 As1 O2 112.0(2) 6 . ? As1 O1 Zn2 129.2(3) . 3_545 ? As1 O1 Zn1 116.0(3) . 3 ? Zn2 O1 Zn1 113.9(2) 3_545 3 ? As1 O2 Zn1 124.6(3) . 5 ? As1 O2 Zn1 124.6(3) . . ? Zn1 O2 Zn1 96.2(3) 5 . ? As1 O2 O2 148.1(6) . 5 ? Zn1 O2 O2 48.08(16) 5 5 ? Zn1 O2 O2 48.08(16) . 5 ? As1 O2 O4 87.0(2) . 3_544 ? Zn1 O2 O4 42.27(14) 5 3_544 ? Zn1 O2 O4 137.8(3) . 3_544 ? O2 O2 O4 90.1(2) 5 3_544 ? As1 O3 Zn2 128.6(4) . . ? As1 O3 Zn2 127.6(5) . 5_565 ? Zn2 O3 Zn2 103.8(4) . 5_565 ? As1 O3 O3 178.2(6) . 5_565 ? Zn2 O3 O3 53.2(3) . 5_565 ? Zn2 O3 O3 50.6(3) 5_565 5_565 ? Zn2 O4 Zn1 124.7(2) . 3 ? Zn2 O4 Zn1 124.7(2) . 7_665 ? Zn1 O4 Zn1 93.5(3) 3 7_665 ? Zn2 O4 O4 146.3(5) . 5_665 ? Zn1 O4 O4 46.76(16) 3 5_665 ? Zn1 O4 O4 46.76(16) 7_665 5_665 ? Zn2 O4 H1 127.8 . . ? Zn1 O4 H1 87.2 3 . ? Zn1 O4 H1 87.2 7_665 . ? O4 O4 H1 85.9 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 1.07 2.08 2.859(8) 127.7 5_665 O4 H1 O1 1.07 2.08 2.859(8) 127.7 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.847 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.195 _iucr_refine_instructions_details ; TITL ADA_300C Pnnm ba-c CELL 0.71073 8.5469 8.3535 6.0609 90.000 90.000 90.000 ZERR 4 0.0005 0.0005 0.0003 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 BOND $H L.S. 4 LIST 4 FMAP 2 PLAN 35 WGHT 0.022700 2.576700 EXTI 0.018355 FVAR 0.42892 ZN1 4 0.000000 0.000000 0.252720 10.50000 0.03811 0.04625 = 0.02519 0.00000 0.00000 -0.01244 ZN2 4 0.136628 0.633942 0.000000 10.50000 0.02901 0.02588 = 0.03076 0.00000 0.00000 0.00067 AS1 2 0.242483 0.250518 0.000000 10.50000 0.02273 0.02083 = 0.02508 0.00000 0.00000 -0.00082 O1 3 0.357650 0.268644 0.223195 11.00000 0.04235 0.02775 = 0.02858 0.00675 -0.00796 -0.00708 O2 3 0.142484 0.076443 0.000000 10.50000 0.03391 0.02669 = 0.02849 0.00000 0.00000 -0.00802 O3 3 0.106586 0.394288 0.000000 10.50000 0.02929 0.02487 = 0.06242 0.00000 0.00000 -0.00356 O4 3 0.373369 0.608062 0.000000 10.50000 0.03224 0.02721 = 0.02900 0.00000 0.00000 0.00118 AFIX 3 H1 1 0.459831 0.699868 0.000000 10.50000 -1.20000 HKLF 4 REM ADA_300C Pnnm ba-c REM R1 = 0.0358 for 422 Fo > 4sig(Fo) and 0.0433 for all 495 data REM 46 parameters refined using 0 restraints END WGHT 0.0215 2.6822 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 4.6 1.0 0 -1 0 3.7 1.5 0 2 0 481.7 5.5 0 -2 0 486.0 5.3 0 3 0 1.1 3.8 0 -3 0 -0.4 3.6 0 4 0 1112.1 10.4 0 -4 0 1236.0 10.8 0 5 0 -1.2 5.0 0 -5 0 1.5 4.8 0 6 0 258.4 6.3 0 -6 0 318.4 6.7 0 7 0 -6.8 5.5 0 -7 0 -4.6 5.3 0 8 0 2291.0 17.4 0 -8 0 2833.6 19.5 0 9 0 -14.3 4.7 0 -9 0 2.0 4.6 0 10 0 126.2 5.1 0 -10 0 158.5 5.4 1 0 0 -1.2 1.0 1 1 0 1269.8 6.0 1 -1 0 1159.8 6.2 1 2 0 1369.8 8.5 1 -2 0 1240.7 8.5 1 3 0 2790.2 14.0 1 -3 0 2609.0 14.1 1 4 0 22.4 3.6 1 -4 0 27.7 3.0 1 5 0 1263.2 11.9 1 -5 0 1416.0 12.6 1 6 0 443.8 7.9 1 -6 0 566.9 8.7 1 7 0 5.0 5.3 1 -7 0 15.4 5.3 1 8 0 38.4 4.1 1 -8 0 49.6 4.1 1 9 0 43.4 4.0 1 -9 0 56.5 4.0 1 10 0 11.4 3.8 1 -10 0 6.8 4.4 2 0 0 230.6 3.0 2 1 0 974.8 6.4 2 -1 0 859.4 6.2 2 2 0 5590.8 17.1 2 -2 0 4857.2 17.2 2 3 0 167.0 4.0 2 -3 0 182.4 4.3 2 4 0 26.7 3.0 2 -4 0 38.7 3.3 2 5 0 320.4 6.5 2 -5 0 371.7 7.1 2 6 0 1871.5 15.2 2 -6 0 2275.6 16.9 2 7 0 9.2 4.8 2 -7 0 3.2 5.4 2 8 0 84.3 4.7 2 -8 0 123.2 5.1 2 9 0 221.7 6.4 2 -9 0 283.5 6.9 2 10 0 365.9 7.8 2 -10 0 524.1 9.2 3 0 0 -4.2 2.4 3 1 0 2914.8 12.3 3 -1 0 1888.8 10.1 3 2 0 370.0 5.0 3 -2 0 333.0 5.1 3 3 0 171.4 4.1 3 -3 0 151.7 4.3 3 4 0 11.5 4.3 3 -4 0 13.5 4.7 3 5 0 120.6 4.7 3 -5 0 123.0 4.9 3 6 0 170.8 5.7 3 -6 0 185.2 5.8 3 7 0 914.0 11.4 3 -7 0 1142.6 12.8 3 8 0 3.8 4.9 3 -8 0 16.5 4.9 3 9 0 63.0 4.0 3 -9 0 84.5 4.5 3 10 0 0.9 4.0 3 -10 0 9.2 3.9 4 0 0 81.8 3.1 4 1 0 46.6 2.3 4 -1 0 44.0 2.3 4 2 0 21.8 2.5 4 -2 0 19.5 3.1 4 3 0 20.7 2.6 4 -3 0 19.8 2.8 4 4 0 5119.1 21.5 4 -4 0 4404.5 21.1 4 5 0 155.1 5.0 4 -5 0 140.3 5.3 4 6 0 5.9 5.0 4 -6 0 16.2 5.5 4 7 0 6.0 4.9 4 -7 0 -2.0 5.2 4 8 0 115.3 5.0 4 -8 0 148.2 5.5 4 9 0 -4.9 4.2 4 -9 0 -2.9 4.0 5 0 0 5.9 2.8 5 1 0 1208.2 9.6 5 -1 0 1143.0 9.3 5 2 0 962.9 8.9 5 -2 0 902.4 8.8 5 3 0 218.7 5.0 5 -3 0 215.6 5.2 5 4 0 33.7 3.4 5 -4 0 38.2 3.9 5 5 0 126.6 4.9 5 -5 0 107.6 4.9 5 6 0 221.8 6.0 5 -6 0 230.4 6.2 5 7 0 274.1 6.6 5 -7 0 288.4 7.0 5 8 0 46.9 4.0 5 -8 0 56.4 4.1 5 9 0 43.5 4.1 5 -9 0 51.0 4.0 6 0 0 103.4 3.6 6 1 0 543.9 7.0 6 -1 0 546.9 6.9 6 2 0 1721.6 12.6 6 -2 0 1618.9 12.3 6 3 0 144.2 4.6 6 -3 0 134.8 4.6 6 4 0 104.1 4.3 6 -4 0 96.7 4.5 6 5 0 57.6 4.3 6 -5 0 57.9 4.2 6 6 0 835.3 10.6 6 -6 0 781.4 10.4 6 7 0 91.1 4.9 6 -7 0 88.5 4.8 6 8 0 14.0 4.5 6 -8 0 15.3 3.2 7 0 0 3.6 3.8 7 1 0 103.3 3.9 7 -1 0 108.3 4.1 7 2 0 46.2 3.4 7 -2 0 37.0 4.1 7 3 0 690.2 8.6 7 -3 0 614.0 8.5 7 4 0 16.5 2.8 7 -4 0 1.9 4.4 7 5 0 292.2 6.4 7 -5 0 293.0 6.6 7 6 0 -7.1 4.3 7 -6 0 0.0 4.5 7 7 0 36.2 3.7 7 -7 0 31.3 3.7 8 0 0 2815.5 16.7 8 1 0 355.1 6.4 8 -1 0 332.7 6.1 8 2 0 65.3 3.5 8 -2 0 62.8 3.5 8 3 0 2.0 4.0 8 -3 0 9.4 3.5 8 4 0 208.9 5.6 8 -4 0 181.1 5.2 8 5 0 12.2 4.1 8 -5 0 10.2 4.2 8 6 0 42.5 3.7 8 -6 0 50.1 3.8 8 -7 0 32.6 3.8 9 0 0 2.6 3.8 9 1 0 70.9 3.7 9 -1 0 68.3 3.7 9 2 0 207.6 5.3 9 -2 0 189.9 5.1 9 3 0 131.7 4.5 9 -3 0 109.8 4.3 9 4 0 2.5 3.7 9 -4 0 -1.3 3.9 9 5 0 58.8 3.8 9 -5 0 55.0 3.8 10 0 0 186.9 5.1 10 1 0 -9.8 3.7 10 -1 0 -2.8 3.8 10 2 0 519.4 8.1 10 -2 0 463.5 7.5 10 3 0 65.5 3.6 10 -3 0 58.1 3.6 0 0 -1 31.3 1.3 0 1 -1 1526.0 7.2 0 -1 -1 1570.9 7.1 0 2 -1 20.4 3.3 0 -2 -1 15.4 2.5 0 3 -1 1691.3 11.3 0 -3 -1 1698.0 10.7 0 4 -1 7.2 4.5 0 -4 -1 9.0 3.9 0 5 -1 336.4 6.9 0 -5 -1 332.7 6.3 0 6 -1 -0.8 5.5 0 -6 -1 6.1 5.0 0 7 -1 371.9 7.7 0 -7 -1 396.7 7.5 0 8 -1 3.8 4.9 0 -8 -1 -2.6 4.4 0 9 -1 77.3 4.6 0 -9 -1 105.1 4.6 0 10 -1 -3.5 3.9 0 -10 -1 1.0 3.7 1 0 -1 1268.0 6.0 1 1 -1 881.8 6.6 1 -1 -1 863.3 6.0 1 2 -1 20.8 3.3 1 -2 -1 14.8 3.5 1 3 -1 2489.0 14.3 1 -3 -1 2527.4 13.8 1 4 -1 516.2 7.7 1 -4 -1 567.6 7.6 1 5 -1 2606.8 17.0 1 -5 -1 2852.7 17.4 1 6 -1 4.4 5.4 1 -6 -1 2.2 5.2 1 7 -1 315.2 7.2 1 -7 -1 368.6 7.4 1 8 -1 53.0 4.4 1 -8 -1 84.3 4.5 1 9 -1 36.9 3.8 1 -9 -1 45.3 3.8 1 10 -1 13.2 4.0 1 -10 -1 18.0 3.6 2 0 -1 2.0 4.2 2 1 -1 29.7 4.7 2 -1 -1 29.7 4.3 2 2 -1 816.0 8.4 2 -2 -1 846.6 8.5 2 3 -1 46.8 3.9 2 -3 -1 50.0 4.0 2 4 -1 44.5 3.5 2 -4 -1 57.9 3.6 2 5 -1 6.7 5.1 2 -5 -1 1.0 5.1 2 6 -1 176.1 5.8 2 -6 -1 231.2 6.1 2 7 -1 12.9 5.2 2 -7 -1 12.4 5.1 2 8 -1 62.6 4.5 2 -8 -1 86.5 4.6 2 9 -1 0.0 4.4 2 -9 -1 0.0 4.5 2 10 -1 35.2 3.5 2 -10 -1 41.4 3.6 3 0 -1 1767.0 9.5 3 1 -1 2403.4 12.2 3 -1 -1 2662.8 13.9 3 2 -1 27.3 3.2 3 -2 -1 26.1 3.8 3 3 -1 820.9 9.1 3 -3 -1 806.7 9.1 3 4 -1 380.9 6.9 3 -4 -1 444.0 7.5 3 5 -1 208.8 5.9 3 -5 -1 243.0 6.3 3 6 -1 6.1 5.5 3 -6 -1 0.2 5.8 3 7 -1 511.6 8.9 3 -7 -1 648.3 9.7 3 8 -1 101.5 5.0 3 -8 -1 152.9 5.6 3 9 -1 431.7 8.4 3 -9 -1 587.0 9.6 4 0 -1 2.4 3.1 4 1 -1 719.2 7.3 4 -1 -1 638.0 7.1 4 2 -1 199.7 4.4 4 -2 -1 194.5 4.8 4 3 -1 800.1 9.0 4 -3 -1 747.9 9.2 4 4 -1 5.7 4.8 4 -4 -1 8.4 5.3 4 5 -1 207.0 6.1 4 -5 -1 236.3 6.6 4 6 -1 26.3 3.9 4 -6 -1 37.4 4.2 4 7 -1 202.7 6.2 4 -7 -1 285.8 7.1 4 8 -1 -0.6 4.7 4 -8 -1 1.8 4.6 4 9 -1 35.2 3.9 4 -9 -1 50.8 3.9 5 0 -1 46.7 2.7 5 1 -1 2134.5 12.9 5 -1 -1 1978.4 12.7 5 2 -1 67.4 3.3 5 -2 -1 71.7 3.6 5 3 -1 243.3 5.4 5 -3 -1 228.9 5.7 5 4 -1 276.1 6.3 5 -4 -1 272.9 6.5 5 5 -1 11.0 4.9 5 -5 -1 26.5 5.3 5 6 -1 33.6 3.7 5 -6 -1 36.8 4.0 5 7 -1 480.8 8.9 5 -7 -1 569.5 9.5 5 8 -1 -4.0 4.7 5 -8 -1 1.4 4.8 5 9 -1 437.8 8.7 5 -9 -1 580.2 9.6 6 0 -1 0.5 3.6 6 1 -1 3.4 4.1 6 -1 -1 10.4 4.0 6 2 -1 271.3 5.6 6 -2 -1 252.4 5.7 6 3 -1 40.6 3.4 6 -3 -1 35.1 3.8 6 4 -1 14.0 4.9 6 -4 -1 15.4 5.0 6 5 -1 2.3 4.7 6 -5 -1 -1.1 5.1 6 6 -1 67.1 4.2 6 -6 -1 69.5 4.6 6 7 -1 35.2 3.7 6 -7 -1 36.7 3.9 6 8 -1 20.2 3.4 6 -8 -1 22.2 3.5 7 0 -1 121.1 4.2 7 1 -1 379.9 6.6 7 -1 -1 374.2 6.4 7 2 -1 42.9 3.3 7 -2 -1 51.9 3.6 7 3 -1 474.8 7.4 7 -3 -1 413.9 7.2 7 4 -1 426.0 7.2 7 -4 -1 389.2 7.2 7 5 -1 389.5 7.4 7 -5 -1 359.6 7.3 7 6 -1 63.9 4.2 7 -6 -1 61.5 4.1 7 7 -1 160.3 5.7 7 -7 -1 169.9 5.8 8 0 -1 1.8 3.9 8 1 -1 126.9 4.3 8 -1 -1 127.6 4.3 8 2 -1 131.8 4.2 8 -2 -1 123.7 4.2 8 3 -1 129.8 4.7 8 -3 -1 102.3 4.2 8 4 -1 -1.8 4.0 8 -4 -1 -4.3 4.4 8 5 -1 39.1 3.4 8 -5 -1 39.8 3.5 8 6 -1 21.4 3.1 8 -6 -1 17.0 3.2 9 0 -1 81.5 3.9 9 1 -1 38.5 3.2 9 -1 -1 35.2 3.1 9 2 -1 48.6 3.3 9 -2 -1 46.0 3.3 9 3 -1 443.1 7.3 9 -3 -1 385.7 7.1 9 4 -1 13.8 2.8 9 -4 -1 5.1 4.1 9 5 -1 458.8 8.3 9 -5 -1 415.8 7.9 10 0 -1 -4.1 3.3 10 1 -1 5.0 3.4 10 -1 -1 0.4 3.4 10 2 -1 31.4 2.9 10 -2 -1 33.2 2.9 10 3 -1 24.6 2.9 10 -3 -1 18.4 2.8 0 0 -2 2724.6 10.9 0 1 -2 -3.6 2.5 0 -1 -2 -2.5 2.3 0 2 -2 2974.0 13.4 0 -2 -2 2936.5 13.0 0 3 -2 -2.2 3.4 0 -3 -2 1.9 3.0 0 4 -2 1969.7 13.8 0 -4 -2 2005.7 13.1 0 5 -2 -5.6 4.8 0 -5 -2 1.8 4.1 0 6 -2 1480.3 13.9 0 -6 -2 1537.7 13.4 0 7 -2 -14.9 5.1 0 -7 -2 -5.3 4.7 0 8 -2 348.8 7.6 0 -8 -2 392.7 7.8 0 9 -2 -6.5 4.5 0 -9 -2 0.1 4.0 0 10 -2 376.7 8.0 0 -10 -2 444.5 8.3 1 0 -2 3.5 2.4 1 1 -2 2540.4 11.6 1 -1 -2 2442.9 11.3 1 2 -2 1502.4 10.3 1 -2 -2 1371.8 9.2 1 3 -2 137.3 4.1 1 -3 -2 139.2 3.8 1 4 -2 8.4 4.5 1 -4 -2 11.0 4.1 1 5 -2 340.2 7.0 1 -5 -2 340.6 6.5 1 6 -2 118.7 5.2 1 -6 -2 114.9 4.9 1 7 -2 510.9 8.8 1 -7 -2 533.8 8.6 1 8 -2 9.1 4.6 1 -8 -2 1.2 4.3 1 9 -2 129.8 5.3 1 -9 -2 162.6 5.5 1 10 -2 48.1 4.2 1 -10 -2 53.9 3.7 2 0 -2 4689.1 60.9 2 1 -2 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3.5 0 -1 -6 5.1 3.4 0 2 -6 843.4 9.6 0 -2 -6 873.7 9.8 0 3 -6 -0.1 3.7 0 -3 -6 -3.0 3.5 0 4 -6 174.3 5.1 0 -4 -6 147.0 4.7 0 5 -6 3.4 3.8 0 -5 -6 -3.8 3.6 0 6 -6 534.9 8.9 0 -6 -6 387.3 7.2 1 0 -6 -0.6 3.5 1 1 -6 360.8 6.4 1 -1 -6 368.6 6.3 1 2 -6 161.3 4.6 1 -2 -6 165.5 4.7 1 3 -6 37.6 3.1 1 -3 -6 39.5 3.1 1 4 -6 2.8 3.7 1 -4 -6 6.4 3.5 1 5 -6 97.2 4.3 1 -5 -6 71.4 3.7 1 6 -6 38.3 3.5 1 -6 -6 30.8 3.1 2 0 -6 1081.6 11.0 2 1 -6 14.5 2.6 2 -1 -6 11.3 3.7 2 2 -6 9.8 3.4 2 -2 -6 4.5 3.7 2 3 -6 29.2 3.0 2 -3 -6 25.4 3.0 2 4 -6 684.1 9.1 2 -4 -6 568.6 8.3 2 5 -6 186.5 5.4 2 -5 -6 154.9 4.9 2 6 -6 39.3 3.6 2 -6 -6 14.3 4.1 3 0 -6 7.3 3.5 3 1 -6 77.2 3.7 3 -1 -6 70.4 3.7 3 2 -6 66.1 3.5 3 -2 -6 63.0 3.4 3 3 -6 444.5 7.4 3 -3 -6 398.3 6.9 3 4 -6 8.6 3.7 3 -4 -6 3.1 3.7 3 5 -6 135.1 5.0 3 -5 -6 101.9 4.5 4 0 -6 114.4 4.2 4 1 -6 6.5 3.3 4 -1 -6 -1.0 3.7 4 2 -6 732.6 9.2 4 -2 -6 697.9 9.0 4 3 -6 40.5 3.2 4 -3 -6 30.8 2.9 4 4 -6 332.7 6.8 4 -4 -6 256.6 6.1 4 5 -6 29.3 3.5 4 -5 -6 17.2 3.0 5 0 -6 -2.8 3.2 5 1 -6 71.5 3.4 5 -1 -6 70.4 3.6 5 2 -6 123.6 4.3 5 -2 -6 107.5 3.9 5 3 -6 164.4 5.0 5 -3 -6 149.7 4.9 5 4 -6 9.1 3.7 5 -4 -6 9.0 3.6 6 0 -6 310.3 6.1 6 1 -6 53.3 3.2 6 -1 -6 51.3 3.2 6 2 -6 19.4 3.2 6 -2 -6 18.4 2.4 0 0 -7 -4.9 3.4 0 1 -7 28.4 3.0 0 -1 -7 25.8 2.8 0 2 -7 -2.9 3.4 0 -2 -7 -6.1 3.4 0 3 -7 82.5 3.8 0 -3 -7 79.1 3.7 0 4 -7 0.8 3.4 0 -4 -7 2.5 3.2 1 0 -7 118.4 4.2 1 1 -7 32.1 3.0 1 -1 -7 30.5 2.9 1 2 -7 7.4 3.4 1 -2 -7 5.0 3.3 1 3 -7 205.6 5.3 1 -3 -7 187.6 5.1 1 4 -7 5.3 3.6 1 -4 -7 -0.7 3.7 2 0 -7 0.4 3.5 2 1 -7 3.0 3.5 2 -1 -7 3.0 3.4 2 2 -7 56.3 3.3 2 -2 -7 59.8 3.3 2 3 -7 0.7 3.6 2 -3 -7 1.1 3.5 3 0 -7 130.5 4.4 3 1 -7 294.7 6.2 3 -1 -7 284.6 6.1 3 2 -7 25.9 2.9 3 -2 -7 30.9 2.9 4 0 -7 6.1 3.1 4 1 -7 40.9 3.0 4 -1 -7 41.4 3.1 0 0 0 0.0 0.0 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5561(6) _cell_length_b 8.3686(5) _cell_length_c 6.0664(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 434.37(6) _cell_formula_units_Z 4 _cell_measurement_temperature 673(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.512 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_T_max 0.118 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 955 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.51 _reflns_number_total 496 _reflns_number_gt 423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+2.8860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_secondary difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0134(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 496 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.2529(2) 0.0413(5) Uani 1 2 d S . . Zn2 Zn 0.13689(14) 0.63350(16) 0.0000 0.0317(4) Uani 1 2 d S . . As1 As 0.24209(11) 0.25041(13) 0.0000 0.0248(4) Uani 1 2 d S . . O1 O 0.3573(6) 0.2679(7) 0.2229(8) 0.0365(13) Uani 1 1 d . . . O2 O 0.1414(9) 0.0769(10) 0.0000 0.0341(18) Uani 1 2 d S . . O3 O 0.1062(9) 0.3946(10) 0.0000 0.042(2) Uani 1 2 d S . . O4 O 0.3734(8) 0.6082(10) 0.0000 0.0338(16) Uani 1 2 d S . . H1 H 0.4569 0.6954 0.0000 0.041 Uiso 1 2 d SR . . 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 Zn1 0.0427(7) 0.0537(10) 0.0274(6) 0.000 0.000 -0.0150(6) Zn2 0.0315(7) 0.0297(8) 0.0339(6) 0.000 0.000 0.0008(6) As1 0.0248(5) 0.0231(7) 0.0263(5) 0.000 0.000 -0.0012(4) O1 0.046(3) 0.033(3) 0.030(2) 0.007(2) -0.010(2) -0.008(2) O2 0.043(4) 0.030(4) 0.030(3) 0.000 0.000 -0.009(3) O3 0.032(4) 0.024(4) 0.069(5) 0.000 0.000 -0.001(3) O4 0.037(4) 0.034(4) 0.030(3) 0.000 0.000 0.003(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O2 2.057(5) 5 ? Zn1 O2 2.057(5) . ? Zn1 O4 2.059(5) 3_545 ? Zn1 O4 2.059(5) 7_566 ? Zn1 O1 2.299(5) 4_455 ? Zn1 O1 2.299(5) 3_545 ? Zn1 Zn1 2.998(3) 5_556 ? Zn2 O3 2.016(8) . ? Zn2 O1 2.023(5) 3 ? Zn2 O1 2.023(5) 8_665 ? Zn2 O4 2.034(7) . ? Zn2 O3 2.093(8) 5_565 ? Zn2 Zn2 3.237(3) 5_565 ? As1 O3 1.676(8) . ? As1 O1 1.680(5) . ? As1 O1 1.680(5) 6 ? As1 O2 1.689(8) . ? O1 Zn2 2.023(5) 3_545 ? O1 Zn1 2.299(5) 3 ? O2 Zn1 2.057(5) 5 ? O2 O2 2.741(15) 5 ? O2 O4 3.0471(12) 3_544 ? O3 Zn2 2.093(8) 5_565 ? O3 O3 2.532(16) 5_565 ? O4 Zn1 2.059(5) 3 ? O4 Zn1 2.059(5) 7_665 ? O4 O4 2.824(15) 5_665 ? O4 H1 1.0215 . ? 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 Zn1 O2 83.5(3) 5 . ? O2 Zn1 O4 171.8(3) 5 3_545 ? O2 Zn1 O4 95.5(2) . 3_545 ? O2 Zn1 O4 95.5(2) 5 7_566 ? O2 Zn1 O4 171.8(3) . 7_566 ? O4 Zn1 O4 86.6(3) 3_545 7_566 ? O2 Zn1 O1 90.0(3) 5 4_455 ? O2 Zn1 O1 95.5(3) . 4_455 ? O4 Zn1 O1 82.0(3) 3_545 4_455 ? O4 Zn1 O1 92.6(3) 7_566 4_455 ? O2 Zn1 O1 95.5(3) 5 3_545 ? O2 Zn1 O1 90.0(3) . 3_545 ? O4 Zn1 O1 92.6(3) 3_545 3_545 ? O4 Zn1 O1 82.0(3) 7_566 3_545 ? O1 Zn1 O1 172.7(3) 4_455 3_545 ? O2 Zn1 Zn1 138.23(16) 5 5_556 ? O2 Zn1 Zn1 138.23(16) . 5_556 ? O4 Zn1 Zn1 43.28(16) 3_545 5_556 ? O4 Zn1 Zn1 43.28(16) 7_566 5_556 ? O1 Zn1 Zn1 86.34(13) 4_455 5_556 ? O1 Zn1 Zn1 86.34(13) 3_545 5_556 ? O3 Zn2 O1 123.67(17) . 3 ? O3 Zn2 O1 123.67(17) . 8_665 ? O1 Zn2 O1 112.4(3) 3 8_665 ? O3 Zn2 O4 91.5(3) . . ? O1 Zn2 O4 91.9(2) 3 . ? O1 Zn2 O4 91.9(2) 8_665 . ? O3 Zn2 O3 76.1(4) . 5_565 ? O1 Zn2 O3 95.0(2) 3 5_565 ? O1 Zn2 O3 95.0(2) 8_665 5_565 ? O4 Zn2 O3 167.6(3) . 5_565 ? O3 Zn2 Zn2 38.9(2) . 5_565 ? O1 Zn2 Zn2 113.66(17) 3 5_565 ? O1 Zn2 Zn2 113.66(17) 8_665 5_565 ? O4 Zn2 Zn2 130.4(3) . 5_565 ? O3 Zn2 Zn2 37.2(2) 5_565 5_565 ? O3 As1 O1 110.2(2) . . ? O3 As1 O1 110.2(2) . 6 ? O1 As1 O1 107.2(4) . 6 ? O3 As1 O2 105.4(4) . . ? O1 As1 O2 112.0(2) . . ? O1 As1 O2 112.0(2) 6 . ? As1 O1 Zn2 129.4(3) . 3_545 ? As1 O1 Zn1 115.9(3) . 3 ? Zn2 O1 Zn1 113.8(2) 3_545 3 ? As1 O2 Zn1 124.7(3) . 5 ? As1 O2 Zn1 124.7(3) . . ? Zn1 O2 Zn1 96.5(3) 5 . ? As1 O2 O2 148.7(6) . 5 ? Zn1 O2 O2 48.23(16) 5 5 ? Zn1 O2 O2 48.23(16) . 5 ? As1 O2 O4 87.0(2) . 3_544 ? Zn1 O2 O4 42.27(14) 5 3_544 ? Zn1 O2 O4 138.1(4) . 3_544 ? O2 O2 O4 90.2(2) 5 3_544 ? As1 O3 Zn2 128.6(4) . . ? As1 O3 Zn2 127.5(5) . 5_565 ? Zn2 O3 Zn2 103.9(4) . 5_565 ? As1 O3 O3 178.1(6) . 5_565 ? Zn2 O3 O3 53.3(3) . 5_565 ? Zn2 O3 O3 50.6(3) 5_565 5_565 ? Zn2 O4 Zn1 124.7(2) . 3 ? Zn2 O4 Zn1 124.7(2) . 7_665 ? Zn1 O4 Zn1 93.4(3) 3 7_665 ? Zn2 O4 O4 146.1(6) . 5_665 ? Zn1 O4 O4 46.72(16) 3 5_665 ? Zn1 O4 O4 46.72(16) 7_665 5_665 ? Zn2 O4 H1 128.4 . . ? Zn1 O4 H1 86.9 3 . ? Zn1 O4 H1 86.9 7_665 . ? O4 O4 H1 85.5 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 1.02 2.11 2.866(8) 129.1 5_665 O4 H1 O1 1.02 2.11 2.866(8) 129.1 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.841 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.189 _iucr_refine_instructions_details ; TITL ADA_400C Pnnm ba-c CELL 0.71073 8.5561 8.3686 6.0664 90.000 90.000 90.000 ZERR 4 0.0006 0.0005 0.0006 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 BOND $H L.S. 4 LIST 4 FMAP 2 PLAN 35 WGHT 0.021600 2.886000 EXTI 0.013483 FVAR 0.42024 ZN1 4 0.000000 0.000000 0.252899 10.50000 0.04274 0.05372 = 0.02744 0.00000 0.00000 -0.01500 ZN2 4 0.136895 0.633501 0.000000 10.50000 0.03152 0.02967 = 0.03389 0.00000 0.00000 0.00080 AS1 2 0.242085 0.250410 0.000000 10.50000 0.02480 0.02315 = 0.02634 0.00000 0.00000 -0.00121 O1 3 0.357338 0.267891 0.222915 11.00000 0.04596 0.03326 = 0.03036 0.00659 -0.00967 -0.00761 O2 3 0.141407 0.076869 0.000000 10.50000 0.04317 0.02961 = 0.02965 0.00000 0.00000 -0.00865 O3 3 0.106200 0.394620 0.000000 10.50000 0.03239 0.02375 = 0.06878 0.00000 0.00000 -0.00128 O4 3 0.373382 0.608181 0.000000 10.50000 0.03735 0.03406 = 0.03000 0.00000 0.00000 0.00293 AFIX 3 H1 1 0.456884 0.695418 0.000000 10.50000 -1.20000 HKLF 4 REM ADA_400C Pnnm ba-c REM R1 = 0.0356 for 423 Fo > 4sig(Fo) and 0.0440 for all 496 data REM 46 parameters refined using 0 restraints END WGHT 0.0204 2.9590 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 5.2 1.0 0 -1 0 4.4 0.9 0 2 0 446.2 5.2 0 -2 0 478.3 5.3 0 3 0 3.4 3.7 0 -3 0 -8.4 3.5 0 4 0 1036.3 9.9 0 -4 0 1153.0 10.3 0 5 0 5.7 4.6 0 -5 0 -0.3 4.5 0 6 0 272.7 6.4 0 -6 0 320.3 6.5 0 7 0 -4.6 5.2 0 -7 0 -1.9 4.9 0 8 0 1927.2 15.6 0 -8 0 2437.0 17.4 0 9 0 -6.3 4.3 0 -9 0 -9.6 4.4 0 10 0 115.2 4.8 0 -10 0 146.2 5.1 1 0 0 1.5 1.0 1 1 0 1565.2 6.5 1 -1 0 1127.0 6.0 1 2 0 1321.3 8.1 1 -2 0 1221.6 8.3 1 3 0 2564.4 13.0 1 -3 0 2492.6 13.4 1 4 0 18.1 2.7 1 -4 0 24.0 3.7 1 5 0 1115.0 11.1 1 -5 0 1257.7 11.6 1 6 0 379.1 7.3 1 -6 0 493.8 7.9 1 7 0 6.1 5.3 1 -7 0 4.0 5.0 1 8 0 23.3 3.5 1 -8 0 40.6 3.6 1 9 0 25.4 4.3 1 -9 0 26.2 3.3 1 10 0 6.1 3.7 1 -10 0 8.0 3.9 2 0 0 231.3 3.0 2 1 0 921.2 6.1 2 -1 0 786.2 5.8 2 2 0 5625.1 16.7 2 -2 0 4783.0 16.6 2 3 0 146.6 3.7 2 -3 0 146.1 4.0 2 4 0 32.2 3.6 2 -4 0 42.7 3.3 2 5 0 264.4 5.8 2 -5 0 331.0 6.6 2 6 0 1664.7 13.9 2 -6 0 2048.8 15.7 2 7 0 6.9 4.7 2 -7 0 -0.1 5.3 2 8 0 87.0 4.7 2 -8 0 127.7 5.0 2 9 0 185.1 5.7 2 -9 0 235.2 6.1 2 10 0 295.6 7.0 2 -10 0 404.4 7.9 3 0 0 -1.4 2.4 3 1 0 2083.5 10.4 3 -1 0 1917.4 10.0 3 2 0 336.6 4.7 3 -2 0 297.8 4.7 3 3 0 164.3 4.2 3 -3 0 141.4 4.0 3 4 0 10.3 4.0 3 -4 0 10.4 4.1 3 5 0 94.8 4.2 3 -5 0 102.7 4.6 3 6 0 157.8 5.4 3 -6 0 166.9 5.5 3 7 0 783.6 10.4 3 -7 0 929.8 11.5 3 8 0 2.8 4.4 3 -8 0 3.5 4.5 3 9 0 46.7 3.7 3 -9 0 71.7 4.4 3 10 0 6.4 3.6 3 -10 0 1.7 3.6 4 0 0 84.5 3.1 4 1 0 40.0 2.3 4 -1 0 36.9 2.2 4 2 0 13.1 2.0 4 -2 0 14.5 2.9 4 3 0 21.3 2.5 4 -3 0 19.6 2.5 4 4 0 4852.8 20.3 4 -4 0 4199.4 20.0 4 5 0 152.7 5.0 4 -5 0 146.3 5.2 4 6 0 8.8 4.1 4 -6 0 17.9 3.5 4 7 0 3.1 4.6 4 -7 0 14.4 4.7 4 8 0 89.0 4.6 4 -8 0 121.9 5.1 4 9 0 -4.5 3.9 4 -9 0 -2.7 3.9 5 0 0 1.3 2.8 5 1 0 1100.2 9.1 5 -1 0 1063.3 8.8 5 2 0 927.2 8.7 5 -2 0 852.4 8.4 5 3 0 198.1 4.8 5 -3 0 186.2 4.9 5 4 0 35.8 3.3 5 -4 0 32.4 3.5 5 5 0 93.4 4.3 5 -5 0 91.1 4.5 5 6 0 187.7 5.5 5 -6 0 186.6 5.6 5 7 0 200.8 5.9 5 -7 0 216.5 6.1 5 8 0 43.9 4.0 5 -8 0 51.7 4.0 5 9 0 34.8 3.7 5 -9 0 38.6 3.5 6 0 0 89.2 3.4 6 1 0 528.3 6.8 6 -1 0 493.9 6.6 6 2 0 1622.3 12.0 6 -2 0 1392.8 11.3 6 3 0 141.3 4.5 6 -3 0 127.3 4.5 6 4 0 102.2 4.2 6 -4 0 95.4 4.3 6 5 0 42.6 3.5 6 -5 0 48.5 3.7 6 6 0 735.4 9.8 6 -6 0 635.6 9.3 6 7 0 92.3 4.5 6 -7 0 82.8 4.5 6 8 0 12.3 4.3 6 -8 0 17.4 3.3 7 0 0 7.5 3.7 7 1 0 85.1 3.7 7 -1 0 81.8 3.6 7 2 0 38.1 3.2 7 -2 0 36.7 3.2 7 3 0 592.5 7.9 7 -3 0 517.9 7.6 7 4 0 23.6 2.8 7 -4 0 3.5 4.2 7 5 0 246.2 5.9 7 -5 0 255.1 6.2 7 6 0 -2.9 4.1 7 -6 0 6.2 4.2 7 7 0 30.2 3.7 7 -7 0 26.4 3.3 8 0 0 2486.5 15.5 8 1 0 357.0 6.3 8 -1 0 321.0 6.0 8 2 0 70.1 3.6 8 -2 0 59.6 3.4 8 3 0 2.7 3.9 8 -3 0 -1.6 3.9 8 4 0 172.5 5.1 8 -4 0 161.0 4.9 8 5 0 19.3 4.0 8 -5 0 1.9 4.4 8 6 0 48.5 3.7 8 -6 0 52.6 3.9 8 7 0 35.1 3.8 8 -7 0 24.2 3.5 9 0 0 -3.0 3.7 9 1 0 53.5 3.4 9 -1 0 54.2 3.4 9 2 0 181.4 5.0 9 -2 0 158.4 4.7 9 3 0 103.3 4.2 9 -3 0 93.3 3.9 9 4 0 1.8 3.6 9 -4 0 2.4 3.8 9 5 0 43.9 3.4 9 -5 0 37.0 3.5 10 0 0 163.9 4.8 10 1 0 0.7 3.6 10 -1 0 -5.4 3.7 10 2 0 446.6 7.5 10 -2 0 386.1 6.8 10 3 0 64.1 3.6 10 -3 0 52.8 3.5 0 0 -1 30.2 1.3 0 1 -1 1619.3 7.2 0 -1 -1 1572.5 6.9 0 2 -1 21.2 2.7 0 -2 -1 17.2 2.2 0 3 -1 1580.2 10.8 0 -3 -1 1575.4 10.0 0 4 -1 9.4 4.2 0 -4 -1 5.2 3.7 0 5 -1 330.6 6.6 0 -5 -1 315.6 6.0 0 6 -1 8.7 5.1 0 -6 -1 -0.8 4.7 0 7 -1 327.6 7.2 0 -7 -1 351.6 7.0 0 8 -1 6.4 4.5 0 -8 -1 -1.5 4.3 0 9 -1 62.2 4.4 0 -9 -1 75.4 4.2 0 10 -1 0.0 3.9 0 -10 -1 12.2 3.7 1 0 -1 1290.3 6.1 1 1 -1 857.7 6.3 1 -1 -1 853.0 5.8 1 2 -1 18.9 3.4 1 -2 -1 14.3 3.0 1 3 -1 2343.8 13.5 1 -3 -1 2475.8 13.2 1 4 -1 502.6 7.5 1 -4 -1 513.8 7.1 1 5 -1 2320.5 15.7 1 -5 -1 2714.1 16.4 1 6 -1 6.0 5.1 1 -6 -1 3.5 4.8 1 7 -1 260.2 6.5 1 -7 -1 334.3 6.9 1 8 -1 65.5 4.1 1 -8 -1 76.1 4.2 1 9 -1 23.7 3.4 1 -9 -1 44.6 3.5 1 10 -1 6.2 3.7 1 -10 -1 12.0 2.9 2 0 -1 -3.4 3.4 2 1 -1 54.5 4.0 2 -1 -1 27.2 4.3 2 2 -1 751.5 8.0 2 -2 -1 794.7 8.1 2 3 -1 38.5 3.8 2 -3 -1 40.2 3.7 2 4 -1 34.9 3.4 2 -4 -1 45.4 3.3 2 5 -1 10.3 5.0 2 -5 -1 5.3 4.8 2 6 -1 171.6 5.5 2 -6 -1 222.5 5.9 2 7 -1 4.5 5.0 2 -7 -1 5.8 5.0 2 8 -1 40.3 3.9 2 -8 -1 58.5 4.0 2 9 -1 8.4 3.8 2 -9 -1 2.9 4.1 2 10 -1 22.4 3.2 2 -10 -1 39.3 3.3 3 0 -1 1682.0 9.3 3 1 -1 2332.5 11.8 3 -1 -1 2041.7 12.0 3 2 -1 28.2 3.1 3 -2 -1 24.4 3.5 3 3 -1 758.0 8.4 3 -3 -1 779.9 8.8 3 4 -1 350.6 6.5 3 -4 -1 403.5 7.0 3 5 -1 193.6 5.6 3 -5 -1 247.2 6.0 3 6 -1 6.8 5.1 3 -6 -1 11.8 5.1 3 7 -1 455.5 8.2 3 -7 -1 563.2 8.9 3 8 -1 91.0 4.5 3 -8 -1 127.3 5.0 3 9 -1 370.8 8.0 3 -9 -1 496.3 8.7 4 0 -1 5.2 3.1 4 1 -1 657.6 6.9 4 -1 -1 587.6 6.7 4 2 -1 192.8 4.3 4 -2 -1 183.7 4.6 4 3 -1 695.9 8.2 4 -3 -1 705.7 8.7 4 4 -1 11.3 4.4 4 -4 -1 11.1 5.1 4 5 -1 184.7 5.7 4 -5 -1 217.3 6.2 4 6 -1 23.0 3.6 4 -6 -1 31.3 3.9 4 7 -1 171.9 5.6 4 -7 -1 232.8 6.3 4 8 -1 -9.3 4.5 4 -8 -1 4.3 4.6 4 9 -1 39.7 3.9 4 -9 -1 42.4 3.6 5 0 -1 40.8 2.7 5 1 -1 2076.1 12.6 5 -1 -1 1907.3 12.2 5 2 -1 77.1 3.3 5 -2 -1 80.2 3.6 5 3 -1 215.9 5.0 5 -3 -1 207.9 5.3 5 4 -1 252.1 5.9 5 -4 -1 250.3 6.2 5 5 -1 16.1 3.4 5 -5 -1 24.5 3.8 5 6 -1 25.5 3.4 5 -6 -1 33.8 4.1 5 7 -1 425.8 8.0 5 -7 -1 536.1 9.3 5 8 -1 -2.1 4.5 5 -8 -1 -3.3 4.6 5 9 -1 345.5 7.9 5 -9 -1 509.4 9.0 6 0 -1 -1.4 3.6 6 1 -1 9.1 3.8 6 -1 -1 11.8 3.9 6 2 -1 257.3 5.4 6 -2 -1 219.3 5.2 6 3 -1 41.3 3.2 6 -3 -1 37.9 3.5 6 4 -1 19.7 3.0 6 -4 -1 16.0 3.3 6 5 -1 5.5 4.4 6 -5 -1 -6.3 4.8 6 6 -1 66.4 4.4 6 -6 -1 61.3 4.3 6 7 -1 23.9 3.4 6 -7 -1 35.4 4.0 6 8 -1 12.7 4.7 6 -8 -1 17.8 3.3 7 0 -1 97.4 3.8 7 1 -1 348.2 6.2 7 -1 -1 331.0 6.0 7 2 -1 53.1 3.5 7 -2 -1 52.7 3.4 7 3 -1 431.4 7.0 7 -3 -1 361.7 6.8 7 4 -1 428.3 7.4 7 -4 -1 346.9 7.0 7 5 -1 354.0 7.0 7 -5 -1 304.7 6.7 7 6 -1 55.1 4.0 7 -6 -1 54.3 3.9 7 7 -1 151.6 5.4 7 -7 -1 145.1 5.4 8 0 -1 -7.6 3.8 8 1 -1 117.0 4.1 8 -1 -1 105.4 4.0 8 2 -1 124.0 4.3 8 -2 -1 117.6 4.1 8 3 -1 102.8 4.1 8 -3 -1 84.6 4.0 8 4 -1 -3.7 4.0 8 -4 -1 0.8 4.3 8 5 -1 36.4 3.6 8 -5 -1 29.3 3.4 8 6 -1 20.3 3.1 8 -6 -1 12.1 4.6 9 0 -1 74.2 3.6 9 1 -1 31.4 3.2 9 -1 -1 27.3 3.0 9 2 -1 52.6 3.4 9 -2 -1 41.5 3.3 9 3 -1 407.1 7.2 9 -3 -1 340.2 6.5 9 4 -1 13.1 4.0 9 -4 -1 12.4 2.9 9 5 -1 392.4 7.4 9 -5 -1 359.2 7.3 10 0 -1 0.3 3.2 10 1 -1 5.0 3.3 10 -1 -1 6.3 3.2 10 2 -1 27.0 3.1 10 -2 -1 22.0 2.8 10 3 -1 19.4 3.0 10 -3 -1 16.6 2.8 0 0 -2 2635.5 10.7 0 1 -2 -4.6 2.4 0 -1 -2 1.4 2.2 0 2 -2 2902.0 13.0 0 -2 -2 2950.5 12.8 0 3 -2 -4.5 3.2 0 -3 -2 0.3 2.8 0 4 -2 1781.1 12.7 0 -4 -2 1775.4 12.0 0 5 -2 -2.6 4.6 0 -5 -2 0.1 4.1 0 6 -2 1326.7 13.0 0 -6 -2 1372.1 12.4 0 7 -2 -3.9 4.8 0 -7 -2 -2.9 4.6 0 8 -2 335.9 7.6 0 -8 -2 380.5 7.5 0 9 -2 3.8 4.0 0 -9 -2 -3.6 3.8 0 10 -2 276.3 6.7 0 -10 -2 355.7 7.6 1 0 -2 1.6 2.4 1 1 -2 2440.0 11.2 1 -1 -2 2373.2 11.0 1 2 -2 1442.0 9.7 1 -2 -2 1307.3 8.9 1 3 -2 133.7 3.9 1 -3 -2 127.0 3.5 1 4 -2 9.8 4.5 1 -4 -2 12.5 3.8 1 5 -2 281.2 6.4 1 -5 -2 282.9 5.9 1 6 -2 96.5 5.0 1 -6 -2 108.8 4.6 1 7 -2 435.9 8.3 1 -7 -2 437.3 7.8 1 8 -2 3.7 4.5 1 -8 -2 4.9 4.4 1 9 -2 93.9 4.4 1 -9 -2 115.7 4.7 1 10 -2 38.5 3.5 1 -10 -2 39.1 3.4 2 0 -2 4995.3 16.0 2 1 -2 70.6 2.6 2 -1 -2 67.3 2.5 2 2 -2 29.8 3.7 2 -2 -2 29.8 3.1 2 3 -2 175.7 4.7 2 -3 -2 185.8 4.4 2 4 -2 2282.2 15.5 2 -4 -2 2275.4 14.7 2 5 -2 854.3 10.6 2 -5 -2 896.3 10.0 2 6 -2 47.6 4.3 2 -6 -2 51.8 3.9 2 7 -2 -1.2 4.9 2 -7 -2 -0.4 4.5 2 8 -2 573.0 9.2 2 -8 -2 745.8 10.3 2 9 -2 56.3 3.8 2 -9 -2 80.0 4.2 3 0 -2 2.8 3.1 3 1 -2 405.2 6.3 3 -1 -2 365.0 5.5 3 2 -2 425.2 6.7 3 -2 -2 403.8 6.2 3 3 -2 2122.1 15.0 3 -3 -2 2165.8 14.4 3 4 -2 -2.5 4.8 3 -4 -2 2.9 4.6 3 5 -2 340.0 7.3 3 -5 -2 411.4 7.5 3 6 -2 22.0 4.0 3 -6 -2 29.3 3.9 3 7 -2 -2.0 4.7 3 -7 -2 -7.1 4.5 3 8 -2 5.8 4.7 3 -8 -2 9.8 4.4 3 9 -2 3.7 3.9 3 -9 -2 -1.8 4.0 4 0 -2 822.1 8.7 4 1 -2 12.7 5.0 4 -1 -2 0.7 5.3 4 2 -2 3515.5 19.3 4 -2 -2 3818.0 20.1 4 3 -2 214.5 5.8 4 -3 -2 243.9 6.1 4 4 -2 1431.8 13.4 4 -4 -2 1754.1 14.7 4 5 -2 86.6 5.0 4 -5 -2 107.8 5.0 4 6 -2 1093.5 12.3 4 -6 -2 1412.3 13.6 4 7 -2 16.3 4.7 4 -7 -2 21.3 3.3 4 8 -2 7.2 4.2 4 -8 -2 4.1 4.2 4 9 -2 6.5 4.2 4 -9 -2 2.6 4.2 5 0 -2 8.0 3.5 5 1 -2 275.1 5.5 5 -1 -2 275.0 6.0 5 2 -2 649.0 8.4 5 -2 -2 635.3 9.0 5 3 -2 609.3 8.7 5 -3 -2 639.0 9.3 5 4 -2 26.9 4.8 5 -4 -2 30.4 4.1 5 5 -2 253.6 6.6 5 -5 -2 343.4 7.5 5 6 -2 156.1 5.5 5 -6 -2 196.4 6.0 5 7 -2 8.4 4.7 5 -7 -2 14.9 3.3 5 8 -2 1.7 4.5 5 -8 -2 4.2 4.5 6 0 -2 1357.2 10.9 6 1 -2 153.7 4.6 6 -1 -2 130.5 4.4 6 2 -2 69.9 4.0 6 -2 -2 75.2 4.1 6 3 -2 -1.2 4.8 6 -3 -2 15.6 5.3 6 4 -2 1546.3 13.8 6 -4 -2 1522.9 14.6 6 5 -2 34.1 4.1 6 -5 -2 41.3 4.0 6 6 -2 72.0 4.8 6 -6 -2 91.6 4.9 6 7 -2 2.8 4.5 6 -7 -2 5.5 4.5 6 8 -2 214.8 6.6 6 -8 -2 291.4 7.2 7 0 -2 -2.7 3.8 7 1 -2 491.5 7.3 7 -1 -2 448.2 7.0 7 2 -2 3.6 4.0 7 -2 -2 -0.4 4.3 7 3 -2 2.3 4.2 7 -3 -2 0.4 4.5 7 4 -2 10.0 4.5 7 -4 -2 16.1 4.9 7 5 -2 43.9 3.8 7 -5 -2 53.4 4.2 7 6 -2 29.9 4.0 7 -6 -2 31.2 3.7 7 7 -2 167.1 5.7 7 -7 -2 209.9 6.3 8 0 -2 357.4 6.3 8 1 -2 103.9 4.0 8 -1 -2 90.3 3.8 8 2 -2 587.1 8.3 8 -2 -2 468.8 7.5 8 3 -2 6.8 3.9 8 -3 -2 6.7 4.2 8 4 -2 71.3 4.2 8 -4 -2 60.2 4.4 8 5 -2 17.6 3.7 8 -5 -2 13.2 3.2 8 6 -2 239.9 6.6 8 -6 -2 245.5 6.7 9 0 -2 -3.1 3.2 9 1 -2 102.6 3.9 9 -1 -2 94.8 3.7 9 2 -2 229.8 5.5 9 -2 -2 185.1 5.0 9 3 -2 45.0 3.1 9 -3 -2 37.0 3.4 9 4 -2 2.6 3.6 9 -4 -2 1.5 4.0 9 5 -2 22.5 3.1 9 -5 -2 15.3 4.0 10 0 -2 457.5 7.3 10 1 -2 17.8 2.6 10 -1 -2 16.3 2.5 10 2 -2 10.3 3.2 10 -2 -2 9.5 2.4 0 0 -3 3.5 2.5 0 1 -3 532.7 6.1 0 -1 -3 523.7 5.9 0 2 -3 -2.6 3.0 0 -2 -3 -0.9 2.8 0 3 -3 828.6 8.5 0 -3 -3 757.9 7.9 0 4 -3 -5.8 4.3 0 -4 -3 1.8 3.6 0 5 -3 313.7 6.4 0 -5 -3 267.9 5.7 0 6 -3 -3.7 4.7 0 -6 -3 2.8 4.2 0 7 -3 259.3 6.4 0 -7 -3 237.3 5.9 0 8 -3 8.4 4.7 0 -8 -3 -5.7 4.2 0 9 -3 20.5 3.1 0 -9 -3 23.7 2.9 1 0 -3 1067.3 8.3 1 1 -3 178.0 3.7 1 -1 -3 179.0 3.8 1 2 -3 19.5 2.3 1 -2 -3 19.9 2.2 1 3 -3 1407.7 11.2 1 -3 -3 1280.1 10.3 1 4 -3 133.6 4.7 1 -4 -3 121.8 4.2 1 5 -3 1550.0 13.5 1 -5 -3 1399.1 12.1 1 6 -3 7.2 4.8 1 -6 -3 4.0 4.3 1 7 -3 173.3 5.6 1 -7 -3 162.7 5.3 1 8 -3 60.2 4.1 1 -8 -3 56.7 4.1 1 9 -3 18.3 3.1 1 -9 -3 22.6 2.9 2 0 -3 7.9 1.8 2 1 -3 16.7 2.9 2 -1 -3 8.2 1.9 2 2 -3 484.4 6.5 2 -2 -3 442.9 6.1 2 3 -3 9.9 3.8 2 -3 -3 2.3 3.5 2 4 -3 21.0 4.8 2 -4 -3 -2.2 4.2 2 5 -3 9.0 5.1 2 -5 -3 5.9 4.5 2 6 -3 149.2 5.5 2 -6 -3 146.6 5.2 2 7 -3 2.8 4.9 2 -7 -3 3.4 4.8 2 8 -3 48.6 4.2 2 -8 -3 49.9 4.0 2 9 -3 4.9 3.9 2 -9 -3 -1.1 3.8 3 0 -3 1126.6 9.3 3 1 -3 1783.9 11.7 3 -1 -3 1703.1 11.5 3 2 -3 112.7 3.9 3 -2 -3 91.2 3.4 3 3 -3 649.1 8.6 3 -3 -3 571.3 7.6 3 4 -3 133.9 5.2 3 -4 -3 132.0 4.6 3 5 -3 191.7 6.0 3 -5 -3 199.4 5.7 3 6 -3 3.0 4.9 3 -6 -3 1.8 4.7 3 7 -3 340.0 8.1 3 -7 -3 400.4 7.9 3 8 -3 71.2 4.8 3 -8 -3 95.9 4.9 3 9 -3 285.9 7.1 3 -9 -3 342.4 7.4 4 0 -3 1.5 3.6 4 1 -3 366.4 6.1 4 -1 -3 347.5 5.8 4 2 -3 96.4 4.4 4 -2 -3 74.8 3.7 4 3 -3 295.7 6.8 4 -3 -3 283.7 6.0 4 4 -3 14.2 5.3 4 -4 -3 0.3 4.9 4 5 -3 108.7 4.9 4 -5 -3 110.8 4.9 4 6 -3 19.3 4.6 4 -6 -3 28.4 3.5 4 7 -3 151.0 5.9 4 -7 -3 191.4 5.9 4 8 -3 7.7 4.3 4 -8 -3 2.1 4.3 5 0 -3 12.4 2.7 5 1 -3 1560.6 13.5 5 -1 -3 1571.0 12.9 5 2 -3 17.7 5.2 5 -2 -3 15.1 5.3 5 3 -3 232.8 6.6 5 -3 -3 241.3 6.3 5 4 -3 131.0 5.4 5 -4 -3 151.0 5.5 5 5 -3 34.4 4.3 5 -5 -3 43.6 3.9 5 6 -3 1.6 5.2 5 -6 -3 9.9 5.0 5 7 -3 309.2 7.4 5 -7 -3 426.3 8.4 5 8 -3 4.1 4.2 5 -8 -3 0.9 4.1 6 0 -3 2.5 4.4 6 1 -3 5.2 5.7 6 -1 -3 4.3 5.9 6 2 -3 132.8 5.6 6 -2 -3 151.9 5.9 6 3 -3 12.8 5.8 6 -3 -3 31.2 4.1 6 4 -3 -2.0 5.5 6 -4 -3 -1.9 5.4 6 5 -3 4.0 5.2 6 -5 -3 -0.1 5.1 6 6 -3 51.3 4.6 6 -6 -3 68.5 4.3 6 7 -3 14.9 3.5 6 -7 -3 14.0 5.3 7 0 -3 116.2 4.1 7 1 -3 205.2 5.3 7 -1 -3 196.1 5.7 7 2 -3 23.5 4.1 7 -2 -3 17.8 4.1 7 3 -3 281.1 6.8 7 -3 -3 285.5 7.2 7 4 -3 171.4 5.8 7 -4 -3 224.1 6.7 7 5 -3 199.5 6.3 7 -5 -3 263.7 6.9 7 6 -3 26.3 3.8 7 -6 -3 46.4 4.1 8 0 -3 0.5 3.1 8 1 -3 51.4 3.1 8 -1 -3 47.4 3.2 8 2 -3 66.5 3.6 8 -2 -3 61.3 3.8 8 3 -3 67.7 3.8 8 -3 -3 57.2 4.2 8 4 -3 -7.0 4.0 8 -4 -3 -1.5 4.3 8 5 -3 29.7 3.6 8 -5 -3 26.6 4.5 9 0 -3 65.2 3.3 9 1 -3 8.0 2.2 9 -1 -3 7.5 3.4 9 2 -3 30.6 3.0 9 -2 -3 23.5 2.9 9 3 -3 222.0 6.1 9 -3 -3 203.2 5.7 0 0 -4 7755.2 23.8 0 1 -4 3.3 3.3 0 -1 -4 4.6 3.4 0 2 -4 66.3 3.3 0 -2 -4 73.1 3.3 0 3 -4 3.0 3.9 0 -3 -4 -5.1 3.7 0 4 -4 507.4 7.5 0 -4 -4 460.8 7.0 0 5 -4 -7.7 4.3 0 -5 -4 -2.5 3.9 0 6 -4 93.4 4.4 0 -6 -4 80.6 4.1 0 7 -4 0.6 4.2 0 -7 -4 -9.6 4.1 0 8 -4 1136.6 12.7 0 -8 -4 946.5 11.4 1 0 -4 3.2 3.0 1 1 -4 323.4 5.4 1 -1 -4 326.2 5.5 1 2 -4 363.3 5.9 1 -2 -4 368.0 5.9 1 3 -4 987.5 9.9 1 -3 -4 934.1 9.4 1 4 -4 6.6 4.5 1 -4 -4 4.8 4.0 1 5 -4 480.8 8.2 1 -5 -4 391.0 6.9 1 6 -4 190.9 5.6 1 -6 -4 159.0 5.1 1 7 -4 1.3 4.4 1 -7 -4 -2.4 4.1 1 8 -4 7.6 4.3 1 -8 -4 14.1 4.0 2 0 -4 70.0 3.1 2 1 -4 191.5 4.5 2 -1 -4 188.9 4.4 2 2 -4 2409.4 14.4 2 -2 -4 2277.8 13.9 2 3 -4 14.1 4.3 2 -3 -4 -0.5 4.0 2 4 -4 16.9 3.3 2 -4 -4 24.1 3.5 2 5 -4 171.4 5.2 2 -5 -4 145.4 4.7 2 6 -4 953.0 11.2 2 -6 -4 798.7 10.1 2 7 -4 4.6 4.4 2 -7 -4 5.1 4.1 2 8 -4 60.0 4.1 2 -8 -4 52.6 4.0 3 0 -4 2.2 3.5 3 1 -4 784.9 8.4 3 -1 -4 753.5 8.5 3 2 -4 117.7 4.1 3 -2 -4 115.1 4.1 3 3 -4 60.4 3.8 3 -3 -4 47.7 3.3 3 4 -4 2.7 4.2 3 -4 -4 12.0 4.2 3 5 -4 67.7 4.1 3 -5 -4 56.4 3.7 3 6 -4 81.0 4.5 3 -6 -4 68.1 3.8 3 7 -4 388.8 7.9 3 -7 -4 348.6 7.5 3 8 -4 -1.5 4.2 3 -8 -4 1.5 4.2 4 0 -4 126.2 4.1 4 1 -4 6.7 3.9 4 -1 -4 4.6 4.1 4 2 -4 7.2 4.2 4 -2 -4 -3.3 4.2 4 3 -4 15.3 4.6 4 -3 -4 5.2 4.4 4 4 -4 2464.6 17.2 4 -4 -4 2219.5 15.9 4 5 -4 76.4 4.3 4 -5 -4 66.0 4.2 4 6 -4 32.7 3.7 4 -6 -4 20.5 3.3 4 7 -4 6.3 4.6 4 -7 -4 -1.7 4.2 4 8 -4 66.9 4.5 4 -8 -4 89.9 4.8 5 0 -4 1.9 3.8 5 1 -4 387.3 6.5 5 -1 -4 365.2 6.5 5 2 -4 349.9 6.7 5 -2 -4 319.0 6.2 5 3 -4 85.3 4.4 5 -3 -4 80.1 4.1 5 4 -4 10.1 3.9 5 -4 -4 7.1 4.5 5 5 -4 57.6 4.3 5 -5 -4 57.8 4.2 5 6 -4 71.5 4.9 5 -6 -4 66.3 4.2 5 7 -4 105.4 5.0 5 -7 -4 106.3 4.8 6 0 -4 19.5 2.7 6 1 -4 188.2 5.1 6 -1 -4 172.9 4.9 6 2 -4 783.0 10.6 6 -2 -4 704.4 9.4 6 3 -4 44.7 4.0 6 -3 -4 37.9 3.6 6 4 -4 60.2 4.6 6 -4 -4 55.0 4.0 6 5 -4 25.2 4.0 6 -5 -4 25.5 3.5 6 6 -4 340.4 8.1 6 -6 -4 409.6 8.3 7 0 -4 1.1 3.1 7 1 -4 40.9 3.9 7 -1 -4 32.7 3.7 7 2 -4 21.6 3.6 7 -2 -4 19.7 3.2 7 3 -4 228.5 6.7 7 -3 -4 249.2 6.7 7 4 -4 2.1 4.4 7 -4 -4 4.3 4.3 7 5 -4 94.4 4.8 7 -5 -4 120.5 5.2 8 0 -4 1025.7 11.4 8 1 -4 129.2 5.2 8 -1 -4 149.7 6.1 8 2 -4 25.0 3.5 8 -2 -4 34.6 4.2 8 3 -4 -2.3 4.6 8 -3 -4 3.1 4.4 8 4 -4 79.1 5.2 8 -4 -4 97.4 4.9 9 0 -4 -5.8 3.1 9 1 -4 23.2 3.8 9 -1 -4 25.1 3.5 0 0 -5 8.8 3.5 0 1 -5 230.1 5.0 0 -1 -5 237.3 5.2 0 2 -5 3.8 3.8 0 -2 -5 -2.1 3.7 0 3 -5 231.0 5.2 0 -3 -5 220.4 5.1 0 4 -5 8.9 3.9 0 -4 -5 -3.7 3.6 0 5 -5 36.3 3.3 0 -5 -5 26.3 2.9 0 6 -5 2.8 4.0 0 -6 -5 0.9 3.5 0 7 -5 108.4 4.6 0 -7 -5 92.1 4.2 1 0 -5 86.1 3.6 1 1 -5 237.6 5.1 1 -1 -5 257.1 5.3 1 2 -5 6.3 3.8 1 -2 -5 4.6 3.6 1 3 -5 843.4 9.3 1 -3 -5 822.9 9.3 1 4 -5 158.3 4.9 1 -4 -5 133.6 4.4 1 5 -5 1059.8 11.5 1 -5 -5 796.1 9.7 1 6 -5 -3.0 4.3 1 -6 -5 -2.5 3.9 1 7 -5 160.1 5.4 1 -7 -5 124.9 4.7 2 0 -5 4.4 3.6 2 1 -5 5.6 3.6 2 -1 -5 -1.6 3.8 2 2 -5 216.3 5.1 2 -2 -5 206.8 5.0 2 3 -5 13.6 2.7 2 -3 -5 12.2 2.5 2 4 -5 15.7 2.9 2 -4 -5 10.0 3.8 2 5 -5 1.3 4.1 2 -5 -5 9.3 3.7 2 6 -5 46.1 3.8 2 -6 -5 40.2 3.6 2 7 -5 -3.2 4.3 2 -7 -5 1.5 3.9 3 0 -5 239.2 5.2 3 1 -5 534.9 7.4 3 -1 -5 537.5 7.5 3 2 -5 -3.8 3.9 3 -2 -5 0.9 3.7 3 3 -5 186.9 4.9 3 -3 -5 160.4 4.9 3 4 -5 100.6 4.3 3 -4 -5 73.8 3.8 3 5 -5 80.9 4.2 3 -5 -5 65.6 3.8 3 6 -5 4.3 4.2 3 -6 -5 6.5 4.0 3 7 -5 191.9 5.8 3 -7 -5 154.4 5.4 4 0 -5 -1.8 3.7 4 1 -5 84.5 3.6 4 -1 -5 77.7 3.7 4 2 -5 28.9 2.8 4 -2 -5 25.0 2.8 4 3 -5 201.0 5.3 4 -3 -5 173.6 5.0 4 4 -5 0.1 4.2 4 -4 -5 0.3 3.8 4 5 -5 45.2 3.7 4 -5 -5 29.8 3.2 4 6 -5 4.3 4.3 4 -6 -5 10.8 4.1 5 0 -5 7.8 3.4 5 1 -5 465.1 7.1 5 -1 -5 470.6 7.3 5 2 -5 33.7 3.1 5 -2 -5 32.5 3.1 5 3 -5 63.3 3.7 5 -3 -5 60.1 3.5 5 4 -5 75.0 4.1 5 -4 -5 60.4 3.8 5 5 -5 11.7 3.0 5 -5 -5 11.1 4.0 5 6 -5 29.0 3.4 5 -6 -5 28.4 3.6 6 0 -5 -2.5 3.1 6 1 -5 9.6 3.3 6 -1 -5 11.1 3.4 6 2 -5 82.1 3.8 6 -2 -5 71.7 3.5 6 3 -5 4.2 3.9 6 -3 -5 7.5 3.6 6 4 -5 8.2 4.0 6 -4 -5 4.0 3.8 6 5 -5 3.3 4.0 6 -5 -5 5.0 3.8 7 0 -5 5.3 2.7 7 1 -5 119.0 4.1 7 -1 -5 107.8 4.0 7 2 -5 26.3 3.0 7 -2 -5 26.3 2.8 7 3 -5 199.0 5.8 7 -3 -5 161.2 5.1 7 4 -5 176.4 5.9 8 0 -5 3.2 3.4 8 1 -5 35.7 3.0 8 -1 -5 27.7 3.0 0 0 -6 344.4 6.2 0 1 -6 1.0 3.5 0 -1 -6 0.1 3.4 0 2 -6 762.6 9.4 0 -2 -6 802.8 9.5 0 3 -6 8.5 3.4 0 -3 -6 7.0 3.2 0 4 -6 130.0 4.5 0 -4 -6 108.2 4.2 0 5 -6 -0.6 3.8 0 -5 -6 -2.4 3.4 0 6 -6 445.5 7.9 0 -6 -6 332.9 7.0 1 0 -6 5.8 3.4 1 1 -6 317.0 6.0 1 -1 -6 328.1 6.1 1 2 -6 143.3 4.5 1 -2 -6 149.6 4.5 1 3 -6 34.2 3.1 1 -3 -6 31.5 2.9 1 4 -6 -2.5 3.5 1 -4 -6 7.0 3.4 1 5 -6 81.6 3.9 1 -5 -6 68.1 3.6 1 6 -6 30.5 3.2 1 -6 -6 23.0 3.0 2 0 -6 949.7 10.0 2 1 -6 6.5 3.8 2 -1 -6 6.0 3.7 2 2 -6 6.5 3.6 2 -2 -6 4.4 3.8 2 3 -6 20.9 2.8 2 -3 -6 25.1 2.8 2 4 -6 579.6 8.4 2 -4 -6 497.9 7.9 2 5 -6 159.2 5.0 2 -5 -6 120.3 4.4 2 6 -6 29.4 3.6 2 -6 -6 15.9 3.8 3 0 -6 -3.3 3.5 3 1 -6 64.6 3.4 3 -1 -6 58.6 3.3 3 2 -6 57.6 3.3 3 -2 -6 57.2 3.4 3 3 -6 373.6 6.6 3 -3 -6 348.2 6.5 3 4 -6 3.5 3.5 3 -4 -6 -4.5 3.7 3 5 -6 109.8 4.6 3 -5 -6 77.9 4.0 4 0 -6 82.7 3.8 4 1 -6 3.9 3.4 4 -1 -6 4.2 3.6 4 2 -6 629.2 8.4 4 -2 -6 642.2 8.8 4 3 -6 34.9 3.2 4 -3 -6 30.8 3.1 4 4 -6 288.9 6.4 4 -4 -6 216.2 5.5 4 5 -6 23.8 3.9 4 -5 -6 17.8 3.0 5 0 -6 6.1 2.9 5 1 -6 55.0 3.2 5 -1 -6 56.4 3.3 5 2 -6 95.1 3.8 5 -2 -6 94.4 3.9 5 3 -6 126.9 4.5 5 -3 -6 105.2 4.3 5 4 -6 5.3 3.6 5 -4 -6 4.6 3.5 6 0 -6 263.8 5.7 6 1 -6 50.2 3.1 6 -1 -6 47.5 3.0 6 2 -6 13.9 2.5 6 -2 -6 16.0 2.4 0 0 -7 -3.2 3.3 0 1 -7 18.0 2.6 0 -1 -7 19.8 2.6 0 2 -7 -2.0 3.3 0 -2 -7 0.9 3.2 0 3 -7 67.9 3.7 0 -3 -7 69.1 3.4 0 4 -7 8.5 3.3 0 -4 -7 -1.9 3.2 1 0 -7 92.7 3.8 1 1 -7 30.9 2.9 1 -1 -7 28.9 2.9 1 2 -7 1.4 3.2 1 -2 -7 1.8 3.2 1 3 -7 174.9 5.0 1 -3 -7 168.4 4.9 1 4 -7 2.6 3.4 1 -4 -7 6.0 3.4 2 0 -7 -2.1 3.2 2 1 -7 -2.5 3.5 2 -1 -7 3.6 3.4 2 2 -7 47.9 3.2 2 -2 -7 49.2 3.2 2 3 -7 -0.3 3.5 2 -3 -7 -5.2 3.7 3 0 -7 95.6 4.0 3 1 -7 256.4 5.7 3 -1 -7 245.1 5.7 3 2 -7 25.8 2.9 3 -2 -7 23.1 2.9 4 0 -7 0.2 3.2 4 1 -7 34.6 3.1 4 -1 -7 36.4 3.0 0 0 0 0.0 0.0 #==END data_ADA_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 ; Crystal structure of adamite at high temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_mineral ; ADAMITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As H O5 Zn2' _chemical_formula_weight 286.71 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' 'As' 'As' 0.0499 2.0058 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_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 8.5611(14) _cell_length_b 8.3756(16) _cell_length_c 6.0750(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 435.60(13) _cell_formula_units_Z 4 _cell_measurement_temperature 773(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour 'LIGHT GREEN' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 18.460 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_T_max 0.1118 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_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 500 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 26.54 _reflns_number_total 499 _reflns_number_gt 405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1609P)^2^+4.5938P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_secondary difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 499 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2337 _refine_ls_wR_factor_gt 0.2208 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.2530(4) 0.0474(9) Uani 1 2 d S . . Zn2 Zn 0.1371(3) 0.6331(3) 0.0000 0.0373(8) Uani 1 2 d S . . As1 As 0.24177(19) 0.2500(2) 0.0000 0.0286(7) Uani 1 2 d S . . O1 O 0.3558(12) 0.2679(13) 0.2236(18) 0.044(3) Uani 1 1 d . . . O2 O 0.1424(17) 0.0752(17) 0.0000 0.036(3) Uani 1 2 d S . . O3 O 0.1053(16) 0.3955(17) 0.0000 0.041(4) Uani 1 2 d S . . O4 O 0.3715(17) 0.6085(18) 0.0000 0.038(3) Uani 1 2 d S . . H1 H 0.4322 0.7254 0.0000 0.046 Uiso 1 2 d SR . . 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 Zn1 0.0453(15) 0.0688(19) 0.0280(14) 0.000 0.000 -0.0177(11) Zn2 0.0331(13) 0.0428(14) 0.0359(13) 0.000 0.000 0.0003(10) As1 0.0250(11) 0.0342(12) 0.0267(12) 0.000 0.000 -0.0010(7) O1 0.051(6) 0.049(6) 0.031(5) 0.011(5) -0.018(4) -0.017(5) O2 0.044(8) 0.033(7) 0.030(7) 0.000 0.000 -0.011(6) O3 0.023(6) 0.034(7) 0.067(11) 0.000 0.000 0.000(5) O4 0.041(8) 0.047(8) 0.027(7) 0.000 0.000 0.002(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O2 2.060(10) 5 ? Zn1 O2 2.060(10) . ? Zn1 O4 2.071(11) 3_545 ? Zn1 O4 2.071(11) 7_566 ? Zn1 O1 2.307(9) 4_455 ? Zn1 O1 2.307(9) 3_545 ? Zn1 Zn1 3.001(5) 5_556 ? Zn2 O3 2.009(15) . ? Zn2 O4 2.017(16) . ? Zn2 O1 2.024(10) 3 ? Zn2 O1 2.024(10) 8_665 ? Zn2 O3 2.089(13) 5_565 ? Zn2 Zn2 3.237(5) 5_565 ? As1 O1 1.680(10) . ? As1 O1 1.680(10) 6 ? As1 O3 1.688(14) . ? As1 O2 1.693(14) . ? O1 Zn2 2.024(10) 3_545 ? O1 Zn1 2.307(9) 3 ? O2 Zn1 2.060(10) 5 ? O2 O2 2.74(3) 5 ? O2 O4 3.053(2) 3_544 ? O3 Zn2 2.089(13) 5_565 ? O3 O3 2.51(3) 5_565 ? O4 Zn1 2.071(11) 3 ? O4 Zn1 2.071(11) 7_665 ? O4 O4 2.85(3) 5_665 ? O4 H1 1.1082 . ? 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 Zn1 O2 83.5(6) 5 . ? O2 Zn1 O4 171.5(6) 5 3_545 ? O2 Zn1 O4 95.3(4) . 3_545 ? O2 Zn1 O4 95.3(4) 5 7_566 ? O2 Zn1 O4 171.5(6) . 7_566 ? O4 Zn1 O4 87.1(6) 3_545 7_566 ? O2 Zn1 O1 89.3(5) 5 4_455 ? O2 Zn1 O1 96.0(5) . 4_455 ? O4 Zn1 O1 82.5(5) 3_545 4_455 ? O4 Zn1 O1 92.3(5) 7_566 4_455 ? O2 Zn1 O1 96.0(5) 5 3_545 ? O2 Zn1 O1 89.3(5) . 3_545 ? O4 Zn1 O1 92.3(5) 3_545 3_545 ? O4 Zn1 O1 82.5(5) 7_566 3_545 ? O1 Zn1 O1 172.9(6) 4_455 3_545 ? O2 Zn1 Zn1 138.2(3) 5 5_556 ? O2 Zn1 Zn1 138.2(3) . 5_556 ? O4 Zn1 Zn1 43.6(3) 3_545 5_556 ? O4 Zn1 Zn1 43.6(3) 7_566 5_556 ? O1 Zn1 Zn1 86.5(3) 4_455 5_556 ? O1 Zn1 Zn1 86.5(3) 3_545 5_556 ? O3 Zn2 O4 91.9(6) . . ? O3 Zn2 O1 123.8(3) . 3 ? O4 Zn2 O1 91.6(4) . 3 ? O3 Zn2 O1 123.8(3) . 8_665 ? O4 Zn2 O1 91.6(4) . 8_665 ? O1 Zn2 O1 112.1(7) 3 8_665 ? O3 Zn2 O3 75.6(6) . 5_565 ? O4 Zn2 O3 167.6(6) . 5_565 ? O1 Zn2 O3 95.4(4) 3 5_565 ? O1 Zn2 O3 95.4(4) 8_665 5_565 ? O3 Zn2 Zn2 38.7(4) . 5_565 ? O4 Zn2 Zn2 130.6(5) . 5_565 ? O1 Zn2 Zn2 113.9(3) 3 5_565 ? O1 Zn2 Zn2 113.9(3) 8_665 5_565 ? O3 Zn2 Zn2 36.9(4) 5_565 5_565 ? O1 As1 O1 107.9(7) . 6 ? O1 As1 O3 109.7(5) . . ? O1 As1 O3 109.7(5) 6 . ? O1 As1 O2 111.7(4) . . ? O1 As1 O2 111.7(4) 6 . ? O3 As1 O2 106.0(7) . . ? As1 O1 Zn2 129.7(5) . 3_545 ? As1 O1 Zn1 115.9(5) . 3 ? Zn2 O1 Zn1 113.8(5) 3_545 3 ? As1 O2 Zn1 124.2(5) . 5 ? As1 O2 Zn1 124.2(5) . . ? Zn1 O2 Zn1 96.5(6) 5 . ? As1 O2 O2 147.5(11) . 5 ? Zn1 O2 O2 48.2(3) 5 5 ? Zn1 O2 O2 48.2(3) . 5 ? As1 O2 O4 86.6(4) . 3_544 ? Zn1 O2 O4 42.5(3) 5 3_544 ? Zn1 O2 O4 138.4(7) . 3_544 ? O2 O2 O4 90.4(4) 5 3_544 ? As1 O3 Zn2 128.4(7) . . ? As1 O3 Zn2 127.2(8) . 5_565 ? Zn2 O3 Zn2 104.4(6) . 5_565 ? As1 O3 O3 178.0(11) . 5_565 ? Zn2 O3 O3 53.6(5) . 5_565 ? Zn2 O3 O3 50.7(5) 5_565 5_565 ? Zn2 O4 Zn1 125.0(5) . 3 ? Zn2 O4 Zn1 125.0(5) . 7_665 ? Zn1 O4 Zn1 92.9(6) 3 7_665 ? Zn2 O4 O4 146.3(10) . 5_665 ? Zn1 O4 O4 46.4(3) 3 5_665 ? Zn1 O4 O4 46.4(3) 7_665 5_665 ? Zn2 O4 H1 112.1 . . ? Zn1 O4 H1 98.0 3 . ? Zn1 O4 H1 98.0 7_665 . ? O4 O4 H1 101.6 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 1.11 2.27 2.892(17) 113.4 5_665 O4 H1 O1 1.11 2.27 2.892(17) 113.4 2_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.684 _refine_diff_density_min -2.071 _refine_diff_density_rms 0.503 _iucr_refine_instructions_details ; TITL ADA_500C Pnnm ba-c CELL 0.71073 8.5611 8.3756 6.0750 90.000 90.000 90.000 ZERR 4 0.0014 0.0016 0.0009 0.000 0.000 0.000 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 AS O ZN UNIT 4 4 20 8 MERG 2 ACTA EQIV $1 -x, -y, -z EQIV $2 -x, -y, -z+1 EQIV $3 -x+1,-y+1,-z EQIV $4 -x+1/2,+y-1/2,-z-1/2 EQIV $5 -x,-y+1,-z FREE ZN1 ZN1_$1 BIND O4 O4_$3 BIND O2 O2_$1 BIND O2 O4_$4 BIND O3 O3_$5 BIND ZN1 ZN1_$2 BIND ZN2 ZN2_$5 HTAB O4 O1_$3 EQIV $6 -x+1, -y+1, z HTAB O4 O1_$6 BOND $H L.S. 4 LIST 4 FMAP 2 PLAN 35 WGHT 0.160900 4.593800 FVAR 0.37008 ZN1 4 0.000000 0.000000 0.252972 10.50000 0.04528 0.06877 = 0.02803 0.00000 0.00000 -0.01773 ZN2 4 0.137086 0.633095 0.000000 10.50000 0.03307 0.04283 = 0.03594 0.00000 0.00000 0.00028 AS1 2 0.241767 0.249971 0.000000 10.50000 0.02500 0.03421 = 0.02672 0.00000 0.00000 -0.00101 O1 3 0.355829 0.267922 0.223602 11.00000 0.05063 0.04941 = 0.03055 0.01068 -0.01769 -0.01676 O2 3 0.142360 0.075166 0.000000 10.50000 0.04373 0.03297 = 0.03045 0.00000 0.00000 -0.01123 O3 3 0.105264 0.395478 0.000000 10.50000 0.02260 0.03365 = 0.06678 0.00000 0.00000 -0.00049 O4 3 0.371511 0.608500 0.000000 10.50000 0.04106 0.04676 = 0.02700 0.00000 0.00000 0.00202 AFIX 3 H1 1 0.432213 0.725362 0.000000 10.50000 -1.20000 HKLF 4 REM ADA_500C Pnnm ba-c REM R1 = 0.0825 for 405 Fo > 4sig(Fo) and 0.0941 for all 499 data REM 45 parameters refined using 0 restraints END WGHT 0.1608 4.6339 ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 1 0 3.9 0.8 0 2 0 275.5 3.5 0 3 0 -1.6 2.5 0 4 0 590.0 6.3 0 5 0 2.7 3.3 0 6 0 198.8 5.1 0 7 0 -0.6 3.8 0 8 0 1178.2 10.9 0 9 0 -5.3 3.5 0 10 0 75.6 3.6 1 0 0 1.5 1.0 1 1 0 1192.8 5.3 1 2 0 941.5 6.1 1 3 0 1770.6 9.4 1 4 0 16.3 2.7 1 5 0 660.2 7.4 1 6 0 239.5 5.2 1 7 0 8.1 3.8 1 8 0 10.6 3.6 1 9 0 6.4 3.5 1 10 0 1.6 3.0 2 0 0 246.1 3.2 2 1 0 816.1 5.7 2 2 0 5629.7 15.6 2 3 0 86.7 2.9 2 4 0 29.1 3.0 2 5 0 173.6 4.4 2 6 0 1045.0 9.7 2 7 0 1.5 3.8 2 8 0 69.7 3.8 2 9 0 107.0 4.2 2 10 0 172.3 4.9 3 0 0 -6.5 2.5 3 1 0 2077.9 10.0 3 2 0 278.0 4.2 3 3 0 120.9 3.6 3 4 0 11.2 3.3 3 5 0 54.5 3.6 3 6 0 103.6 4.1 3 7 0 467.2 7.1 3 8 0 2.6 3.3 3 9 0 31.5 3.3 3 10 0 1.5 2.8 4 0 0 53.4 2.9 4 1 0 36.2 2.4 4 2 0 7.4 2.9 4 3 0 17.8 2.3 4 4 0 4135.7 17.5 4 5 0 117.9 4.2 4 6 0 -1.9 4.1 4 7 0 1.9 3.7 4 8 0 54.5 3.6 4 9 0 4.4 3.0 5 0 0 -0.3 2.9 5 1 0 1084.0 8.8 5 2 0 840.0 8.1 5 3 0 139.8 4.1 5 4 0 28.4 3.2 5 5 0 74.6 4.2 5 6 0 121.6 4.4 5 7 0 120.6 4.5 5 8 0 26.6 3.0 5 9 0 15.1 2.6 6 0 0 75.6 3.5 6 1 0 472.4 6.6 6 2 0 1440.0 10.9 6 3 0 129.5 4.3 6 4 0 93.1 4.0 6 5 0 31.5 3.2 6 6 0 483.7 7.5 6 7 0 68.7 3.8 6 8 0 16.8 3.3 7 0 0 -0.8 3.7 7 1 0 70.1 3.7 7 2 0 33.3 3.6 7 3 0 464.0 7.1 7 4 0 15.2 2.7 7 5 0 168.4 5.0 7 6 0 -1.7 3.6 7 7 0 20.5 3.0 7 8 0 9.6 3.2 8 0 0 2363.3 14.8 8 1 0 303.3 6.0 8 2 0 55.5 3.4 8 3 0 4.5 3.7 8 4 0 128.3 4.8 8 5 0 10.5 3.5 8 6 0 43.6 3.5 8 7 0 18.7 2.9 9 0 0 -8.3 3.8 9 1 0 33.4 3.8 9 2 0 138.7 4.9 9 3 0 69.5 3.8 9 4 0 -0.2 3.5 9 5 0 29.3 3.5 10 0 0 152.8 4.8 10 1 0 0.5 3.5 10 2 0 326.6 6.5 10 3 0 51.9 3.5 0 0 -1 26.8 1.3 0 1 -1 1452.4 6.7 0 2 -1 15.9 2.4 0 3 -1 1105.6 7.9 0 4 -1 7.2 3.2 0 5 -1 206.1 5.1 0 6 -1 -7.7 4.1 0 7 -1 189.9 5.4 0 8 -1 4.6 3.7 0 9 -1 39.2 3.9 0 10 -1 10.1 3.1 1 0 -1 1337.8 6.4 1 1 -1 658.3 5.1 1 2 -1 6.0 2.7 1 3 -1 1554.5 9.5 1 4 -1 294.1 5.1 1 5 -1 1521.6 11.1 1 6 -1 2.5 4.0 1 7 -1 153.3 4.9 1 8 -1 39.0 3.5 1 9 -1 23.1 3.1 1 10 -1 2.1 3.2 2 0 -1 22.8 3.2 2 1 -1 21.5 3.2 2 2 -1 443.5 5.3 2 3 -1 22.1 3.0 2 4 -1 16.6 2.8 2 5 -1 -0.2 3.9 2 6 -1 95.5 4.2 2 7 -1 0.3 4.1 2 8 -1 28.5 3.4 2 9 -1 1.3 3.5 2 10 -1 12.0 3.0 3 0 -1 1827.0 10.1 3 1 -1 2142.2 11.0 3 2 -1 15.5 2.7 3 3 -1 514.0 6.3 3 4 -1 221.5 5.0 3 5 -1 128.7 4.4 3 6 -1 4.3 4.1 3 7 -1 262.8 6.0 3 8 -1 64.5 3.9 3 9 -1 202.5 5.5 3 10 -1 15.9 2.8 4 0 -1 7.6 3.4 4 1 -1 620.8 6.8 4 2 -1 152.4 3.9 4 3 -1 520.0 6.7 4 4 -1 -1.7 3.8 4 5 -1 121.4 4.5 4 6 -1 10.8 4.2 4 7 -1 98.5 4.2 4 8 -1 -0.8 3.8 4 9 -1 17.1 3.0 5 0 -1 29.0 3.8 5 1 -1 1990.5 12.3 5 2 -1 71.7 3.3 5 3 -1 168.9 4.7 5 4 -1 185.8 5.2 5 5 -1 9.5 3.5 5 6 -1 11.4 4.3 5 7 -1 269.2 6.3 5 8 -1 -2.2 3.7 5 9 -1 215.9 5.7 6 0 -1 0.0 3.7 6 1 -1 6.6 4.0 6 2 -1 201.2 5.0 6 3 -1 33.0 3.4 6 4 -1 13.2 4.3 6 5 -1 3.9 3.9 6 6 -1 34.7 3.5 6 7 -1 12.0 3.6 6 8 -1 5.5 3.6 7 0 -1 78.6 4.3 7 1 -1 334.1 6.4 7 2 -1 49.1 3.7 7 3 -1 349.1 6.5 7 4 -1 333.6 6.4 7 5 -1 230.7 5.7 7 6 -1 39.0 3.4 7 7 -1 95.4 4.7 8 0 -1 0.7 3.8 8 1 -1 96.9 4.4 8 2 -1 108.4 4.5 8 3 -1 78.4 4.0 8 4 -1 2.4 3.9 8 5 -1 25.4 3.2 8 6 -1 18.3 3.7 9 0 -1 69.1 4.0 9 1 -1 26.2 3.8 9 2 -1 43.7 3.5 9 3 -1 327.3 6.6 9 4 -1 12.1 3.1 9 5 -1 295.3 6.5 10 0 -1 -2.9 3.2 10 1 -1 -4.1 3.5 10 2 -1 22.9 3.0 10 3 -1 11.5 3.4 0 0 -2 2863.9 11.5 0 1 -2 -2.2 2.4 0 2 -2 2691.9 12.1 0 3 -2 -5.5 2.9 0 4 -2 1179.6 9.6 0 5 -2 -2.7 3.7 0 6 -2 768.2 8.8 0 7 -2 -0.9 3.8 0 8 -2 203.9 5.4 0 9 -2 -1.4 3.3 0 10 -2 147.7 4.9 1 0 -2 -2.0 2.5 1 1 -2 2347.6 11.0 1 2 -2 1119.3 8.2 1 3 -2 85.5 3.2 1 4 -2 9.0 3.6 1 5 -2 151.0 4.7 1 6 -2 48.7 4.3 1 7 -2 208.1 5.3 1 8 -2 6.1 3.4 1 9 -2 46.3 3.4 1 10 -2 21.2 2.8 2 0 -2 5276.9 16.9 2 1 -2 59.6 2.8 2 2 -2 20.4 2.9 2 3 -2 102.9 3.4 2 4 -2 1297.0 10.2 2 5 -2 464.5 7.0 2 6 -2 24.6 4.2 2 7 -2 1.9 3.7 2 8 -2 317.2 6.6 2 9 -2 25.7 3.8 3 0 -2 1.6 3.2 3 1 -2 264.3 4.9 3 2 -2 247.9 4.8 3 3 -2 1226.1 9.8 3 4 -2 -2.2 3.7 3 5 -2 182.9 5.1 3 6 -2 13.7 4.2 3 7 -2 -2.3 3.8 3 8 -2 16.3 3.3 3 9 -2 4.4 3.2 4 0 -2 598.0 7.1 4 1 -2 11.4 3.7 4 2 -2 2148.7 12.8 4 3 -2 126.5 4.0 4 4 -2 819.8 8.8 4 5 -2 41.5 3.8 4 6 -2 584.3 8.3 4 7 -2 12.1 3.2 4 8 -2 -4.2 3.7 4 9 -2 1.5 3.4 5 0 -2 1.9 3.8 5 1 -2 206.7 4.9 5 2 -2 419.2 6.5 5 3 -2 354.7 6.3 5 4 -2 20.8 3.6 5 5 -2 141.5 4.8 5 6 -2 94.7 4.2 5 7 -2 7.4 3.8 5 8 -2 2.1 3.5 6 0 -2 1305.0 11.1 6 1 -2 130.3 4.9 6 2 -2 62.2 3.8 6 3 -2 7.9 4.1 6 4 -2 943.4 10.1 6 5 -2 5.4 4.2 6 6 -2 45.3 3.7 6 7 -2 3.2 3.6 6 8 -2 106.3 4.4 7 0 -2 -6.8 4.0 7 1 -2 377.9 6.9 7 2 -2 -1.9 3.8 7 3 -2 -2.2 3.8 7 4 -2 10.5 3.8 7 5 -2 28.4 4.2 7 6 -2 14.9 3.0 7 7 -2 78.6 4.2 8 0 -2 314.2 6.7 8 1 -2 75.1 4.2 8 2 -2 426.7 7.4 8 3 -2 5.6 3.8 8 4 -2 35.9 3.2 8 5 -2 6.0 3.7 8 6 -2 133.3 5.0 9 0 -2 -8.1 3.3 9 1 -2 73.6 4.1 9 2 -2 165.4 5.2 9 3 -2 26.2 2.9 9 4 -2 2.4 3.3 9 5 -2 8.6 3.7 10 0 -2 364.4 7.1 10 1 -2 13.4 2.7 10 2 -2 9.2 3.4 0 0 -3 1.8 2.9 0 1 -3 488.2 6.4 0 2 -3 6.8 3.3 0 3 -3 600.5 7.7 0 4 -3 -1.7 4.1 0 5 -3 187.2 5.5 0 6 -3 1.7 4.2 0 7 -3 148.0 5.4 0 8 -3 8.5 3.9 0 9 -3 12.6 3.6 1 0 -3 1111.5 9.1 1 1 -3 170.8 4.3 1 2 -3 21.0 3.6 1 3 -3 1064.3 9.7 1 4 -3 85.7 4.2 1 5 -3 912.7 10.0 1 6 -3 -5.7 4.3 1 7 -3 86.2 4.7 1 8 -3 37.0 4.3 1 9 -3 11.7 3.7 2 0 -3 2.3 3.2 2 1 -3 10.4 3.3 2 2 -3 383.6 6.2 2 3 -3 2.2 3.7 2 4 -3 10.5 4.3 2 5 -3 13.2 4.4 2 6 -3 86.0 4.8 2 7 -3 3.6 4.0 2 8 -3 26.6 4.2 2 9 -3 -2.4 3.4 3 0 -3 1045.3 9.6 3 1 -3 1565.5 11.6 3 2 -3 88.0 3.9 3 3 -3 400.3 6.7 3 4 -3 81.6 4.7 3 5 -3 104.7 4.7 3 6 -3 13.0 4.1 3 7 -3 188.3 5.7 3 8 -3 35.7 3.8 3 9 -3 136.8 5.2 4 0 -3 6.5 4.2 4 1 -3 294.6 6.2 4 2 -3 52.2 3.9 4 3 -3 167.1 5.1 4 4 -3 6.2 4.5 4 5 -3 45.3 3.9 4 6 -3 9.1 4.3 4 7 -3 71.2 4.4 4 8 -3 1.5 3.9 5 0 -3 10.5 4.5 5 1 -3 1109.9 10.9 5 2 -3 5.0 4.7 5 3 -3 113.8 4.6 5 4 -3 66.9 4.0 5 5 -3 23.4 3.5 5 6 -3 0.0 4.5 5 7 -3 179.3 5.7 5 8 -3 -0.1 4.0 6 0 -3 1.4 4.6 6 1 -3 8.8 4.6 6 2 -3 66.9 3.8 6 3 -3 18.2 3.3 6 4 -3 6.3 4.2 6 5 -3 -2.6 4.1 6 6 -3 21.7 3.2 6 7 -3 7.7 4.2 7 0 -3 100.0 4.7 7 1 -3 155.5 5.3 7 2 -3 13.2 4.3 7 3 -3 160.6 5.4 7 4 -3 104.0 4.6 7 5 -3 101.9 4.6 7 6 -3 22.1 4.4 8 0 -3 -12.9 3.7 8 1 -3 41.2 4.0 8 2 -3 40.2 3.2 8 3 -3 38.9 3.4 8 4 -3 -6.7 3.4 8 5 -3 8.8 2.7 9 0 -3 56.8 3.7 9 1 -3 6.7 3.2 9 2 -3 20.0 2.7 9 3 -3 154.3 4.9 9 4 -3 12.5 3.4 0 0 -4 8417.8 26.3 0 1 -4 3.5 3.9 0 2 -4 60.6 4.1 0 3 -4 6.8 4.1 0 4 -4 376.9 7.0 0 5 -4 5.0 4.0 0 6 -4 68.1 4.6 0 7 -4 -5.0 4.0 0 8 -4 605.0 9.1 1 0 -4 0.0 3.6 1 1 -4 297.3 5.9 1 2 -4 310.7 6.4 1 3 -4 769.7 9.3 1 4 -4 1.3 4.5 1 5 -4 283.9 6.6 1 6 -4 107.5 4.8 1 7 -4 -0.7 4.1 1 8 -4 4.6 3.7 2 0 -4 72.1 3.9 2 1 -4 162.8 4.8 2 2 -4 1986.4 13.8 2 3 -4 8.8 4.4 2 4 -4 14.6 4.2 2 5 -4 97.4 4.6 2 6 -4 516.7 8.5 2 7 -4 -4.6 3.9 2 8 -4 37.6 3.6 3 0 -4 9.0 3.9 3 1 -4 648.5 8.4 3 2 -4 82.2 4.2 3 3 -4 40.2 4.0 3 4 -4 2.5 4.2 3 5 -4 36.3 4.0 3 6 -4 40.6 3.9 3 7 -4 173.2 5.5 3 8 -4 -6.8 3.9 4 0 -4 123.8 4.9 4 1 -4 2.4 4.3 4 2 -4 5.3 4.4 4 3 -4 2.1 4.4 4 4 -4 1391.0 12.6 4 5 -4 40.2 3.8 4 6 -4 11.0 3.9 4 7 -4 1.2 3.8 4 8 -4 39.2 3.6 5 0 -4 -3.5 4.3 5 1 -4 296.9 6.6 5 2 -4 230.8 6.0 5 3 -4 46.7 3.6 5 4 -4 11.7 4.1 5 5 -4 29.7 4.0 5 6 -4 26.3 3.4 5 7 -4 37.2 3.8 6 0 -4 10.3 4.1 6 1 -4 129.2 5.5 6 2 -4 422.8 7.5 6 3 -4 25.5 4.2 6 4 -4 23.9 3.3 6 5 -4 9.4 4.1 6 6 -4 139.3 5.1 7 0 -4 -3.5 3.5 7 1 -4 20.4 3.4 7 2 -4 2.7 4.0 7 3 -4 90.6 4.2 7 4 -4 -3.7 3.6 7 5 -4 40.4 3.4 8 0 -4 583.4 8.9 8 1 -4 67.3 3.7 8 2 -4 8.5 3.7 8 3 -4 -0.3 3.5 8 4 -4 35.3 3.2 9 0 -4 0.8 3.6 9 1 -4 13.1 3.9 0 0 -5 8.4 4.2 0 1 -5 182.4 6.1 0 2 -5 4.8 4.4 0 3 -5 160.0 5.6 0 4 -5 10.9 4.3 0 5 -5 25.9 3.8 0 6 -5 1.1 4.2 0 7 -5 66.9 4.9 1 0 -5 71.1 5.3 1 1 -5 202.9 6.3 1 2 -5 -2.8 4.7 1 3 -5 624.6 9.2 1 4 -5 98.0 5.2 1 5 -5 619.2 9.4 1 6 -5 12.0 4.1 1 7 -5 84.0 5.1 2 0 -5 4.4 4.4 2 1 -5 12.5 4.5 2 2 -5 160.1 5.7 2 3 -5 3.1 4.6 2 4 -5 4.1 4.5 2 5 -5 2.1 4.5 2 6 -5 26.9 4.4 2 7 -5 -6.5 4.3 3 0 -5 180.1 5.5 3 1 -5 420.8 7.6 3 2 -5 0.0 4.1 3 3 -5 124.3 4.9 3 4 -5 46.6 4.1 3 5 -5 50.7 4.1 3 6 -5 1.7 3.9 3 7 -5 89.8 4.7 4 0 -5 -5.3 4.0 4 1 -5 50.9 4.2 4 2 -5 24.8 4.1 4 3 -5 119.4 5.3 4 4 -5 5.1 4.0 4 5 -5 23.2 3.6 4 6 -5 2.2 3.8 5 0 -5 -5.8 4.1 5 1 -5 392.7 7.4 5 2 -5 28.5 3.5 5 3 -5 41.9 3.8 5 4 -5 42.8 3.8 5 5 -5 9.3 4.3 5 6 -5 13.9 4.0 6 0 -5 -2.7 3.6 6 1 -5 3.8 3.7 6 2 -5 53.2 4.0 6 3 -5 5.4 3.7 6 4 -5 1.4 3.6 6 5 -5 -11.1 3.8 7 0 -5 -4.4 3.5 7 1 -5 79.5 4.1 7 2 -5 19.6 3.6 7 3 -5 93.0 4.3 7 4 -5 81.9 4.3 8 0 -5 4.9 3.5 8 1 -5 21.5 3.8 0 0 -6 261.2 6.6 0 1 -6 -1.5 4.1 0 2 -6 599.4 9.4 0 3 -6 0.9 4.1 0 4 -6 75.5 4.8 0 5 -6 3.9 4.0 0 6 -6 256.2 6.8 1 0 -6 -1.0 4.1 1 1 -6 243.9 6.6 1 2 -6 116.5 5.2 1 3 -6 33.3 4.5 1 4 -6 -1.7 4.1 1 5 -6 44.9 4.0 1 6 -6 16.3 4.0 2 0 -6 775.1 10.2 2 1 -6 0.3 4.5 2 2 -6 9.9 4.1 2 3 -6 14.5 4.5 2 4 -6 393.9 8.0 2 5 -6 95.8 4.9 2 6 -6 11.3 4.5 3 0 -6 -2.2 4.3 3 1 -6 47.5 4.4 3 2 -6 39.7 4.3 3 3 -6 246.4 6.7 3 4 -6 -0.4 4.3 3 5 -6 50.8 4.9 4 0 -6 58.9 4.3 4 1 -6 -2.8 4.2 4 2 -6 485.5 8.7 4 3 -6 25.9 4.3 4 4 -6 171.4 6.0 4 5 -6 17.2 3.9 5 0 -6 1.2 3.5 5 1 -6 45.1 3.9 5 2 -6 65.1 4.3 5 3 -6 77.6 4.9 5 4 -6 -5.8 4.1 6 0 -6 207.6 6.4 6 1 -6 31.3 3.9 6 2 -6 15.6 3.8 0 0 -7 1.6 3.9 0 1 -7 14.2 3.1 0 2 -7 4.0 3.9 0 3 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