data_shelx _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Fe0.90 H20 Mg0.05 Mn0.60 O23 P3 Zn2.40' _chemical_formula_weight 722.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 21/m' _space_group_name_Hall '-P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.3710(13) _cell_length_b 11.020(2) _cell_length_c 13.016(3) _cell_angle_alpha 90 _cell_angle_beta 99.34(3) _cell_angle_gamma 90 _cell_volume 901.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.661 _exptl_crystal_F_000 720 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 4.661 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6570 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.435 _diffrn_reflns_theta_max 20.789 _diffrn_reflns_theta_full 20.789 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.987 _reflns_number_total 995 _reflns_number_gt 935 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+33.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 995 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5853(4) 0.7500 0.7916(2) 0.0199(14) Uani 0.76(8) 2 d S T P . . Fe1 Fe 0.5853(4) 0.7500 0.7916(2) 0.0199(14) Uani 0.24(8) 2 d S T P . . Zn2 Zn 0.2477(3) 0.50006(17) 0.50898(15) 0.0189(11) Uani 0.54(6) 1 d . . P . . Fe2 Fe 0.2477(3) 0.50006(17) 0.50898(15) 0.0189(11) Uani 0.36(6) 1 d . . P . . Mg2 Mg 0.2477(3) 0.50006(17) 0.50898(15) 0.0189(11) Uani 0.1 1 d . . P . . Mn Mn 0.2190(4) 0.2500 0.8328(2) 0.0185(15) Uani 0.51(6) 2 d S T P . . Zn3 Zn 0.2190(4) 0.2500 0.8328(2) 0.0185(15) Uani 0.49(6) 2 d S T P . . Fe Fe 0.0453(4) 0.7500 0.6275(2) 0.0182(11) Uani 1 2 d S T P . . P2 P 0.5296(8) 0.7500 0.5674(4) 0.0173(15) Uani 1 2 d S T P . . P1 P 0.2772(6) 0.5301(3) 0.7650(3) 0.0191(12) Uani 1 1 d . . . . . O5 O 0.357(2) 0.7500 0.6367(11) 0.023(4) Uani 1 2 d S T P . . O7 O 0.5114(15) 0.6333(8) 0.5024(8) 0.022(2) Uani 1 1 d . . . . . O6 O 0.738(2) 0.7500 0.6473(11) 0.022(4) Uani 1 2 d S T P . . O1 O 0.2110(14) 0.4318(9) 0.8361(7) 0.021(2) Uani 1 1 d . . . . . O2 O 0.3323(14) 0.4750(8) 0.6644(7) 0.020(2) Uani 1 1 d . . . . . O3 O 0.0900(14) 0.6187(8) 0.7360(7) 0.019(2) Uani 1 1 d . . . . . O4 O 0.4758(14) 0.5947(9) 0.8226(7) 0.024(3) Uani 1 1 d . . . . . OH O 0.0052(15) 0.6236(8) 0.5156(7) 0.021(2) Uani 1 1 d . . . . . OW1 O 0.2286(15) 0.5269(9) 0.3441(8) 0.024(3) Uani 1 1 d . . . . . OW2 O 0.443(2) 0.2500 0.9729(11) 0.026(4) Uani 1 2 d S T P . . OW3 O -0.034(2) 0.2500 0.9220(11) 0.024(3) Uani 1 2 d S T P . . OW4 O 0.460(2) 0.2500 0.7336(11) 0.023(3) Uani 1 2 d S T P . . OW5 O -0.028(2) 0.2500 0.6889(10) 0.023(3) Uani 1 2 d S T P . . OW6 O 0.872(2) 0.7500 0.8746(12) 0.042(4) Uani 1 2 d S T P . . OW7 O 0.7247(16) 0.4450(9) 0.9632(7) 0.027(3) Uani 1 1 d . . . . . 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 0.0176(19) 0.0095(18) 0.032(2) 0.000 0.0020(12) 0.000 Fe1 0.0176(19) 0.0095(18) 0.032(2) 0.000 0.0020(12) 0.000 Zn2 0.0154(15) 0.0124(14) 0.0287(16) -0.0006(9) 0.0033(9) 0.0021(9) Fe2 0.0154(15) 0.0124(14) 0.0287(16) -0.0006(9) 0.0033(9) 0.0021(9) Mg2 0.0154(15) 0.0124(14) 0.0287(16) -0.0006(9) 0.0033(9) 0.0021(9) Mn 0.017(2) 0.0101(19) 0.029(2) 0.000 0.0059(12) 0.000 Zn3 0.017(2) 0.0101(19) 0.029(2) 0.000 0.0059(12) 0.000 Fe 0.0129(18) 0.0145(18) 0.027(2) 0.000 0.0046(13) 0.000 P2 0.008(3) 0.008(3) 0.036(4) 0.000 0.004(2) 0.000 P1 0.017(2) 0.012(2) 0.028(2) 0.0009(18) 0.0047(17) 0.0012(17) O5 0.008(8) 0.017(8) 0.042(9) 0.000 0.002(7) 0.000 O7 0.022(6) 0.006(5) 0.035(6) -0.004(5) -0.001(4) 0.002(4) O6 0.014(8) 0.030(9) 0.024(8) 0.000 0.009(6) 0.000 O1 0.018(5) 0.021(6) 0.025(6) 0.002(5) 0.008(4) -0.002(5) O2 0.017(5) 0.014(6) 0.032(6) -0.005(5) 0.010(4) -0.010(4) O3 0.014(5) 0.014(6) 0.029(6) -0.001(4) 0.006(4) -0.002(4) O4 0.014(5) 0.028(6) 0.028(6) 0.002(5) 0.000(4) 0.001(5) OH 0.021(5) 0.009(5) 0.033(6) -0.007(4) 0.007(4) -0.005(4) OW1 0.017(6) 0.016(6) 0.038(6) -0.002(5) 0.004(5) 0.009(5) OW2 0.032(9) 0.009(7) 0.037(9) 0.000 0.001(7) 0.000 OW3 0.023(8) 0.017(8) 0.032(9) 0.000 0.006(7) 0.000 OW4 0.024(8) 0.017(8) 0.029(9) 0.000 0.010(7) 0.000 OW5 0.013(8) 0.030(9) 0.024(8) 0.000 -0.001(6) 0.000 OW6 0.016(9) 0.071(13) 0.040(10) 0.000 0.010(7) 0.000 OW7 0.032(6) 0.020(6) 0.031(6) 0.001(5) 0.006(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.915(10) 4_575 ? Zn1 O4 1.915(10) . ? Zn1 OW6 1.967(15) . ? Zn1 O6 2.253(13) . ? Zn1 O5 2.286(14) . ? Zn1 P2 2.882(6) . ? Zn2 O2 2.026(10) . ? Zn2 OH 2.072(9) . ? Zn2 OH 2.095(9) 3_566 ? Zn2 O7 2.147(9) 3_666 ? Zn2 OW1 2.150(10) . ? Zn2 O7 2.243(10) . ? Zn2 Mg2 3.127(4) 3_566 ? Zn2 Zn2 3.127(4) 3_566 ? Zn2 Mg2 3.261(4) 3_666 ? Mn O1 2.005(10) . ? Mn O1 2.005(10) 4_565 ? Mn OW2 2.125(14) . ? Mn OW3 2.136(14) . ? Mn OW4 2.158(13) . ? Mn OW5 2.242(13) . ? Fe O5 1.971(13) . ? Fe OH 2.001(9) . ? Fe OH 2.001(9) 4_575 ? Fe O3 2.010(9) . ? Fe O3 2.010(9) 4_575 ? Fe O6 2.014(13) 1_455 ? P2 O5 1.530(15) . ? P2 O7 1.534(10) . ? P2 O7 1.534(10) 4_575 ? P2 O6 1.549(15) . ? P1 O1 1.527(10) . ? P1 O2 1.536(10) . ? P1 O4 1.537(10) . ? P1 O3 1.540(10) . ? O7 Mg2 2.147(9) 3_666 ? O7 Fe2 2.147(9) 3_666 ? O7 Zn2 2.147(9) 3_666 ? O6 Fe 2.014(13) 1_655 ? OH Mg2 2.095(9) 3_566 ? OH Zn2 2.095(9) 3_566 ? OH Fe2 2.095(9) 3_566 ? 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 126.6(6) 4_575 . ? O4 Zn1 OW6 102.8(3) 4_575 . ? O4 Zn1 OW6 102.8(3) . . ? O4 Zn1 O6 113.4(3) 4_575 . ? O4 Zn1 O6 113.4(3) . . ? OW6 Zn1 O6 88.2(6) . . ? O4 Zn1 O5 89.1(3) 4_575 . ? O4 Zn1 O5 89.1(3) . . ? OW6 Zn1 O5 152.3(6) . . ? O6 Zn1 O5 64.1(5) . . ? O4 Zn1 P2 102.9(3) 4_575 . ? O4 Zn1 P2 102.9(3) . . ? OW6 Zn1 P2 120.4(5) . . ? O6 Zn1 P2 32.3(4) . . ? O5 Zn1 P2 31.9(4) . . ? O2 Zn2 OH 97.3(4) . . ? O2 Zn2 OH 97.9(4) . 3_566 ? OH Zn2 OH 82.7(4) . 3_566 ? O2 Zn2 O7 84.2(4) . 3_666 ? OH Zn2 O7 177.3(4) . 3_666 ? OH Zn2 O7 94.9(4) 3_566 3_666 ? O2 Zn2 OW1 168.0(4) . . ? OH Zn2 OW1 91.7(4) . . ? OH Zn2 OW1 91.1(4) 3_566 . ? O7 Zn2 OW1 87.2(4) 3_666 . ? O2 Zn2 O7 92.7(4) . . ? OH Zn2 O7 98.0(4) . . ? OH Zn2 O7 169.2(4) 3_566 . ? O7 Zn2 O7 84.1(4) 3_666 . ? OW1 Zn2 O7 78.1(4) . . ? O2 Zn2 Mg2 100.1(3) . 3_566 ? OH Zn2 Mg2 41.6(3) . 3_566 ? OH Zn2 Mg2 41.1(3) 3_566 3_566 ? O7 Zn2 Mg2 135.9(3) 3_666 3_566 ? OW1 Zn2 Mg2 91.9(3) . 3_566 ? O7 Zn2 Mg2 138.6(3) . 3_566 ? O2 Zn2 Zn2 100.1(3) . 3_566 ? OH Zn2 Zn2 41.6(3) . 3_566 ? OH Zn2 Zn2 41.1(3) 3_566 3_566 ? O7 Zn2 Zn2 135.9(3) 3_666 3_566 ? OW1 Zn2 Zn2 91.9(3) . 3_566 ? O7 Zn2 Zn2 138.6(3) . 3_566 ? Mg2 Zn2 Zn2 0.0 3_566 3_566 ? O2 Zn2 Mg2 88.1(3) . 3_666 ? OH Zn2 Mg2 138.9(3) . 3_666 ? OH Zn2 Mg2 137.0(3) 3_566 3_666 ? O7 Zn2 Mg2 43.2(3) 3_666 3_666 ? OW1 Zn2 Mg2 79.9(3) . 3_666 ? O7 Zn2 Mg2 40.9(2) . 3_666 ? Mg2 Zn2 Mg2 171.72(13) 3_566 3_666 ? Zn2 Zn2 Mg2 171.72(13) 3_566 3_666 ? O1 Mn O1 175.9(5) . 4_565 ? O1 Mn OW2 89.9(3) . . ? O1 Mn OW2 89.8(3) 4_565 . ? O1 Mn OW3 88.0(3) . . ? O1 Mn OW3 88.0(3) 4_565 . ? OW2 Mn OW3 89.7(6) . . ? O1 Mn OW4 92.0(3) . . ? O1 Mn OW4 92.0(3) 4_565 . ? OW2 Mn OW4 94.0(6) . . ? OW3 Mn OW4 176.3(6) . . ? O1 Mn OW5 90.1(3) . . ? O1 Mn OW5 90.1(3) 4_565 . ? OW2 Mn OW5 177.6(5) . . ? OW3 Mn OW5 88.0(5) . . ? OW4 Mn OW5 88.3(5) . . ? O5 Fe OH 93.0(4) . . ? O5 Fe OH 93.0(4) . 4_575 ? OH Fe OH 88.2(6) . 4_575 ? O5 Fe O3 86.0(4) . . ? OH Fe O3 89.8(4) . . ? OH Fe O3 177.8(4) 4_575 . ? O5 Fe O3 86.0(4) . 4_575 ? OH Fe O3 177.8(4) . 4_575 ? OH Fe O3 89.8(4) 4_575 4_575 ? O3 Fe O3 92.1(5) . 4_575 ? O5 Fe O6 169.3(6) . 1_455 ? OH Fe O6 94.6(4) . 1_455 ? OH Fe O6 94.6(4) 4_575 1_455 ? O3 Fe O6 86.5(4) . 1_455 ? O3 Fe O6 86.5(4) 4_575 1_455 ? O5 P2 O7 109.2(5) . . ? O5 P2 O7 109.2(5) . 4_575 ? O7 P2 O7 114.0(8) . 4_575 ? O5 P2 O6 103.0(8) . . ? O7 P2 O6 110.5(5) . . ? O7 P2 O6 110.5(5) 4_575 . ? O5 P2 Zn1 52.1(5) . . ? O7 P2 Zn1 123.0(4) . . ? O7 P2 Zn1 123.0(4) 4_575 . ? O6 P2 Zn1 50.9(5) . . ? O1 P1 O2 111.1(5) . . ? O1 P1 O4 108.6(6) . . ? O2 P1 O4 108.4(5) . . ? O1 P1 O3 108.6(5) . . ? O2 P1 O3 108.5(5) . . ? O4 P1 O3 111.7(5) . . ? P2 O5 Fe 141.0(9) . . ? P2 O5 Zn1 96.1(6) . . ? Fe O5 Zn1 123.0(7) . . ? P2 O7 Mg2 128.4(6) . 3_666 ? P2 O7 Fe2 128.4(6) . 3_666 ? Mg2 O7 Fe2 0.00(12) 3_666 3_666 ? P2 O7 Zn2 128.4(6) . 3_666 ? Mg2 O7 Zn2 0.0 3_666 3_666 ? Fe2 O7 Zn2 0.0 3_666 3_666 ? P2 O7 Zn2 121.2(6) . . ? Mg2 O7 Zn2 95.9 3_666 . ? Fe2 O7 Zn2 95.9 3_666 . ? Zn2 O7 Zn2 95.9(4) 3_666 . ? P2 O6 Fe 131.3(8) . 1_655 ? P2 O6 Zn1 96.8(6) . . ? Fe O6 Zn1 131.9(7) 1_655 . ? P1 O1 Mn 133.3(6) . . ? P1 O2 Zn2 137.5(6) . . ? P1 O3 Fe 130.1(5) . . ? P1 O4 Zn1 127.6(6) . . ? Fe OH Zn2 118.7(5) . . ? Fe OH Mg2 124.6(5) . 3_566 ? Zn2 OH Mg2 97.3 . 3_566 ? Fe OH Zn2 124.6(5) . 3_566 ? Zn2 OH Zn2 97.3(4) . 3_566 ? Mg2 OH Zn2 0.0 3_566 3_566 ? Fe OH Fe2 124.6(5) . 3_566 ? Zn2 OH Fe2 97.3 . 3_566 ? Mg2 OH Fe2 0.00(7) 3_566 3_566 ? Zn2 OH Fe2 0.00(7) 3_566 3_566 ? _refine_diff_density_max 1.265 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.196 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL p2onm_a.res in P2(1)/m CELL 0.71073 6.3710 11.0200 13.0160 90.000 99.339 90.000 ZERR 2.000 0.0013 0.0022 0.0026 0.000 0.030 0.000 LATT 1 SYMM -X, 1/2+Y, -Z SFAC O H P FE ZN MN MG UNIT 46 40 6 1.8 4.8 1.2 0.1 SHEL 15 1.0 ACTA L.S. 6 BOND $H LIST 4 FMAP 2 PLAN 60 EXYZ ZN1 FE1 EADP ZN1 FE1 EXYZ MN ZN3 EADP MN ZN3 EXYZ ZN2 FE2 MG2 EADP ZN2 FE2 MG2 WGHT 0.030000 33.000000 EXTI 0.012179 FVAR 0.47114 0.76416 0.59925 0.48616 ZN1 5 0.585275 0.750000 0.791643 20.50000 0.01761 0.00947 = 0.03188 0.00000 0.00200 0.00000 FE1 4 0.585275 0.750000 0.791643 -20.50000 0.01761 0.00947 = 0.03188 0.00000 0.00200 0.00000 ZN2 5 0.247726 0.500060 0.508977 30.90000 0.01536 0.01239 = 0.02872 -0.00063 0.00329 0.00213 FE2 4 0.247726 0.500060 0.508977 -30.90000 0.01536 0.01239 = 0.02872 -0.00063 0.00329 0.00213 MG2 7 0.247726 0.500060 0.508977 10.10000 0.01536 0.01239 = 0.02872 -0.00063 0.00329 0.00213 MN 6 0.218997 0.250000 0.832778 -40.50000 0.01720 0.01008 = 0.02883 0.00000 0.00594 0.00000 ZN3 5 0.218997 0.250000 0.832778 40.50000 0.01720 0.01008 = 0.02883 0.00000 0.00594 0.00000 FE 4 0.045336 0.750000 0.627457 10.50000 0.01294 0.01449 = 0.02748 0.00000 0.00455 0.00000 P2 3 0.529606 0.750000 0.567450 10.50000 0.00817 0.00816 = 0.03574 0.00000 0.00374 0.00000 P1 3 0.277159 0.530110 0.765030 11.00000 0.01689 0.01240 = 0.02840 0.00087 0.00467 0.00115 O5 1 0.357241 0.750000 0.636720 10.50000 0.00805 0.01746 = 0.04202 0.00000 0.00226 0.00000 O7 1 0.511378 0.633276 0.502386 11.00000 0.02241 0.00571 = 0.03473 -0.00357 -0.00093 0.00246 O6 1 0.738326 0.750000 0.647259 10.50000 0.01420 0.03013 = 0.02434 0.00000 0.00908 0.00000 O1 1 0.211031 0.431846 0.836085 11.00000 0.01828 0.02083 = 0.02480 0.00186 0.00806 -0.00216 O2 1 0.332261 0.475020 0.664366 11.00000 0.01678 0.01395 = 0.03182 -0.00490 0.00983 -0.01035 O3 1 0.089958 0.618696 0.736033 11.00000 0.01358 0.01419 = 0.02931 -0.00079 0.00644 -0.00235 O4 1 0.475847 0.594743 0.822602 11.00000 0.01427 0.02764 = 0.02821 0.00226 0.00006 0.00105 OH 1 0.005153 0.623590 0.515605 11.00000 0.02096 0.00915 = 0.03275 -0.00690 0.00710 -0.00451 OW1 1 0.228594 0.526936 0.344106 11.00000 0.01672 0.01640 = 0.03758 -0.00199 0.00360 0.00878 OW2 1 0.442884 0.250000 0.972862 10.50000 0.03195 0.00851 = 0.03709 0.00000 0.00128 0.00000 OW3 1 -0.034288 0.250000 0.922042 10.50000 0.02315 0.01690 = 0.03199 0.00000 0.00562 0.00000 OW4 1 0.459517 0.250000 0.733580 10.50000 0.02372 0.01743 = 0.02888 0.00000 0.00964 0.00000 OW5 1 -0.028009 0.250000 0.688893 10.50000 0.01304 0.02980 = 0.02354 0.00000 -0.00087 0.00000 OW6 1 0.872333 0.750000 0.874635 10.50000 0.01633 0.07078 = 0.03977 0.00000 0.00967 0.00000 OW7 1 0.724748 0.444960 0.963249 11.00000 0.03164 0.02000 = 0.03054 0.00128 0.00572 -0.00105 HKLF 4 REM p2onm_a.res in P2(1)/m REM R1 = 0.0566 for 935 Fo > 4sig(Fo) and 0.0594 for all 995 data REM 161 parameters refined using 0 restraints END WGHT 0.0233 35.8533 REM Highest difference peak 1.265, deepest hole -0.750, 1-sigma level 0.196 Q1 1 0.5944 0.7500 0.8799 10.50000 0.05 1.27 Q2 1 0.5719 0.7500 0.6778 10.50000 0.05 1.16 Q3 1 0.2218 0.5004 0.4212 11.00000 0.05 1.07 Q4 1 0.2733 0.4977 0.5888 11.00000 0.05 1.00 Q5 1 0.5063 0.7500 0.4618 10.50000 0.05 0.90 Q6 1 0.5161 0.2500 0.6227 10.50000 0.05 0.89 Q7 1 0.0965 0.7500 0.7226 10.50000 0.05 0.89 Q8 1 0.0327 0.7500 0.5342 10.50000 0.05 0.84 Q9 1 0.4014 0.4464 0.8458 11.00000 0.05 0.82 Q10 1 0.2355 0.2500 0.9297 10.50000 0.05 0.76 Q11 1 0.1943 0.2500 0.7484 10.50000 0.05 0.73 Q12 1 -0.1164 0.1703 0.9162 11.00000 0.05 0.67 Q13 1 -0.1040 0.5561 0.4995 11.00000 0.05 0.67 Q14 1 0.3562 0.4995 0.3387 11.00000 0.05 0.64 Q15 1 0.9833 0.7500 0.8818 10.50000 0.05 0.60 Q16 1 0.2185 0.6015 0.5164 11.00000 0.05 0.58 Q17 1 0.3158 0.2500 1.0265 10.50000 0.05 0.57 Q18 1 -0.1270 0.7500 0.6049 10.50000 0.05 0.57 Q19 1 0.2358 0.7744 0.6343 11.00000 0.05 0.57 Q20 1 0.0916 0.2500 0.6848 10.50000 0.05 0.57 Q21 1 0.1446 0.4835 0.3007 11.00000 0.05 0.57 Q22 1 0.0610 0.6371 0.6414 11.00000 0.05 0.55 Q23 1 0.3778 0.4514 0.7792 11.00000 0.05 0.53 Q24 1 -0.0033 0.6474 0.4387 11.00000 0.05 0.53 Q25 1 -0.0217 0.2500 0.7626 10.50000 0.05 0.52 Q26 1 0.2565 0.4083 0.5006 11.00000 0.05 0.52 Q27 1 0.4440 0.4440 0.9146 11.00000 0.05 0.51 Q28 1 0.9057 0.7500 0.9562 10.50000 0.05 0.51 Q29 1 0.4398 0.1726 0.6926 11.00000 0.05 0.51 Q30 1 -0.0121 0.2500 0.8573 10.50000 0.05 0.50 Q31 1 0.1468 0.7500 0.8165 10.50000 0.05 0.50 Q32 1 -0.1312 0.1809 0.7005 11.00000 0.05 0.49 Q33 1 0.4882 0.1629 0.9664 11.00000 0.05 0.49 Q34 1 0.6011 0.2500 1.0367 10.50000 0.05 0.49 Q35 1 0.0044 0.1297 0.6830 11.00000 0.05 0.49 Q36 1 0.5514 0.1681 0.9806 11.00000 0.05 0.49 Q37 1 1.1813 0.7957 0.8836 11.00000 0.05 0.48 Q38 1 0.6437 0.5008 0.9151 11.00000 0.05 0.47 Q39 1 -0.2291 0.2500 0.7853 10.50000 0.05 0.47 Q40 1 0.6112 0.1692 0.9969 11.00000 0.05 0.46 Q41 1 0.2750 0.1619 0.8411 11.00000 0.05 0.46 Q42 1 0.1816 0.5949 0.3535 11.00000 0.05 0.46 Q43 1 0.4562 0.5012 0.6627 11.00000 0.05 0.44 Q44 1 0.0593 0.3439 0.7745 11.00000 0.05 0.44 Q45 1 0.0802 0.5499 0.5113 11.00000 0.05 0.44 Q46 1 0.3844 0.5751 0.5052 11.00000 0.05 0.43 Q47 1 0.3146 0.6644 0.8874 11.00000 0.05 0.43 Q48 1 0.9774 0.7500 0.8120 10.50000 0.05 0.43 Q49 1 0.2683 0.6544 0.7790 11.00000 0.05 0.43 Q50 1 0.3320 0.6566 0.3082 11.00000 0.05 0.43 Q51 1 -0.2531 0.2500 0.6986 10.50000 0.05 0.42 Q52 1 0.3506 0.7500 0.8263 10.50000 0.05 0.41 Q53 1 -0.2818 0.2169 0.6147 11.00000 0.05 0.41 Q54 1 0.1037 0.1523 0.9506 11.00000 0.05 0.40 Q55 1 0.6644 0.6170 0.8853 11.00000 0.05 0.40 Q56 1 -0.1829 0.2500 0.8753 10.50000 0.05 0.39 Q57 1 0.2379 0.3798 0.7633 11.00000 0.05 0.39 Q58 1 0.9348 0.4524 0.9226 11.00000 0.05 0.39 Q59 1 0.4759 0.1512 1.0424 11.00000 0.05 0.39 Q60 1 0.4994 0.2500 0.8001 10.50000 0.05 0.38 ; _shelx_res_checksum 15337 _shelx_hkl_file ; 0 0 -2 105.87 7.40 0 0 -2 94.65 6.34 0 0 2 103.96 7.25 0 0 2 95.94 6.41 0 0 -3 3649.25 217.08 0 0 -3 3769.85 224.10 0 0 3 3606.51 214.41 0 0 3 3755.35 223.26 0 0 -4 2218.10 132.12 0 0 -4 2273.05 135.25 0 0 4 2118.87 126.17 0 0 4 2194.44 130.60 0 0 -5 61.52 6.87 0 0 -5 63.58 6.18 0 0 5 55.87 6.34 0 0 5 65.49 6.18 0 0 -6 5610.13 333.63 0 0 -6 5733.01 340.81 0 0 6 5314.74 316.00 0 0 6 5627.68 334.47 0 0 -7 4301.86 255.85 0 0 -7 4381.24 260.43 0 0 7 4154.55 247.15 0 0 7 4285.83 254.78 0 0 -8 1141.11 68.39 0 0 -8 1149.50 68.70 0 0 8 1085.39 65.11 0 0 8 1112.10 66.48 0 0 -9 952.58 57.32 0 0 -9 924.34 55.49 0 0 9 949.52 57.09 0 0 9 917.47 55.03 0 0 -10 17.63 6.34 0 0 -10 12.75 5.57 0 0 10 13.82 6.11 0 0 10 20.00 5.80 0 0 -11 256.00 17.17 0 0 11 248.60 16.79 0 0 11 229.29 15.34 0 0 -12 490.26 30.30 0 0 12 485.60 29.84 0 0 12 510.48 31.45 0 0 -13 362.33 22.67 0 0 13 314.55 20.15 0 0 13 291.88 18.40 0 0 -14 170.29 12.29 0 0 14 165.48 11.98 0 0 14 158.69 11.07 0 0 -15 548.42 33.43 0 0 15 526.05 32.21 0 0 15 534.22 32.44 0 0 -16 31.37 6.56 0 0 -16 22.21 14.12 0 0 16 37.40 6.49 0 0 16 36.03 6.11 0 0 17 86.40 8.01 0 0 17 61.75 7.25 0 -1 17 90.30 7.94 0 -1 17 92.28 8.24 0 1 -17 103.65 9.54 0 -1 16 12.06 5.50 0 -1 16 16.94 6.11 0 1 -16 14.81 17.63 0 1 -16 12.06 6.03 0 -1 15 147.39 10.46 0 -1 15 198.30 13.66 0 1 -15 161.97 11.75 0 -1 14 63.28 6.64 0 -1 14 70.76 7.71 0 1 -14 76.56 8.01 0 1 -14 77.17 14.27 0 -1 13 578.57 35.19 0 -1 13 540.79 32.74 0 1 -13 563.53 34.27 0 1 -13 567.20 35.87 0 -1 12 109.84 9.16 0 -1 12 118.08 9.77 0 1 -12 125.33 10.69 0 1 -12 126.25 11.83 0 -1 11 389.12 24.27 0 -1 11 400.80 25.04 0 1 -11 380.65 23.97 0 -1 10 20.61 5.57 0 -1 10 23.20 5.88 0 1 -10 26.49 6.49 0 1 -10 20.38 5.95 0 -1 9 94.04 8.09 0 -1 9 90.37 8.24 0 1 -9 93.81 8.85 0 1 -9 90.83 7.86 0 -1 8 1168.59 69.99 0 -1 8 1150.27 68.70 0 1 -8 1186.14 71.06 0 1 -8 1109.81 66.33 0 -1 7 839.61 50.30 0 -1 7 822.06 49.46 0 1 -7 843.43 50.83 0 1 -7 801.45 48.16 0 -1 6 777.02 46.79 0 -1 6 762.37 45.72 0 1 -6 796.10 48.01 0 1 -6 743.67 44.65 0 -1 5 25.95 4.81 0 -1 5 30.00 5.57 0 1 -5 25.34 6.03 0 1 -5 30.00 4.96 0 -1 4 1207.51 72.05 0 -1 4 1167.82 69.76 0 1 -4 1188.43 70.91 0 1 -4 1168.59 69.84 0 -1 3 20.84 4.12 0 -1 3 12.29 4.20 0 1 -3 16.03 3.82 0 1 -3 21.37 5.04 0 -1 2 1918.13 114.11 0 -1 2 1905.92 113.35 0 1 -2 1945.61 115.79 0 1 -2 1937.97 115.33 0 -1 1 1115.16 66.33 0 -1 1 1076.99 64.12 0 1 -1 1071.65 63.73 0 1 -1 1112.10 66.18 0 -1 0 2.44 0.99 0 -1 0 1.60 0.92 0 1 0 1.76 0.99 0 1 0 2.14 0.92 0 -1 -1 1099.13 65.41 0 -1 -1 1089.20 64.80 0 1 1 1118.21 66.56 0 1 1 1062.49 63.28 0 -1 -2 1883.02 111.97 0 -1 -2 1859.36 110.68 0 1 2 1944.08 115.64 0 1 2 1929.58 114.80 0 -1 -3 25.04 4.96 0 -1 -3 19.23 4.50 0 1 3 28.24 5.27 0 1 3 22.75 4.43 0 -1 -4 1219.73 72.89 0 -1 -4 1234.23 73.66 0 1 4 1235.75 73.81 0 1 4 1180.03 70.53 0 -1 -5 28.78 5.80 0 -1 -5 26.87 4.96 0 1 5 33.51 5.42 0 1 5 29.00 6.11 0 -1 -6 807.55 48.54 0 -1 -6 817.48 49.00 0 1 6 789.23 47.55 0 1 6 749.54 45.03 0 -1 -7 912.12 54.65 0 -1 -7 856.40 51.52 0 1 7 815.19 48.93 0 1 7 822.82 49.69 0 -1 -8 1196.06 71.60 0 -1 -8 1199.12 71.67 0 1 8 1134.24 67.86 0 1 8 1127.37 67.55 0 -1 -9 88.69 8.63 0 1 9 73.89 7.02 0 1 9 71.44 7.71 0 -1 -10 26.79 6.72 0 -1 -10 21.98 5.72 0 1 10 19.46 5.95 0 1 10 22.14 5.95 0 -1 -11 437.67 27.33 0 -1 -11 384.62 24.27 0 1 11 409.50 25.72 0 1 11 375.99 23.51 0 1 12 75.26 8.78 0 1 12 87.70 8.47 0 -1 -13 556.51 34.58 0 -1 -13 589.03 35.87 0 1 13 592.38 36.18 0 1 13 522.24 31.75 0 -1 -14 67.02 7.94 0 -1 -14 42.51 9.77 0 1 14 52.44 7.94 0 1 14 56.10 6.79 0 -1 -15 139.68 10.61 0 -1 -15 137.01 13.13 0 1 15 109.84 9.01 0 -1 -16 8.17 5.80 0 -1 -16 15.57 11.30 0 1 16 10.15 6.41 0 1 16 11.07 5.80 0 -1 -17 80.98 7.63 0 1 17 83.81 7.79 0 1 17 82.43 8.01 0 -2 17 29.69 5.80 0 -2 17 28.62 6.03 0 2 -17 36.26 8.09 0 2 -17 38.16 16.94 0 -2 16 -3.82 5.50 0 -2 16 -1.76 6.03 0 2 -16 -0.61 5.95 0 2 -16 -2.90 17.25 0 -2 15 18.70 5.72 0 -2 15 5.04 6.34 0 2 -15 1.91 6.11 0 2 -15 -15.34 16.72 0 -2 14 10.00 5.34 0 -2 14 3.89 6.26 0 2 -14 11.37 16.56 0 2 -14 17.94 6.56 0 -2 13 71.60 7.79 0 -2 13 80.68 7.17 0 2 -13 77.70 7.71 0 -2 12 820.53 49.46 0 -2 12 806.79 48.54 0 2 -12 759.62 45.87 0 2 -12 1000.66 61.22 0 -2 11 1110.58 66.48 0 -2 11 1190.72 71.37 0 2 -11 1092.26 65.57 0 2 -11 1278.50 76.94 0 -2 10 9.31 6.18 0 -2 10 9.24 5.11 0 2 -10 13.74 7.17 0 2 -10 12.14 7.40 0 -2 9 40.15 6.11 0 -2 9 36.26 5.72 0 2 -9 31.45 7.25 0 2 -9 32.52 7.10 0 -2 8 841.14 50.45 0 -2 8 851.82 51.14 0 2 -8 957.16 57.55 0 2 -8 878.54 52.90 0 -2 7 645.43 38.93 0 -2 7 689.85 41.45 0 2 -7 667.87 40.38 0 2 -7 758.02 45.72 0 -2 6 744.66 44.73 0 -2 6 710.92 42.82 0 2 -6 806.03 48.47 0 2 -6 746.03 44.96 0 -2 5 3379.05 200.97 0 -2 5 3392.03 201.74 0 2 -5 3546.21 210.89 0 2 -5 3495.07 207.92 0 -2 4 3673.68 218.45 0 -2 4 4156.84 247.15 0 2 -4 4308.73 256.23 0 2 -4 4188.89 248.98 0 -2 3 486.82 29.39 0 -2 3 439.12 26.49 0 2 -3 443.24 26.71 0 2 -3 482.85 29.31 0 -2 2 1689.91 100.60 0 -2 2 1660.90 98.92 0 2 -2 1703.65 101.44 0 2 -2 1724.26 102.59 0 -2 1 1346.43 80.14 0 -2 1 1283.08 76.40 0 2 -1 1286.13 76.56 0 2 -1 1294.53 77.09 0 -2 0 136.09 8.47 0 -2 0 136.32 8.40 0 2 0 136.78 8.47 0 2 0 140.98 8.70 0 -2 -1 1296.82 77.24 0 -2 -1 1352.54 80.53 0 2 1 1313.61 78.24 0 2 1 1328.11 79.08 0 -2 -2 1740.28 103.58 0 -2 -2 1777.68 105.79 0 2 2 1784.55 106.25 0 2 2 1687.62 100.45 0 -2 -3 458.96 27.71 0 -2 -3 507.05 30.61 0 2 3 496.06 30.00 0 2 3 463.47 28.01 0 -2 -4 3991.20 237.38 0 -2 -4 4222.48 251.12 0 2 4 4224.77 251.27 0 2 4 4133.94 245.93 0 -2 -5 3305.78 196.70 0 -2 -5 3634.75 216.16 0 2 5 3413.40 203.03 0 2 5 3660.70 217.76 0 -2 -6 748.55 45.03 0 -2 -6 772.44 46.33 0 2 6 773.21 46.48 0 2 6 781.60 47.17 0 -2 -7 718.25 43.35 0 -2 -7 722.90 43.43 0 2 7 698.63 42.36 0 2 7 736.03 44.35 0 -2 -8 914.41 54.96 0 -2 -8 893.80 53.58 0 2 8 883.88 53.12 0 2 8 870.14 52.36 0 -2 -9 42.21 5.95 0 -2 -9 44.04 7.79 0 2 9 37.32 6.95 0 -2 -10 13.59 5.95 0 -2 -10 23.97 7.10 0 2 10 18.78 7.17 0 2 10 11.91 6.11 0 -2 -11 1199.88 71.90 0 -2 -11 1280.02 76.79 0 2 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-6.64 7.02 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12823