data_hydroredmondite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'hydroredmondite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H10 O22 Pb8 S8 Zn' _chemical_formula_weight 2341.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5991(9) _cell_length_b 9.2819(4) _cell_length_c 12.9774(9) _cell_angle_alpha 90 _cell_angle_beta 90.443(6) _cell_angle_gamma 90 _cell_volume 1517.57(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11384 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'equant' _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 5.124 _exptl_crystal_F_000 2000 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 45.604 _shelx_estimated_absorpt_T_min 0.040 _shelx_estimated_absorpt_T_max 0.462 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.232 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 14486 _diffrn_reflns_av_unetI/netI 0.0785 _diffrn_reflns_av_R_equivalents 0.1210 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.140 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3463 _reflns_number_gt 3022 _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_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _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^)+(0.0166P)^2^+33.0300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3463 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Pb1 Pb 0.61677(4) 0.66695(6) 0.44080(4) 0.02205(14) Uani 1 1 d . . . . . Pb2 Pb 0.61349(4) 0.80577(6) 0.70161(4) 0.02628(15) Uani 1 1 d . . . . . Pb3 Pb 0.77559(4) 0.98853(6) 0.50887(5) 0.02992(16) Uani 1 1 d . . . . . Pb4 Pb 0.87410(4) 0.62549(6) 0.61858(4) 0.02559(15) Uani 1 1 d . . . . . Zn Zn 0.500000 0.000000 0.500000 0.0205(5) Uani 1 2 d S . P . . S1 S 0.3735(3) 0.5826(4) 0.2955(3) 0.0282(8) Uani 1 1 d . . . . . S2 S 0.8735(3) 0.6134(4) 0.3621(3) 0.0259(8) Uani 1 1 d . . . . . O1 O 0.4183(10) 0.5182(15) 0.3862(11) 0.058(4) Uani 1 1 d . . . . . O2 O 0.3088(11) 0.7084(14) 0.3145(12) 0.056(4) Uani 1 1 d . . . . . O3 O 0.3111(11) 0.4765(14) 0.2376(12) 0.056(4) Uani 1 1 d . . . . . S1A S 0.4940(5) 0.6416(8) 0.2072(5) 0.0736(19) Uani 1 1 d . . . . . O4 O 0.7985(9) 0.7133(13) 0.3186(9) 0.040(3) Uani 1 1 d . . . . . O5 O 0.9301(9) 0.5340(14) 0.2825(8) 0.039(3) Uani 1 1 d . . . . . O6 O 0.8183(8) 0.5147(11) 0.4329(8) 0.030(2) Uani 1 1 d . . . . . S2A S 0.9816(3) 0.7235(5) 0.4475(3) 0.0392(10) Uani 1 1 d . . . . . O7 O 0.7325(7) 0.7639(10) 0.5731(7) 0.0180(19) Uani 1 1 d . . . . . OH8 O 0.6289(7) 0.9180(11) 0.4097(7) 0.024(2) Uani 1 1 d . . . . . OH9 O 0.3767(8) 0.9706(10) 0.3947(8) 0.025(2) Uani 1 1 d . . . . . OH10 O 0.5019(8) 0.7886(10) 0.5566(8) 0.023(2) Uani 1 1 d . . . . . OW11 O 0.7149(9) 0.2475(12) 0.4004(10) 0.040(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 Pb1 0.0209(3) 0.0228(3) 0.0224(3) -0.0040(2) -0.0022(2) 0.00144(19) Pb2 0.0283(3) 0.0335(3) 0.0171(3) 0.0022(2) 0.0014(2) 0.0100(2) Pb3 0.0216(3) 0.0298(3) 0.0383(3) 0.0100(2) -0.0028(2) -0.0043(2) Pb4 0.0259(3) 0.0306(3) 0.0202(3) 0.0016(2) -0.0015(2) 0.0080(2) Zn 0.0212(10) 0.0184(11) 0.0218(11) 0.0012(9) -0.0034(9) 0.0034(8) S1 0.0276(18) 0.0189(18) 0.038(2) 0.0020(15) -0.0120(15) -0.0030(14) S2 0.0212(16) 0.038(2) 0.0183(16) -0.0041(15) 0.0013(13) 0.0036(15) O1 0.043(7) 0.061(9) 0.070(9) 0.058(8) -0.026(7) -0.025(6) O2 0.056(8) 0.037(8) 0.074(11) -0.019(7) -0.009(7) 0.003(6) O3 0.055(8) 0.038(7) 0.076(10) -0.020(7) -0.026(8) -0.004(6) S1A 0.072(4) 0.089(5) 0.059(4) 0.031(4) 0.004(3) 0.005(3) O4 0.036(6) 0.042(7) 0.042(7) 0.018(6) 0.006(5) 0.014(5) O5 0.033(6) 0.057(8) 0.027(6) -0.019(6) 0.003(5) 0.004(5) O6 0.029(5) 0.028(6) 0.032(6) -0.008(5) 0.001(4) 0.002(4) S2A 0.040(2) 0.048(3) 0.030(2) -0.0075(19) 0.0077(17) -0.019(2) O7 0.019(4) 0.017(5) 0.018(5) 0.007(4) 0.001(4) -0.003(4) OH8 0.031(5) 0.025(5) 0.016(5) 0.003(4) -0.001(4) -0.004(4) OH9 0.029(5) 0.017(5) 0.029(5) -0.001(4) -0.011(4) -0.001(4) OH10 0.029(5) 0.018(5) 0.023(5) -0.001(4) -0.001(4) 0.004(4) OW11 0.048(7) 0.027(6) 0.046(7) -0.009(5) -0.001(6) -0.015(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 Pb1 OH8 2.370(10) . ? Pb1 OH10 2.379(10) . ? Pb1 O7 2.418(9) . ? Pb1 O4 2.828(12) . ? Pb1 O1 2.864(11) 3_666 ? Pb1 O6 2.908(10) . ? Pb1 O1 2.938(11) . ? Pb1 S1A 3.401(7) . ? Pb1 S2 3.436(4) . ? Pb1 Zn 3.5112(5) 1_565 ? Pb1 Pb2 3.6221(8) . ? Pb1 S1 3.671(3) . ? Pb1 Pb3 3.6968(8) . ? Pb1 Pb4 3.9832(8) . ? Pb1 OH9 3.985(10) 3_676 ? Pb2 O7 2.284(9) . ? Pb2 OH10 2.346(9) . ? Pb2 OH9 2.426(10) 3_676 ? Pb2 O2 2.857(13) 4_676 ? Pb2 O3 2.894(14) 3_666 ? Pb2 O5 2.947(12) 4_576 ? Pb2 O3 3.238(13) 4_676 ? Pb2 O1 3.239(15) 3_666 ? Pb2 Zn 3.4759(5) 1_565 ? Pb2 S1 3.608(4) 3_666 ? Pb2 S2A 3.620(4) 4_576 ? Pb2 S1 3.637(3) 4_676 ? Pb2 Pb3 3.6583(9) . ? Pb2 S2 3.760(4) 4_576 ? Pb3 O7 2.311(9) . ? Pb3 OH9 2.330(11) 3_676 ? Pb3 OH8 2.338(9) . ? Pb3 OW11 2.886(12) 1_565 ? Pb3 O3 3.016(15) 4_676 ? Pb3 Zn 3.4748(6) 1_565 ? Pb3 O4 3.566(13) . ? Pb3 S2A 3.668(5) . ? Pb3 O2 3.786(14) 3_676 ? Pb3 Pb4 3.8594(8) . ? Pb3 S1A 3.943(7) 4_676 ? Pb3 S1 3.965(4) 4_676 ? Pb3 OH10 3.969(10) . ? Pb4 O7 2.272(9) . ? Pb4 O6 2.708(10) . ? Pb4 S2A 2.763(4) . ? Pb4 S1A 2.872(6) 4_676 ? Pb4 O2 3.091(16) 4_676 ? Pb4 O5 3.143(11) 3_766 ? Pb4 O3 3.144(17) 3_666 ? Pb4 S2 3.331(4) . ? Pb4 S1 3.552(4) 4_676 ? Pb4 OH9 3.692(10) 4_676 ? Pb4 S2A 3.816(5) 3_766 ? Pb4 S1 3.841(4) 3_666 ? Zn OH9 2.079(9) 3_666 ? Zn OH9 2.079(9) 1_545 ? Zn OH10 2.095(10) 3_666 ? Zn OH10 2.095(10) 1_545 ? Zn OH8 2.149(10) 3_666 ? Zn OH8 2.149(10) 1_545 ? S1 O1 1.432(11) . ? S1 O2 1.446(14) . ? S1 O3 1.464(12) . ? S1 S1A 1.987(8) . ? S2 O4 1.437(11) . ? S2 O5 1.459(11) . ? S2 O6 1.476(12) . ? S2 S2A 2.026(5) . ? O2 OH9 2.779(16) . ? O6 OW11 2.832(15) . ? OH10 OW11 2.812(15) 3_666 ? 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 OH8 Pb1 OH10 71.4(3) . . ? OH8 Pb1 O7 73.5(3) . . ? OH10 Pb1 O7 75.0(3) . . ? OH8 Pb1 O4 72.6(3) . . ? OH10 Pb1 O4 141.3(4) . . ? O7 Pb1 O4 81.7(3) . . ? OH8 Pb1 O1 137.2(4) . 3_666 ? OH10 Pb1 O1 72.0(4) . 3_666 ? O7 Pb1 O1 76.3(3) . 3_666 ? O4 Pb1 O1 131.4(3) . 3_666 ? OH8 Pb1 O6 114.5(3) . . ? OH10 Pb1 O6 142.0(3) . . ? O7 Pb1 O6 71.6(3) . . ? O4 Pb1 O6 49.0(3) . . ? O1 Pb1 O6 82.9(4) 3_666 . ? OH8 Pb1 O1 118.5(3) . . ? OH10 Pb1 O1 81.6(4) . . ? O7 Pb1 O1 148.6(4) . . ? O4 Pb1 O1 128.9(4) . . ? O1 Pb1 O1 76.8(4) 3_666 . ? O6 Pb1 O1 120.3(4) . . ? OH8 Pb1 S1A 86.9(3) . . ? OH10 Pb1 S1A 108.7(3) . . ? O7 Pb1 S1A 157.9(2) . . ? O4 Pb1 S1A 82.8(3) . . ? O1 Pb1 S1A 125.8(3) 3_666 . ? O6 Pb1 S1A 109.0(2) . . ? O1 Pb1 S1A 51.1(3) . . ? OH8 Pb1 S2 91.7(2) . . ? OH10 Pb1 S2 146.6(2) . . ? O7 Pb1 S2 72.6(2) . . ? O4 Pb1 S2 24.1(2) . . ? O1 Pb1 S2 107.3(3) 3_666 . ? O6 Pb1 S2 25.2(2) . . ? O1 Pb1 S2 131.4(3) . . ? S1A Pb1 S2 98.50(13) . . ? OH8 Pb1 Zn 36.8(2) . 1_565 ? OH10 Pb1 Zn 35.5(2) . 1_565 ? O7 Pb1 Zn 76.6(2) . 1_565 ? O4 Pb1 Zn 109.3(2) . 1_565 ? O1 Pb1 Zn 106.8(3) 3_666 1_565 ? O6 Pb1 Zn 143.4(2) . 1_565 ? O1 Pb1 Zn 96.3(3) . 1_565 ? S1A Pb1 Zn 93.87(13) . 1_565 ? S2 Pb1 Zn 126.12(7) . 1_565 ? OH8 Pb1 Pb2 79.1(2) . . ? OH10 Pb1 Pb2 39.6(2) . . ? O7 Pb1 Pb2 38.3(2) . . ? O4 Pb1 Pb2 119.0(3) . . ? O1 Pb1 Pb2 58.5(3) 3_666 . ? O6 Pb1 Pb2 102.8(2) . . ? O1 Pb1 Pb2 112.1(3) . . ? S1A Pb1 Pb2 148.12(12) . . ? S2 Pb1 Pb2 110.30(6) . . ? Zn Pb1 Pb2 58.298(12) 1_565 . ? OH8 Pb1 S1 100.2(2) . . ? OH10 Pb1 S1 85.2(2) . . ? O7 Pb1 S1 160.2(2) . . ? O4 Pb1 S1 114.9(3) . . ? O1 Pb1 S1 98.1(2) 3_666 . ? O6 Pb1 S1 127.2(2) . . ? O1 Pb1 S1 21.6(2) . . ? S1A Pb1 S1 32.34(13) . . ? S2 Pb1 S1 126.93(9) . . ? Zn Pb1 S1 87.17(6) 1_565 . ? Pb2 Pb1 S1 122.70(7) . . ? OH8 Pb1 Pb3 37.9(2) . . ? OH10 Pb1 Pb3 78.3(2) . . ? O7 Pb1 Pb3 37.6(2) . . ? O4 Pb1 Pb3 64.7(3) . . ? O1 Pb1 Pb3 112.6(3) 3_666 . ? O6 Pb1 Pb3 86.0(2) . . ? O1 Pb1 Pb3 153.5(3) . . ? S1A Pb1 Pb3 120.69(12) . . ? S2 Pb1 Pb3 71.27(7) . . ? Zn Pb1 Pb3 57.573(13) 1_565 . ? Pb2 Pb1 Pb3 59.969(16) . . ? S1 Pb1 Pb3 138.01(6) . . ? OH8 Pb1 Pb4 98.1(2) . . ? OH10 Pb1 Pb4 100.2(2) . . ? O7 Pb1 Pb4 30.8(2) . . ? O4 Pb1 Pb4 71.4(2) . . ? O1 Pb1 Pb4 67.5(2) 3_666 . ? O6 Pb1 Pb4 42.8(2) . . ? O1 Pb1 Pb4 141.4(2) . . ? S1A Pb1 Pb4 150.72(12) . . ? S2 Pb1 Pb4 52.72(6) . . ? Zn Pb1 Pb4 107.389(15) 1_565 . ? Pb2 Pb1 Pb4 60.546(15) . . ? S1 Pb1 Pb4 161.73(6) . . ? Pb3 Pb1 Pb4 60.196(14) . . ? OH8 Pb1 OH9 42.3(3) . 3_676 ? OH10 Pb1 OH9 43.2(3) . 3_676 ? O7 Pb1 OH9 45.2(3) . 3_676 ? O4 Pb1 OH9 99.1(3) . 3_676 ? O1 Pb1 OH9 95.1(4) 3_666 3_676 ? O6 Pb1 OH9 114.5(2) . 3_676 ? O1 Pb1 OH9 122.7(4) . 3_676 ? S1A Pb1 OH9 122.91(18) . 3_676 ? S2 Pb1 OH9 105.43(16) . 3_676 ? Zn Pb1 OH9 31.40(13) 1_565 3_676 ? Pb2 Pb1 OH9 36.81(15) . 3_676 ? S1 Pb1 OH9 117.97(15) . 3_676 ? Pb3 Pb1 OH9 35.07(15) . 3_676 ? Pb4 Pb1 OH9 75.99(13) . 3_676 ? O7 Pb2 OH10 78.2(3) . . ? O7 Pb2 OH9 74.5(3) . 3_676 ? OH10 Pb2 OH9 71.2(3) . 3_676 ? O7 Pb2 O2 78.4(4) . 4_676 ? OH10 Pb2 O2 156.5(4) . 4_676 ? OH9 Pb2 O2 104.9(3) 3_676 4_676 ? O7 Pb2 O3 80.1(4) . 3_666 ? OH10 Pb2 O3 110.5(3) . 3_666 ? OH9 Pb2 O3 153.7(4) 3_676 3_666 ? O2 Pb2 O3 62.5(4) 4_676 3_666 ? O7 Pb2 O5 150.1(3) . 4_576 ? OH10 Pb2 O5 81.6(3) . 4_576 ? OH9 Pb2 O5 78.2(3) 3_676 4_576 ? O2 Pb2 O5 121.0(4) 4_676 4_576 ? O3 Pb2 O5 128.0(4) 3_666 4_576 ? O7 Pb2 O3 72.7(4) . 4_676 ? OH10 Pb2 O3 127.9(4) . 4_676 ? OH9 Pb2 O3 59.9(3) 3_676 4_676 ? O2 Pb2 O3 45.3(3) 4_676 4_676 ? O3 Pb2 O3 105.97(14) 3_666 4_676 ? O5 Pb2 O3 103.7(4) 4_576 4_676 ? O7 Pb2 O1 70.5(3) . 3_666 ? OH10 Pb2 O1 65.4(3) . 3_666 ? OH9 Pb2 O1 128.3(3) 3_676 3_666 ? O2 Pb2 O1 104.0(3) 4_676 3_666 ? O3 Pb2 O1 45.2(3) 3_666 3_666 ? O5 Pb2 O1 119.9(3) 4_576 3_666 ? O3 Pb2 O1 136.3(4) 4_676 3_666 ? O7 Pb2 Zn 78.9(2) . 1_565 ? OH10 Pb2 Zn 36.0(2) . 1_565 ? OH9 Pb2 Zn 36.0(2) 3_676 1_565 ? O2 Pb2 Zn 139.2(3) 4_676 1_565 ? O3 Pb2 Zn 143.8(3) 3_666 1_565 ? O5 Pb2 Zn 71.8(2) 4_576 1_565 ? O3 Pb2 Zn 95.5(2) 4_676 1_565 ? O1 Pb2 Zn 99.65(19) 3_666 1_565 ? O7 Pb2 S1 78.9(2) . 3_666 ? OH10 Pb2 S1 88.1(2) . 3_666 ? OH9 Pb2 S1 149.0(3) 3_676 3_666 ? O2 Pb2 S1 84.8(3) 4_676 3_666 ? O3 Pb2 S1 22.8(2) 3_666 3_666 ? O5 Pb2 S1 122.4(2) 4_576 3_666 ? O3 Pb2 S1 126.0(2) 4_676 3_666 ? O1 Pb2 S1 23.3(2) 3_666 3_666 ? Zn Pb2 S1 122.97(6) 1_565 3_666 ? O7 Pb2 S2A 159.9(2) . 4_576 ? OH10 Pb2 S2A 115.2(3) . 4_576 ? OH9 Pb2 S2A 122.9(3) 3_676 4_576 ? O2 Pb2 S2A 86.8(3) 4_676 4_576 ? O3 Pb2 S2A 81.0(3) 3_666 4_576 ? O5 Pb2 S2A 50.0(2) 4_576 4_576 ? O3 Pb2 S2A 106.1(3) 4_676 4_576 ? O1 Pb2 S2A 100.6(3) 3_666 4_576 ? Zn Pb2 S2A 120.91(7) 1_565 4_576 ? S1 Pb2 S2A 86.39(10) 3_666 4_576 ? O7 Pb2 Pb1 41.0(2) . . ? OH10 Pb2 Pb1 40.3(2) . . ? OH9 Pb2 Pb1 79.8(2) 3_676 . ? O2 Pb2 Pb1 116.5(3) 4_676 . ? O3 Pb2 Pb1 85.8(3) 3_666 . ? O5 Pb2 Pb1 121.8(2) 4_576 . ? O3 Pb2 Pb1 110.0(3) 4_676 . ? O1 Pb2 Pb1 49.0(2) 3_666 . ? Zn Pb2 Pb1 59.254(12) 1_565 . ? S1 Pb2 Pb1 69.72(7) 3_666 . ? S2A Pb2 Pb1 143.69(8) 4_576 . ? O7 Pb2 S1 72.4(2) . 4_676 ? OH10 Pb2 S1 145.2(3) . 4_676 ? OH9 Pb2 S1 83.1(2) 3_676 4_676 ? O2 Pb2 S1 21.8(3) 4_676 4_676 ? O3 Pb2 S1 82.7(2) 3_666 4_676 ? O5 Pb2 S1 116.3(2) 4_576 4_676 ? O3 Pb2 S1 23.7(2) 4_676 4_676 ? O1 Pb2 S1 119.4(2) 3_666 4_676 ? Zn Pb2 S1 117.95(7) 1_565 4_676 ? S1 Pb2 S1 103.91(7) 3_666 4_676 ? S2A Pb2 S1 98.29(10) 4_576 4_676 ? Pb1 Pb2 S1 113.44(7) . 4_676 ? O7 Pb2 Pb3 37.5(2) . . ? OH10 Pb2 Pb3 79.5(3) . . ? OH9 Pb2 Pb3 38.8(2) 3_676 . ? O2 Pb2 Pb3 83.6(3) 4_676 . ? O3 Pb2 Pb3 115.0(3) 3_666 . ? O5 Pb2 Pb3 116.9(2) 4_576 . ? O3 Pb2 Pb3 51.4(3) 4_676 . ? O1 Pb2 Pb3 105.0(2) 3_666 . ? Zn Pb2 Pb3 58.228(13) 1_565 . ? S1 Pb2 Pb3 116.40(7) 3_666 . ? S2A Pb2 Pb3 154.17(8) 4_576 . ? Pb1 Pb2 Pb3 61.029(16) . . ? S1 Pb2 Pb3 65.85(7) 4_676 . ? O7 Pb2 S2 166.8(2) . 4_576 ? OH10 Pb2 S2 88.8(3) . 4_576 ? OH9 Pb2 S2 99.1(3) 3_676 4_576 ? O2 Pb2 S2 114.7(3) 4_676 4_576 ? O3 Pb2 S2 107.1(3) 3_666 4_576 ? O5 Pb2 S2 21.0(2) 4_576 4_576 ? O3 Pb2 S2 114.6(3) 4_676 4_576 ? O1 Pb2 S2 106.4(3) 3_666 4_576 ? Zn Pb2 S2 89.17(6) 1_565 4_576 ? S1 Pb2 S2 103.32(9) 3_666 4_576 ? S2A Pb2 S2 31.80(8) 4_576 4_576 ? Pb1 Pb2 S2 127.13(6) . 4_576 ? S1 Pb2 S2 118.91(9) 4_676 4_576 ? Pb3 Pb2 S2 137.87(6) . 4_576 ? O7 Pb3 OH9 75.9(3) . 3_676 ? O7 Pb3 OH8 76.1(3) . . ? OH9 Pb3 OH8 72.0(3) 3_676 . ? O7 Pb3 OW11 149.9(3) . 1_565 ? OH9 Pb3 OW11 84.9(3) 3_676 1_565 ? OH8 Pb3 OW11 76.1(3) . 1_565 ? O7 Pb3 O3 77.0(3) . 4_676 ? OH9 Pb3 O3 64.5(4) 3_676 4_676 ? OH8 Pb3 O3 133.0(4) . 4_676 ? OW11 Pb3 O3 115.3(3) 1_565 4_676 ? O7 Pb3 Zn 78.6(2) . 1_565 ? OH9 Pb3 Zn 35.5(2) 3_676 1_565 ? OH8 Pb3 Zn 37.3(2) . 1_565 ? OW11 Pb3 Zn 72.4(2) 1_565 1_565 ? O3 Pb3 Zn 99.8(3) 4_676 1_565 ? O7 Pb3 O4 67.9(3) . . ? OH9 Pb3 O4 124.1(3) 3_676 . ? OH8 Pb3 O4 59.1(3) . . ? OW11 Pb3 O4 106.3(3) 1_565 . ? O3 Pb3 O4 138.3(3) 4_676 . ? Zn Pb3 O4 94.90(18) 1_565 . ? O7 Pb3 Pb2 37.0(2) . . ? OH9 Pb3 Pb2 40.7(2) 3_676 . ? OH8 Pb3 Pb2 78.7(2) . . ? OW11 Pb3 Pb2 124.9(3) 1_565 . ? O3 Pb3 Pb2 57.1(3) 4_676 . ? Zn Pb3 Pb2 58.257(13) 1_565 . ? O4 Pb3 Pb2 100.95(19) . . ? O7 Pb3 S2A 69.0(2) . . ? OH9 Pb3 S2A 144.4(2) 3_676 . ? OH8 Pb3 S2A 104.5(3) . . ? OW11 Pb3 S2A 129.6(3) 1_565 . ? O3 Pb3 S2A 100.7(3) 4_676 . ? Zn Pb3 S2A 136.22(7) 1_565 . ? O4 Pb3 S2A 46.22(18) . . ? Pb2 Pb3 S2A 103.72(7) . . ? O7 Pb3 Pb1 39.6(2) . . ? OH9 Pb3 Pb1 79.2(2) 3_676 . ? OH8 Pb3 Pb1 38.6(2) . . ? OW11 Pb3 Pb1 114.5(2) 1_565 . ? O3 Pb3 Pb1 113.4(3) 4_676 . ? Zn Pb3 Pb1 58.530(12) 1_565 . ? O4 Pb3 Pb1 45.80(19) . . ? Pb2 Pb3 Pb1 59.002(15) . . ? S2A Pb3 Pb1 77.84(7) . . ? O7 Pb3 O2 112.6(3) . 3_676 ? OH9 Pb3 O2 47.0(3) 3_676 3_676 ? OH8 Pb3 O2 108.5(3) . 3_676 ? OW11 Pb3 O2 66.5(3) 1_565 3_676 ? O3 Pb3 O2 50.5(3) 4_676 3_676 ? Zn Pb3 O2 73.3(2) 1_565 3_676 ? O4 Pb3 O2 167.4(3) . 3_676 ? Pb2 Pb3 O2 76.7(2) . 3_676 ? S2A Pb3 O2 146.3(2) . 3_676 ? Pb1 Pb3 O2 126.2(2) . 3_676 ? O7 Pb3 Pb4 32.3(2) . . ? OH9 Pb3 Pb4 102.0(2) 3_676 . ? OH8 Pb3 Pb4 102.1(2) . . ? OW11 Pb3 Pb4 172.1(3) 1_565 . ? O3 Pb3 Pb4 71.7(2) 4_676 . ? Zn Pb3 Pb4 110.940(17) 1_565 . ? O4 Pb3 Pb4 66.57(17) . . ? Pb2 Pb3 Pb4 61.483(15) . . ? S2A Pb3 Pb4 42.98(7) . . ? Pb1 Pb3 Pb4 63.583(15) . . ? O2 Pb3 Pb4 121.1(2) 3_676 . ? O7 Pb3 S1A 69.7(2) . 4_676 ? OH9 Pb3 S1A 105.8(2) 3_676 4_676 ? OH8 Pb3 S1A 144.9(3) . 4_676 ? OW11 Pb3 S1A 139.0(2) 1_565 4_676 ? O3 Pb3 S1A 45.0(3) 4_676 4_676 ? Zn Pb3 S1A 136.31(11) 1_565 4_676 ? O4 Pb3 S1A 99.94(19) . 4_676 ? Pb2 Pb3 S1A 78.59(11) . 4_676 ? S2A Pb3 S1A 56.27(11) . 4_676 ? Pb1 Pb3 S1A 106.40(11) . 4_676 ? O2 Pb3 S1A 91.7(2) 3_676 4_676 ? Pb4 Pb3 S1A 43.19(10) . 4_676 ? O7 Pb3 S1 65.4(2) . 4_676 ? OH9 Pb3 S1 77.0(2) 3_676 4_676 ? OH8 Pb3 S1 135.1(2) . 4_676 ? OW11 Pb3 S1 132.5(2) 1_565 4_676 ? O3 Pb3 S1 18.5(2) 4_676 4_676 ? Zn Pb3 S1 109.86(6) 1_565 4_676 ? O4 Pb3 S1 120.27(18) . 4_676 ? Pb2 Pb3 S1 56.82(6) . 4_676 ? S2A Pb3 S1 82.90(9) . 4_676 ? Pb1 Pb3 S1 104.69(6) . 4_676 ? O2 Pb3 S1 69.1(2) 3_676 4_676 ? Pb4 Pb3 S1 53.97(5) . 4_676 ? S1A Pb3 S1 29.10(11) 4_676 4_676 ? O7 Pb3 OH10 46.8(3) . . ? OH9 Pb3 OH10 43.3(3) 3_676 . ? OH8 Pb3 OH10 43.2(3) . . ? OW11 Pb3 OH10 103.8(3) 1_565 . ? O3 Pb3 OH10 91.1(3) 4_676 . ? Zn Pb3 OH10 31.82(13) 1_565 . ? O4 Pb3 OH10 81.3(2) . . ? Pb2 Pb3 OH10 35.53(14) . . ? S2A Pb3 OH10 109.72(15) . . ? Pb1 Pb3 OH10 35.94(14) . . ? O2 Pb3 OH10 90.3(3) 3_676 . ? Pb4 Pb3 OH10 79.14(13) . . ? S1A Pb3 OH10 110.96(17) 4_676 . ? S1 Pb3 OH10 92.30(15) 4_676 . ? O7 Pb4 O6 77.6(3) . . ? O7 Pb4 S2A 89.7(2) . . ? O6 Pb4 S2A 62.3(2) . . ? O7 Pb4 S1A 95.0(3) . 4_676 ? O6 Pb4 S1A 140.7(3) . 4_676 ? S2A Pb4 S1A 79.30(17) . 4_676 ? O7 Pb4 O2 73.6(3) . 4_676 ? O6 Pb4 O2 148.5(3) . 4_676 ? S2A Pb4 O2 129.2(3) . 4_676 ? S1A Pb4 O2 55.8(3) 4_676 4_676 ? O7 Pb4 O5 169.9(3) . 3_766 ? O6 Pb4 O5 112.5(3) . 3_766 ? S2A Pb4 O5 95.5(2) . 3_766 ? S1A Pb4 O5 77.4(3) 4_676 3_766 ? O2 Pb4 O5 96.4(3) 4_676 3_766 ? O7 Pb4 O3 74.9(3) . 3_666 ? O6 Pb4 O3 103.0(3) . 3_666 ? S2A Pb4 O3 161.1(3) . 3_666 ? S1A Pb4 O3 112.3(3) 4_676 3_666 ? O2 Pb4 O3 57.2(3) 4_676 3_666 ? O5 Pb4 O3 101.5(3) 3_766 3_666 ? O7 Pb4 S2 76.4(2) . . ? O6 Pb4 S2 25.7(2) . . ? S2A Pb4 S2 37.40(11) . . ? S1A Pb4 S2 115.00(16) 4_676 . ? O2 Pb4 S2 147.2(2) 4_676 . ? O5 Pb4 S2 112.8(2) 3_766 . ? O3 Pb4 S2 126.0(2) 3_666 . ? O7 Pb4 S1 74.4(2) . 4_676 ? O6 Pb4 S1 149.7(2) . 4_676 ? S2A Pb4 S1 105.76(12) . 4_676 ? S1A Pb4 S1 33.98(14) 4_676 4_676 ? O2 Pb4 S1 23.9(3) 4_676 4_676 ? O5 Pb4 S1 95.8(2) 3_766 4_676 ? O3 Pb4 S1 80.8(2) 3_666 4_676 ? S2 Pb4 S1 132.22(10) . 4_676 ? O7 Pb4 OH9 112.9(3) . 4_676 ? O6 Pb4 OH9 140.5(3) . 4_676 ? S2A Pb4 OH9 149.12(17) . 4_676 ? S1A Pb4 OH9 78.0(2) 4_676 4_676 ? O2 Pb4 OH9 47.4(3) 4_676 4_676 ? O5 Pb4 OH9 59.2(3) 3_766 4_676 ? O3 Pb4 OH9 49.7(3) 3_666 4_676 ? S2 Pb4 OH9 164.08(17) . 4_676 ? S1 Pb4 OH9 63.70(16) 4_676 4_676 ? O7 Pb4 Pb2 129.3(2) . 2_646 ? O6 Pb4 Pb2 105.1(2) . 2_646 ? S2A Pb4 Pb2 137.44(11) . 2_646 ? S1A Pb4 Pb2 108.95(15) 4_676 2_646 ? O2 Pb4 Pb2 83.9(2) 4_676 2_646 ? O5 Pb4 Pb2 49.4(2) 3_766 2_646 ? O3 Pb4 Pb2 54.9(2) 3_666 2_646 ? S2 Pb4 Pb2 126.20(7) . 2_646 ? S1 Pb4 Pb2 101.55(7) 4_676 2_646 ? OH9 Pb4 Pb2 37.89(15) 4_676 2_646 ? O7 Pb4 S2A 142.8(2) . 3_766 ? O6 Pb4 S2A 66.3(2) . 3_766 ? S2A Pb4 S2A 82.04(14) . 3_766 ? S1A Pb4 S2A 118.62(15) 4_676 3_766 ? O2 Pb4 S2A 137.6(2) 4_676 3_766 ? O5 Pb4 S2A 47.0(2) 3_766 3_766 ? O3 Pb4 S2A 103.6(2) 3_666 3_766 ? S2 Pb4 S2A 75.16(9) . 3_766 ? S1 Pb4 S2A 142.80(8) 4_676 3_766 ? OH9 Pb4 S2A 90.71(17) 4_676 3_766 ? Pb2 Pb4 S2A 56.94(7) 2_646 3_766 ? O7 Pb4 S1 73.9(2) . 3_666 ? O6 Pb4 S1 82.0(2) . 3_666 ? S2A Pb4 S1 143.40(10) . 3_666 ? S1A Pb4 S1 133.46(15) 4_676 3_666 ? O2 Pb4 S1 77.9(3) 4_676 3_666 ? O5 Pb4 S1 106.3(2) 3_766 3_666 ? O3 Pb4 S1 21.3(2) 3_666 3_666 ? S2 Pb4 S1 106.12(9) . 3_666 ? S1 Pb4 S1 100.96(4) 4_676 3_666 ? OH9 Pb4 S1 66.31(16) 4_676 3_666 ? Pb2 Pb4 S1 57.02(5) 2_646 3_666 ? S2A Pb4 S1 91.60(9) 3_766 3_666 ? O7 Pb4 Pb2 32.5(2) . . ? O6 Pb4 Pb2 101.4(2) . . ? S2A Pb4 Pb2 120.44(11) . . ? S1A Pb4 Pb2 90.45(14) 4_676 . ? O2 Pb4 Pb2 47.1(2) 4_676 . ? O5 Pb4 Pb2 139.4(2) 3_766 . ? O3 Pb4 Pb2 47.6(2) 3_666 . ? S2 Pb4 Pb2 107.43(6) . . ? S1 Pb4 Pb2 58.73(6) 4_676 . ? OH9 Pb4 Pb2 80.48(15) 4_676 . ? Pb2 Pb4 Pb2 101.540(15) 2_646 . ? S2A Pb4 Pb2 147.30(6) 3_766 . ? S1 Pb4 Pb2 55.99(6) 3_666 . ? O7 Pb4 Pb3 33.0(2) . . ? O6 Pb4 Pb3 85.6(2) . . ? S2A Pb4 Pb3 64.82(11) . . ? S1A Pb4 Pb3 69.96(15) 4_676 . ? O2 Pb4 Pb3 77.4(2) 4_676 . ? O5 Pb4 Pb3 144.2(2) 3_766 . ? O3 Pb4 Pb3 104.1(2) 3_666 . ? S2 Pb4 Pb3 70.29(7) . . ? S1 Pb4 Pb3 64.54(6) 4_676 . ? OH9 Pb4 Pb3 124.70(15) 4_676 . ? Pb2 Pb4 Pb3 157.73(2) 2_646 . ? S2A Pb4 Pb3 144.17(7) 3_766 . ? S1 Pb4 Pb3 106.64(6) 3_666 . ? Pb2 Pb4 Pb3 56.684(14) . . ? OH9 Zn OH9 180.0 3_666 1_545 ? OH9 Zn OH10 96.5(4) 3_666 3_666 ? OH9 Zn OH10 83.5(4) 1_545 3_666 ? OH9 Zn OH10 83.5(4) 3_666 1_545 ? OH9 Zn OH10 96.5(4) 1_545 1_545 ? OH10 Zn OH10 180.0 3_666 1_545 ? OH9 Zn OH8 99.1(4) 3_666 3_666 ? OH9 Zn OH8 80.9(4) 1_545 3_666 ? OH10 Zn OH8 81.5(4) 3_666 3_666 ? OH10 Zn OH8 98.5(4) 1_545 3_666 ? OH9 Zn OH8 80.9(4) 3_666 1_545 ? OH9 Zn OH8 99.1(4) 1_545 1_545 ? OH10 Zn OH8 98.5(4) 3_666 1_545 ? OH10 Zn OH8 81.5(4) 1_545 1_545 ? OH8 Zn OH8 180.0(4) 3_666 1_545 ? OH9 Zn Pb3 40.6(3) 3_666 1_545 ? OH9 Zn Pb3 139.4(3) 1_545 1_545 ? OH10 Zn Pb3 92.8(3) 3_666 1_545 ? OH10 Zn Pb3 87.2(3) 1_545 1_545 ? OH8 Zn Pb3 138.7(2) 3_666 1_545 ? OH8 Zn Pb3 41.3(2) 1_545 1_545 ? OH9 Zn Pb3 139.4(3) 3_666 3_666 ? OH9 Zn Pb3 40.6(3) 1_545 3_666 ? OH10 Zn Pb3 87.2(3) 3_666 3_666 ? OH10 Zn Pb3 92.8(3) 1_545 3_666 ? OH8 Zn Pb3 41.3(2) 3_666 3_666 ? OH8 Zn Pb3 138.7(2) 1_545 3_666 ? Pb3 Zn Pb3 180.0 1_545 3_666 ? OH9 Zn Pb2 43.3(3) 3_666 1_545 ? OH9 Zn Pb2 136.7(3) 1_545 1_545 ? OH10 Zn Pb2 138.9(3) 3_666 1_545 ? OH10 Zn Pb2 41.1(3) 1_545 1_545 ? OH8 Zn Pb2 94.7(2) 3_666 1_545 ? OH8 Zn Pb2 85.3(2) 1_545 1_545 ? Pb3 Zn Pb2 63.515(14) 1_545 1_545 ? Pb3 Zn Pb2 116.485(14) 3_666 1_545 ? OH9 Zn Pb2 136.7(3) 3_666 3_666 ? OH9 Zn Pb2 43.3(3) 1_545 3_666 ? OH10 Zn Pb2 41.1(3) 3_666 3_666 ? OH10 Zn Pb2 138.9(3) 1_545 3_666 ? OH8 Zn Pb2 85.3(2) 3_666 3_666 ? OH8 Zn Pb2 94.7(2) 1_545 3_666 ? Pb3 Zn Pb2 116.485(14) 1_545 3_666 ? Pb3 Zn Pb2 63.515(14) 3_666 3_666 ? Pb2 Zn Pb2 180.0 1_545 3_666 ? OH9 Zn Pb1 93.0(3) 3_666 3_666 ? OH9 Zn Pb1 87.0(3) 1_545 3_666 ? OH10 Zn Pb1 41.3(3) 3_666 3_666 ? OH10 Zn Pb1 138.7(3) 1_545 3_666 ? OH8 Zn Pb1 41.3(3) 3_666 3_666 ? OH8 Zn Pb1 138.7(3) 1_545 3_666 ? Pb3 Zn Pb1 116.103(13) 1_545 3_666 ? Pb3 Zn Pb1 63.897(13) 3_666 3_666 ? Pb2 Zn Pb1 117.553(13) 1_545 3_666 ? Pb2 Zn Pb1 62.447(13) 3_666 3_666 ? OH9 Zn Pb1 87.0(3) 3_666 1_545 ? OH9 Zn Pb1 93.0(3) 1_545 1_545 ? OH10 Zn Pb1 138.7(3) 3_666 1_545 ? OH10 Zn Pb1 41.3(3) 1_545 1_545 ? OH8 Zn Pb1 138.7(3) 3_666 1_545 ? OH8 Zn Pb1 41.3(3) 1_545 1_545 ? Pb3 Zn Pb1 63.897(13) 1_545 1_545 ? Pb3 Zn Pb1 116.103(13) 3_666 1_545 ? Pb2 Zn Pb1 62.447(13) 1_545 1_545 ? Pb2 Zn Pb1 117.553(13) 3_666 1_545 ? Pb1 Zn Pb1 180.0 3_666 1_545 ? O1 S1 O2 114.6(10) . . ? O1 S1 O3 110.4(8) . . ? O2 S1 O3 109.2(7) . . ? O1 S1 S1A 106.9(6) . . ? O2 S1 S1A 108.0(7) . . ? O3 S1 S1A 107.4(7) . . ? O1 S1 Pb4 147.9(5) . 4_575 ? O2 S1 Pb4 59.9(7) . 4_575 ? O3 S1 Pb4 100.7(6) . 4_575 ? S1A S1 Pb4 53.9(2) . 4_575 ? O1 S1 Pb2 63.7(6) . 3_666 ? O2 S1 Pb2 146.1(6) . 3_666 ? O3 S1 Pb2 50.0(5) . 3_666 ? S1A S1 Pb2 104.3(3) . 3_666 ? Pb4 S1 Pb2 140.21(13) 4_575 3_666 ? O1 S1 Pb2 138.0(6) . 4_575 ? O2 S1 Pb2 47.1(5) . 4_575 ? O3 S1 Pb2 62.7(5) . 4_575 ? S1A S1 Pb2 114.7(2) . 4_575 ? Pb4 S1 Pb2 64.69(6) 4_575 4_575 ? Pb2 S1 Pb2 109.20(9) 3_666 4_575 ? O1 S1 Pb1 49.0(5) . . ? O2 S1 Pb1 102.1(5) . . ? O3 S1 Pb1 148.2(6) . . ? S1A S1 Pb1 66.3(2) . . ? Pb4 S1 Pb1 99.40(9) 4_575 . ? Pb2 S1 Pb1 99.79(8) 3_666 . ? Pb2 S1 Pb1 149.06(12) 4_575 . ? O1 S1 Pb4 82.4(5) . 3_666 ? O2 S1 Pb4 84.1(6) . 3_666 ? O3 S1 Pb4 51.4(7) . 3_666 ? S1A S1 Pb4 158.8(3) . 3_666 ? Pb4 S1 Pb4 125.24(9) 4_575 3_666 ? Pb2 S1 Pb4 62.08(6) 3_666 3_666 ? Pb2 S1 Pb4 60.61(6) 4_575 3_666 ? Pb1 S1 Pb4 129.42(11) . 3_666 ? O1 S1 Pb3 145.0(7) . 4_575 ? O2 S1 Pb3 97.0(6) . 4_575 ? O3 S1 Pb3 40.9(6) . 4_575 ? S1A S1 Pb3 74.8(2) . 4_575 ? Pb4 S1 Pb3 61.49(6) 4_575 4_575 ? Pb2 S1 Pb3 81.79(8) 3_666 4_575 ? Pb2 S1 Pb3 57.33(5) 4_575 4_575 ? Pb1 S1 Pb3 140.33(12) . 4_575 ? Pb4 S1 Pb3 86.63(7) 3_666 4_575 ? O1 S1 Pb1 22.6(5) . 3_666 ? O2 S1 Pb1 108.9(7) . 3_666 ? O3 S1 Pb1 93.5(6) . 3_666 ? S1A S1 Pb1 127.9(2) . 3_666 ? Pb4 S1 Pb1 164.28(12) 4_575 3_666 ? Pb2 S1 Pb1 55.30(5) 3_666 3_666 ? Pb2 S1 Pb1 117.26(10) 4_575 3_666 ? Pb1 S1 Pb1 71.03(6) . 3_666 ? Pb4 S1 Pb1 59.80(6) 3_666 3_666 ? Pb3 S1 Pb1 133.67(10) 4_575 3_666 ? O4 S2 O5 111.8(7) . . ? O4 S2 O6 109.5(6) . . ? O5 S2 O6 111.3(7) . . ? O4 S2 S2A 109.0(6) . . ? O5 S2 S2A 108.2(5) . . ? O6 S2 S2A 106.9(5) . . ? O4 S2 Pb4 111.5(5) . . ? O5 S2 Pb4 136.7(5) . . ? O6 S2 Pb4 52.8(4) . . ? S2A S2 Pb4 55.92(15) . . ? O4 S2 Pb1 53.5(5) . . ? O5 S2 Pb1 138.6(5) . . ? O6 S2 Pb1 57.0(4) . . ? S2A S2 Pb1 113.23(19) . . ? Pb4 S2 Pb1 72.10(7) . . ? O4 S2 Pb2 100.5(5) . 4_675 ? O5 S2 Pb2 46.3(5) . 4_675 ? O6 S2 Pb2 148.7(4) . 4_675 ? S2A S2 Pb2 70.29(15) . 4_675 ? Pb4 S2 Pb2 123.46(10) . 4_675 ? Pb1 S2 Pb2 153.97(12) . 4_675 ? O4 S2 Pb4 158.4(5) . 3_766 ? O5 S2 Pb4 49.7(5) . 3_766 ? O6 S2 Pb4 89.7(4) . 3_766 ? S2A S2 Pb4 72.92(17) . 3_766 ? Pb4 S2 Pb4 87.67(8) . 3_766 ? Pb1 S2 Pb4 146.70(12) . 3_766 ? Pb2 S2 Pb4 59.22(5) 4_675 3_766 ? O4 S2 Pb3 56.1(5) . . ? O5 S2 Pb3 153.5(6) . . ? O6 S2 Pb3 95.2(4) . . ? S2A S2 Pb3 61.81(17) . . ? Pb4 S2 Pb3 60.82(6) . . ? Pb1 S2 Pb3 57.28(6) . . ? Pb2 S2 Pb3 109.21(10) 4_675 . ? Pb4 S2 Pb3 133.94(9) 3_766 . ? S1 O1 Pb1 146.3(7) . 3_666 ? S1 O1 Pb1 109.4(6) . . ? Pb1 O1 Pb1 103.2(4) 3_666 . ? S1 O1 Pb2 93.0(7) . 3_666 ? Pb1 O1 Pb2 72.5(3) 3_666 3_666 ? Pb1 O1 Pb2 128.6(5) . 3_666 ? S1 O1 Pb4 76.4(5) . 3_666 ? Pb1 O1 Pb4 70.0(2) 3_666 3_666 ? Pb1 O1 Pb4 164.2(6) . 3_666 ? Pb2 O1 Pb4 64.2(2) 3_666 3_666 ? S1 O2 OH9 126.8(7) . . ? S1 O2 Pb2 111.1(7) . 4_575 ? OH9 O2 Pb2 119.6(5) . 4_575 ? S1 O2 Pb4 96.2(8) . 4_575 ? OH9 O2 Pb4 77.7(4) . 4_575 ? Pb2 O2 Pb4 80.5(4) 4_575 4_575 ? S1 O2 Pb3 149.8(8) . 3_676 ? OH9 O2 Pb3 37.8(3) . 3_676 ? Pb2 O2 Pb3 95.7(4) 4_575 3_676 ? Pb4 O2 Pb3 101.8(4) 4_575 3_676 ? S1 O2 Pb4 74.7(6) . 3_666 ? OH9 O2 Pb4 141.3(6) . 3_666 ? Pb2 O2 Pb4 64.9(3) 4_575 3_666 ? Pb4 O2 Pb4 136.8(4) 4_575 3_666 ? Pb3 O2 Pb4 106.4(4) 3_676 3_666 ? S1 O3 Pb2 107.2(7) . 3_666 ? S1 O3 Pb3 120.5(8) . 4_575 ? Pb2 O3 Pb3 114.3(4) 3_666 4_575 ? S1 O3 Pb4 107.2(8) . 3_666 ? Pb2 O3 Pb4 79.0(4) 3_666 3_666 ? Pb3 O3 Pb4 120.8(4) 4_575 3_666 ? S1 O3 Pb2 93.6(6) . 4_575 ? Pb2 O3 Pb2 148.8(5) 3_666 4_575 ? Pb3 O3 Pb2 71.5(3) 4_575 4_575 ? Pb4 O3 Pb2 72.6(3) 3_666 4_575 ? S1 O3 Pb4 58.7(5) . 4_575 ? Pb2 O3 Pb4 149.0(5) 3_666 4_575 ? Pb3 O3 Pb4 63.8(3) 4_575 4_575 ? Pb4 O3 Pb4 130.1(4) 3_666 4_575 ? Pb2 O3 Pb4 62.1(2) 4_575 4_575 ? S1 S1A Pb4 92.1(3) . 4_575 ? S1 S1A Pb1 81.3(2) . . ? Pb4 S1A Pb1 122.6(3) 4_575 . ? S1 S1A Pb3 76.1(2) . 4_575 ? Pb4 S1A Pb3 66.86(13) 4_575 4_575 ? Pb1 S1A Pb3 156.0(2) . 4_575 ? S1 S1A Pb3 144.0(3) . 2_645 ? Pb4 S1A Pb3 110.10(17) 4_575 2_645 ? Pb1 S1A Pb3 107.45(16) . 2_645 ? Pb3 S1A Pb3 86.80(14) 4_575 2_645 ? S1 S1A Pb2 50.6(2) . 3_666 ? Pb4 S1A Pb2 129.6(2) 4_575 3_666 ? Pb1 S1A Pb2 88.01(13) . 3_666 ? Pb3 S1A Pb2 71.40(12) 4_575 3_666 ? Pb3 S1A Pb2 94.14(15) 2_645 3_666 ? S2 O4 Pb1 102.4(6) . . ? S2 O4 Pb3 104.3(6) . . ? Pb1 O4 Pb3 69.5(3) . . ? S2 O4 Pb4 49.4(4) . . ? Pb1 O4 Pb4 67.6(2) . . ? Pb3 O4 Pb4 60.16(19) . . ? S2 O5 Pb2 112.7(6) . 4_675 ? S2 O5 Pb4 109.6(6) . 3_766 ? Pb2 O5 Pb4 76.6(3) 4_675 3_766 ? S2 O6 Pb4 101.4(5) . . ? S2 O6 OW11 132.0(7) . . ? Pb4 O6 OW11 125.6(5) . . ? S2 O6 Pb1 97.9(5) . . ? Pb4 O6 Pb1 90.3(3) . . ? OW11 O6 Pb1 91.7(4) . . ? S2 O6 Pb4 69.4(4) . 3_766 ? Pb4 O6 Pb4 91.5(3) . 3_766 ? OW11 O6 Pb4 97.5(4) . 3_766 ? Pb1 O6 Pb4 167.2(4) . 3_766 ? S2 S2A Pb4 86.68(17) . . ? S2 S2A Pb2 77.91(16) . 4_675 ? Pb4 S2A Pb2 156.17(17) . 4_675 ? S2 S2A Pb3 89.06(18) . . ? Pb4 S2A Pb3 72.21(10) . . ? Pb2 S2A Pb3 124.89(14) 4_675 . ? S2 S2A Pb4 76.57(17) . 3_766 ? Pb4 S2A Pb4 97.96(14) . 3_766 ? Pb2 S2A Pb4 61.00(7) 4_675 3_766 ? Pb3 S2A Pb4 163.21(12) . 3_766 ? S2 S2A Pb3 154.5(2) . 3_776 ? Pb4 S2A Pb3 118.29(13) . 3_776 ? Pb2 S2A Pb3 79.83(8) 4_675 3_776 ? Pb3 S2A Pb3 93.52(10) . 3_776 ? Pb4 S2A Pb3 103.20(10) 3_766 3_776 ? Pb4 O7 Pb2 115.2(4) . . ? Pb4 O7 Pb3 114.7(4) . . ? Pb2 O7 Pb3 105.5(4) . . ? Pb4 O7 Pb1 116.2(4) . . ? Pb2 O7 Pb1 100.7(3) . . ? Pb3 O7 Pb1 102.8(3) . . ? Zn OH8 Pb3 101.4(4) 1_565 . ? Zn OH8 Pb1 101.9(4) 1_565 . ? Pb3 OH8 Pb1 103.5(4) . . ? Zn OH8 O5 98.8(4) 1_565 2_655 ? Pb3 OH8 O5 125.7(5) . 2_655 ? Pb1 OH8 O5 120.7(5) . 2_655 ? Zn OH8 Pb2 61.7(2) 1_565 . ? Pb3 OH8 Pb2 65.7(2) . . ? Pb1 OH8 Pb2 64.7(2) . . ? O5 OH8 Pb2 160.2(4) 2_655 . ? Zn OH9 Pb3 103.9(4) 1_565 3_676 ? Zn OH9 Pb2 100.7(4) 1_565 3_676 ? Pb3 OH9 Pb2 100.5(4) 3_676 3_676 ? Zn OH9 O2 126.0(5) 1_565 . ? Pb3 OH9 O2 95.2(4) 3_676 . ? Pb2 OH9 O2 125.0(5) 3_676 . ? Zn OH9 Pb4 132.1(4) 1_565 4_575 ? Pb3 OH9 Pb4 124.0(3) 3_676 4_575 ? Pb2 OH9 Pb4 73.0(2) 3_676 4_575 ? O2 OH9 Pb4 54.9(4) . 4_575 ? Zn OH9 Pb1 61.6(2) 1_565 3_676 ? Pb3 OH9 Pb1 65.7(2) 3_676 3_676 ? Pb2 OH9 Pb1 63.4(2) 3_676 3_676 ? O2 OH9 Pb1 160.9(5) . 3_676 ? Pb4 OH9 Pb1 136.4(3) 4_575 3_676 ? Zn OH10 Pb2 102.9(4) 1_565 . ? Zn OH10 Pb1 103.2(4) 1_565 . ? Pb2 OH10 Pb1 100.1(3) . . ? Zn OH10 OW11 99.9(4) 1_565 3_666 ? Pb2 OH10 OW11 115.2(5) . 3_666 ? Pb1 OH10 OW11 131.7(4) . 3_666 ? Zn OH10 Pb3 61.0(2) 1_565 . ? Pb2 OH10 Pb3 65.0(2) . . ? Pb1 OH10 Pb3 65.8(2) . . ? OW11 OH10 Pb3 158.9(4) 3_666 . ? Zn OH10 Pb3 56.9(2) 1_565 3_676 ? Pb2 OH10 Pb3 129.0(3) . 3_676 ? Pb1 OH10 Pb3 128.6(3) . 3_676 ? OW11 OH10 Pb3 44.0(3) 3_666 3_676 ? Pb3 OH10 Pb3 117.9(2) . 3_676 ? O6 OW11 O4 105.6(5) . 2_645 ? O6 OW11 Pb3 122.5(5) . 1_545 ? O4 OW11 Pb3 113.9(5) 2_645 1_545 ? O6 OW11 Pb1 44.9(3) . . ? O4 OW11 Pb1 102.5(4) 2_645 . ? Pb3 OW11 Pb1 143.5(4) 1_545 . ? _refine_diff_density_max 3.289 _refine_diff_density_min -2.263 _refine_diff_density_rms 0.536 _shelx_res_file ; TITL hydroredmondite R4.res created by SHELXL-2016/6 at 11:50:39 on 17-Jul-2021 CELL 0.71075 12.59910 9.28187 12.97740 90.00000 90.44330 90.00000 ZERR 2 0.00089 0.00035 0.00091 0.00000 0.00640 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC H O PB S ZN UNIT 20 44 16 16 2 L.S. 20 omit -5 7 9 CONN 15 3.0 PB1 CONN 15 3.0 PB2 CONN 15 3.0 PB3 CONN 15 3.0 PB4 EQIV $1 1.5-x, 0.5+y, 0.5-z EQIV $2 1-x, 1-y, 1-z EQIV $3 1.5-x, -0.5+y, 0.5-z BIND OH8 O5_$1 BIND OH9 O2 BIND OH10 OW11_$2 BIND OW11 O4_$3 BIND OW11 O6 FMAP 2 PLAN 20 ACTA SIZE 0.200 0.025 0.020 WGHT 0.016600 33.029999 FVAR 0.10936 PB1 3 0.616769 0.666946 0.440800 11.00000 0.02094 0.02278 = 0.02238 -0.00397 -0.00223 0.00144 PB2 3 0.613490 0.805774 0.701606 11.00000 0.02827 0.03352 = 0.01707 0.00217 0.00142 0.01000 PB3 3 0.775588 0.988527 0.508872 11.00000 0.02161 0.02980 = 0.03831 0.00998 -0.00276 -0.00425 PB4 3 0.874098 0.625487 0.618576 11.00000 0.02589 0.03061 = 0.02024 0.00160 -0.00146 0.00801 ZN 5 0.500000 0.000000 0.500000 10.50000 0.02119 0.01840 = 0.02176 0.00122 -0.00340 0.00338 S1 4 0.373483 0.582569 0.295536 11.00000 0.02764 0.01893 = 0.03768 0.00197 -0.01201 -0.00300 S2 4 0.873546 0.613351 0.362078 11.00000 0.02117 0.03841 = 0.01825 -0.00413 0.00129 0.00356 O1 2 0.418299 0.518183 0.386191 11.00000 0.04288 0.06118 = 0.06995 0.05834 -0.02628 -0.02461 O2 2 0.308785 0.708380 0.314526 11.00000 0.05599 0.03658 = 0.07442 -0.01883 -0.00942 0.00252 O3 2 0.311063 0.476484 0.237640 11.00000 0.05483 0.03774 = 0.07597 -0.01975 -0.02578 -0.00411 S1A 4 0.493986 0.641623 0.207207 11.00000 0.07232 0.08928 = 0.05923 0.03083 0.00372 0.00506 O4 2 0.798532 0.713349 0.318621 11.00000 0.03553 0.04152 = 0.04189 0.01830 0.00611 0.01370 O5 2 0.930130 0.534021 0.282476 11.00000 0.03281 0.05667 = 0.02723 -0.01912 0.00297 0.00361 O6 2 0.818267 0.514691 0.432924 11.00000 0.02932 0.02782 = 0.03179 -0.00767 0.00135 0.00167 S2A 4 0.981612 0.723504 0.447548 11.00000 0.03950 0.04832 = 0.02998 -0.00754 0.00774 -0.01860 O7 2 0.732534 0.763947 0.573144 11.00000 0.01930 0.01668 = 0.01803 0.00734 0.00150 -0.00316 OH8 2 0.628873 0.917957 0.409687 11.00000 0.03127 0.02489 = 0.01565 0.00286 -0.00148 -0.00436 OH9 2 0.376728 0.970607 0.394653 11.00000 0.02878 0.01714 = 0.02931 -0.00128 -0.01058 -0.00137 OH10 2 0.501906 0.788599 0.556567 11.00000 0.02881 0.01831 = 0.02297 -0.00092 -0.00107 0.00436 OW11 2 0.714859 0.247503 0.400354 11.00000 0.04777 0.02692 = 0.04608 -0.00916 -0.00108 -0.01487 HKLF 4 REM hydroredmondite REM R1 = 0.0473 for 3022 Fo > 4sig(Fo) and 0.0545 for all 3463 data REM 178 parameters refined using 0 restraints END WGHT 0.0166 33.0346 REM Highest difference peak 3.289, deepest hole -2.263, 1-sigma level 0.536 Q1 1 0.8162 0.6257 0.5791 11.00000 0.05 3.29 Q2 1 0.7073 0.9865 0.4845 11.00000 0.05 3.27 Q3 1 0.8372 0.9950 0.5461 11.00000 0.05 3.08 Q4 1 0.6820 0.6761 0.4599 11.00000 0.05 2.90 Q5 1 0.9259 0.6285 0.6626 11.00000 0.05 2.86 Q6 1 0.6743 0.8085 0.7233 11.00000 0.05 2.76 Q7 1 0.5601 0.8126 0.6635 11.00000 0.05 2.73 Q8 1 0.5581 0.6624 0.4074 11.00000 0.05 2.59 Q9 1 0.9175 0.6312 0.5820 11.00000 0.05 2.50 Q10 1 0.7431 0.6670 0.5010 11.00000 0.05 2.39 Q11 1 0.8168 0.7177 0.5474 11.00000 0.05 2.36 Q12 1 0.6426 0.6632 0.3799 11.00000 0.05 2.36 Q13 1 0.7426 0.6290 0.5587 11.00000 0.05 2.07 Q14 1 0.6162 0.4835 0.4428 11.00000 0.05 2.02 Q15 1 0.7684 0.9713 0.4535 11.00000 0.05 1.82 Q16 1 0.3838 0.3780 0.2967 11.00000 0.05 1.79 Q17 1 0.6295 0.9626 0.4430 11.00000 0.05 1.78 Q18 1 0.6547 0.8032 0.6657 11.00000 0.05 1.78 Q19 1 0.8737 0.5288 0.5615 11.00000 0.05 1.76 Q20 1 0.5436 0.8651 0.6351 11.00000 0.05 1.73 ; _shelx_res_checksum 28573 _shelx_hkl_file ; -1 -1 1 2315.81 91.39 1 -1 -1 1757.34 88.62 0 0 -2 1049.65 43.84 0 0 2 1036.84 40.33 -1 -1 -1 2358.94 116.93 -1 1 -1 2288.66 119.01 1 -1 1 2314.97 115.21 -1 -1 -1 2518.40 131.06 1 1 1 2110.05 106.88 -1 1 -1 2358.42 116.54 1 1 1 2291.96 120.78 1 -1 1 2154.21 118.91 -2 0 0 235.24 6.58 2 0 0 237.60 6.59 -2 0 0 232.24 6.45 2 0 0 243.36 8.25 -1 0 2 14.18 0.74 1 0 -2 9.33 0.74 -1 0 -2 3.93 1.30 1 0 2 9.67 1.24 -1 0 -2 3.89 0.87 2 0 -1 4.18 0.77 2 0 1 2.11 1.12 2 0 1 2.08 0.76 -2 0 -1 4.53 0.72 -2 0 -1 2.64 1.62 0 1 2 211.35 6.73 0 -1 -2 228.57 9.19 0 1 -2 183.80 7.04 0 -1 2 206.89 6.38 -2 -1 0 454.54 14.02 2 -1 0 442.88 15.09 2 1 0 373.43 13.58 -2 1 0 437.24 13.25 -2 -1 0 444.48 12.99 2 1 0 444.37 13.10 -1 -1 2 24.73 0.72 -1 1 2 23.21 1.58 1 1 -2 21.47 0.96 1 -1 -2 17.30 1.59 -1 1 -2 55.96 2.96 -1 1 -2 59.37 3.44 -1 -1 -2 65.09 2.33 -1 -1 -2 68.97 3.42 1 1 2 69.99 4.64 1 -1 2 65.20 4.80 2 -1 -1 80.55 3.71 2 1 -1 77.13 2.57 -2 -1 1 79.27 1.81 2 -1 1 1581.47 77.58 2 -1 1 1493.29 71.89 2 1 1 1363.00 68.55 -2 -1 -1 1619.64 73.60 2 1 1 1507.45 68.39 -2 1 -1 1430.29 74.17 -2 1 -1 1518.33 71.50 -2 -1 -1 1626.36 79.72 0 -2 0 13.99 1.07 2 0 -2 2274.53 114.61 -2 0 -2 21.23 4.08 2 0 2 23.35 1.70 2 0 2 23.99 2.72 -2 0 -2 16.95 1.66 0 2 1 578.85 21.49 0 -2 -1 640.11 23.09 -1 -2 0 564.56 13.87 1 -2 0 495.48 14.20 1 2 0 520.58 16.57 -1 -2 0 562.68 19.13 1 2 0 507.02 12.76 -1 2 0 514.04 13.53 0 0 3 0.91 0.87 0 0 -3 0.72 0.87 3 0 0 3.50 1.08 3 0 0 2.83 0.97 -3 0 0 3.49 1.42 -3 0 0 4.69 0.90 -1 -2 1 308.92 7.64 1 -2 -1 251.78 9.84 1 2 1 41.02 3.25 1 -2 1 30.44 1.89 -1 -2 -1 37.02 1.44 -1 2 -1 37.15 1.77 -1 -2 -1 43.98 2.03 1 2 1 39.15 1.47 1 0 -3 125.26 5.41 -1 0 3 116.59 5.06 -1 0 -3 564.72 30.71 1 0 3 514.72 26.96 2 -1 -2 2.51 0.92 -2 1 -2 10.21 1.68 -2 1 -2 12.62 1.34 2 -1 2 14.04 1.94 2 -1 2 16.06 1.36 2 1 2 9.91 1.81 -2 -1 -2 7.31 1.84 2 1 2 8.94 1.89 -3 0 1 1462.34 68.81 3 0 -1 1451.65 64.79 3 0 -1 1437.54 68.35 -3 0 -1 365.89 13.12 3 0 1 367.62 13.23 3 0 1 354.13 19.32 -3 0 -1 354.48 14.66 0 -1 -3 1649.35 79.27 0 1 -3 949.13 51.20 0 -1 3 1363.47 67.76 0 1 3 1545.95 74.27 -3 -1 0 17.72 1.43 3 1 0 23.81 2.18 -3 1 0 13.56 2.18 3 1 0 15.49 1.52 -3 -1 0 17.00 2.21 3 -1 0 11.37 1.75 3 -1 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1.95 2.05 5 -9 -7 -8.86 8.73 -5 -8 -9 16.26 4.44 -5 -8 -9 28.44 12.69 5 8 9 13.52 9.47 5 -8 9 23.83 11.90 -5 8 -9 26.78 5.45 9 5 -10 124.57 17.08 9 -5 -10 118.44 17.47 9 -5 -10 140.22 19.00 9 1 12 35.87 16.25 -9 -1 -12 31.14 11.77 -9 1 -12 54.37 12.33 -9 -1 -12 40.32 17.10 -9 1 -12 51.02 23.33 9 -1 12 64.33 26.05 -1 2 15 47.22 13.20 1 -2 -15 39.09 16.59 1 2 -15 58.83 12.64 -1 -2 15 83.26 10.34 -6 -10 0 2.28 3.60 6 -10 0 0.78 5.20 11 7 3 7.12 5.18 11 -7 3 11.25 11.56 -11 -7 -3 25.76 4.95 11 7 3 15.94 8.01 -11 -7 -3 32.52 12.19 11 -7 3 2.78 10.23 -11 7 -3 4.38 5.70 11 -6 -6 46.57 10.95 11 6 -6 50.71 14.46 11 -6 -6 62.72 13.19 14 1 -5 3.20 9.09 14 1 -5 7.14 6.77 14 -1 -5 6.32 5.19 14 1 -5 4.61 2.91 14 -1 -5 3.55 9.61 -3 0 15 128.96 15.41 3 0 -15 115.75 31.94 14 -3 -3 57.47 13.97 14 -3 -3 58.56 15.03 14 3 -3 61.88 12.65 12 -1 -9 5.52 4.53 12 1 -9 2.45 5.34 12 -1 -9 7.70 5.40 12 -1 -9 0.53 2.97 4 -5 -13 550.45 57.71 -14 0 -5 1.69 5.28 14 0 5 -3.57 7.11 -14 0 -5 -7.64 5.29 14 0 5 -2.10 5.73 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119.72 39.30 8 -7 -11 217.61 32.71 -8 -3 -14 -2.21 10.42 -8 3 -14 3.53 7.65 -8 -3 -14 5.72 10.86 8 -3 14 12.93 14.06 -8 3 -14 8.27 10.94 -10 -4 -12 33.79 16.05 10 -4 12 22.18 15.14 -10 -4 -12 12.54 9.20 -10 4 -12 18.75 9.83 -10 4 -12 17.75 10.59 -13 -1 -10 209.82 40.83 -13 1 -10 216.86 37.73 6 10 7 10.66 7.82 -6 -10 -7 21.30 11.14 6 -10 7 15.90 11.32 12 -7 -6 0.23 10.60 12 -7 -6 36.85 9.95 13 -7 -3 240.84 56.98 13 -7 -3 215.34 33.63 -1 -12 1 4.86 8.78 1 -12 -1 11.23 10.26 -12 2 -11 209.44 35.43 -12 -2 -11 198.99 42.02 -3 3 -16 103.37 23.16 -9 0 -14 0.63 6.93 -5 4 -15 -1.36 8.33 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12445