data_sulfatoredmondite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'sulfatoredmondite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H16.62 O28.69 Pb8 S4.61 Zn' _chemical_formula_weight 2346.72 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 12 _space_group_name_H-M_alt 'C 2/m' _space_group_name_Hall '-C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 17.294(2) _cell_length_b 7.3668(9) _cell_length_c 12.7271(18) _cell_angle_alpha 90 _cell_angle_beta 110.622(9) _cell_angle_gamma 90 _cell_volume 1517.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12692 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'equant' _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 5.136 _exptl_crystal_F_000 2012 _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 45.397 _shelx_estimated_absorpt_T_min 0.106 _shelx_estimated_absorpt_T_max 0.171 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.486 _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 14253 _diffrn_reflns_av_unetI/netI 0.0437 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.038 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 1871 _reflns_number_gt 1661 _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^)+(0.0241P)^2^+40.7468P] 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 1871 _refine_ls_number_parameters 125 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.104 _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 0.32052(2) 0.25364(5) 0.37682(3) 0.02621(13) Uani 1 1 d . . . . . Pb2 Pb 0.57524(4) 0.500000 0.78939(5) 0.0511(2) Uani 1 2 d S T P . . Pb3 Pb 0.18145(3) 0.500000 0.10691(4) 0.03115(15) Uani 1 2 d S T P . . Zn Zn 0.500000 0.500000 0.500000 0.0257(5) Uani 1 4 d S T P . . S1 S 0.3743(2) 0.000000 0.6473(3) 0.0288(7) Uani 1 2 d S T P . . S2 S 0.2313(2) 0.000000 0.1086(3) 0.0302(7) Uani 1 2 d DS T P . . O1 O 0.4126(13) 0.000000 0.7687(13) 0.147(11) Uani 1 2 d S T P . . O2 O 0.4379(7) 0.000000 0.5967(10) 0.044(3) Uani 1 2 d S T P . . O3 O 0.3202(7) 0.1569(15) 0.6059(11) 0.084(4) Uani 1 1 d . . . . . O4 O 0.2140(8) 0.000000 0.9897(10) 0.069(4) Uani 1 2 d S T P . . O5 O 0.1962(7) 0.8444(13) 0.1429(9) 0.070(3) Uani 1 1 d . . . . . O6 O 0.3210(12) 0.000000 0.169(2) 0.14(2) Uani 0.69(3) 2 d DS T P . . S2A S 0.3526(8) 0.000000 0.1757(16) 0.042(6) Uani 0.31(3) 2 d DS T P . . O7 O 0.2999(6) 0.500000 0.2584(7) 0.0235(19) Uani 1 2 d S T P . . OH8 O 0.5451(4) 0.6895(11) 0.6314(6) 0.0341(16) Uani 1 1 d . . . . . OH9 O 0.3758(6) 0.500000 0.4936(8) 0.027(2) Uani 1 2 d S T P . . OW10 O 0.0952(7) 0.000000 0.2745(9) 0.039(3) Uani 1 2 d S T P . . OW11 O 0.4399(18) 0.161(4) 0.128(2) 0.060(12) Uiso 0.33(3) 1 d . . . . . OW12 O 0.500000 0.424(8) 0.000000 0.10(3) Uiso 0.38(6) 2 d S . . . . OW13 O 0.500000 0.233(13) 0.000000 0.26(6) Uiso 0.62(11) 2 d S . . . . 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 0.0277(2) 0.0222(2) 0.0277(2) 0.00101(13) 0.00837(16) 0.00117(13) Pb2 0.0316(3) 0.1030(6) 0.0198(3) 0.000 0.0105(2) 0.000 Pb3 0.0280(3) 0.0417(3) 0.0215(3) 0.000 0.0058(2) 0.000 Zn 0.0193(10) 0.0372(12) 0.0190(10) 0.000 0.0049(8) 0.000 S1 0.0273(17) 0.0297(18) 0.0328(19) 0.000 0.0150(15) 0.000 S2 0.0331(19) 0.0345(19) 0.0237(17) 0.000 0.0108(15) 0.000 O1 0.104(15) 0.31(4) 0.039(9) 0.000 0.044(10) 0.000 O2 0.032(6) 0.054(7) 0.063(8) 0.000 0.036(6) 0.000 O3 0.075(7) 0.068(7) 0.140(11) 0.039(7) 0.076(7) 0.027(6) O4 0.053(8) 0.123(14) 0.020(6) 0.000 -0.001(5) 0.000 O5 0.104(8) 0.036(5) 0.090(8) -0.004(5) 0.058(7) -0.012(5) O6 0.013(13) 0.36(6) 0.036(13) 0.000 -0.007(12) 0.000 S2A 0.011(9) 0.072(12) 0.035(8) 0.000 -0.003(7) 0.000 O7 0.026(5) 0.019(4) 0.023(5) 0.000 0.006(4) 0.000 OH8 0.021(3) 0.045(4) 0.033(4) -0.013(3) 0.005(3) 0.004(3) OH9 0.024(5) 0.030(5) 0.028(5) 0.000 0.011(4) 0.000 OW10 0.039(6) 0.041(6) 0.039(6) 0.000 0.015(5) 0.000 _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 O7 2.305(5) . ? Pb1 OH9 2.328(6) . ? Pb1 OH8 2.400(7) 5_666 ? Pb1 O3 2.604(10) 7_556 ? Pb1 O3 3.004(12) . ? Pb1 O5 3.082(12) 2_565 ? Pb1 O6 3.24(3) . ? Pb1 S2A 3.369(16) . ? Pb1 O2 3.382(10) . ? Pb1 Zn 3.4580(5) . ? Pb1 Pb1 3.6298(8) 2_565 ? Pb1 Pb2 3.7019(7) 5_666 ? Pb1 S2 3.717(3) . ? Pb1 S1 3.735(3) . ? Pb1 Pb1 3.7370(8) 2 ? Pb2 OH8 2.351(8) 2_565 ? Pb2 OH8 2.351(8) . ? Pb2 O7 2.441(9) 5_666 ? Pb2 OW11 2.76(3) 5_666 ? Pb2 OW11 2.76(3) 6_656 ? Pb2 OW10 2.768(11) 7_556 ? Pb2 O4 2.820(12) 3 ? Pb2 OW12 3.413(10) 5_666 ? Pb2 OW12 3.413(10) 1_556 ? Pb2 Zn 3.4471(8) . ? Pb2 S2A 3.864(4) 5_666 ? Pb2 S2A 3.864(4) 5_656 ? Pb2 OW13 3.90(5) 5_666 ? Pb3 O7 2.265(9) . ? Pb3 O4 2.520(14) 7_556 ? Pb3 O5 2.575(10) 2_565 ? Pb3 O5 2.575(10) . ? Pb3 O1 2.638(17) 7_556 ? Pb3 OW11 3.21(3) 7 ? Pb3 OW11 3.21(3) 8 ? Pb3 OW13 3.41(5) 7 ? Pb3 OW13 3.41(5) 3_455 ? Pb3 S2A 3.43(2) 7 ? Pb3 O6 3.50(3) 7 ? Pb3 S2 3.565(4) 7 ? Pb3 S1 3.583(4) 7_556 ? Pb3 S2 3.7813(10) . ? Pb3 S2 3.7813(10) 1_565 ? Zn OH8 2.106(7) 5_666 ? Zn OH8 2.106(7) 6_656 ? Zn OH8 2.106(7) 2_565 ? Zn OH8 2.106(7) . ? Zn OH9 2.120(9) 5_666 ? Zn OH9 2.120(9) . ? S1 O1 1.451(17) . ? S1 O2 1.458(10) . ? S1 O3 1.463(10) 2 ? S1 O3 1.463(10) . ? S2 O4 1.435(12) 1_554 ? S2 O5 1.435(10) 1_545 ? S2 O5 1.435(10) 2_565 ? S2 O6 1.470(18) . ? S2 S2A 1.967(13) . ? O6 S2A 0.52(2) . ? S2A OW11 2.17(3) 2 ? S2A OW11 2.17(3) . ? OW12 OW12 1.12(12) 5_665 ? OW12 OW13 1.40(8) . ? 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 O7 Pb1 OH9 74.8(3) . . ? O7 Pb1 OH8 76.3(3) . 5_666 ? OH9 Pb1 OH8 72.9(3) . 5_666 ? O7 Pb1 O3 85.5(3) . 7_556 ? OH9 Pb1 O3 86.3(4) . 7_556 ? OH8 Pb1 O3 155.2(3) 5_666 7_556 ? O7 Pb1 O3 140.2(3) . . ? OH9 Pb1 O3 72.9(3) . . ? OH8 Pb1 O3 114.6(3) 5_666 . ? O3 Pb1 O3 69.9(4) 7_556 . ? O7 Pb1 O5 70.0(3) . 2_565 ? OH9 Pb1 O5 142.2(3) . 2_565 ? OH8 Pb1 O5 110.8(3) 5_666 2_565 ? O3 Pb1 O5 77.7(4) 7_556 2_565 ? O3 Pb1 O5 130.0(3) . 2_565 ? O7 Pb1 O6 88.0(4) . . ? OH9 Pb1 O6 148.5(4) . . ? OH8 Pb1 O6 77.5(4) 5_666 . ? O3 Pb1 O6 119.1(5) 7_556 . ? O3 Pb1 O6 131.0(4) . . ? O5 Pb1 O6 43.8(4) 2_565 . ? O7 Pb1 S2A 88.2(3) . . ? OH9 Pb1 S2A 141.0(3) . . ? OH8 Pb1 S2A 69.1(3) 5_666 . ? O3 Pb1 S2A 127.8(4) 7_556 . ? O3 Pb1 S2A 131.5(3) . . ? O5 Pb1 S2A 51.8(3) 2_565 . ? O6 Pb1 S2A 8.8(3) . . ? O7 Pb1 O2 152.3(3) . . ? OH9 Pb1 O2 84.9(2) . . ? OH8 Pb1 O2 79.9(2) 5_666 . ? O3 Pb1 O2 112.1(3) 7_556 . ? O3 Pb1 O2 43.3(2) . . ? O5 Pb1 O2 132.9(2) 2_565 . ? O6 Pb1 O2 100.5(3) . . ? S2A Pb1 O2 96.3(3) . . ? O7 Pb1 Zn 77.9(2) . . ? OH9 Pb1 Zn 36.9(2) . . ? OH8 Pb1 Zn 36.85(17) 5_666 . ? O3 Pb1 Zn 123.0(3) 7_556 . ? O3 Pb1 Zn 89.6(2) . . ? O5 Pb1 Zn 140.37(19) 2_565 . ? O6 Pb1 Zn 114.4(4) . . ? S2A Pb1 Zn 105.9(2) . . ? O2 Pb1 Zn 74.54(13) . . ? O7 Pb1 Pb1 38.07(17) . 2_565 ? OH9 Pb1 Pb1 38.76(18) . 2_565 ? OH8 Pb1 Pb1 79.95(19) 5_666 2_565 ? O3 Pb1 Pb1 75.3(3) 7_556 2_565 ? O3 Pb1 Pb1 103.7(2) . 2_565 ? O5 Pb1 Pb1 103.55(18) 2_565 2_565 ? O6 Pb1 Pb1 125.2(3) . 2_565 ? S2A Pb1 Pb1 123.69(19) . 2_565 ? O2 Pb1 Pb1 123.53(12) . 2_565 ? Zn Pb1 Pb1 58.343(8) . 2_565 ? O7 Pb1 Pb2 40.1(2) . 5_666 ? OH9 Pb1 Pb2 79.0(2) . 5_666 ? OH8 Pb1 Pb2 38.33(18) 5_666 5_666 ? O3 Pb1 Pb2 125.6(2) 7_556 5_666 ? O3 Pb1 Pb2 147.0(2) . 5_666 ? O5 Pb1 Pb2 82.94(19) 2_565 5_666 ? O6 Pb1 Pb2 71.0(4) . 5_666 ? S2A Pb1 Pb2 66.06(18) . 5_666 ? O2 Pb1 Pb2 118.18(16) . 5_666 ? Zn Pb1 Pb2 57.438(13) . 5_666 ? Pb1 Pb1 Pb2 60.643(8) 2_565 5_666 ? O7 Pb1 S2 82.91(18) . . ? OH9 Pb1 S2 157.35(19) . . ? OH8 Pb1 S2 98.21(17) 5_666 . ? O3 Pb1 S2 96.1(3) 7_556 . ? O3 Pb1 S2 129.1(2) . . ? O5 Pb1 S2 21.91(18) 2_565 . ? O6 Pb1 S2 23.1(3) . . ? S2A Pb1 S2 31.7(2) . . ? O2 Pb1 S2 114.59(13) . . ? Zn Pb1 S2 134.12(6) . . ? Pb1 Pb1 S2 120.18(3) 2_565 . ? Pb2 Pb1 S2 81.36(5) 5_666 . ? O7 Pb1 S1 158.04(17) . . ? OH9 Pb1 S1 83.60(19) . . ? OH8 Pb1 S1 101.36(18) 5_666 . ? O3 Pb1 S1 89.2(3) 7_556 . ? O3 Pb1 S1 21.8(2) . . ? O5 Pb1 S1 129.47(19) 2_565 . ? O6 Pb1 S1 113.1(3) . . ? S2A Pb1 S1 111.6(2) . . ? O2 Pb1 S1 22.96(17) . . ? Zn Pb1 S1 87.27(5) . . ? Pb1 Pb1 S1 120.02(3) 2_565 . ? Pb2 Pb1 S1 139.35(5) 5_666 . ? S2 Pb1 S1 118.89(4) . . ? O7 Pb1 Pb1 141.93(17) . 2 ? OH9 Pb1 Pb1 141.24(18) . 2 ? OH8 Pb1 Pb1 100.05(19) 5_666 2 ? O3 Pb1 Pb1 104.7(3) 7_556 2 ? O3 Pb1 Pb1 76.3(2) . 2 ? O5 Pb1 Pb1 76.45(18) 2_565 2 ? O6 Pb1 Pb1 54.8(3) . 2 ? S2A Pb1 Pb1 56.31(19) . 2 ? O2 Pb1 Pb1 56.47(12) . 2 ? Zn Pb1 Pb1 121.657(8) . 2 ? Pb1 Pb1 Pb1 180.0 2_565 2 ? Pb2 Pb1 Pb1 119.357(8) 5_666 2 ? S2 Pb1 Pb1 59.82(3) . 2 ? S1 Pb1 Pb1 59.98(3) . 2 ? OH8 Pb2 OH8 72.9(4) 2_565 . ? OH8 Pb2 O7 74.7(2) 2_565 5_666 ? OH8 Pb2 O7 74.7(2) . 5_666 ? OH8 Pb2 OW11 147.4(6) 2_565 5_666 ? OH8 Pb2 OW11 76.6(6) . 5_666 ? O7 Pb2 OW11 107.9(6) 5_666 5_666 ? OH8 Pb2 OW11 76.6(6) 2_565 6_656 ? OH8 Pb2 OW11 147.4(6) . 6_656 ? O7 Pb2 OW11 107.9(6) 5_666 6_656 ? OW11 Pb2 OW11 129.6(12) 5_666 6_656 ? OH8 Pb2 OW10 81.7(2) 2_565 7_556 ? OH8 Pb2 OW10 81.7(2) . 7_556 ? O7 Pb2 OW10 150.6(3) 5_666 7_556 ? OW11 Pb2 OW10 83.0(6) 5_666 7_556 ? OW11 Pb2 OW10 83.0(6) 6_656 7_556 ? OH8 Pb2 O4 129.4(2) 2_565 3 ? OH8 Pb2 O4 129.4(3) . 3 ? O7 Pb2 O4 71.3(4) 5_666 3 ? OW11 Pb2 O4 79.6(6) 5_666 3 ? OW11 Pb2 O4 79.6(6) 6_656 3 ? OW10 Pb2 O4 138.1(4) 7_556 3 ? OH8 Pb2 OW12 137.6(7) 2_565 5_666 ? OH8 Pb2 OW12 122.9(8) . 5_666 ? O7 Pb2 OW12 144.2(3) 5_666 5_666 ? OW11 Pb2 OW12 55.8(12) 5_666 5_666 ? OW11 Pb2 OW12 74.5(11) 6_656 5_666 ? OW10 Pb2 OW12 64.5(2) 7_556 5_666 ? O4 Pb2 OW12 74.2(3) 3 5_666 ? OH8 Pb2 OW12 122.9(8) 2_565 1_556 ? OH8 Pb2 OW12 137.6(7) . 1_556 ? O7 Pb2 OW12 144.2(3) 5_666 1_556 ? OW11 Pb2 OW12 74.5(11) 5_666 1_556 ? OW11 Pb2 OW12 55.8(12) 6_656 1_556 ? OW10 Pb2 OW12 64.5(2) 7_556 1_556 ? O4 Pb2 OW12 74.2(3) 3 1_556 ? OW12 Pb2 OW12 18.8(19) 5_666 1_556 ? OH8 Pb2 Zn 36.82(18) 2_565 . ? OH8 Pb2 Zn 36.82(18) . . ? O7 Pb2 Zn 76.6(2) 5_666 . ? OW11 Pb2 Zn 111.0(6) 5_666 . ? OW11 Pb2 Zn 111.0(6) 6_656 . ? OW10 Pb2 Zn 74.0(2) 7_556 . ? O4 Pb2 Zn 147.9(3) 3 . ? OW12 Pb2 Zn 137.25(18) 5_666 . ? OW12 Pb2 Zn 137.25(18) 1_556 . ? OH8 Pb2 Pb1 39.29(17) 2_565 6_656 ? OH8 Pb2 Pb1 78.95(17) . 6_656 ? O7 Pb2 Pb1 37.45(12) 5_666 6_656 ? OW11 Pb2 Pb1 142.5(6) 5_666 6_656 ? OW11 Pb2 Pb1 84.6(6) 6_656 6_656 ? OW10 Pb2 Pb1 120.98(19) 7_556 6_656 ? O4 Pb2 Pb1 94.9(2) 3 6_656 ? OW12 Pb2 Pb1 157.8(9) 5_666 6_656 ? OW12 Pb2 Pb1 140.0(9) 1_556 6_656 ? Zn Pb2 Pb1 57.722(12) . 6_656 ? OH8 Pb2 Pb1 78.95(17) 2_565 5_666 ? OH8 Pb2 Pb1 39.29(17) . 5_666 ? O7 Pb2 Pb1 37.45(12) 5_666 5_666 ? OW11 Pb2 Pb1 84.6(6) 5_666 5_666 ? OW11 Pb2 Pb1 142.5(6) 6_656 5_666 ? OW10 Pb2 Pb1 120.98(19) 7_556 5_666 ? O4 Pb2 Pb1 94.9(3) 3 5_666 ? OW12 Pb2 Pb1 140.0(9) 5_666 5_666 ? OW12 Pb2 Pb1 157.8(9) 1_556 5_666 ? Zn Pb2 Pb1 57.723(13) . 5_666 ? Pb1 Pb2 Pb1 58.714(16) 6_656 5_666 ? OH8 Pb2 S2A 129.0(3) 2_565 5_666 ? OH8 Pb2 S2A 59.8(3) . 5_666 ? O7 Pb2 S2A 75.5(2) 5_666 5_666 ? OW11 Pb2 S2A 33.3(7) 5_666 5_666 ? OW11 Pb2 S2A 152.7(7) 6_656 5_666 ? OW10 Pb2 S2A 107.53(19) 7_556 5_666 ? O4 Pb2 S2A 76.0(2) 3 5_666 ? OW12 Pb2 S2A 87.2(10) 5_666 5_666 ? OW12 Pb2 S2A 105.2(10) 1_556 5_666 ? Zn Pb2 S2A 96.2(3) . 5_666 ? Pb1 Pb2 S2A 109.3(3) 6_656 5_666 ? Pb1 Pb2 S2A 52.8(3) 5_666 5_666 ? OH8 Pb2 S2A 59.8(3) 2_565 5_656 ? OH8 Pb2 S2A 129.0(3) . 5_656 ? O7 Pb2 S2A 75.5(2) 5_666 5_656 ? OW11 Pb2 S2A 152.7(7) 5_666 5_656 ? OW11 Pb2 S2A 33.3(7) 6_656 5_656 ? OW10 Pb2 S2A 107.53(19) 7_556 5_656 ? O4 Pb2 S2A 76.0(2) 3 5_656 ? OW12 Pb2 S2A 105.2(10) 5_666 5_656 ? OW12 Pb2 S2A 87.2(10) 1_556 5_656 ? Zn Pb2 S2A 96.2(3) . 5_656 ? Pb1 Pb2 S2A 52.8(3) 6_656 5_656 ? Pb1 Pb2 S2A 109.3(3) 5_666 5_656 ? S2A Pb2 S2A 144.8(4) 5_666 5_656 ? OH8 Pb2 OW13 149.3(5) 2_565 5_666 ? OH8 Pb2 OW13 105.2(11) . 5_666 ? O7 Pb2 OW13 135.3(7) 5_666 5_666 ? OW11 Pb2 OW13 35.0(14) 5_666 5_666 ? OW11 Pb2 OW13 95.3(13) 6_656 5_666 ? OW10 Pb2 OW13 67.9(3) 7_556 5_666 ? O4 Pb2 OW13 76.2(3) 3 5_666 ? OW12 Pb2 OW13 20.8(11) 5_666 5_666 ? OW12 Pb2 OW13 39.7(19) 1_556 5_666 ? Zn Pb2 OW13 130.0(6) . 5_666 ? Pb1 Pb2 OW13 171.00(9) 6_656 5_666 ? Pb1 Pb2 OW13 119.6(12) 5_666 5_666 ? S2A Pb2 OW13 67.3(12) 5_666 5_666 ? S2A Pb2 OW13 125.0(12) 5_656 5_666 ? O7 Pb3 O4 80.0(3) . 7_556 ? O7 Pb3 O5 81.1(3) . 2_565 ? O4 Pb3 O5 92.5(2) 7_556 2_565 ? O7 Pb3 O5 81.1(3) . . ? O4 Pb3 O5 92.5(2) 7_556 . ? O5 Pb3 O5 160.4(5) 2_565 . ? O7 Pb3 O1 93.0(5) . 7_556 ? O4 Pb3 O1 173.0(5) 7_556 7_556 ? O5 Pb3 O1 86.4(2) 2_565 7_556 ? O5 Pb3 O1 86.4(2) . 7_556 ? O7 Pb3 OW11 152.9(6) . 7 ? O4 Pb3 OW11 83.9(6) 7_556 7 ? O5 Pb3 OW11 78.0(6) 2_565 7 ? O5 Pb3 OW11 121.4(6) . 7 ? O1 Pb3 OW11 102.6(7) 7_556 7 ? O7 Pb3 OW11 152.9(6) . 8 ? O4 Pb3 OW11 83.9(6) 7_556 8 ? O5 Pb3 OW11 121.4(6) 2_565 8 ? O5 Pb3 OW11 78.0(6) . 8 ? O1 Pb3 OW11 102.6(7) 7_556 8 ? OW11 Pb3 OW11 43.4(11) 7 8 ? O7 Pb3 OW13 140.2(10) . 7 ? O4 Pb3 OW13 121.5(5) 7_556 7 ? O5 Pb3 OW13 66.1(14) 2_565 7 ? O5 Pb3 OW13 126.0(14) . 7 ? O1 Pb3 OW13 64.2(5) 7_556 7 ? OW11 Pb3 OW13 40.1(5) 7 7 ? OW11 Pb3 OW13 66.9(11) 8 7 ? O7 Pb3 OW13 140.2(10) . 3_455 ? O4 Pb3 OW13 121.5(5) 7_556 3_455 ? O5 Pb3 OW13 126.0(14) 2_565 3_455 ? O5 Pb3 OW13 66.1(14) . 3_455 ? O1 Pb3 OW13 64.2(5) 7_556 3_455 ? OW11 Pb3 OW13 66.9(11) 7 3_455 ? OW11 Pb3 OW13 40.1(5) 8 3_455 ? OW13 Pb3 OW13 61(3) 7 3_455 ? O7 Pb3 S2A 131.4(3) . 7 ? O4 Pb3 S2A 51.4(3) 7_556 7 ? O5 Pb3 S2A 99.0(2) 2_565 7 ? O5 Pb3 S2A 99.0(2) . 7 ? O1 Pb3 S2A 135.5(5) 7_556 7 ? OW11 Pb3 S2A 38.0(6) 7 7 ? OW11 Pb3 S2A 38.0(6) 8 7 ? OW13 Pb3 S2A 77.8(3) 7 7 ? OW13 Pb3 S2A 77.8(3) 3_455 7 ? O7 Pb3 O6 122.9(4) . 7 ? O4 Pb3 O6 42.9(4) 7_556 7 ? O5 Pb3 O6 98.3(2) 2_565 7 ? O5 Pb3 O6 98.3(2) . 7 ? O1 Pb3 O6 144.1(5) 7_556 7 ? OW11 Pb3 O6 45.1(6) 7 7 ? OW11 Pb3 O6 45.1(6) 8 7 ? OW13 Pb3 O6 85.1(3) 7 7 ? OW13 Pb3 O6 85.1(3) 3_455 7 ? S2A Pb3 O6 8.6(3) 7 7 ? O7 Pb3 S2 98.9(2) . 7 ? O4 Pb3 S2 18.9(3) 7_556 7 ? O5 Pb3 S2 95.4(2) 2_565 7 ? O5 Pb3 S2 95.4(2) . 7 ? O1 Pb3 S2 168.1(4) 7_556 7 ? OW11 Pb3 S2 66.4(5) 7 7 ? OW11 Pb3 S2 66.4(5) 8 7 ? OW13 Pb3 S2 105.8(2) 7 7 ? OW13 Pb3 S2 105.8(2) 3_455 7 ? S2A Pb3 S2 32.6(2) 7 7 ? O6 Pb3 S2 24.0(3) 7 7 ? O7 Pb3 S1 72.4(2) . 7_556 ? O4 Pb3 S1 152.4(3) 7_556 7_556 ? O5 Pb3 S1 83.4(2) 2_565 7_556 ? O5 Pb3 S1 83.4(2) . 7_556 ? O1 Pb3 S1 20.6(4) 7_556 7_556 ? OW11 Pb3 S1 121.5(5) 7 7_556 ? OW11 Pb3 S1 121.5(5) 8 7_556 ? OW13 Pb3 S1 81.71(13) 7 7_556 ? OW13 Pb3 S1 81.71(13) 3_455 7_556 ? S2A Pb3 S1 156.2(2) 7 7_556 ? O6 Pb3 S1 164.8(3) 7 7_556 ? S2 Pb3 S1 171.25(8) 7 7_556 ? O7 Pb3 S2 81.91(7) . . ? O4 Pb3 S2 78.54(6) 7_556 . ? O5 Pb3 S2 14.3(2) 2_565 . ? O5 Pb3 S2 161.9(3) . . ? O1 Pb3 S2 100.61(8) 7_556 . ? OW11 Pb3 S2 73.6(6) 7 . ? OW11 Pb3 S2 116.0(6) 8 . ? OW13 Pb3 S2 71.8(14) 7 . ? OW13 Pb3 S2 132.0(14) 3_455 . ? S2A Pb3 S2 87.74(7) 7 . ? O6 Pb3 S2 85.86(9) 7 . ? S2 Pb3 S2 81.19(5) 7 . ? S1 Pb3 S2 97.24(5) 7_556 . ? O7 Pb3 S2 81.91(7) . 1_565 ? O4 Pb3 S2 78.54(6) 7_556 1_565 ? O5 Pb3 S2 161.9(3) 2_565 1_565 ? O5 Pb3 S2 14.3(2) . 1_565 ? O1 Pb3 S2 100.61(8) 7_556 1_565 ? OW11 Pb3 S2 116.0(6) 7 1_565 ? OW11 Pb3 S2 73.6(6) 8 1_565 ? OW13 Pb3 S2 132.0(14) 7 1_565 ? OW13 Pb3 S2 71.8(14) 3_455 1_565 ? S2A Pb3 S2 87.73(7) 7 1_565 ? O6 Pb3 S2 85.85(9) 7 1_565 ? S2 Pb3 S2 81.19(5) 7 1_565 ? S1 Pb3 S2 97.24(5) 7_556 1_565 ? S2 Pb3 S2 153.86(11) . 1_565 ? OH8 Zn OH8 83.0(4) 5_666 6_656 ? OH8 Zn OH8 97.0(4) 5_666 2_565 ? OH8 Zn OH8 180.0(3) 6_656 2_565 ? OH8 Zn OH8 180.0 5_666 . ? OH8 Zn OH8 97.0(4) 6_656 . ? OH8 Zn OH8 83.0(4) 2_565 . ? OH8 Zn OH9 96.7(3) 5_666 5_666 ? OH8 Zn OH9 96.7(3) 6_656 5_666 ? OH8 Zn OH9 83.3(3) 2_565 5_666 ? OH8 Zn OH9 83.3(3) . 5_666 ? OH8 Zn OH9 83.3(3) 5_666 . ? OH8 Zn OH9 83.3(3) 6_656 . ? OH8 Zn OH9 96.7(3) 2_565 . ? OH8 Zn OH9 96.7(3) . . ? OH9 Zn OH9 180.0 5_666 . ? OH8 Zn Pb2 138.0(2) 5_666 . ? OH8 Zn Pb2 138.0(2) 6_656 . ? OH8 Zn Pb2 42.0(2) 2_565 . ? OH8 Zn Pb2 42.0(2) . . ? OH9 Zn Pb2 87.9(2) 5_666 . ? OH9 Zn Pb2 92.1(2) . . ? OH8 Zn Pb2 42.0(2) 5_666 5_666 ? OH8 Zn Pb2 42.0(2) 6_656 5_666 ? OH8 Zn Pb2 138.0(2) 2_565 5_666 ? OH8 Zn Pb2 138.0(2) . 5_666 ? OH9 Zn Pb2 92.1(2) 5_666 5_666 ? OH9 Zn Pb2 87.9(2) . 5_666 ? Pb2 Zn Pb2 180.0 . 5_666 ? OH8 Zn Pb1 136.89(19) 5_666 5_666 ? OH8 Zn Pb1 91.96(19) 6_656 5_666 ? OH8 Zn Pb1 88.04(19) 2_565 5_666 ? OH8 Zn Pb1 43.11(19) . 5_666 ? OH9 Zn Pb1 41.18(15) 5_666 5_666 ? OH9 Zn Pb1 138.82(15) . 5_666 ? Pb2 Zn Pb1 64.839(13) . 5_666 ? Pb2 Zn Pb1 115.161(13) 5_666 5_666 ? OH8 Zn Pb1 91.96(19) 5_666 6_656 ? OH8 Zn Pb1 136.89(19) 6_656 6_656 ? OH8 Zn Pb1 43.11(19) 2_565 6_656 ? OH8 Zn Pb1 88.04(19) . 6_656 ? OH9 Zn Pb1 41.18(15) 5_666 6_656 ? OH9 Zn Pb1 138.82(15) . 6_656 ? Pb2 Zn Pb1 64.839(13) . 6_656 ? Pb2 Zn Pb1 115.161(13) 5_666 6_656 ? Pb1 Zn Pb1 63.315(15) 5_666 6_656 ? OH8 Zn Pb1 88.04(19) 5_666 2_565 ? OH8 Zn Pb1 43.11(19) 6_656 2_565 ? OH8 Zn Pb1 136.89(19) 2_565 2_565 ? OH8 Zn Pb1 91.96(19) . 2_565 ? OH9 Zn Pb1 138.82(15) 5_666 2_565 ? OH9 Zn Pb1 41.18(15) . 2_565 ? Pb2 Zn Pb1 115.161(13) . 2_565 ? Pb2 Zn Pb1 64.839(13) 5_666 2_565 ? Pb1 Zn Pb1 116.685(15) 5_666 2_565 ? Pb1 Zn Pb1 180.000(12) 6_656 2_565 ? OH8 Zn Pb1 43.11(19) 5_666 . ? OH8 Zn Pb1 88.04(19) 6_656 . ? OH8 Zn Pb1 91.96(19) 2_565 . ? OH8 Zn Pb1 136.89(19) . . ? OH9 Zn Pb1 138.82(15) 5_666 . ? OH9 Zn Pb1 41.18(15) . . ? Pb2 Zn Pb1 115.161(13) . . ? Pb2 Zn Pb1 64.839(13) 5_666 . ? Pb1 Zn Pb1 180.0 5_666 . ? Pb1 Zn Pb1 116.685(15) 6_656 . ? Pb1 Zn Pb1 63.315(15) 2_565 . ? O1 S1 O2 109.8(9) . . ? O1 S1 O3 112.2(7) . 2 ? O2 S1 O3 109.1(5) . 2 ? O1 S1 O3 112.2(7) . . ? O2 S1 O3 109.1(5) . . ? O3 S1 O3 104.3(10) 2 . ? O1 S1 Pb3 39.9(8) . 7_556 ? O2 S1 Pb3 149.6(5) . 7_556 ? O3 S1 Pb3 88.8(5) 2 7_556 ? O3 S1 Pb3 88.8(5) . 7_556 ? O1 S1 Pb1 148.6(2) . 2 ? O2 S1 Pb1 64.8(4) . 2 ? O3 S1 Pb1 49.7(5) 2 2 ? O3 S1 Pb1 98.2(6) . 2 ? Pb3 S1 Pb1 138.46(7) 7_556 2 ? O1 S1 Pb1 148.6(2) . . ? O2 S1 Pb1 64.8(4) . . ? O3 S1 Pb1 98.2(5) 2 . ? O3 S1 Pb1 49.7(5) . . ? Pb3 S1 Pb1 138.46(7) 7_556 . ? Pb1 S1 Pb1 60.03(6) 2 . ? O1 S1 Pb1 98.5(7) . 8_546 ? O2 S1 Pb1 139.6(4) . 8_546 ? O3 S1 Pb1 31.2(4) 2 8_546 ? O3 S1 Pb1 84.9(5) . 8_546 ? Pb3 S1 Pb1 63.93(6) 7_556 8_546 ? Pb1 S1 Pb1 75.95(5) 2 8_546 ? Pb1 S1 Pb1 104.02(9) . 8_546 ? O1 S1 Pb1 98.5(7) . 7_556 ? O2 S1 Pb1 139.6(3) . 7_556 ? O3 S1 Pb1 84.9(5) 2 7_556 ? O3 S1 Pb1 31.2(4) . 7_556 ? Pb3 S1 Pb1 63.93(6) 7_556 7_556 ? Pb1 S1 Pb1 104.02(9) 2 7_556 ? Pb1 S1 Pb1 75.95(5) . 7_556 ? Pb1 S1 Pb1 58.01(5) 8_546 7_556 ? O4 S2 O5 111.6(5) 1_554 1_545 ? O4 S2 O5 111.6(5) 1_554 2_565 ? O5 S2 O5 106.0(8) 1_545 2_565 ? O4 S2 O6 110.0(14) 1_554 . ? O5 S2 O6 108.8(8) 1_545 . ? O5 S2 O6 108.8(8) 2_565 . ? O4 S2 S2A 104.6(8) 1_554 . ? O5 S2 S2A 111.6(6) 1_545 . ? O5 S2 S2A 111.6(6) 2_565 . ? O6 S2 S2A 5.4(16) . . ? O4 S2 Pb3 34.6(6) 1_554 7 ? O5 S2 Pb3 124.9(4) 1_545 7 ? O5 S2 Pb3 124.9(4) 2_565 7 ? O6 S2 Pb3 75.4(12) . 7 ? S2A S2 Pb3 70.1(6) . 7 ? O4 S2 Pb1 146.4(2) 1_554 . ? O5 S2 Pb1 101.8(5) 1_545 . ? O5 S2 Pb1 53.3(5) 2_565 . ? O6 S2 Pb1 59.9(10) . . ? S2A S2 Pb1 64.3(5) . . ? Pb3 S2 Pb1 123.73(9) 7 . ? O4 S2 Pb1 146.4(2) 1_554 2 ? O5 S2 Pb1 53.3(5) 1_545 2 ? O5 S2 Pb1 101.8(5) 2_565 2 ? O6 S2 Pb1 59.9(10) . 2 ? S2A S2 Pb1 64.3(5) . 2 ? Pb3 S2 Pb1 123.73(9) 7 2 ? Pb1 S2 Pb1 60.35(6) . 2 ? O4 S2 Pb3 91.81(14) 1_554 1_545 ? O5 S2 Pb3 26.3(4) 1_545 1_545 ? O5 S2 Pb3 131.3(4) 2_565 1_545 ? O6 S2 Pb3 101.51(15) . 1_545 ? S2A S2 Pb3 102.04(8) . 1_545 ? Pb3 S2 Pb3 98.81(5) 7 1_545 ? Pb1 S2 Pb3 120.99(8) . 1_545 ? Pb1 S2 Pb3 62.33(3) 2 1_545 ? O4 S2 Pb3 91.81(14) 1_554 . ? O5 S2 Pb3 131.3(4) 1_545 . ? O5 S2 Pb3 26.3(4) 2_565 . ? O6 S2 Pb3 101.51(15) . . ? S2A S2 Pb3 102.04(8) . . ? Pb3 S2 Pb3 98.81(5) 7 . ? Pb1 S2 Pb3 62.33(3) . . ? Pb1 S2 Pb3 120.99(8) 2 . ? Pb3 S2 Pb3 153.86(11) 1_545 . ? O4 S2 Pb2 27.8(6) 1_554 3_444 ? O5 S2 Pb2 95.9(5) 1_545 3_444 ? O5 S2 Pb2 95.9(5) 2_565 3_444 ? O6 S2 Pb2 137.9(12) . 3_444 ? S2A S2 Pb2 132.5(6) . 3_444 ? Pb3 S2 Pb2 62.40(6) 7 3_444 ? Pb1 S2 Pb2 147.61(5) . 3_444 ? Pb1 S2 Pb2 147.61(5) 2 3_444 ? Pb3 S2 Pb2 85.61(6) 1_545 3_444 ? Pb3 S2 Pb2 85.61(6) . 3_444 ? S1 O1 Pb3 119.5(11) . 7_556 ? S1 O2 Pb1 92.2(4) . 2 ? S1 O2 Pb1 92.2(4) . . ? Pb1 O2 Pb1 67.1(2) 2 . ? S1 O3 Pb1 131.9(6) . 7_556 ? S1 O3 Pb1 108.5(6) . . ? Pb1 O3 Pb1 110.1(4) 7_556 . ? S1 O3 Pb3 68.8(4) . 7_556 ? Pb1 O3 Pb3 71.1(2) 7_556 7_556 ? Pb1 O3 Pb3 176.2(4) . 7_556 ? S1 O3 Pb1 73.2(4) . 8_546 ? Pb1 O3 Pb1 64.4(2) 7_556 8_546 ? Pb1 O3 Pb1 116.8(4) . 8_546 ? Pb3 O3 Pb1 60.20(16) 7_556 8_546 ? S2 O4 Pb3 126.5(8) 1_556 7_556 ? S2 O4 Pb2 138.5(8) 1_556 3_445 ? Pb3 O4 Pb2 95.0(4) 7_556 3_445 ? S2 O4 Pb3 67.6(2) 1_556 1_556 ? Pb3 O4 Pb3 113.1(2) 7_556 1_556 ? Pb2 O4 Pb3 98.5(2) 3_445 1_556 ? S2 O4 Pb3 67.6(2) 1_556 1_546 ? Pb3 O4 Pb3 113.1(2) 7_556 1_546 ? Pb2 O4 Pb3 98.5(2) 3_445 1_546 ? Pb3 O4 Pb3 128.7(3) 1_556 1_546 ? S2 O5 Pb3 139.4(6) 1_565 . ? S2 O5 Pb1 104.8(6) 1_565 2_565 ? Pb3 O5 Pb1 86.1(3) . 2_565 ? S2A O6 S2 159(6) . . ? S2A O6 Pb1 100(4) . 2 ? S2 O6 Pb1 97.0(11) . 2 ? S2A O6 Pb1 100(4) . . ? S2 O6 Pb1 97.0(11) . . ? Pb1 O6 Pb1 70.4(6) 2 . ? S2A O6 Pb3 79(5) . 7 ? S2 O6 Pb3 80.6(12) . 7 ? Pb1 O6 Pb3 144.8(3) 2 7 ? Pb1 O6 Pb3 144.8(3) . 7 ? S2A O6 Pb2 65.7(3) . 5_666 ? S2 O6 Pb2 113.9(3) . 5_666 ? Pb1 O6 Pb2 123.1(7) 2 5_666 ? Pb1 O6 Pb2 59.83(15) . 5_666 ? Pb3 O6 Pb2 88.8(5) 7 5_666 ? S2A O6 Pb2 65.7(3) . 5_656 ? S2 O6 Pb2 113.9(3) . 5_656 ? Pb1 O6 Pb2 59.83(15) 2 5_656 ? Pb1 O6 Pb2 123.1(7) . 5_656 ? Pb3 O6 Pb2 88.8(5) 7 5_656 ? Pb2 O6 Pb2 130.9(5) 5_666 5_656 ? O6 S2A S2 15(4) . . ? O6 S2A OW11 138(3) . 2 ? S2 S2A OW11 128.2(10) . 2 ? O6 S2A OW11 138(3) . . ? S2 S2A OW11 128.2(10) . . ? OW11 S2A OW11 66.2(17) 2 . ? O6 S2A Pb1 71(4) . 2 ? S2 S2A Pb1 83.9(5) . 2 ? OW11 S2A Pb1 103.2(9) 2 2 ? OW11 S2A Pb1 146.5(10) . 2 ? O6 S2A Pb1 71(4) . . ? S2 S2A Pb1 83.9(5) . . ? OW11 S2A Pb1 146.5(10) 2 . ? OW11 S2A Pb1 103.2(9) . . ? Pb1 S2A Pb1 67.4(4) 2 . ? O6 S2A Pb3 93(5) . 7 ? S2 S2A Pb3 77.4(6) . 7 ? OW11 S2A Pb3 65.4(9) 2 7 ? OW11 S2A Pb3 65.4(9) . 7 ? Pb1 S2A Pb3 141.5(3) 2 7 ? Pb1 S2A Pb3 141.5(3) . 7 ? O6 S2A Pb2 107.2(4) . 5_666 ? S2 S2A Pb2 107.57(19) . 5_666 ? OW11 S2A Pb2 108.9(9) 2 5_666 ? OW11 S2A Pb2 44.2(8) . 5_666 ? Pb1 S2A Pb2 125.1(5) 2 5_666 ? Pb1 S2A Pb2 61.12(13) . 5_666 ? Pb3 S2A Pb2 92.8(3) 7 5_666 ? O6 S2A Pb2 107.2(4) . 5_656 ? S2 S2A Pb2 107.57(19) . 5_656 ? OW11 S2A Pb2 44.2(8) 2 5_656 ? OW11 S2A Pb2 108.9(9) . 5_656 ? Pb1 S2A Pb2 61.12(13) 2 5_656 ? Pb1 S2A Pb2 125.1(5) . 5_656 ? Pb3 S2A Pb2 92.8(3) 7 5_656 ? Pb2 S2A Pb2 144.8(4) 5_666 5_656 ? Pb3 O7 Pb1 116.2(3) . . ? Pb3 O7 Pb1 116.2(3) . 2_565 ? Pb1 O7 Pb1 103.9(3) . 2_565 ? Pb3 O7 Pb2 113.7(4) . 5_666 ? Pb1 O7 Pb2 102.5(3) . 5_666 ? Pb1 O7 Pb2 102.5(3) 2_565 5_666 ? Zn OH8 Pb2 101.2(3) . . ? Zn OH8 Pb1 100.0(3) . 5_666 ? Pb2 OH8 Pb1 102.4(3) . 5_666 ? Zn OH8 Pb1 60.09(17) . 6_656 ? Pb2 OH8 Pb1 65.69(17) . 6_656 ? Pb1 OH8 Pb1 63.70(15) 5_666 6_656 ? Zn OH8 Pb1 57.23(15) . 2_565 ? Pb2 OH8 Pb1 126.7(3) . 2_565 ? Pb1 OH8 Pb1 127.5(3) 5_666 2_565 ? Pb1 OH8 Pb1 117.33(17) 6_656 2_565 ? Zn OH9 Pb1 102.0(3) . . ? Zn OH9 Pb1 102.0(3) . 2_565 ? Pb1 OH9 Pb1 102.5(4) . 2_565 ? Zn OH9 Pb2 60.0(2) . 5_666 ? Pb1 OH9 Pb2 65.9(2) . 5_666 ? Pb1 OH9 Pb2 65.9(2) 2_565 5_666 ? Zn OH9 Pb2 56.9(2) . . ? Pb1 OH9 Pb2 127.45(19) . . ? Pb1 OH9 Pb2 127.45(19) 2_565 . ? Pb2 OH9 Pb2 116.8(2) 5_666 . ? Pb2 OW10 Pb1 152.66(8) 7_556 . ? Pb2 OW10 Pb1 152.66(8) 7_556 2 ? Pb1 OW10 Pb1 54.25(14) . 2 ? S2A OW11 Pb2 102.5(11) . 5_666 ? S2A OW11 Pb3 76.6(10) . 7 ? Pb2 OW11 Pb3 124.8(10) 5_666 7 ? OW12 OW12 OW13 180.0 5_665 . ? OW12 OW12 Pb2 80.6(10) 5_665 5_666 ? OW13 OW12 Pb2 99.4(10) . 5_666 ? OW12 OW12 Pb2 80.6(10) 5_665 1_554 ? OW13 OW12 Pb2 99.4(10) . 1_554 ? Pb2 OW12 Pb2 161.2(19) 5_666 1_554 ? OW12 OW13 Pb3 120.3(14) . 7 ? OW12 OW13 Pb3 120.3(14) . 3_545 ? Pb3 OW13 Pb3 119(3) 7 3_545 ? OW12 OW13 Pb2 59.8(12) . 5_666 ? Pb3 OW13 Pb2 92.59(10) 7 5_666 ? Pb3 OW13 Pb2 117.55(6) 3_545 5_666 ? OW12 OW13 Pb2 59.8(12) . 1_554 ? Pb3 OW13 Pb2 117.55(6) 7 1_554 ? Pb3 OW13 Pb2 92.59(10) 3_545 1_554 ? Pb2 OW13 Pb2 120(2) 5_666 1_554 ? _refine_diff_density_max 1.916 _refine_diff_density_min -2.154 _refine_diff_density_rms 0.331 _shelx_res_file ; TITL Redmond-3A R3A.res created by SHELXL-2016/6 at 20:11:43 on 29-Aug-2021 CELL 0.71075 17.29390 7.36675 12.72710 90.00000 110.62200 90.00000 ZERR 2 0.00230 0.00091 0.00175 0.00000 0.00900 0.00000 LATT 7 SYMM +X, -Y, +Z SFAC H O PB S ZN UNIT 33.24 57.39 16 9.23 2 L.S. 20 CONN 15 3.0 PB1 CONN 15 3.0 PB2 CONN 15 3.0 PB3 DFIX 1.47 0.02 S2 O6 DFIX 2.01 0.02 S2 S2A FMAP 2 PLAN 20 ACTA SIZE 0.090 0.090 0.060 WGHT 0.024100 40.746807 FVAR 0.08801 0.69178 PB1 3 0.320525 0.253640 0.376823 11.00000 0.02765 0.02220 = 0.02766 0.00101 0.00837 0.00117 PB2 3 0.575239 0.500000 0.789389 10.50000 0.03159 0.10298 = 0.01979 0.00000 0.01055 0.00000 PB3 3 0.181450 0.500000 0.106905 10.50000 0.02796 0.04166 = 0.02149 0.00000 0.00578 0.00000 ZN 5 0.500000 0.500000 0.500000 10.25000 0.01934 0.03724 = 0.01898 0.00000 0.00490 0.00000 S1 4 0.374286 0.000000 0.647302 10.50000 0.02734 0.02975 = 0.03281 0.00000 0.01500 0.00000 S2 4 0.231304 0.000000 0.108560 10.50000 0.03313 0.03452 = 0.02371 0.00000 0.01080 0.00000 O1 2 0.412561 0.000000 0.768736 10.50000 0.10432 0.31170 = 0.03881 0.00000 0.04417 0.00000 O2 2 0.437918 0.000000 0.596656 10.50000 0.03170 0.05360 = 0.06271 0.00000 0.03630 0.00000 O3 2 0.320172 0.156855 0.605934 11.00000 0.07460 0.06763 = 0.13956 0.03856 0.07552 0.02735 O4 2 0.214004 0.000000 0.989730 10.50000 0.05294 0.12310 = 0.01981 0.00000 -0.00128 0.00000 O5 2 0.196248 0.844377 0.142897 11.00000 0.10384 0.03558 = 0.08992 -0.00364 0.05770 -0.01188 O6 2 0.321034 0.000000 0.169131 20.50000 0.01264 0.36336 = 0.03631 0.00000 -0.00693 0.00000 S2A 4 0.352597 0.000000 0.175735 -20.50000 0.01052 0.07239 = 0.03452 0.00000 -0.00322 0.00000 O7 2 0.299857 0.500000 0.258384 10.50000 0.02643 0.01924 = 0.02282 0.00000 0.00629 0.00000 OH8 2 0.545085 0.689523 0.631400 11.00000 0.02124 0.04506 = 0.03283 -0.01295 0.00541 0.00377 OH9 2 0.375839 0.500000 0.493639 10.50000 0.02368 0.02980 = 0.02809 0.00000 0.01068 0.00000 OW10 2 0.095223 0.000000 0.274480 10.50000 0.03935 0.04135 = 0.03868 0.00000 0.01527 0.00000 OW11 2 0.439943 0.161061 0.127583 0.32710 0.06047 OW12 2 0.500000 0.424200 0.000000 0.18909 0.10341 OW13 2 0.500000 0.233486 0.000000 0.31142 0.25994 HKLF 4 REM Redmond-3A REM R1 = 0.0344 for 1661 Fo > 4sig(Fo) and 0.0398 for all 1871 data REM 125 parameters refined using 2 restraints END WGHT 0.0241 40.7003 REM Highest difference peak 1.916, deepest hole -2.154, 1-sigma level 0.331 Q1 1 0.2366 0.5000 0.1870 10.50000 0.05 1.92 Q2 1 0.6253 0.5000 0.8264 10.50000 0.05 1.84 Q3 1 0.1304 0.5000 0.0687 10.50000 0.05 1.73 Q4 1 0.2723 0.2507 0.3426 11.00000 0.05 1.58 Q5 1 0.3706 0.2239 0.4167 11.00000 0.05 1.43 Q6 1 0.3440 0.1501 0.6944 11.00000 0.05 1.35 Q7 1 0.5714 0.5732 0.7577 11.00000 0.05 1.25 Q8 1 0.2412 0.5000 0.1265 10.50000 0.05 1.22 Q9 1 0.1796 0.0000 0.1028 10.50000 0.05 1.22 Q10 1 0.5110 0.5000 0.8105 10.50000 0.05 1.22 Q11 1 0.4793 0.0000 -0.0378 10.50000 0.05 1.18 Q12 1 0.6414 0.5546 0.7806 11.00000 0.05 1.14 Q13 1 0.1520 1.0000 0.1659 10.50000 0.05 1.13 Q14 1 0.5223 0.5000 0.7036 10.50000 0.05 1.13 Q15 1 0.2011 1.0000 0.2171 10.50000 0.05 1.12 Q16 1 0.2933 0.0000 0.5581 10.50000 0.05 1.11 Q17 1 0.3436 0.5000 0.3527 10.50000 0.05 1.10 Q18 1 0.4626 0.0000 0.7937 10.50000 0.05 1.09 Q19 1 0.3140 0.5000 0.4102 10.50000 0.05 1.08 Q20 1 0.5328 0.5753 0.7681 11.00000 0.05 1.06 ; _shelx_res_checksum 48892 _shelx_hkl_file ; -1 1 0 228.22 3.67 -1 1 0 249.05 4.84 -1 -1 0 190.73 3.80 1 -1 0 195.04 3.83 1 1 0 225.09 4.55 -1 -1 0 256.65 5.06 -1 -1 1 1049.81 32.10 1 -1 -1 1001.01 29.70 -1 -1 1 1144.65 30.13 1 1 -1 1079.58 30.96 1 1 -1 998.20 30.63 -1 1 1 1108.45 27.58 -1 -1 1 1118.90 32.09 -1 1 1 1056.14 31.87 -1 1 1 1235.53 29.34 0 0 -2 223.30 4.03 0 0 -2 219.02 6.46 0 0 2 209.90 5.30 0 0 2 202.34 4.30 0 0 2 219.77 5.21 -2 0 2 935.57 24.53 2 0 -2 918.91 21.77 2 0 -2 984.36 25.87 -2 0 2 871.97 23.22 -2 0 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107.47 26.50 0 6 12 53.68 17.80 -13 5 13 -0.03 14.24 13 -5 -13 0.02 11.77 13 5 -13 31.35 19.11 13 5 -13 45.16 9.77 -13 -5 13 63.64 22.96 7 9 0 -5.33 9.15 7 9 0 -7.84 14.15 -7 9 0 7.63 6.07 7 9 0 2.53 6.38 4 8 -9 128.13 34.03 -4 8 9 153.24 23.08 -15 -7 2 34.72 17.30 -15 7 2 38.94 12.62 -15 -7 2 26.64 11.55 15 7 -2 23.80 16.40 15 7 -2 27.08 12.77 15 7 -2 42.99 22.87 20 2 1 12.41 9.64 20 2 1 34.43 9.30 20 2 1 29.65 12.69 -20 2 -1 55.64 13.32 -20 -2 -1 17.65 13.93 20 -2 1 15.67 11.01 -3 -1 16 56.95 15.34 5 5 -14 12.04 7.36 5 5 -14 6.59 7.93 -5 -5 14 19.55 10.23 5 -5 -14 13.06 19.01 14 2 8 11.59 13.72 14 2 8 15.75 8.53 14 -2 8 11.60 9.18 -21 3 3 23.37 10.46 21 3 -3 1.26 12.89 21 3 -3 0.36 6.99 -3 9 -4 -7.26 7.26 8 2 12 5.86 10.53 -8 -2 -12 17.55 7.09 -8 -2 -12 27.28 13.27 8 -2 12 11.38 7.39 8 4 -15 122.04 24.32 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 54642