data_twin5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 O34 Pb9.81 S6.02 Si2.09 Zn0.93' _chemical_formula_weight 2891.05 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3175(4) _cell_length_b 11.1973(5) _cell_length_c 10.8318(5) _cell_angle_alpha 120.374(2) _cell_angle_beta 90.511(2) _cell_angle_gamma 56.471(2) _cell_volume 753.13(6) _cell_formula_units_Z 1 _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_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 55.960 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1663 _exptl_absorpt_correction_T_max 0.2131 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5286 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 32.62 _reflns_number_total 5286 _reflns_number_gt 4543 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+1.9928P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00076(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5286 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.25929(4) 0.11301(4) 0.25132(4) 0.01533(8) Uani 1 1 d . . . Pb2 Pb 0.26564(4) 0.08114(4) 0.64895(3) 0.01200(7) Uani 1 1 d . . . Pb3 Pb 0.92660(4) 0.23610(4) 0.02931(3) 0.01273(7) Uani 1 1 d . . . Pb4 Pb 0.72237(4) 0.41691(4) 0.75348(4) 0.01446(8) Uani 1 1 d . . . Pb5 Pb 0.31236(4) 0.46321(4) 0.53615(3) 0.01209(7) Uani 1 1 d . . . Zn Zn 0.0000 0.5000 0.0000 0.0119(3) Uani 1 2 d S . . S1 S 0.9580(3) 0.0793(3) 0.3619(2) 0.0107(4) Uani 1 1 d . . . S2 S 0.5697(3) 0.1765(3) 0.1512(2) 0.0093(3) Uani 1 1 d . . . S3 S 0.4433(3) 0.3275(3) 0.8370(2) 0.0096(3) Uani 1 1 d . . . Si Si 0.0259(3) 0.4474(3) 0.6572(2) 0.0077(4) Uani 1 1 d . . . O1 O 0.7667(9) 0.2146(9) 0.4768(7) 0.0195(13) Uani 1 1 d . . . O2 O 0.0929(10) 0.0688(9) 0.4360(8) 0.0249(15) Uani 1 1 d . . . O3 O 0.0017(9) 0.0971(8) 0.7301(7) 0.0152(12) Uani 1 1 d . . . O4 O 0.9727(10) 0.1230(9) 0.2571(8) 0.0219(14) Uani 1 1 d . . . O5 O 0.5321(9) 0.1389(8) 0.2552(7) 0.0145(12) Uani 1 1 d . . . O6 O 0.4389(9) 0.1985(9) 0.0717(7) 0.0220(14) Uani 1 1 d . . . O7 O 0.7616(8) 0.0297(8) 0.0375(7) 0.0159(12) Uani 1 1 d . . . O8 O 0.5482(9) 0.3422(8) 0.2466(8) 0.0171(13) Uani 1 1 d . . . O9 O 0.5779(8) 0.3031(9) 0.9108(8) 0.0189(13) Uani 1 1 d . . . O10 O 0.4526(9) 0.3892(9) 0.7476(8) 0.0196(13) Uani 1 1 d . . . O11 O 0.2489(8) 0.4725(8) 0.9598(7) 0.0139(11) Uani 1 1 d . . . O12 O 0.4688(9) 0.1611(8) 0.7378(7) 0.0181(13) Uani 1 1 d . . . O13 O 0.2242(8) 0.2933(8) 0.5076(6) 0.0133(11) Uani 1 1 d . . . O14 O 0.0338(8) 0.3846(7) 0.7657(6) 0.0106(11) Uani 1 1 d . . . O15 O 0.9897(8) 0.3735(8) 0.2570(7) 0.0119(11) Uani 1 1 d . . . O16 O 0.8516(8) 0.4772(8) 0.6090(7) 0.0136(11) Uani 1 1 d . . . OH O 0.1362(8) 0.2497(7) 0.9300(6) 0.0094(10) 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 0.01361(15) 0.01550(15) 0.01213(14) 0.00608(12) -0.00526(12) -0.00900(13) Pb2 0.01039(14) 0.01015(14) 0.01172(14) 0.00497(12) -0.00228(11) -0.00616(12) Pb3 0.01486(15) 0.01272(14) 0.01227(13) 0.00732(12) -0.00398(11) -0.00968(12) Pb4 0.01538(15) 0.01725(16) 0.01611(15) 0.01183(13) -0.00891(12) -0.01129(13) Pb5 0.01448(14) 0.01688(15) 0.01268(14) 0.01023(12) -0.00782(11) -0.01242(13) Zn 0.0156(6) 0.0104(6) 0.0109(6) 0.0062(5) -0.0045(5) -0.0090(5) S1 0.0131(9) 0.0122(9) 0.0096(8) 0.0056(8) -0.0040(7) -0.0102(8) S2 0.0079(8) 0.0071(8) 0.0077(8) 0.0033(7) -0.0007(7) -0.0034(7) S3 0.0093(8) 0.0109(9) 0.0108(8) 0.0066(7) -0.0036(7) -0.0073(7) Si 0.0098(10) 0.0099(10) 0.0077(9) 0.0069(8) -0.0041(8) -0.0069(8) O1 0.020(3) 0.021(3) 0.014(3) 0.006(3) 0.000(3) -0.016(3) O2 0.029(4) 0.024(4) 0.030(4) 0.015(3) -0.021(3) -0.022(3) O3 0.020(3) 0.012(3) 0.013(3) 0.005(2) -0.003(2) -0.012(3) O4 0.028(4) 0.027(4) 0.015(3) 0.014(3) -0.006(3) -0.019(3) O5 0.018(3) 0.016(3) 0.012(3) 0.011(2) -0.003(2) -0.010(3) O6 0.013(3) 0.027(4) 0.018(3) 0.013(3) -0.010(3) -0.011(3) O7 0.008(3) 0.013(3) 0.018(3) 0.009(3) -0.001(2) -0.002(2) O8 0.016(3) 0.009(3) 0.024(3) 0.009(3) -0.008(3) -0.008(3) O9 0.010(3) 0.023(3) 0.024(3) 0.015(3) -0.010(3) -0.011(3) O10 0.028(4) 0.031(4) 0.023(3) 0.022(3) -0.013(3) -0.024(3) O11 0.013(3) 0.010(3) 0.009(3) 0.001(2) 0.001(2) -0.006(2) O12 0.012(3) 0.013(3) 0.019(3) 0.005(3) -0.004(2) -0.008(3) O13 0.011(3) 0.013(3) 0.006(2) 0.000(2) 0.003(2) -0.007(2) O14 0.014(3) 0.009(3) 0.009(2) 0.007(2) -0.005(2) -0.006(2) O15 0.015(3) 0.007(3) 0.012(3) 0.005(2) -0.002(2) -0.007(2) O16 0.011(3) 0.019(3) 0.018(3) 0.015(3) -0.010(2) -0.010(2) OH 0.014(3) 0.007(2) 0.009(2) 0.005(2) -0.005(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O13 2.347(6) . ? Pb1 O15 2.558(6) 1_455 ? Pb1 O4 2.610(7) 1_455 ? Pb1 O5 2.711(6) . ? Pb1 O12 2.761(6) 2_656 ? Pb1 O7 2.767(6) 2_655 ? Pb1 O2 2.925(7) . ? Pb1 O6 3.052(7) 2_655 ? Pb1 O9 3.326(6) 2_656 ? Pb1 S1 3.3384(19) 1_455 ? Pb1 O6 3.348(7) . ? Pb1 S2 3.4901(19) 2_655 ? Pb2 O14 2.325(6) . ? Pb2 OH 2.454(5) . ? Pb2 O3 2.500(6) . ? Pb2 O12 2.505(6) . ? Pb2 O2 2.791(6) . ? Pb2 O5 2.850(6) 2_656 ? Pb2 O1 3.074(6) 2_656 ? Pb2 O13 3.284(6) . ? Pb2 Si 3.366(2) . ? Pb2 S1 3.3914(19) 2_656 ? Pb2 Zn 3.4483(4) 1_556 ? Pb2 O12 3.509(7) 2_656 ? Pb3 OH 2.352(6) 1_654 ? Pb3 O15 2.436(6) . ? Pb3 O7 2.476(6) 2_755 ? Pb3 O11 2.656(6) 2_666 ? Pb3 O3 2.674(6) 1_654 ? Pb3 O10 3.074(7) 2_666 ? Pb3 O4 3.154(7) 2_755 ? Pb3 O4 3.228(6) . ? Pb3 O9 3.313(6) 1_554 ? Pb3 O7 3.443(6) . ? Pb3 O8 3.475(6) . ? Pb3 S3 3.490(2) 2_666 ? Pb4 O8 2.474(6) 2_666 ? Pb4 O16 2.520(6) . ? Pb4 O1 2.531(6) . ? Pb4 O10 2.694(6) . ? Pb4 O14 2.730(6) 1_655 ? Pb4 O11 2.777(6) 2_667 ? Pb4 O3 2.909(6) 1_655 ? Pb4 O6 3.008(7) 2_666 ? Pb4 O9 3.137(7) 2_667 ? Pb4 O9 3.236(7) . ? Pb4 Si 3.268(2) 1_655 ? Pb4 O2 3.275(7) 1_655 ? Pb5 O16 2.268(5) 2_666 ? Pb5 O13 2.350(6) . ? Pb5 O15 2.563(6) 2_666 ? Pb5 O5 2.713(6) . ? Pb5 O10 2.883(6) . ? Pb5 O8 3.006(7) . ? Pb5 O4 3.091(7) 2_666 ? Pb5 Si 3.113(2) . ? Pb5 O8 3.140(6) 2_666 ? Pb5 O1 3.339(6) 2_666 ? Pb5 O1 3.362(7) . ? Pb5 S2 3.4031(19) . ? Zn OH 1.994(5) 2_566 ? Zn OH 1.994(5) 1_554 ? Zn O14 2.111(5) 1_554 ? Zn O14 2.111(5) 2_566 ? Zn O11 2.181(6) 1_554 ? Zn O11 2.181(6) 2_566 ? Zn Pb2 3.4483(4) 2_566 ? Zn Pb2 3.4483(4) 1_554 ? Zn Pb3 3.5335(3) 2_665 ? Zn Pb3 3.5335(3) 1_455 ? Zn Pb4 3.8354(3) 2_666 ? Zn Pb4 3.8354(3) 1_454 ? S1 O2 1.467(7) 1_655 ? S1 O1 1.473(7) . ? S1 O4 1.478(6) . ? S1 O3 1.494(6) 2_656 ? S1 Pb1 3.3384(19) 1_655 ? S1 Pb2 3.3914(19) 2_656 ? S1 Pb3 3.5122(19) 2_755 ? S1 Pb5 3.725(2) 2_666 ? S1 Pb4 4.008(2) 2_756 ? S2 O6 1.467(6) . ? S2 O7 1.470(6) . ? S2 O8 1.484(6) . ? S2 O5 1.490(6) . ? S2 Pb4 3.2872(19) 2_666 ? S2 Pb1 3.4901(19) 2_655 ? S2 Pb3 3.7775(19) 2_755 ? S3 O9 1.453(6) . ? S3 O10 1.472(6) . ? S3 O12 1.475(6) . ? S3 O11 1.515(6) . ? S3 Pb3 3.490(2) 2_666 ? S3 Pb4 3.557(2) 2_667 ? S3 Pb1 3.619(2) 2_656 ? Si O16 1.608(6) 1_455 ? Si O14 1.630(6) . ? Si O15 1.644(6) 2_666 ? Si O13 1.649(6) . ? Si Pb4 3.268(2) 1_455 ? Si Pb1 3.597(2) 2_566 ? Si Pb3 3.718(2) 2_666 ? Si Pb5 3.721(2) 2_566 ? O1 Pb2 3.074(6) 2_656 ? O1 Pb5 3.339(6) 2_666 ? O2 S1 1.467(7) 1_455 ? O2 Pb4 3.275(7) 1_455 ? O3 S1 1.494(6) 2_656 ? O3 Pb3 2.674(6) 1_456 ? O3 Pb4 2.909(6) 1_455 ? O4 Pb1 2.610(7) 1_655 ? O4 Pb5 3.091(7) 2_666 ? O4 Pb3 3.154(7) 2_755 ? O5 Pb2 2.850(6) 2_656 ? O6 Pb4 3.008(7) 2_666 ? O6 Pb1 3.052(7) 2_655 ? O7 Pb3 2.476(6) 2_755 ? O7 Pb1 2.767(6) 2_655 ? O8 Pb4 2.474(6) 2_666 ? O8 Pb5 3.140(6) 2_666 ? O9 Pb4 3.137(7) 2_667 ? O9 Pb3 3.313(6) 1_556 ? O9 Pb1 3.326(6) 2_656 ? O10 Pb3 3.074(7) 2_666 ? O11 Zn 2.181(6) 1_556 ? O11 Pb3 2.656(6) 2_666 ? O11 Pb4 2.777(6) 2_667 ? O12 Pb1 2.761(6) 2_656 ? O12 Pb2 3.509(7) 2_656 ? O14 Zn 2.111(5) 1_556 ? O14 Pb4 2.730(6) 1_455 ? O15 Si 1.644(6) 2_666 ? O15 Pb1 2.558(6) 1_655 ? O15 Pb5 2.563(6) 2_666 ? O16 Si 1.608(6) 1_655 ? O16 Pb5 2.268(5) 2_666 ? O16 Pb1 3.491(6) 2_666 ? O16 Pb1 3.639(6) 1_655 ? OH Zn 1.994(5) 1_556 ? OH Pb3 2.352(6) 1_456 ? 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 O13 Pb1 O15 95.2(2) . 1_455 ? O13 Pb1 O4 107.8(2) . 1_455 ? O15 Pb1 O4 68.1(2) 1_455 1_455 ? O13 Pb1 O5 70.36(19) . . ? O15 Pb1 O5 106.04(18) 1_455 . ? O4 Pb1 O5 173.9(2) 1_455 . ? O13 Pb1 O12 82.8(2) . 2_656 ? O15 Pb1 O12 175.74(18) 1_455 2_656 ? O4 Pb1 O12 108.8(2) 1_455 2_656 ? O5 Pb1 O12 76.89(18) . 2_656 ? O13 Pb1 O7 167.64(19) . 2_655 ? O15 Pb1 O7 72.47(18) 1_455 2_655 ? O4 Pb1 O7 68.55(19) 1_455 2_655 ? O5 Pb1 O7 111.92(18) . 2_655 ? O12 Pb1 O7 109.53(18) 2_656 2_655 ? O13 Pb1 O2 72.00(19) . . ? O15 Pb1 O2 106.49(18) 1_455 . ? O4 Pb1 O2 51.08(19) 1_455 . ? O5 Pb1 O2 131.67(17) . . ? O12 Pb1 O2 69.33(19) 2_656 . ? O7 Pb1 O2 111.39(18) 2_655 . ? O13 Pb1 O6 140.42(18) . 2_655 ? O15 Pb1 O6 111.76(18) 1_455 2_655 ? O4 Pb1 O6 108.89(19) 1_455 2_655 ? O5 Pb1 O6 74.51(17) . 2_655 ? O12 Pb1 O6 71.86(18) 2_656 2_655 ? O7 Pb1 O6 48.52(16) 2_655 2_655 ? O2 Pb1 O6 123.00(19) . 2_655 ? O13 Pb1 O9 120.41(19) . 2_656 ? O15 Pb1 O9 133.94(16) 1_455 2_656 ? O4 Pb1 O9 73.35(19) 1_455 2_656 ? O5 Pb1 O9 112.65(16) . 2_656 ? O12 Pb1 O9 45.51(16) 2_656 2_656 ? O7 Pb1 O9 70.62(17) 2_655 2_656 ? O2 Pb1 O9 64.16(18) . 2_656 ? O6 Pb1 O9 58.84(18) 2_655 2_656 ? O13 Pb1 S1 91.45(14) . 1_455 ? O15 Pb1 S1 87.98(13) 1_455 1_455 ? O4 Pb1 S1 25.16(14) 1_455 1_455 ? O5 Pb1 S1 157.63(12) . 1_455 ? O12 Pb1 S1 88.30(14) 2_656 1_455 ? O7 Pb1 S1 88.67(13) 2_655 1_455 ? O2 Pb1 S1 26.03(13) . 1_455 ? O6 Pb1 S1 116.97(13) 2_655 1_455 ? O9 Pb1 S1 64.77(11) 2_656 1_455 ? O13 Pb1 O6 102.73(18) . . ? O15 Pb1 O6 72.13(17) 1_455 . ? O4 Pb1 O6 131.22(17) 1_455 . ? O5 Pb1 O6 45.43(16) . . ? O12 Pb1 O6 111.96(17) 2_656 . ? O7 Pb1 O6 73.45(16) 2_655 . ? O2 Pb1 O6 174.53(17) . . ? O6 Pb1 O6 62.0(2) 2_655 . ? O9 Pb1 O6 120.73(16) 2_656 . ? S1 Pb1 O6 156.34(11) 1_455 . ? O13 Pb1 S2 163.62(14) . 2_655 ? O15 Pb1 S2 91.48(13) 1_455 2_655 ? O4 Pb1 S2 88.53(15) 1_455 2_655 ? O5 Pb1 S2 93.42(13) . 2_655 ? O12 Pb1 S2 91.43(14) 2_656 2_655 ? O7 Pb1 S2 23.76(12) 2_655 2_655 ? O2 Pb1 S2 120.27(13) . 2_655 ? O6 Pb1 S2 24.77(12) 2_655 2_655 ? O9 Pb1 S2 62.85(12) 2_656 2_655 ? S1 Pb1 S2 103.75(5) 1_455 2_655 ? O6 Pb1 S2 65.19(11) . 2_655 ? O14 Pb2 OH 69.61(18) . . ? O14 Pb2 O3 83.9(2) . . ? OH Pb2 O3 68.42(19) . . ? O14 Pb2 O12 85.8(2) . . ? OH Pb2 O12 77.0(2) . . ? O3 Pb2 O12 145.4(2) . . ? O14 Pb2 O2 78.81(19) . . ? OH Pb2 O2 131.0(2) . . ? O3 Pb2 O2 71.9(2) . . ? O12 Pb2 O2 137.6(2) . . ? O14 Pb2 O5 137.21(18) . 2_656 ? OH Pb2 O5 68.14(17) . 2_656 ? O3 Pb2 O5 86.94(19) . 2_656 ? O12 Pb2 O5 78.59(19) . 2_656 ? O2 Pb2 O5 136.70(19) . 2_656 ? O14 Pb2 O1 129.07(19) . 2_656 ? OH Pb2 O1 103.44(17) . 2_656 ? O3 Pb2 O1 49.50(18) . 2_656 ? O12 Pb2 O1 143.7(2) . 2_656 ? O2 Pb2 O1 69.04(19) . 2_656 ? O5 Pb2 O1 68.52(18) 2_656 2_656 ? O14 Pb2 O13 53.92(17) . . ? OH Pb2 O13 118.90(15) . . ? O3 Pb2 O13 120.64(17) . . ? O12 Pb2 O13 77.52(18) . . ? O2 Pb2 O13 61.48(17) . . ? O5 Pb2 O13 152.42(16) 2_656 . ? O1 Pb2 O13 128.53(16) 2_656 . ? O14 Pb2 Si 25.91(14) . . ? OH Pb2 Si 94.78(13) . . ? O3 Pb2 Si 98.88(15) . . ? O12 Pb2 Si 85.28(15) . . ? O2 Pb2 Si 64.18(14) . . ? O5 Pb2 Si 158.65(13) 2_656 . ? O1 Pb2 Si 130.21(13) 2_656 . ? O13 Pb2 Si 28.68(10) . . ? O14 Pb2 S1 105.81(15) . 2_656 ? OH Pb2 S1 85.04(13) . 2_656 ? O3 Pb2 S1 23.75(14) . 2_656 ? O12 Pb2 S1 153.82(16) . 2_656 ? O2 Pb2 S1 68.42(15) . 2_656 ? O5 Pb2 S1 77.07(13) 2_656 2_656 ? O1 Pb2 S1 25.75(12) 2_656 2_656 ? O13 Pb2 S1 128.35(11) . 2_656 ? Si Pb2 S1 115.45(5) . 2_656 ? O14 Pb2 Zn 36.81(13) . 1_556 ? OH Pb2 Zn 34.57(12) . 1_556 ? O3 Pb2 Zn 81.15(13) . 1_556 ? O12 Pb2 Zn 71.04(14) . 1_556 ? O2 Pb2 Zn 112.46(15) . 1_556 ? O5 Pb2 Zn 100.48(12) 2_656 1_556 ? O1 Pb2 Zn 128.80(12) 2_656 1_556 ? O13 Pb2 Zn 84.58(10) . 1_556 ? Si Pb2 Zn 60.64(4) . 1_556 ? S1 Pb2 Zn 104.14(3) 2_656 1_556 ? O14 Pb2 O12 112.74(17) . 2_656 ? OH Pb2 O12 167.54(17) . 2_656 ? O3 Pb2 O12 123.59(17) . 2_656 ? O12 Pb2 O12 90.80(18) . 2_656 ? O2 Pb2 O12 60.57(18) . 2_656 ? O5 Pb2 O12 107.12(16) 2_656 2_656 ? O1 Pb2 O12 84.67(15) 2_656 2_656 ? O13 Pb2 O12 59.82(14) . 2_656 ? Si Pb2 O12 86.84(11) . 2_656 ? S1 Pb2 O12 105.45(10) 2_656 2_656 ? Zn Pb2 O12 143.16(10) 1_556 2_656 ? OH Pb3 O15 79.46(18) 1_654 . ? OH Pb3 O7 75.0(2) 1_654 2_755 ? O15 Pb3 O7 79.9(2) . 2_755 ? OH Pb3 O11 68.32(18) 1_654 2_666 ? O15 Pb3 O11 90.95(18) . 2_666 ? O7 Pb3 O11 143.19(19) 2_755 2_666 ? OH Pb3 O3 66.96(18) 1_654 1_654 ? O15 Pb3 O3 146.40(18) . 1_654 ? O7 Pb3 O3 90.0(2) 2_755 1_654 ? O11 Pb3 O3 78.20(18) 2_666 1_654 ? OH Pb3 O10 111.17(17) 1_654 2_666 ? O15 Pb3 O10 77.26(18) . 2_666 ? O7 Pb3 O10 154.57(19) 2_755 2_666 ? O11 Pb3 O10 48.60(16) 2_666 2_666 ? O3 Pb3 O10 115.31(18) 1_654 2_666 ? OH Pb3 O4 102.37(18) 1_654 2_755 ? O15 Pb3 O4 146.05(18) . 2_755 ? O7 Pb3 O4 68.3(2) 2_755 2_755 ? O11 Pb3 O4 121.58(17) 2_666 2_755 ? O3 Pb3 O4 48.16(17) 1_654 2_755 ? O10 Pb3 O4 130.42(18) 2_666 2_755 ? OH Pb3 O4 124.11(18) 1_654 . ? O15 Pb3 O4 59.54(18) . . ? O7 Pb3 O4 62.57(19) 2_755 . ? O11 Pb3 O4 140.18(18) 2_666 . ? O3 Pb3 O4 141.14(18) 1_654 . ? O10 Pb3 O4 95.91(17) 2_666 . ? O4 Pb3 O4 94.23(16) 2_755 . ? OH Pb3 O9 119.34(17) 1_654 1_554 ? O15 Pb3 O9 141.32(18) . 1_554 ? O7 Pb3 O9 135.44(19) 2_755 1_554 ? O11 Pb3 O9 69.13(17) 2_666 1_554 ? O3 Pb3 O9 63.61(17) 1_654 1_554 ? O10 Pb3 O9 64.61(16) 2_666 1_554 ? O4 Pb3 O9 67.42(17) 2_755 1_554 ? O4 Pb3 O9 116.35(17) . 1_554 ? OH Pb3 O7 155.33(16) 1_654 . ? O15 Pb3 O7 114.29(17) . . ? O7 Pb3 O7 87.04(18) 2_755 . ? O11 Pb3 O7 128.61(16) 2_666 . ? O3 Pb3 O7 96.86(16) 1_654 . ? O10 Pb3 O7 92.35(15) 2_666 . ? O4 Pb3 O7 54.49(15) 2_755 . ? O4 Pb3 O7 57.40(16) . . ? O9 Pb3 O7 63.39(15) 1_554 . ? OH Pb3 O8 164.23(16) 1_654 . ? O15 Pb3 O8 92.01(17) . . ? O7 Pb3 O8 116.88(17) 2_755 . ? O11 Pb3 O8 98.86(16) 2_666 . ? O3 Pb3 O8 120.88(17) 1_654 . ? O10 Pb3 O8 53.56(15) 2_666 . ? O4 Pb3 O8 92.13(16) 2_755 . ? O4 Pb3 O8 59.88(16) . . ? O9 Pb3 O8 60.67(15) 1_554 . ? O7 Pb3 O8 40.41(14) . . ? OH Pb3 S3 90.52(14) 1_654 2_666 ? O15 Pb3 S3 86.18(14) . 2_666 ? O7 Pb3 S3 161.39(15) 2_755 2_666 ? O11 Pb3 S3 23.97(13) 2_666 2_666 ? O3 Pb3 S3 95.04(14) 1_654 2_666 ? O10 Pb3 S3 24.89(11) 2_666 2_666 ? O4 Pb3 S3 127.40(13) 2_755 2_666 ? O4 Pb3 S3 119.96(13) . 2_666 ? O9 Pb3 S3 61.97(12) 1_554 2_666 ? O7 Pb3 S3 110.06(10) . 2_666 ? O8 Pb3 S3 75.58(10) . 2_666 ? O8 Pb4 O16 73.8(2) 2_666 . ? O8 Pb4 O1 84.1(2) 2_666 . ? O16 Pb4 O1 75.71(19) . . ? O8 Pb4 O10 70.1(2) 2_666 . ? O16 Pb4 O10 131.93(18) . . ? O1 Pb4 O10 70.1(2) . . ? O8 Pb4 O14 122.63(18) 2_666 1_655 ? O16 Pb4 O14 58.53(17) . 1_655 ? O1 Pb4 O14 110.42(18) . 1_655 ? O10 Pb4 O14 167.23(18) . 1_655 ? O8 Pb4 O11 114.30(19) 2_666 2_667 ? O16 Pb4 O11 114.38(18) . 2_667 ? O1 Pb4 O11 160.47(19) . 2_667 ? O10 Pb4 O11 108.89(18) . 2_667 ? O14 Pb4 O11 66.08(17) 1_655 2_667 ? O8 Pb4 O3 167.20(18) 2_666 1_655 ? O16 Pb4 O3 114.22(18) . 1_655 ? O1 Pb4 O3 88.23(19) . 1_655 ? O10 Pb4 O3 97.67(18) . 1_655 ? O14 Pb4 O3 69.74(16) 1_655 1_655 ? O11 Pb4 O3 72.45(17) 2_667 1_655 ? O8 Pb4 O6 51.53(18) 2_666 2_666 ? O16 Pb4 O6 65.37(19) . 2_666 ? O1 Pb4 O6 126.6(2) . 2_666 ? O10 Pb4 O6 111.17(19) . 2_666 ? O14 Pb4 O6 79.14(17) 1_655 2_666 ? O11 Pb4 O6 72.52(17) 2_667 2_666 ? O3 Pb4 O6 140.16(16) 1_655 2_666 ? O8 Pb4 O9 74.33(19) 2_666 2_667 ? O16 Pb4 O9 126.82(18) . 2_667 ? O1 Pb4 O9 140.33(18) . 2_667 ? O10 Pb4 O9 71.33(18) . 2_667 ? O14 Pb4 O9 109.25(16) 1_655 2_667 ? O11 Pb4 O9 47.85(16) 2_667 2_667 ? O3 Pb4 O9 105.85(17) 1_655 2_667 ? O6 Pb4 O9 61.45(18) 2_666 2_667 ? O8 Pb4 O9 108.66(18) 2_666 . ? O16 Pb4 O9 174.85(18) . . ? O1 Pb4 O9 99.88(18) . . ? O10 Pb4 O9 47.10(17) . . ? O14 Pb4 O9 121.69(15) 1_655 . ? O11 Pb4 O9 69.05(16) 2_667 . ? O3 Pb4 O9 62.54(16) 1_655 . ? O6 Pb4 O9 119.75(17) 2_666 . ? O9 Pb4 O9 58.3(2) 2_667 . ? O8 Pb4 Si 97.62(15) 2_666 1_655 ? O16 Pb4 Si 28.71(13) . 1_655 ? O1 Pb4 Si 93.73(14) . 1_655 ? O10 Pb4 Si 160.16(13) . 1_655 ? O14 Pb4 Si 29.84(12) 1_655 1_655 ? O11 Pb4 Si 90.21(13) 2_667 1_655 ? O3 Pb4 Si 93.11(12) 1_655 1_655 ? O6 Pb4 Si 68.68(13) 2_666 1_655 ? O9 Pb4 Si 121.49(12) 2_667 1_655 ? O9 Pb4 Si 151.39(11) . 1_655 ? O8 Pb4 O2 119.8(2) 2_666 1_655 ? O16 Pb4 O2 62.77(19) . 1_655 ? O1 Pb4 O2 47.39(18) . 1_655 ? O10 Pb4 O2 111.05(19) . 1_655 ? O14 Pb4 O2 65.18(16) 1_655 1_655 ? O11 Pb4 O2 120.47(17) 2_667 1_655 ? O3 Pb4 O2 60.14(17) 1_655 1_655 ? O6 Pb4 O2 126.94(18) 2_666 1_655 ? O9 Pb4 O2 165.80(17) 2_667 1_655 ? O9 Pb4 O2 112.31(17) . 1_655 ? Si Pb4 O2 60.70(12) 1_655 1_655 ? O16 Pb5 O13 86.3(2) 2_666 . ? O16 Pb5 O15 89.0(2) 2_666 2_666 ? O13 Pb5 O15 63.16(18) . 2_666 ? O16 Pb5 O5 78.9(2) 2_666 . ? O13 Pb5 O5 70.28(18) . . ? O15 Pb5 O5 132.50(18) 2_666 . ? O16 Pb5 O10 166.31(19) 2_666 . ? O13 Pb5 O10 82.42(19) . . ? O15 Pb5 O10 79.09(19) 2_666 . ? O5 Pb5 O10 104.20(19) . . ? O16 Pb5 O8 67.63(19) 2_666 . ? O13 Pb5 O8 116.93(17) . . ? O15 Pb5 O8 156.21(18) 2_666 . ? O5 Pb5 O8 49.50(16) . . ? O10 Pb5 O8 124.65(18) . . ? O16 Pb5 O4 76.3(2) 2_666 2_666 ? O13 Pb5 O4 121.07(19) . 2_666 ? O15 Pb5 O4 60.75(17) 2_666 2_666 ? O5 Pb5 O4 151.66(17) . 2_666 ? O10 Pb5 O4 103.12(18) . 2_666 ? O8 Pb5 O4 107.29(16) . 2_666 ? O16 Pb5 Si 86.28(15) 2_666 . ? O13 Pb5 Si 31.35(14) . . ? O15 Pb5 Si 31.83(13) 2_666 . ? O5 Pb5 Si 101.06(13) . . ? O10 Pb5 Si 80.04(13) . . ? O8 Pb5 Si 142.62(12) . . ? O4 Pb5 Si 90.90(13) 2_666 . ? O16 Pb5 O8 130.25(19) 2_666 2_666 ? O13 Pb5 O8 140.22(19) . 2_666 ? O15 Pb5 O8 97.76(17) 2_666 2_666 ? O5 Pb5 O8 125.02(18) . 2_666 ? O10 Pb5 O8 58.96(17) . 2_666 ? O8 Pb5 O8 94.55(17) . 2_666 ? O4 Pb5 O8 65.08(17) 2_666 2_666 ? Si Pb5 O8 122.82(13) . 2_666 ? O16 Pb5 O1 63.80(19) 2_666 2_666 ? O13 Pb5 O1 147.99(19) . 2_666 ? O15 Pb5 O1 103.11(16) 2_666 2_666 ? O5 Pb5 O1 111.68(16) . 2_666 ? O10 Pb5 O1 125.25(17) . 2_666 ? O8 Pb5 O1 63.55(15) . 2_666 ? O4 Pb5 O1 43.93(16) 2_666 2_666 ? Si Pb5 O1 128.71(12) . 2_666 ? O8 Pb5 O1 66.67(16) 2_666 2_666 ? O16 Pb5 O1 134.55(19) 2_666 . ? O13 Pb5 O1 106.30(18) . . ? O15 Pb5 O1 135.97(17) 2_666 . ? O5 Pb5 O1 65.69(17) . . ? O10 Pb5 O1 56.89(17) . . ? O8 Pb5 O1 67.80(16) . . ? O4 Pb5 O1 125.98(17) 2_666 . ? Si Pb5 O1 126.56(11) . . ? O8 Pb5 O1 61.98(15) 2_666 . ? O1 Pb5 O1 103.00(15) 2_666 . ? O16 Pb5 S2 65.70(16) 2_666 . ? O13 Pb5 S2 91.26(14) . . ? O15 Pb5 S2 145.75(13) 2_666 . ? O5 Pb5 S2 25.10(12) . . ? O10 Pb5 S2 122.02(14) . . ? O8 Pb5 S2 25.84(12) . . ? O4 Pb5 S2 128.00(12) 2_666 . ? Si Pb5 S2 119.24(5) . . ? O8 Pb5 S2 116.08(13) 2_666 . ? O1 Pb5 S2 86.58(11) 2_666 . ? O1 Pb5 S2 70.43(11) . . ? OH Zn OH 180.0 2_566 1_554 ? OH Zn O14 96.7(2) 2_566 1_554 ? OH Zn O14 83.3(2) 1_554 1_554 ? OH Zn O14 83.3(2) 2_566 2_566 ? OH Zn O14 96.7(2) 1_554 2_566 ? O14 Zn O14 180.0(4) 1_554 2_566 ? OH Zn O11 85.0(2) 2_566 1_554 ? OH Zn O11 95.0(2) 1_554 1_554 ? O14 Zn O11 91.2(2) 1_554 1_554 ? O14 Zn O11 88.8(2) 2_566 1_554 ? OH Zn O11 95.0(2) 2_566 2_566 ? OH Zn O11 85.0(2) 1_554 2_566 ? O14 Zn O11 88.8(2) 1_554 2_566 ? O14 Zn O11 91.2(2) 2_566 2_566 ? O11 Zn O11 180.00(6) 1_554 2_566 ? OH Zn Pb2 44.29(15) 2_566 2_566 ? OH Zn Pb2 135.71(15) 1_554 2_566 ? O14 Zn Pb2 138.72(15) 1_554 2_566 ? O14 Zn Pb2 41.28(15) 2_566 2_566 ? O11 Zn Pb2 96.68(15) 1_554 2_566 ? O11 Zn Pb2 83.32(15) 2_566 2_566 ? OH Zn Pb2 135.71(15) 2_566 1_554 ? OH Zn Pb2 44.29(15) 1_554 1_554 ? O14 Zn Pb2 41.28(15) 1_554 1_554 ? O14 Zn Pb2 138.72(15) 2_566 1_554 ? O11 Zn Pb2 83.32(15) 1_554 1_554 ? O11 Zn Pb2 96.68(15) 2_566 1_554 ? Pb2 Zn Pb2 180.0 2_566 1_554 ? OH Zn Pb3 39.13(16) 2_566 2_665 ? OH Zn Pb3 140.87(16) 1_554 2_665 ? O14 Zn Pb3 83.61(15) 1_554 2_665 ? O14 Zn Pb3 96.39(15) 2_566 2_665 ? O11 Zn Pb3 48.62(16) 1_554 2_665 ? O11 Zn Pb3 131.38(16) 2_566 2_665 ? Pb2 Zn Pb3 72.163(8) 2_566 2_665 ? Pb2 Zn Pb3 107.837(8) 1_554 2_665 ? OH Zn Pb3 140.87(16) 2_566 1_455 ? OH Zn Pb3 39.13(16) 1_554 1_455 ? O14 Zn Pb3 96.39(15) 1_554 1_455 ? O14 Zn Pb3 83.61(15) 2_566 1_455 ? O11 Zn Pb3 131.38(16) 1_554 1_455 ? O11 Zn Pb3 48.62(16) 2_566 1_455 ? Pb2 Zn Pb3 107.837(8) 2_566 1_455 ? Pb2 Zn Pb3 72.163(8) 1_554 1_455 ? Pb3 Zn Pb3 180.0 2_665 1_455 ? OH Zn Pb4 85.71(16) 2_566 2_666 ? OH Zn Pb4 94.29(16) 1_554 2_666 ? O14 Zn Pb4 136.33(16) 1_554 2_666 ? O14 Zn Pb4 43.67(16) 2_566 2_666 ? O11 Zn Pb4 45.37(15) 1_554 2_666 ? O11 Zn Pb4 134.63(15) 2_566 2_666 ? Pb2 Zn Pb4 65.931(8) 2_566 2_666 ? Pb2 Zn Pb4 114.069(8) 1_554 2_666 ? Pb3 Zn Pb4 71.076(7) 2_665 2_666 ? Pb3 Zn Pb4 108.924(7) 1_455 2_666 ? OH Zn Pb4 94.29(16) 2_566 1_454 ? OH Zn Pb4 85.71(16) 1_554 1_454 ? O14 Zn Pb4 43.67(16) 1_554 1_454 ? O14 Zn Pb4 136.33(16) 2_566 1_454 ? O11 Zn Pb4 134.63(15) 1_554 1_454 ? O11 Zn Pb4 45.37(15) 2_566 1_454 ? Pb2 Zn Pb4 114.069(8) 2_566 1_454 ? Pb2 Zn Pb4 65.931(8) 1_554 1_454 ? Pb3 Zn Pb4 108.924(7) 2_665 1_454 ? Pb3 Zn Pb4 71.076(7) 1_455 1_454 ? Pb4 Zn Pb4 180.000(10) 2_666 1_454 ? O2 S1 O1 111.5(4) 1_655 . ? O2 S1 O4 109.4(4) 1_655 . ? O1 S1 O4 109.9(4) . . ? O2 S1 O3 109.7(4) 1_655 2_656 ? O1 S1 O3 107.4(4) . 2_656 ? O4 S1 O3 108.9(4) . 2_656 ? O2 S1 Pb1 61.0(3) 1_655 1_655 ? O1 S1 Pb1 132.4(3) . 1_655 ? O4 S1 Pb1 48.7(3) . 1_655 ? O3 S1 Pb1 119.5(3) 2_656 1_655 ? O2 S1 Pb2 125.3(3) 1_655 2_656 ? O1 S1 Pb2 65.0(2) . 2_656 ? O4 S1 Pb2 123.3(3) . 2_656 ? O3 S1 Pb2 42.4(2) 2_656 2_656 ? Pb1 S1 Pb2 160.80(7) 1_655 2_656 ? O2 S1 Pb4 70.9(3) 1_655 . ? O1 S1 Pb4 41.1(3) . . ? O4 S1 Pb4 119.1(3) . . ? O3 S1 Pb4 128.9(2) 2_656 . ? Pb1 S1 Pb4 105.43(5) 1_655 . ? Pb2 S1 Pb4 93.59(5) 2_656 . ? O2 S1 Pb3 124.7(3) 1_655 2_755 ? O1 S1 Pb3 122.5(3) . 2_755 ? O4 S1 Pb3 63.9(3) . 2_755 ? O3 S1 Pb3 45.0(2) 2_656 2_755 ? Pb1 S1 Pb3 88.56(5) 1_655 2_755 ? Pb2 S1 Pb3 73.10(4) 2_656 2_755 ? Pb4 S1 Pb3 163.45(6) . 2_755 ? O2 S1 Pb5 102.4(3) 1_655 2_666 ? O1 S1 Pb5 63.5(3) . 2_666 ? O4 S1 Pb5 53.8(3) . 2_666 ? O3 S1 Pb5 147.5(3) 2_656 2_666 ? Pb1 S1 Pb5 72.24(4) 1_655 2_666 ? Pb2 S1 Pb5 119.15(6) 2_656 2_666 ? Pb4 S1 Pb5 66.47(4) . 2_666 ? Pb3 S1 Pb5 110.97(5) 2_755 2_666 ? O2 S1 Pb4 75.1(3) 1_655 2_756 ? O1 S1 Pb4 119.6(3) . 2_756 ? O4 S1 Pb4 124.5(3) . 2_756 ? O3 S1 Pb4 34.7(2) 2_656 2_756 ? Pb1 S1 Pb4 104.27(5) 1_655 2_756 ? Pb2 S1 Pb4 64.38(3) 2_656 2_756 ? Pb4 S1 Pb4 114.44(5) . 2_756 ? Pb3 S1 Pb4 69.20(4) 2_755 2_756 ? Pb5 S1 Pb4 176.45(6) 2_666 2_756 ? O6 S2 O7 110.0(4) . . ? O6 S2 O8 110.9(4) . . ? O7 S2 O8 108.0(4) . . ? O6 S2 O5 109.3(4) . . ? O7 S2 O5 110.5(4) . . ? O8 S2 O5 108.2(4) . . ? O6 S2 Pb4 66.1(3) . 2_666 ? O7 S2 Pb4 128.5(3) . 2_666 ? O8 S2 Pb4 45.1(2) . 2_666 ? O5 S2 Pb4 119.2(3) . 2_666 ? O6 S2 Pb5 107.0(3) . . ? O7 S2 Pb5 142.7(3) . . ? O8 S2 Pb5 62.0(3) . . ? O5 S2 Pb5 50.6(2) . . ? Pb4 S2 Pb5 72.10(4) 2_666 . ? O6 S2 Pb1 60.7(3) . 2_655 ? O7 S2 Pb1 49.3(3) . 2_655 ? O8 S2 Pb1 126.6(3) . 2_655 ? O5 S2 Pb1 124.7(3) . 2_655 ? Pb4 S2 Pb1 105.73(5) 2_666 2_655 ? Pb5 S2 Pb1 166.08(6) . 2_655 ? O6 S2 Pb1 67.3(3) . . ? O7 S2 Pb1 124.3(3) . . ? O8 S2 Pb1 125.4(3) . . ? O5 S2 Pb1 42.0(2) . . ? Pb4 S2 Pb1 102.21(5) 2_666 . ? Pb5 S2 Pb1 66.82(3) . . ? Pb1 S2 Pb1 100.90(5) 2_655 . ? O6 S2 Pb3 125.0(3) . 2_755 ? O7 S2 Pb3 21.9(2) . 2_755 ? O8 S2 Pb3 111.0(3) . 2_755 ? O5 S2 Pb3 89.3(3) . 2_755 ? Pb4 S2 Pb3 145.69(6) 2_666 2_755 ? Pb5 S2 Pb3 123.51(5) . 2_755 ? Pb1 S2 Pb3 66.15(3) 2_655 2_755 ? Pb1 S2 Pb3 112.01(5) . 2_755 ? O9 S3 O10 111.7(4) . . ? O9 S3 O12 110.9(4) . . ? O10 S3 O12 110.5(4) . . ? O9 S3 O11 109.3(4) . . ? O10 S3 O11 106.2(4) . . ? O12 S3 O11 108.0(3) . . ? O9 S3 Pb3 117.8(3) . 2_666 ? O10 S3 Pb3 61.5(3) . 2_666 ? O12 S3 Pb3 130.0(3) . 2_666 ? O11 S3 Pb3 45.4(2) . 2_666 ? O9 S3 Pb4 66.7(3) . . ? O10 S3 Pb4 45.1(3) . . ? O12 S3 Pb4 126.7(3) . . ? O11 S3 Pb4 123.3(2) . . ? Pb3 S3 Pb4 84.52(4) 2_666 . ? O9 S3 Pb4 61.6(3) . 2_667 ? O10 S3 Pb4 125.9(3) . 2_667 ? O12 S3 Pb4 122.1(3) . 2_667 ? O11 S3 Pb4 47.8(2) . 2_667 ? Pb3 S3 Pb4 75.00(4) 2_666 2_667 ? Pb4 S3 Pb4 103.65(5) . 2_667 ? O9 S3 Pb1 66.8(3) . 2_656 ? O10 S3 Pb1 130.7(3) . 2_656 ? O12 S3 Pb1 44.2(3) . 2_656 ? O11 S3 Pb1 121.0(2) . 2_656 ? Pb3 S3 Pb1 166.04(6) 2_666 2_656 ? Pb4 S3 Pb1 108.98(5) . 2_656 ? Pb4 S3 Pb1 97.71(5) 2_667 2_656 ? O9 S3 Pb2 133.9(3) . . ? O10 S3 Pb2 105.8(3) . . ? O12 S3 Pb2 27.7(2) . . ? O11 S3 Pb2 83.9(2) . . ? Pb3 S3 Pb2 103.05(5) 2_666 . ? Pb4 S3 Pb2 141.87(6) . . ? Pb4 S3 Pb2 114.44(5) 2_667 . ? Pb1 S3 Pb2 68.73(3) 2_656 . ? O16 Si O14 105.2(3) 1_455 . ? O16 Si O15 112.7(3) 1_455 2_666 ? O14 Si O15 113.1(3) . 2_666 ? O16 Si O13 113.1(3) 1_455 . ? O14 Si O13 109.8(3) . . ? O15 Si O13 103.1(3) 2_666 . ? O16 Si Pb5 126.8(2) 1_455 . ? O14 Si Pb5 127.6(2) . . ? O15 Si Pb5 55.3(2) 2_666 . ? O13 Si Pb5 47.8(2) . . ? O16 Si Pb4 48.8(2) 1_455 1_455 ? O14 Si Pb4 56.5(2) . 1_455 ? O15 Si Pb4 127.7(2) 2_666 1_455 ? O13 Si Pb4 129.2(2) . 1_455 ? Pb5 Si Pb4 174.78(8) . 1_455 ? O16 Si Pb2 110.7(2) 1_455 . ? O14 Si Pb2 38.6(2) . . ? O15 Si Pb2 133.8(2) 2_666 . ? O13 Si Pb2 72.9(2) . . ? Pb5 Si Pb2 107.54(6) . . ? Pb4 Si Pb2 73.64(4) 1_455 . ? O16 Si Pb1 80.2(2) 1_455 . ? O14 Si Pb1 118.1(2) . . ? O15 Si Pb1 121.0(2) 2_666 . ? O13 Si Pb1 33.0(2) . . ? Pb5 Si Pb1 70.77(4) . . ? Pb4 Si Pb1 104.64(6) 1_455 . ? Pb2 Si Pb1 81.03(5) . . ? O16 Si Pb1 73.2(2) 1_455 2_566 ? O14 Si Pb1 130.5(2) . 2_566 ? O15 Si Pb1 39.7(2) 2_666 2_566 ? O13 Si Pb1 116.1(2) . 2_566 ? Pb5 Si Pb1 76.59(4) . 2_566 ? Pb4 Si Pb1 103.25(6) 1_455 2_566 ? Pb2 Si Pb1 168.50(7) . 2_566 ? Pb1 Si Pb1 110.44(5) . 2_566 ? O16 Si Pb3 131.9(2) 1_455 2_666 ? O14 Si Pb3 84.3(2) . 2_666 ? O15 Si Pb3 30.0(2) 2_666 2_666 ? O13 Si Pb3 107.0(2) . 2_666 ? Pb5 Si Pb3 66.62(4) . 2_666 ? Pb4 Si Pb3 118.20(6) 1_455 2_666 ? Pb2 Si Pb3 105.51(5) . 2_666 ? Pb1 Si Pb3 136.89(6) . 2_666 ? Pb1 Si Pb3 65.79(4) 2_566 2_666 ? O16 Si Pb5 19.4(2) 1_455 2_566 ? O14 Si Pb5 124.5(2) . 2_566 ? O15 Si Pb5 103.0(2) 2_666 2_566 ? O13 Si Pb5 100.8(2) . 2_566 ? Pb5 Si Pb5 107.36(6) . 2_566 ? Pb4 Si Pb5 68.24(4) 1_455 2_566 ? Pb2 Si Pb5 123.12(6) . 2_566 ? Pb1 Si Pb5 70.05(4) . 2_566 ? Pb1 Si Pb5 63.93(4) 2_566 2_566 ? Pb3 Si Pb5 129.22(6) 2_666 2_566 ? S1 O1 Pb4 116.3(3) . . ? S1 O1 Pb2 89.3(3) . 2_656 ? Pb4 O1 Pb2 125.3(2) . 2_656 ? S1 O1 Pb5 93.3(3) . 2_666 ? Pb4 O1 Pb5 83.05(17) . 2_666 ? Pb2 O1 Pb5 146.4(2) 2_656 2_666 ? S1 O1 Pb5 145.7(4) . . ? Pb4 O1 Pb5 95.33(19) . . ? Pb2 O1 Pb5 82.17(15) 2_656 . ? Pb5 O1 Pb5 77.00(15) 2_666 . ? S1 O2 Pb2 162.0(5) 1_455 . ? S1 O2 Pb1 92.9(3) 1_455 . ? Pb2 O2 Pb1 103.7(2) . . ? S1 O2 Pb4 84.1(3) 1_455 1_455 ? Pb2 O2 Pb4 81.50(18) . 1_455 ? Pb1 O2 Pb4 121.0(2) . 1_455 ? S1 O3 Pb2 113.9(3) 2_656 . ? S1 O3 Pb3 111.7(3) 2_656 1_456 ? Pb2 O3 Pb3 105.2(2) . 1_456 ? S1 O3 Pb4 128.2(3) 2_656 1_455 ? Pb2 O3 Pb4 94.35(18) . 1_455 ? Pb3 O3 Pb4 100.34(19) 1_456 1_455 ? S1 O4 Pb1 106.2(4) . 1_655 ? S1 O4 Pb5 103.5(3) . 2_666 ? Pb1 O4 Pb5 93.8(2) 1_655 2_666 ? S1 O4 Pb3 91.3(3) . 2_755 ? Pb1 O4 Pb3 111.9(2) 1_655 2_755 ? Pb5 O4 Pb3 145.6(2) 2_666 2_755 ? S1 O4 Pb3 168.6(4) . . ? Pb1 O4 Pb3 85.11(17) 1_655 . ? Pb5 O4 Pb3 73.57(15) 2_666 . ? Pb3 O4 Pb3 85.77(16) 2_755 . ? S2 O5 Pb1 116.4(3) . . ? S2 O5 Pb5 104.3(3) . . ? Pb1 O5 Pb5 91.21(18) . . ? S2 O5 Pb2 138.8(4) . 2_656 ? Pb1 O5 Pb2 96.22(17) . 2_656 ? Pb5 O5 Pb2 99.13(18) . 2_656 ? S2 O6 Pb4 87.4(3) . 2_666 ? S2 O6 Pb1 94.6(3) . 2_655 ? Pb4 O6 Pb1 126.2(2) 2_666 2_655 ? S2 O6 Pb1 88.8(3) . . ? Pb4 O6 Pb1 115.8(2) 2_666 . ? Pb1 O6 Pb1 118.0(2) 2_655 . ? S2 O7 Pb3 145.3(4) . 2_755 ? S2 O7 Pb1 106.9(3) . 2_655 ? Pb3 O7 Pb1 98.4(2) 2_755 2_655 ? S2 O7 Pb3 105.2(3) . . ? Pb3 O7 Pb3 92.96(18) 2_755 . ? Pb1 O7 Pb3 100.23(18) 2_655 . ? S2 O8 Pb4 109.8(3) . 2_666 ? S2 O8 Pb5 92.2(3) . . ? Pb4 O8 Pb5 91.35(19) 2_666 . ? S2 O8 Pb5 147.9(3) . 2_666 ? Pb4 O8 Pb5 102.30(19) 2_666 2_666 ? Pb5 O8 Pb5 85.45(17) . 2_666 ? S2 O8 Pb3 103.4(3) . . ? Pb4 O8 Pb3 103.6(2) 2_666 . ? Pb5 O8 Pb3 153.0(2) . . ? Pb5 O8 Pb3 69.60(12) 2_666 . ? S3 O9 Pb4 94.4(3) . 2_667 ? S3 O9 Pb4 89.0(3) . . ? Pb4 O9 Pb4 121.7(2) 2_667 . ? S3 O9 Pb3 169.9(4) . 1_556 ? Pb4 O9 Pb3 93.95(16) 2_667 1_556 ? Pb4 O9 Pb3 81.85(14) . 1_556 ? S3 O9 Pb1 89.6(3) . 2_656 ? Pb4 O9 Pb1 113.45(19) 2_667 2_656 ? Pb4 O9 Pb1 124.8(2) . 2_656 ? Pb3 O9 Pb1 92.23(15) 1_556 2_656 ? S3 O10 Pb4 112.1(3) . . ? S3 O10 Pb5 143.6(4) . . ? Pb4 O10 Pb5 103.86(19) . . ? S3 O10 Pb3 93.6(3) . 2_666 ? Pb4 O10 Pb3 109.5(2) . 2_666 ? Pb5 O10 Pb3 78.83(16) . 2_666 ? S3 O11 Zn 135.6(3) . 1_556 ? S3 O11 Pb3 110.6(3) . 2_666 ? Zn O11 Pb3 93.3(2) 1_556 2_666 ? S3 O11 Pb4 108.3(3) . 2_667 ? Zn O11 Pb4 100.6(2) 1_556 2_667 ? Pb3 O11 Pb4 104.28(19) 2_666 2_667 ? S3 O12 Pb2 136.4(4) . . ? S3 O12 Pb1 113.9(3) . 2_656 ? Pb2 O12 Pb1 103.6(2) . 2_656 ? S3 O12 Pb2 111.0(3) . 2_656 ? Pb2 O12 Pb2 89.20(18) . 2_656 ? Pb1 O12 Pb2 90.81(17) 2_656 2_656 ? Si O13 Pb1 124.5(3) . . ? Si O13 Pb5 100.8(3) . . ? Pb1 O13 Pb5 111.2(2) . . ? Si O13 Pb2 78.4(2) . . ? Pb1 O13 Pb2 104.71(19) . . ? Pb5 O13 Pb2 135.6(2) . . ? Si O14 Zn 133.3(3) . 1_556 ? Si O14 Pb2 115.5(3) . . ? Zn O14 Pb2 101.9(2) 1_556 . ? Si O14 Pb4 93.7(2) . 1_455 ? Zn O14 Pb4 104.1(2) 1_556 1_455 ? Pb2 O14 Pb4 103.5(2) . 1_455 ? Si O15 Pb3 130.3(3) 2_666 . ? Si O15 Pb1 116.0(3) 2_666 1_655 ? Pb3 O15 Pb1 105.4(2) . 1_655 ? Si O15 Pb5 92.9(3) 2_666 2_666 ? Pb3 O15 Pb5 98.4(2) . 2_666 ? Pb1 O15 Pb5 109.3(2) 1_655 2_666 ? Si O16 Pb5 146.9(3) 1_655 2_666 ? Si O16 Pb4 102.4(3) 1_655 . ? Pb5 O16 Pb4 110.6(2) 2_666 . ? Si O16 Pb1 80.6(2) 1_655 2_666 ? Pb5 O16 Pb1 81.61(16) 2_666 2_666 ? Pb4 O16 Pb1 126.5(2) . 2_666 ? Si O16 Pb1 74.0(2) 1_655 1_655 ? Pb5 O16 Pb1 86.69(17) 2_666 1_655 ? Pb4 O16 Pb1 121.4(2) . 1_655 ? Pb1 O16 Pb1 110.83(16) 2_666 1_655 ? Zn OH Pb3 108.5(2) 1_556 1_456 ? Zn OH Pb2 101.1(2) 1_556 . ? Pb3 OH Pb2 117.7(2) 1_456 . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 32.62 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 3.323 _refine_diff_density_min -2.790 _refine_diff_density_rms 0.446