data_fassinaite-black-forest _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C O6 Pb2 S2' _chemical_formula_weight 586.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.326(3) _cell_length_b 8.773(2) _cell_length_c 4.5830(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 656.4(2) _cell_formula_units_Z 4 _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 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 51.840 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1221 _exptl_absorpt_correction_T_max 0.3054 _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 1781 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 30.02 _reflns_number_total 1018 _reflns_number_gt 770 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0500P)^2^+0.0000P] 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 0.00073(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1018 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.135969(19) 0.48701(4) 0.58424(9) 0.02049(17) Uani 1 1 d . . . S1 S 0.00297(16) 0.2500 0.0734(7) 0.0155(6) Uani 1 2 d S . . C C 0.7115(7) 0.2500 0.373(3) 0.017(3) Uani 1 2 d S . . O1 O 0.0604(5) 0.2500 0.8267(19) 0.021(2) Uani 1 2 d S . . O2 O 0.2758(4) 0.6203(7) 0.5023(15) 0.0272(16) Uani 1 1 d . . . O3 O 0.0138(3) 0.1110(6) 0.2515(15) 0.0188(12) Uani 1 1 d . . . O4 O 0.1872(6) 0.2500 0.394(2) 0.028(2) Uani 1 2 d S . . S2 S 0.88526(19) 0.2500 0.9276(8) 0.0197(6) Uani 1 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 Pb 0.0186(2) 0.0187(2) 0.0242(2) -0.00070(14) -0.00106(13) -0.00107(11) S1 0.0131(14) 0.0144(13) 0.0189(15) 0.000 0.0002(14) 0.000 C 0.013(5) 0.018(5) 0.020(7) 0.000 0.006(5) 0.000 O1 0.016(4) 0.027(5) 0.019(5) 0.000 0.007(4) 0.000 O2 0.023(3) 0.027(3) 0.032(4) -0.012(3) 0.009(3) -0.006(3) O3 0.019(3) 0.015(3) 0.022(3) 0.002(3) -0.004(3) -0.005(2) O4 0.037(5) 0.030(5) 0.018(5) 0.000 0.011(5) 0.000 S2 0.0167(13) 0.0211(14) 0.0213(17) 0.000 -0.0043(14) 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 Pb O4 2.405(5) . ? Pb O2 2.575(6) 2_565 ? Pb O2 2.593(6) . ? Pb O3 2.654(6) 7_565 ? Pb O1 2.661(5) . ? Pb O3 2.780(5) 3_556 ? Pb O2 3.174(7) 2_564 ? Pb C 3.201(10) 6_556 ? Pb S2 3.232(3) 5_667 ? Pb S2 3.308(3) 5_666 ? S1 O1 1.469(9) 1_554 ? S1 O3 1.478(6) 7_565 ? S1 O3 1.478(6) . ? S1 S2 2.035(4) 1_454 ? S1 Pb 3.596(2) 5_566 ? S1 Pb 3.596(2) 3_546 ? S1 Pb 3.750(2) 1_554 ? S1 Pb 3.750(2) 7_564 ? S1 Pb 3.810(3) 7_565 ? S1 Pb 4.422(3) 3_545 ? S1 Pb 4.422(3) 5_565 ? C O4 1.287(14) 6_656 ? C O2 1.289(8) 5_666 ? C O2 1.289(8) 3_646 ? C Pb 3.201(10) 4 ? C Pb 3.201(10) 6_656 ? C Pb 3.400(8) 5_666 ? C Pb 3.400(8) 3_646 ? C Pb 3.467(10) 6_657 ? C Pb 3.467(10) 4_556 ? O1 S1 1.469(9) 1_556 ? O1 Pb 2.661(5) 7_565 ? O1 Pb 4.231(8) 1_556 ? O1 Pb 4.231(8) 7_566 ? O1 Pb 4.376(7) 3_546 ? O1 Pb 4.376(7) 5_566 ? O2 C 1.289(8) 5_666 ? O2 Pb 2.575(6) 2_564 ? O2 Pb 3.174(7) 2_565 ? O2 Pb 4.011(6) 8_665 ? O2 Pb 4.150(6) 7_575 ? O2 Pb 4.420(6) 8_666 ? O3 Pb 2.654(6) 7_565 ? O3 Pb 2.780(5) 3_546 ? O3 Pb 3.751(6) 7_564 ? O3 Pb 4.357(5) 5_566 ? O4 C 1.287(14) 6_556 ? O4 Pb 2.405(5) 7_565 ? O4 Pb 3.959(7) 2_564 ? O4 Pb 3.959(7) 8_655 ? O4 Pb 4.334(9) 7_564 ? O4 Pb 4.334(9) 1_554 ? S2 S1 2.035(4) 1_656 ? S2 Pb 3.232(3) 5_667 ? S2 Pb 3.232(3) 3_647 ? S2 Pb 3.308(3) 3_646 ? S2 Pb 3.308(3) 5_666 ? S2 Pb 4.571(3) 4_556 ? S2 Pb 4.571(3) 6_657 ? S2 Pb 4.853(3) 1_655 ? S2 Pb 4.853(3) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Pb O2 76.1(3) . 2_565 ? O4 Pb O2 91.8(2) . . ? O2 Pb O2 77.31(17) 2_565 . ? O4 Pb O3 76.9(3) . 7_565 ? O2 Pb O3 136.83(18) 2_565 7_565 ? O2 Pb O3 136.5(2) . 7_565 ? O4 Pb O1 68.7(2) . . ? O2 Pb O1 70.3(2) 2_565 . ? O2 Pb O1 145.2(2) . . ? O3 Pb O1 68.8(2) 7_565 . ? O4 Pb O3 137.9(2) . 3_556 ? O2 Pb O3 115.7(2) 2_565 3_556 ? O2 Pb O3 129.60(18) . 3_556 ? O3 Pb O3 67.7(2) 7_565 3_556 ? O1 Pb O3 77.58(18) . 3_556 ? O4 Pb O2 44.0(2) . 2_564 ? O2 Pb O2 105.3(2) 2_565 2_564 ? O2 Pb O2 67.21(18) . 2_564 ? O3 Pb O2 76.23(17) 7_565 2_564 ? O1 Pb O2 109.23(18) . 2_564 ? O3 Pb O2 137.96(18) 3_556 2_564 ? O4 Pb C 21.0(2) . 6_556 ? O2 Pb C 92.0(3) 2_565 6_556 ? O2 Pb C 81.9(2) . 6_556 ? O3 Pb C 72.7(2) 7_565 6_556 ? O1 Pb C 86.8(2) . 6_556 ? O3 Pb C 140.4(2) 3_556 6_556 ? O2 Pb C 23.32(18) 2_564 6_556 ? O4 Pb S2 154.9(2) . 5_667 ? O2 Pb S2 78.81(16) 2_565 5_667 ? O2 Pb S2 82.68(15) . 5_667 ? O3 Pb S2 123.25(13) 7_565 5_667 ? O1 Pb S2 102.65(16) . 5_667 ? O3 Pb S2 55.88(14) 3_556 5_667 ? O2 Pb S2 147.36(12) 2_564 5_667 ? C Pb S2 163.45(19) 6_556 5_667 ? O4 Pb S2 112.5(2) . 5_666 ? O2 Pb S2 147.26(14) 2_565 5_666 ? O2 Pb S2 71.04(17) . 5_666 ? O3 Pb S2 74.91(13) 7_565 5_666 ? O1 Pb S2 142.43(18) . 5_666 ? O3 Pb S2 80.04(14) 3_556 5_666 ? O2 Pb S2 70.04(12) 2_564 5_666 ? C Pb S2 91.65(18) 6_556 5_666 ? S2 Pb S2 88.95(2) 5_667 5_666 ? O1 S1 O3 110.4(3) 1_554 7_565 ? O1 S1 O3 110.4(3) 1_554 . ? O3 S1 O3 111.2(5) 7_565 . ? O1 S1 S2 110.5(4) 1_554 1_454 ? O3 S1 S2 107.1(2) 7_565 1_454 ? O3 S1 S2 107.1(2) . 1_454 ? O1 S1 Pb 137.61(12) 1_554 5_566 ? O3 S1 Pb 46.0(2) 7_565 5_566 ? O3 S1 Pb 111.3(3) . 5_566 ? S2 S1 Pb 63.10(9) 1_454 5_566 ? O1 S1 Pb 137.61(12) 1_554 3_546 ? O3 S1 Pb 111.3(3) 7_565 3_546 ? O3 S1 Pb 46.0(2) . 3_546 ? S2 S1 Pb 63.10(9) 1_454 3_546 ? Pb S1 Pb 79.83(6) 5_566 3_546 ? O1 S1 Pb 33.93(5) 1_554 1_554 ? O3 S1 Pb 78.7(3) 7_565 1_554 ? O3 S1 Pb 135.9(2) . 1_554 ? S2 S1 Pb 110.52(13) 1_454 1_554 ? Pb S1 Pb 105.68(2) 5_566 1_554 ? Pb S1 Pb 169.06(9) 3_546 1_554 ? O1 S1 Pb 33.93(5) 1_554 7_564 ? O3 S1 Pb 135.9(2) 7_565 7_564 ? O3 S1 Pb 78.7(3) . 7_564 ? S2 S1 Pb 110.52(13) 1_454 7_564 ? Pb S1 Pb 169.06(9) 5_566 7_564 ? Pb S1 Pb 105.68(2) 3_546 7_564 ? Pb S1 Pb 67.35(5) 1_554 7_564 ? O1 S1 Pb 96.3(3) 1_554 . ? O3 S1 Pb 31.0(2) 7_565 . ? O3 S1 Pb 92.5(3) . . ? S2 S1 Pb 137.74(10) 1_454 . ? Pb S1 Pb 75.01(4) 5_566 . ? Pb S1 Pb 116.20(9) 3_546 . ? Pb S1 Pb 74.62(4) 1_554 . ? Pb S1 Pb 109.87(7) 7_564 . ? O1 S1 Pb 96.3(3) 1_554 7_565 ? O3 S1 Pb 92.5(3) 7_565 7_565 ? O3 S1 Pb 31.0(2) . 7_565 ? S2 S1 Pb 137.74(10) 1_454 7_565 ? Pb S1 Pb 116.20(9) 5_566 7_565 ? Pb S1 Pb 75.01(4) 3_546 7_565 ? Pb S1 Pb 109.87(7) 1_554 7_565 ? Pb S1 Pb 74.62(4) 7_564 7_565 ? Pb S1 Pb 66.14(5) . 7_565 ? O1 S1 Pb 78.6(3) 1_554 3_545 ? O3 S1 Pb 150.2(2) 7_565 3_545 ? O3 S1 Pb 90.4(2) . 3_545 ? S2 S1 Pb 44.89(9) 1_454 3_545 ? Pb S1 Pb 107.97(6) 5_566 3_545 ? Pb S1 Pb 68.84(4) 3_546 3_545 ? Pb S1 Pb 100.30(7) 1_554 3_545 ? Pb S1 Pb 66.44(4) 7_564 3_545 ? Pb S1 Pb 174.77(8) . 3_545 ? Pb S1 Pb 115.238(17) 7_565 3_545 ? O1 S1 Pb 78.6(3) 1_554 5_565 ? O3 S1 Pb 90.4(2) 7_565 5_565 ? O3 S1 Pb 150.2(2) . 5_565 ? S2 S1 Pb 44.89(9) 1_454 5_565 ? Pb S1 Pb 68.84(4) 5_566 5_565 ? Pb S1 Pb 107.97(6) 3_546 5_565 ? Pb S1 Pb 66.44(4) 1_554 5_565 ? Pb S1 Pb 100.30(7) 7_564 5_565 ? Pb S1 Pb 115.238(17) . 5_565 ? Pb S1 Pb 174.77(8) 7_565 5_565 ? Pb S1 Pb 62.90(4) 3_545 5_565 ? O4 C O2 118.0(6) 6_656 5_666 ? O4 C O2 118.0(6) 6_656 3_646 ? O2 C O2 123.9(12) 5_666 3_646 ? O4 C Pb 42.1(2) 6_656 4 ? O2 C Pb 157.6(7) 5_666 4 ? O2 C Pb 77.2(5) 3_646 4 ? O4 C Pb 42.1(2) 6_656 6_656 ? O2 C Pb 77.2(5) 5_666 6_656 ? O2 C Pb 157.6(7) 3_646 6_656 ? Pb C Pb 81.0(3) 4 6_656 ? O4 C Pb 106.3(5) 6_656 5_666 ? O2 C Pb 42.1(4) 5_666 5_666 ? O2 C Pb 117.2(7) 3_646 5_666 ? Pb C Pb 139.5(4) 4 5_666 ? Pb C Pb 83.04(13) 6_656 5_666 ? O4 C Pb 106.3(5) 6_656 3_646 ? O2 C Pb 117.2(7) 5_666 3_646 ? O2 C Pb 42.1(4) 3_646 3_646 ? Pb C Pb 83.04(13) 4 3_646 ? Pb C Pb 139.5(4) 6_656 3_646 ? Pb C Pb 85.5(3) 5_666 3_646 ? O4 C Pb 124.9(5) 6_656 6_657 ? O2 C Pb 37.9(5) 5_666 6_657 ? O2 C Pb 105.6(7) 3_646 6_657 ? Pb C Pb 136.2(4) 4 6_657 ? Pb C Pb 86.74(14) 6_656 6_657 ? Pb C Pb 79.20(16) 5_666 6_657 ? Pb C Pb 128.8(4) 3_646 6_657 ? O4 C Pb 124.9(5) 6_656 4_556 ? O2 C Pb 105.6(7) 5_666 4_556 ? O2 C Pb 37.9(5) 3_646 4_556 ? Pb C Pb 86.74(14) 4 4_556 ? Pb C Pb 136.2(4) 6_656 4_556 ? Pb C Pb 128.8(4) 5_666 4_556 ? Pb C Pb 79.20(16) 3_646 4_556 ? Pb C Pb 73.7(2) 6_657 4_556 ? S1 O1 Pb 128.12(16) 1_556 7_565 ? S1 O1 Pb 128.12(16) 1_556 . ? Pb O1 Pb 102.8(3) 7_565 . ? S1 O1 Pb 63.5(3) 1_556 1_556 ? Pb O1 Pb 126.3(3) 7_565 1_556 ? Pb O1 Pb 79.84(14) . 1_556 ? S1 O1 Pb 63.5(3) 1_556 7_566 ? Pb O1 Pb 79.84(14) 7_565 7_566 ? Pb O1 Pb 126.3(3) . 7_566 ? Pb O1 Pb 58.88(12) 1_556 7_566 ? S1 O1 Pb 82.1(3) 1_556 3_546 ? Pb O1 Pb 75.39(13) 7_565 3_546 ? Pb O1 Pb 124.9(3) . 3_546 ? Pb O1 Pb 145.7(2) 1_556 3_546 ? Pb O1 Pb 107.92(9) 7_566 3_546 ? S1 O1 Pb 82.1(3) 1_556 5_566 ? Pb O1 Pb 124.9(3) 7_565 5_566 ? Pb O1 Pb 75.39(13) . 5_566 ? Pb O1 Pb 107.92(9) 1_556 5_566 ? Pb O1 Pb 145.7(2) 7_566 5_566 ? Pb O1 Pb 63.63(12) 3_546 5_566 ? C O2 Pb 124.2(6) 5_666 2_564 ? C O2 Pb 118.4(6) 5_666 . ? Pb O2 Pb 115.8(2) 2_564 . ? C O2 Pb 79.5(6) 5_666 2_565 ? Pb O2 Pb 105.3(2) 2_564 2_565 ? Pb O2 Pb 98.3(2) . 2_565 ? C O2 Pb 56.3(6) 5_666 8_665 ? Pb O2 Pb 74.76(15) 2_564 8_665 ? Pb O2 Pb 138.3(2) . 8_665 ? Pb O2 Pb 118.46(17) 2_565 8_665 ? C O2 Pb 46.8(6) 5_666 7_575 ? Pb O2 Pb 132.7(2) 2_564 7_575 ? Pb O2 Pb 82.92(15) . 7_575 ? Pb O2 Pb 114.83(17) 2_565 7_575 ? Pb O2 Pb 64.85(10) 8_665 7_575 ? C O2 Pb 16.0(6) 5_666 8_666 ? Pb O2 Pb 122.21(19) 2_564 8_666 ? Pb O2 Pb 121.86(19) . 8_666 ? Pb O2 Pb 63.97(11) 2_565 8_666 ? Pb O2 Pb 65.65(9) 8_665 8_666 ? Pb O2 Pb 61.35(8) 7_575 8_666 ? S1 O3 Pb 132.4(3) . 7_565 ? S1 O3 Pb 111.5(3) . 3_546 ? Pb O3 Pb 112.3(2) 7_565 3_546 ? S1 O3 Pb 78.6(3) . 7_564 ? Pb O3 Pb 89.69(15) 7_565 7_564 ? Pb O3 Pb 126.79(19) 3_546 7_564 ? S1 O3 Pb 66.7(2) . . ? Pb O3 Pb 71.62(12) 7_565 . ? Pb O3 Pb 129.4(2) 3_546 . ? Pb O3 Pb 103.08(12) 7_564 . ? S1 O3 Pb 50.2(2) . 5_566 ? Pb O3 Pb 125.8(2) 7_565 5_566 ? Pb O3 Pb 77.07(12) 3_546 5_566 ? Pb O3 Pb 128.66(16) 7_564 5_566 ? Pb O3 Pb 64.04(8) . 5_566 ? C O4 Pb 116.9(3) 6_556 7_565 ? C O4 Pb 116.9(3) 6_556 . ? Pb O4 Pb 119.7(4) 7_565 . ? C O4 Pb 55.5(4) 6_556 2_564 ? Pb O4 Pb 152.5(3) 7_565 2_564 ? Pb O4 Pb 83.09(11) . 2_564 ? C O4 Pb 55.5(4) 6_556 8_655 ? Pb O4 Pb 83.09(11) 7_565 8_655 ? Pb O4 Pb 152.5(3) . 8_655 ? Pb O4 Pb 71.29(15) 2_564 8_655 ? C O4 Pb 41.0(4) 6_556 7_564 ? Pb O4 Pb 80.15(17) 7_565 7_564 ? Pb O4 Pb 131.2(3) . 7_564 ? Pb O4 Pb 96.52(19) 2_564 7_564 ? Pb O4 Pb 63.54(11) 8_655 7_564 ? C O4 Pb 41.0(4) 6_556 1_554 ? Pb O4 Pb 131.2(3) 7_565 1_554 ? Pb O4 Pb 80.15(17) . 1_554 ? Pb O4 Pb 63.54(11) 2_564 1_554 ? Pb O4 Pb 96.52(19) 8_655 1_554 ? Pb O4 Pb 57.33(13) 7_564 1_554 ? S1 S2 Pb 82.76(11) 1_656 5_667 ? S1 S2 Pb 82.76(11) 1_656 3_647 ? Pb S2 Pb 91.08(9) 5_667 3_647 ? S1 S2 Pb 109.38(11) 1_656 3_646 ? Pb S2 Pb 167.76(11) 5_667 3_646 ? Pb S2 Pb 88.95(2) 3_647 3_646 ? S1 S2 Pb 109.38(11) 1_656 5_666 ? Pb S2 Pb 88.95(2) 5_667 5_666 ? Pb S2 Pb 167.76(11) 3_647 5_666 ? Pb S2 Pb 88.43(9) 3_646 5_666 ? S1 S2 Pb 147.66(9) 1_656 4_556 ? Pb S2 Pb 103.74(8) 5_667 4_556 ? Pb S2 Pb 65.67(4) 3_647 4_556 ? Pb S2 Pb 65.23(4) 3_646 4_556 ? Pb S2 Pb 102.45(7) 5_666 4_556 ? S1 S2 Pb 147.66(9) 1_656 6_657 ? Pb S2 Pb 65.67(4) 5_667 6_657 ? Pb S2 Pb 103.74(8) 3_647 6_657 ? Pb S2 Pb 102.45(7) 3_646 6_657 ? Pb S2 Pb 65.23(4) 5_666 6_657 ? Pb S2 Pb 54.12(4) 4_556 6_657 ? S1 S2 Pb 46.36(10) 1_656 1_655 ? Pb S2 Pb 90.52(4) 5_667 1_655 ? Pb S2 Pb 128.36(8) 3_647 1_655 ? Pb S2 Pb 99.05(8) 3_646 1_655 ? Pb S2 Pb 63.88(5) 5_666 1_655 ? Pb S2 Pb 160.40(9) 4_556 1_655 ? Pb S2 Pb 123.52(3) 6_657 1_655 ? S1 S2 Pb 46.36(10) 1_656 7_665 ? Pb S2 Pb 128.36(8) 5_667 7_665 ? Pb S2 Pb 90.52(4) 3_647 7_665 ? Pb S2 Pb 63.88(5) 3_646 7_665 ? Pb S2 Pb 99.05(8) 5_666 7_665 ? Pb S2 Pb 123.52(3) 4_556 7_665 ? Pb S2 Pb 160.40(9) 6_657 7_665 ? Pb S2 Pb 50.74(4) 1_655 7_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.690 _refine_diff_density_min -2.614 _refine_diff_density_rms 0.424