data_eclarite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag0.12 Bi12.76 Cu0.77 Fe0.45 Pb8.25 S28' _chemical_formula_weight 5360.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pmcn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 4.03070(10) _cell_length_b 22.7011(6) _cell_length_c 54.6145(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4997.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8893 _exptl_absorpt_coefficient_mu 74.087 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 34772 _diffrn_reflns_av_R_equivalents 0.1089 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 25.23 _reflns_number_total 4976 _reflns_number_gt 4141 _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^)+(0.0480P)^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 0.000008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4976 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.7500 0.14778(4) 0.070090(18) 0.0244(2) Uani 1 2 d S . . Bi2 Bi 0.7500 0.33131(4) 0.065868(18) 0.0245(2) Uani 1 2 d S . . Bi3 Bi 0.2500 0.22287(4) 0.125515(17) 0.0247(2) Uani 1 2 d S . . Bi4 Bi 0.2500 0.40900(4) 0.123206(18) 0.0251(2) Uani 1 2 d S . . Bi5 Bi 0.2500 0.03474(4) 0.244920(18) 0.0238(2) Uani 1 2 d S . . Bi6 Bi 0.2500 0.37471(4) 0.251522(18) 0.0252(2) Uani 1 2 d S . . Bi7 Bi 0.2500 0.27823(4) 0.316806(18) 0.0249(2) Uani 1 2 d S . . Bi8 Bi 0.7500 0.44231(4) 0.320094(17) 0.0235(2) Uani 1 2 d S . . ME2 Bi 0.2500 0.42113(4) 0.00591(2) 0.0305(3) Uani 1 2 d S . . ME3 Bi 0.7500 0.32724(5) 0.379705(19) 0.0305(3) Uani 1 2 d S . . ME4 Bi 0.7500 0.20482(4) 0.437853(18) 0.0247(2) Uani 1 2 d S . . ME5 Bi 0.2500 0.36761(4) 0.441339(19) 0.0278(2) Uani 1 2 d S . . Pb1 Pb 0.2500 0.23449(5) 0.00804(2) 0.0348(3) Uani 1 2 d S . . Pb2 Pb 0.7500 0.00411(5) 0.11604(2) 0.0369(3) Uani 1 2 d S . . Pb3 Pb 0.7500 0.11799(5) 0.17909(2) 0.0354(3) Uani 1 2 d S . . Pb4 Pb 0.7500 0.31548(5) 0.18457(2) 0.0355(3) Uani 1 2 d S . . Pb5 Pb 0.7500 0.20538(5) 0.24985(2) 0.0355(3) Uani 1 2 d S . . Pb6A Pb 0.2500 -0.0023(4) 0.3191(3) 0.0347(15) Uani 0.66(3) 2 d SP . . PB6B Bi 0.2500 0.0029(7) 0.3258(3) 0.0347(15) Uani 0.34(3) 2 d SP . . Pb7A Pb 0.2500 0.1385(5) 0.36909(5) 0.0413(12) Uani 0.83(3) 2 d SP . . PB7B Bi 0.2500 0.1187(15) 0.3691(3) 0.0413(12) Uani 0.17(3) 2 d SP . . Pb8A Pb 0.2500 0.0297(5) 0.42879(14) 0.0371(12) Uani 0.76(3) 2 d SP . . PB8B Bi 0.2500 0.0453(8) 0.4332(3) 0.0371(12) Uani 0.24(3) 2 d SP . . Cu Cu 0.7500 0.134(3) 0.3039(16) 0.032(8) Uani 0.55(9) 2 d SP . . Fe Fe 0.7500 0.144(4) 0.307(2) 0.032(8) Uani 0.45(9) 2 d SP . . Bi9 Bi 0.2500 0.04446(5) 0.02586(2) 0.0325(5) Uani 0.854(5) 2 d SP . . Cu1 Cu 0.2500 0.0828(9) 0.0112(4) 0.036(8) Uiso 0.179(14) 2 d SP . . Cu2 Cu 0.2500 -0.0022(12) 0.0457(5) 0.030(11) Uiso 0.113(12) 2 d SP . . S1 S 0.7500 0.1345(3) 0.02197(11) 0.0254(14) Uani 1 2 d S . . S2 S 0.7500 0.3242(3) 0.01839(11) 0.0238(14) Uani 1 2 d S . . S3 S 0.2500 0.0654(3) 0.07563(11) 0.0241(14) Uani 1 2 d S . . S4 S 0.2500 0.2393(3) 0.06419(12) 0.0256(14) Uani 1 2 d S . . S5 S 0.2500 0.4160(3) 0.06584(12) 0.0297(15) Uani 1 2 d S . . S6 S 0.7500 0.1412(3) 0.12451(11) 0.0222(13) Uani 1 2 d S . . S7 S 0.7500 0.3157(3) 0.12540(12) 0.0284(15) Uani 1 2 d S . . S8 S 0.7500 0.4908(3) 0.12326(12) 0.0271(15) Uani 1 2 d S . . S9 S 0.2500 0.0348(3) 0.15253(11) 0.0227(14) Uani 1 2 d S . . S10 S 0.2500 0.2180(3) 0.17193(11) 0.0244(14) Uani 1 2 d S . . S11 S 0.2500 0.4081(3) 0.17113(11) 0.0213(13) Uani 1 2 d S . . S12 S 0.2500 0.1330(3) 0.22145(11) 0.0205(13) Uani 1 2 d S . . S13 S 0.2500 0.2805(3) 0.22606(12) 0.0250(14) Uani 1 2 d S . . S14 S 0.7500 0.4170(3) 0.22461(11) 0.0214(13) Uani 1 2 d S . . S15 S 0.7500 0.0607(3) 0.27513(13) 0.0308(15) Uani 1 2 d S . . S16 S 0.2500 0.1819(3) 0.29259(12) 0.0235(14) Uani 1 2 d S . . S17 S 0.7500 0.3227(3) 0.28608(12) 0.0267(15) Uani 1 2 d S . . S18 S 0.2500 0.4882(3) 0.29170(12) 0.0252(14) Uani 1 2 d S . . S19 S 0.7500 0.0800(3) 0.33918(12) 0.0262(14) Uani 1 2 d S . . S20 S 0.7500 0.2303(3) 0.34716(13) 0.0307(16) Uani 1 2 d S . . S21 S 0.2500 0.3920(3) 0.35300(11) 0.0228(13) Uani 1 2 d S . . S22 S 0.7500 0.1033(3) 0.40848(11) 0.0247(14) Uani 1 2 d S . . S23 S 0.2500 0.2693(3) 0.40563(11) 0.0246(14) Uani 1 2 d S . . S24 S 0.7500 0.4190(3) 0.41180(13) 0.0303(15) Uani 1 2 d S . . S25 S 0.7500 0.0364(3) 0.47613(12) 0.0277(15) Uani 1 2 d S . . S26 S 0.2500 0.1636(3) 0.46463(13) 0.0295(15) Uani 1 2 d S . . S27 S 0.7500 0.3068(3) 0.46660(11) 0.0242(14) Uani 1 2 d S . . S28 S 0.2500 0.4629(3) 0.47310(12) 0.0308(15) 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 Bi1 0.0256(5) 0.0255(5) 0.0219(5) -0.0008(4) 0.000 0.000 Bi2 0.0258(5) 0.0259(5) 0.0218(5) 0.0006(4) 0.000 0.000 Bi3 0.0248(5) 0.0285(5) 0.0209(5) -0.0011(4) 0.000 0.000 Bi4 0.0241(5) 0.0290(5) 0.0221(5) -0.0010(4) 0.000 0.000 Bi5 0.0241(5) 0.0240(5) 0.0232(5) -0.0004(4) 0.000 0.000 Bi6 0.0260(5) 0.0245(5) 0.0251(5) -0.0015(4) 0.000 0.000 Bi7 0.0243(5) 0.0250(5) 0.0253(5) -0.0025(4) 0.000 0.000 Bi8 0.0238(5) 0.0241(5) 0.0226(5) 0.0006(4) 0.000 0.000 ME2 0.0228(5) 0.0344(6) 0.0344(6) 0.0001(5) 0.000 0.000 ME3 0.0301(5) 0.0351(6) 0.0263(6) 0.0001(5) 0.000 0.000 ME4 0.0239(5) 0.0269(5) 0.0233(5) 0.0026(4) 0.000 0.000 ME5 0.0261(5) 0.0284(6) 0.0290(6) 0.0012(4) 0.000 0.000 Pb1 0.0284(5) 0.0368(6) 0.0392(7) -0.0046(5) 0.000 0.000 Pb2 0.0292(6) 0.0491(7) 0.0325(6) 0.0040(5) 0.000 0.000 Pb3 0.0312(6) 0.0373(6) 0.0378(7) -0.0043(5) 0.000 0.000 Pb4 0.0296(6) 0.0329(6) 0.0440(7) 0.0045(5) 0.000 0.000 Pb5 0.0334(6) 0.0435(7) 0.0296(6) 0.0038(5) 0.000 0.000 Pb6A 0.0324(6) 0.0293(16) 0.042(5) -0.004(2) 0.000 0.000 PB6B 0.0324(6) 0.0293(16) 0.042(5) -0.004(2) 0.000 0.000 Pb7A 0.0467(7) 0.049(4) 0.0285(7) 0.0008(13) 0.000 0.000 PB7B 0.0467(7) 0.049(4) 0.0285(7) 0.0008(13) 0.000 0.000 Pb8A 0.0324(6) 0.039(3) 0.0402(19) 0.0055(19) 0.000 0.000 PB8B 0.0324(6) 0.039(3) 0.0402(19) 0.0055(19) 0.000 0.000 Cu 0.030(2) 0.03(2) 0.038(19) 0.007(12) 0.000 0.000 Fe 0.030(2) 0.03(2) 0.038(19) 0.007(12) 0.000 0.000 Bi9 0.0339(8) 0.0322(8) 0.0315(8) -0.0041(6) 0.000 0.000 S1 0.029(3) 0.031(4) 0.016(3) 0.003(3) 0.000 0.000 S2 0.025(3) 0.024(3) 0.022(3) 0.009(3) 0.000 0.000 S3 0.026(3) 0.025(3) 0.021(3) 0.001(3) 0.000 0.000 S4 0.023(3) 0.022(3) 0.032(4) 0.002(3) 0.000 0.000 S5 0.031(4) 0.029(4) 0.029(4) 0.003(3) 0.000 0.000 S6 0.023(3) 0.026(3) 0.018(3) 0.000(3) 0.000 0.000 S7 0.029(3) 0.024(3) 0.032(4) 0.000(3) 0.000 0.000 S8 0.025(3) 0.027(3) 0.029(4) 0.005(3) 0.000 0.000 S9 0.023(3) 0.021(3) 0.024(4) 0.002(3) 0.000 0.000 S10 0.027(3) 0.026(3) 0.020(3) -0.002(3) 0.000 0.000 S11 0.024(3) 0.021(3) 0.019(3) 0.000(3) 0.000 0.000 S12 0.020(3) 0.027(3) 0.014(3) 0.001(3) 0.000 0.000 S13 0.026(3) 0.025(3) 0.024(4) 0.002(3) 0.000 0.000 S14 0.023(3) 0.021(3) 0.020(3) 0.005(3) 0.000 0.000 S15 0.024(3) 0.039(4) 0.029(4) -0.001(3) 0.000 0.000 S16 0.024(3) 0.020(3) 0.027(4) -0.003(3) 0.000 0.000 S17 0.025(3) 0.034(4) 0.022(4) 0.003(3) 0.000 0.000 S18 0.020(3) 0.033(4) 0.023(4) 0.004(3) 0.000 0.000 S19 0.028(3) 0.030(4) 0.021(3) -0.005(3) 0.000 0.000 S20 0.026(3) 0.031(4) 0.035(4) 0.009(3) 0.000 0.000 S21 0.027(3) 0.024(3) 0.017(3) 0.000(3) 0.000 0.000 S22 0.023(3) 0.029(4) 0.022(3) 0.001(3) 0.000 0.000 S23 0.021(3) 0.030(4) 0.023(3) 0.003(3) 0.000 0.000 S24 0.028(3) 0.026(4) 0.037(4) 0.007(3) 0.000 0.000 S25 0.032(4) 0.027(4) 0.024(4) 0.002(3) 0.000 0.000 S26 0.022(3) 0.036(4) 0.031(4) 0.013(3) 0.000 0.000 S27 0.029(3) 0.023(3) 0.020(3) 0.000(3) 0.000 0.000 S28 0.037(4) 0.030(4) 0.025(4) -0.003(3) 0.000 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 Bi1 S1 2.645(6) . ? Bi1 S3 2.766(4) . ? Bi1 S3 2.766(4) 1_655 ? Bi1 S4 2.912(4) 1_655 ? Bi1 S4 2.912(4) . ? Bi1 S6 2.976(6) . ? Bi2 S2 2.598(6) . ? Bi2 S5 2.785(5) 1_655 ? Bi2 S5 2.785(5) . ? Bi2 S4 2.904(4) . ? Bi2 S4 2.904(4) 1_655 ? Bi3 S10 2.537(6) . ? Bi3 S6 2.740(4) 1_455 ? Bi3 S6 2.740(4) . ? Bi3 S7 2.916(5) . ? Bi3 S7 2.916(5) 1_455 ? Bi4 S11 2.617(6) . ? Bi4 S8 2.740(4) . ? Bi4 S8 2.740(4) 1_455 ? Bi4 S7 2.926(5) 1_455 ? Bi4 S7 2.926(5) . ? Bi4 S5 3.137(7) . ? Bi5 S12 2.573(6) . ? Bi5 S15 2.670(5) . ? Bi5 S15 2.670(5) 1_455 ? Bi5 S18 3.029(5) 2_545 ? Bi5 S18 3.029(5) 2_645 ? Bi6 S13 2.551(6) . ? Bi6 S14 2.673(4) . ? Bi6 S14 2.673(4) 1_455 ? Bi6 S17 3.003(5) 1_455 ? Bi6 S17 3.003(5) . ? Bi7 S16 2.556(6) . ? Bi7 S17 2.810(4) . ? Bi7 S17 2.810(4) 1_455 ? Bi7 S20 2.827(5) 1_455 ? Bi7 S20 2.827(5) . ? Bi8 S9 2.577(6) 2_655 ? Bi8 S18 2.748(4) . ? Bi8 S18 2.748(4) 1_655 ? Bi8 S21 2.932(4) 1_655 ? Bi8 S21 2.932(4) . ? ME2 S25 2.763(5) 6_465 ? ME2 S25 2.763(5) 6_565 ? ME2 S25 2.794(6) 2_655 ? ME2 S26 2.963(6) 6_565 ? ME2 S2 3.061(5) 1_455 ? ME2 S2 3.061(5) . ? ME3 S24 2.722(7) . ? ME3 S23 2.792(4) 1_655 ? ME3 S23 2.792(4) . ? ME3 S20 2.829(7) . ? ME3 S21 2.889(4) . ? ME3 S21 2.889(4) 1_655 ? ME4 S26 2.660(4) 1_655 ? ME4 S26 2.660(4) . ? ME4 S27 2.798(6) . ? ME4 S22 2.807(6) . ? ME4 S23 3.050(5) . ? ME4 S23 3.050(5) 1_655 ? ME5 S28 2.773(7) . ? ME5 S27 2.805(4) 1_455 ? ME5 S27 2.805(4) . ? ME5 S24 2.833(5) . ? ME5 S24 2.833(5) 1_455 ? ME5 S23 2.964(7) . ? Pb1 S2 2.920(5) . ? Pb1 S2 2.920(5) 1_455 ? Pb1 S4 3.069(7) . ? Pb1 S1 3.130(5) 1_455 ? Pb1 S1 3.130(5) . ? Pb2 S9 2.918(5) 1_655 ? Pb2 S9 2.918(5) . ? Pb2 S21 3.056(6) 2_645 ? Pb3 S6 3.027(6) . ? Pb3 S10 3.061(5) 1_655 ? Pb3 S10 3.061(5) . ? Pb3 S12 3.087(5) 1_655 ? Pb3 S12 3.087(5) . ? Pb3 S9 3.120(5) . ? Pb3 S9 3.120(5) 1_655 ? Pb4 S11 3.003(4) 1_655 ? Pb4 S11 3.003(4) . ? Pb4 S10 3.071(5) . ? Pb4 S10 3.071(5) 1_655 ? Pb5 S13 2.942(5) . ? Pb5 S13 2.942(5) 1_655 ? Pb5 S12 3.027(4) . ? Pb5 S12 3.027(4) 1_655 ? Pb5 S16 3.130(5) 1_655 ? Pb5 S16 3.130(5) . ? Pb5 Cu 3.36(9) . ? Pb6A S11 2.914(7) 2_545 ? Pb6A S11 2.914(7) 2_645 ? Pb6A S14 3.009(16) 2_645 ? Pb6A S19 2.958(10) . ? Pb6A S19 2.958(10) 1_455 ? PB6B S19 2.767(11) . ? PB6B S19 2.767(11) 1_455 ? PB6B S8 2.796(16) 2_645 ? PB6B S11 2.954(13) 2_545 ? PB6B S11 2.954(13) 2_645 ? PB6B PB7B 3.54(3) . ? Pb7A PB7B 0.45(2) . ? Pb7A S19 2.915(7) 1_455 ? Pb7A S19 2.915(7) . ? Pb7A S22 3.054(6) 1_455 ? Pb7A S22 3.054(6) . ? PB7B S19 2.742(16) 1_455 ? PB7B S19 2.742(16) . ? PB7B S8 2.93(3) 2_645 ? PB7B S22 2.966(14) 1_455 ? PB7B S22 2.966(14) . ? Pb8A S22 2.843(6) . ? Pb8A S22 2.843(6) 1_455 ? Pb8A S8 2.977(12) 2_645 ? PB8B S22 2.760(11) . ? PB8B S22 2.760(11) 1_455 ? PB8B S25 3.100(14) 1_455 ? PB8B S25 3.100(14) . ? Cu S15 2.29(7) . ? Cu S19 2.29(9) . ? Cu S16 2.37(4) . ? Cu S16 2.37(4) 1_655 ? Fe S15 2.56(8) . ? Fe S19 2.28(14) . ? Fe S16 2.33(7) . ? Fe S16 2.33(7) 1_655 ? Bi9 Cu1 1.18(2) . ? Bi9 Cu2 1.52(3) . ? Bi9 S28 2.738(4) 2_545 ? Bi9 S28 2.738(4) 2_645 ? Bi9 S3 2.760(6) . ? Bi9 S28 2.886(7) 6_565 ? Bi9 S1 2.878(5) . ? Bi9 S1 2.878(5) 1_455 ? Cu1 S28 2.32(2) 6_565 ? Cu1 S1 2.405(11) . ? Cu1 S1 2.405(11) 1_455 ? Cu1 Cu2 2.70(4) . ? Cu2 S3 2.24(3) . ? Cu2 S28 2.397(16) 2_545 ? Cu2 S28 2.397(16) 2_645 ? S1 Cu1 2.405(11) 1_655 ? S1 Bi9 2.878(5) 1_655 ? S1 Pb1 3.130(5) 1_655 ? S2 Pb1 2.920(5) 1_655 ? S2 ME2 3.061(5) 1_655 ? S3 Bi1 2.766(4) 1_455 ? S4 Bi2 2.904(4) 1_455 ? S4 Bi1 2.912(4) 1_455 ? S5 Bi2 2.785(5) 1_455 ? S6 Bi3 2.740(4) 1_655 ? S7 Bi3 2.916(5) 1_655 ? S7 Bi4 2.926(5) 1_655 ? S8 Bi4 2.740(4) 1_655 ? S8 PB7B 2.93(3) 2_655 ? S8 PB6B 2.796(16) 2_655 ? S8 Pb8A 2.977(12) 2_655 ? S9 Bi8 2.577(6) 2_645 ? S9 Pb2 2.918(5) 1_455 ? S9 Pb3 3.120(5) 1_455 ? S10 Pb3 3.061(5) 1_455 ? S10 Pb4 3.071(5) 1_455 ? S11 Pb6A 2.914(7) 2_655 ? S11 Pb6A 2.914(7) 2 ? S11 PB6B 2.954(13) 2_655 ? S11 PB6B 2.954(13) 2 ? S11 Pb4 3.003(4) 1_455 ? S12 Pb5 3.027(4) 1_455 ? S12 Pb3 3.087(5) 1_455 ? S13 Pb5 2.942(5) 1_455 ? S14 Bi6 2.673(4) 1_655 ? S14 Pb6A 3.009(16) 2_655 ? S15 Bi5 2.670(5) 1_655 ? S16 Fe 2.33(7) 1_455 ? S16 Cu 2.37(4) 1_455 ? S16 Pb5 3.130(5) 1_455 ? S17 Bi7 2.810(4) 1_655 ? S17 Bi6 3.003(5) 1_655 ? S18 Bi8 2.748(4) 1_455 ? S18 Bi5 3.029(5) 2 ? S18 Bi5 3.029(5) 2_655 ? S19 PB7B 2.742(16) 1_655 ? S19 PB6B 2.767(11) 1_655 ? S19 Pb7A 2.915(7) 1_655 ? S19 Pb6A 2.958(10) 1_655 ? S20 Bi7 2.827(5) 1_655 ? S21 ME3 2.889(4) 1_455 ? S21 Bi8 2.932(4) 1_455 ? S21 Pb2 3.056(6) 2_655 ? S22 PB8B 2.760(11) 1_655 ? S22 Pb8A 2.843(6) 1_655 ? S22 PB7B 2.966(15) 1_655 ? S22 Pb7A 3.054(6) 1_655 ? S23 ME3 2.792(4) 1_455 ? S23 ME4 3.050(5) 1_455 ? S24 ME5 2.833(5) 1_655 ? S25 ME2 2.763(5) 6_666 ? S25 ME2 2.763(5) 6_566 ? S25 ME2 2.794(6) 2_645 ? S25 PB8B 3.100(14) 1_655 ? S26 ME4 2.660(4) 1_455 ? S26 ME2 2.963(6) 6_566 ? S27 ME5 2.805(4) 1_655 ? S28 Cu1 2.32(2) 6_566 ? S28 Cu2 2.397(16) 2 ? S28 Cu2 2.397(16) 2_655 ? S28 Bi9 2.738(4) 2_655 ? S28 Bi9 2.738(4) 2 ? S28 Bi9 2.886(7) 6_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Bi1 S3 91.81(16) . . ? S1 Bi1 S3 91.81(16) . 1_655 ? S3 Bi1 S3 93.55(19) . 1_655 ? S1 Bi1 S4 88.37(16) . 1_655 ? S3 Bi1 S4 177.00(13) . 1_655 ? S3 Bi1 S4 89.43(12) 1_655 1_655 ? S1 Bi1 S4 88.37(16) . . ? S3 Bi1 S4 89.43(12) . . ? S3 Bi1 S4 177.00(13) 1_655 . ? S4 Bi1 S4 87.58(17) 1_655 . ? S1 Bi1 S6 170.56(18) . . ? S3 Bi1 S6 81.76(15) . . ? S3 Bi1 S6 81.76(15) 1_655 . ? S4 Bi1 S6 98.42(16) 1_655 . ? S4 Bi1 S6 98.42(16) . . ? S2 Bi2 S5 92.43(17) . 1_655 ? S2 Bi2 S5 92.43(17) . . ? S5 Bi2 S5 92.7(2) 1_655 . ? S2 Bi2 S4 85.63(16) . . ? S5 Bi2 S4 177.00(17) 1_655 . ? S5 Bi2 S4 89.68(13) . . ? S2 Bi2 S4 85.63(16) . 1_655 ? S5 Bi2 S4 89.68(13) 1_655 1_655 ? S5 Bi2 S4 177.00(17) . 1_655 ? S4 Bi2 S4 87.89(17) . 1_655 ? S10 Bi3 S6 89.47(16) . 1_455 ? S10 Bi3 S6 89.47(16) . . ? S6 Bi3 S6 94.72(19) 1_455 . ? S10 Bi3 S7 91.92(17) . . ? S6 Bi3 S7 176.13(14) 1_455 . ? S6 Bi3 S7 88.90(13) . . ? S10 Bi3 S7 91.92(17) . 1_455 ? S6 Bi3 S7 88.90(13) 1_455 1_455 ? S6 Bi3 S7 176.13(14) . 1_455 ? S7 Bi3 S7 87.44(17) . 1_455 ? S11 Bi4 S8 90.25(17) . . ? S11 Bi4 S8 90.25(17) . 1_455 ? S8 Bi4 S8 94.7(2) . 1_455 ? S11 Bi4 S7 87.31(16) . 1_455 ? S8 Bi4 S7 175.53(16) . 1_455 ? S8 Bi4 S7 89.07(13) 1_455 1_455 ? S11 Bi4 S7 87.31(16) . . ? S8 Bi4 S7 89.07(13) . . ? S8 Bi4 S7 175.53(16) 1_455 . ? S7 Bi4 S7 87.07(17) 1_455 . ? S11 Bi4 S5 177.56(18) . . ? S8 Bi4 S5 88.09(16) . . ? S8 Bi4 S5 88.09(16) 1_455 . ? S7 Bi4 S5 94.45(16) 1_455 . ? S7 Bi4 S5 94.45(16) . . ? S12 Bi5 S15 96.71(18) . . ? S12 Bi5 S15 96.71(18) . 1_455 ? S15 Bi5 S15 98.0(2) . 1_455 ? S12 Bi5 S18 88.47(16) . 2_545 ? S15 Bi5 S18 170.71(16) . 2_545 ? S15 Bi5 S18 89.00(14) 1_455 2_545 ? S12 Bi5 S18 88.47(16) . 2_645 ? S15 Bi5 S18 89.00(14) . 2_645 ? S15 Bi5 S18 170.71(16) 1_455 2_645 ? S18 Bi5 S18 83.41(16) 2_545 2_645 ? S13 Bi6 S14 90.08(16) . . ? S13 Bi6 S14 90.08(16) . 1_455 ? S14 Bi6 S14 97.89(19) . 1_455 ? S13 Bi6 S17 90.75(16) . 1_455 ? S14 Bi6 S17 173.17(13) . 1_455 ? S14 Bi6 S17 88.89(13) 1_455 1_455 ? S13 Bi6 S17 90.75(16) . . ? S14 Bi6 S17 88.89(13) . . ? S14 Bi6 S17 173.17(13) 1_455 . ? S17 Bi6 S17 84.32(16) 1_455 . ? S16 Bi7 S17 89.93(17) . . ? S16 Bi7 S17 89.93(17) . 1_455 ? S17 Bi7 S17 91.63(19) . 1_455 ? S16 Bi7 S20 88.51(18) . 1_455 ? S17 Bi7 S20 178.4(2) . 1_455 ? S17 Bi7 S20 88.70(13) 1_455 1_455 ? S16 Bi7 S20 88.51(18) . . ? S17 Bi7 S20 88.70(13) . . ? S17 Bi7 S20 178.4(2) 1_455 . ? S20 Bi7 S20 90.94(19) 1_455 . ? S9 Bi8 S18 91.06(17) 2_655 . ? S9 Bi8 S18 91.06(17) 2_655 1_655 ? S18 Bi8 S18 94.3(2) . 1_655 ? S9 Bi8 S21 87.81(16) 2_655 1_655 ? S18 Bi8 S21 176.12(13) . 1_655 ? S18 Bi8 S21 89.41(13) 1_655 1_655 ? S9 Bi8 S21 87.81(16) 2_655 . ? S18 Bi8 S21 89.41(13) . . ? S18 Bi8 S21 176.12(13) 1_655 . ? S21 Bi8 S21 86.84(17) 1_655 . ? S25 ME2 S25 93.7(2) 6_465 6_565 ? S25 ME2 S25 83.09(17) 6_465 2_655 ? S25 ME2 S25 83.09(17) 6_565 2_655 ? S25 ME2 S26 77.23(16) 6_465 6_565 ? S25 ME2 S26 77.23(16) 6_565 6_565 ? S25 ME2 S26 151.0(2) 2_655 6_565 ? S25 ME2 S2 84.36(14) 6_465 1_455 ? S25 ME2 S2 149.56(18) 6_565 1_455 ? S25 ME2 S2 126.52(14) 2_655 1_455 ? S26 ME2 S2 72.70(15) 6_565 1_455 ? S25 ME2 S2 149.56(18) 6_465 . ? S25 ME2 S2 84.36(14) 6_565 . ? S25 ME2 S2 126.52(14) 2_655 . ? S26 ME2 S2 72.70(15) 6_565 . ? S2 ME2 S2 82.36(15) 1_455 . ? S24 ME3 S23 91.95(17) . 1_655 ? S24 ME3 S23 91.95(17) . . ? S23 ME3 S23 92.40(19) 1_655 . ? S24 ME3 S20 178.85(19) . . ? S23 ME3 S20 87.25(16) 1_655 . ? S23 ME3 S20 87.25(16) . . ? S24 ME3 S21 86.32(16) . . ? S23 ME3 S21 177.44(15) 1_655 . ? S23 ME3 S21 89.55(13) . . ? S20 ME3 S21 94.50(16) . . ? S24 ME3 S21 86.32(16) . 1_655 ? S23 ME3 S21 89.55(13) 1_655 1_655 ? S23 ME3 S21 177.44(15) . 1_655 ? S20 ME3 S21 94.50(16) . 1_655 ? S21 ME3 S21 88.45(17) . 1_655 ? S26 ME4 S26 98.5(2) 1_655 . ? S26 ME4 S27 89.00(18) 1_655 . ? S26 ME4 S27 89.00(18) . . ? S26 ME4 S22 91.46(18) 1_655 . ? S26 ME4 S22 91.46(18) . . ? S27 ME4 S22 179.29(18) . . ? S26 ME4 S23 170.66(16) 1_655 . ? S26 ME4 S23 89.16(13) . . ? S27 ME4 S23 85.80(15) . . ? S22 ME4 S23 93.67(16) . . ? S26 ME4 S23 89.16(13) 1_655 1_655 ? S26 ME4 S23 170.66(16) . 1_655 ? S27 ME4 S23 85.80(15) . 1_655 ? S22 ME4 S23 93.67(16) . 1_655 ? S23 ME4 S23 82.73(16) . 1_655 ? S28 ME5 S27 94.36(16) . 1_455 ? S28 ME5 S27 94.36(16) . . ? S27 ME5 S27 91.85(18) 1_455 . ? S28 ME5 S24 92.01(17) . . ? S27 ME5 S24 173.6(2) 1_455 . ? S27 ME5 S24 88.37(13) . . ? S28 ME5 S24 92.01(17) . 1_455 ? S27 ME5 S24 88.37(13) 1_455 1_455 ? S27 ME5 S24 173.6(2) . 1_455 ? S24 ME5 S24 90.70(19) . 1_455 ? S28 ME5 S23 177.59(19) . . ? S27 ME5 S23 87.31(15) 1_455 . ? S27 ME5 S23 87.31(15) . . ? S24 ME5 S23 86.30(17) . . ? S24 ME5 S23 86.30(17) 1_455 . ? S2 Pb1 S2 87.28(17) . 1_455 ? S2 Pb1 S4 77.40(15) . . ? S2 Pb1 S4 77.40(15) 1_455 . ? S2 Pb1 S1 154.58(17) . 1_455 ? S2 Pb1 S1 90.83(12) 1_455 1_455 ? S4 Pb1 S1 77.45(14) . 1_455 ? S2 Pb1 S1 90.83(12) . . ? S2 Pb1 S1 154.58(17) 1_455 . ? S4 Pb1 S1 77.45(14) . . ? S1 Pb1 S1 80.17(15) 1_455 . ? S9 Pb2 S9 87.35(17) 1_655 . ? S9 Pb2 S21 79.68(15) 1_655 2_645 ? S9 Pb2 S21 79.68(15) . 2_645 ? S6 Pb3 S10 75.23(14) . 1_655 ? S6 Pb3 S10 75.23(14) . . ? S10 Pb3 S10 82.34(16) 1_655 . ? S6 Pb3 S12 135.95(9) . 1_655 ? S10 Pb3 S12 65.42(15) 1_655 1_655 ? S10 Pb3 S12 116.34(15) . 1_655 ? S6 Pb3 S12 135.95(9) . . ? S10 Pb3 S12 116.34(15) 1_655 . ? S10 Pb3 S12 65.42(15) . . ? S12 Pb3 S12 81.52(14) 1_655 . ? S6 Pb3 S9 69.34(14) . . ? S10 Pb3 S9 144.57(16) 1_655 . ? S10 Pb3 S9 87.96(12) . . ? S12 Pb3 S9 146.83(16) 1_655 . ? S12 Pb3 S9 89.64(12) . . ? S6 Pb3 S9 69.34(14) . 1_655 ? S10 Pb3 S9 87.96(13) 1_655 1_655 ? S10 Pb3 S9 144.57(16) . 1_655 ? S12 Pb3 S9 89.64(12) 1_655 1_655 ? S12 Pb3 S9 146.83(16) . 1_655 ? S9 Pb3 S9 80.47(15) . 1_655 ? S11 Pb4 S11 84.31(15) 1_655 . ? S11 Pb4 S10 152.83(17) 1_655 . ? S11 Pb4 S10 90.50(12) . . ? S11 Pb4 S10 90.50(12) 1_655 1_655 ? S11 Pb4 S10 152.83(17) . 1_655 ? S10 Pb4 S10 82.03(15) . 1_655 ? S13 Pb5 S13 86.47(17) . 1_655 ? S13 Pb5 S12 68.42(15) . . ? S13 Pb5 S12 122.97(16) 1_655 . ? S13 Pb5 S12 122.97(16) . 1_655 ? S13 Pb5 S12 68.42(15) 1_655 1_655 ? S12 Pb5 S12 83.47(15) . 1_655 ? S13 Pb5 S16 150.37(17) . 1_655 ? S13 Pb5 S16 89.26(13) 1_655 1_655 ? S12 Pb5 S16 135.90(15) . 1_655 ? S12 Pb5 S16 82.00(13) 1_655 1_655 ? S13 Pb5 S16 89.26(13) . . ? S13 Pb5 S16 150.37(17) 1_655 . ? S12 Pb5 S16 82.00(13) . . ? S12 Pb5 S16 135.90(15) 1_655 . ? S16 Pb5 S16 80.16(16) 1_655 . ? S13 Pb5 Cu 131.7(5) . . ? S13 Pb5 Cu 131.7(5) 1_655 . ? S12 Pb5 Cu 100.9(9) . . ? S12 Pb5 Cu 100.9(9) 1_655 . ? S16 Pb5 Cu 42.6(4) 1_655 . ? S16 Pb5 Cu 42.6(4) . . ? S11 Pb6A S11 87.5(3) 2_545 2_645 ? S11 Pb6A S14 73.7(3) 2_545 2_645 ? S11 Pb6A S14 73.7(3) 2_645 2_645 ? S11 Pb6A S19 147.6(6) 2_545 . ? S11 Pb6A S19 84.3(2) 2_645 . ? S14 Pb6A S19 132.7(3) 2_645 . ? S11 Pb6A S19 84.3(2) 2_545 1_455 ? S11 Pb6A S19 147.6(6) 2_645 1_455 ? S14 Pb6A S19 132.7(3) 2_645 1_455 ? S19 Pb6A S19 85.9(4) . 1_455 ? S19 PB6B S19 93.5(5) . 1_455 ? S19 PB6B S8 78.4(4) . 2_645 ? S19 PB6B S8 78.4(4) 1_455 2_645 ? S19 PB6B S11 160.5(6) . 2_545 ? S19 PB6B S11 87.07(17) 1_455 2_545 ? S8 PB6B S11 82.6(4) 2_645 2_545 ? S19 PB6B S11 87.07(17) . 2_645 ? S19 PB6B S11 160.5(6) 1_455 2_645 ? S8 PB6B S11 82.6(4) 2_645 2_645 ? S11 PB6B S11 86.0(5) 2_545 2_645 ? S19 PB6B PB7B 49.7(3) . . ? S19 PB6B PB7B 49.7(3) 1_455 . ? S8 PB6B PB7B 53.7(5) 2_645 . ? S11 PB6B PB7B 120.2(4) 2_545 . ? S11 PB6B PB7B 120.2(4) 2_645 . ? PB7B Pb7A S19 63.1(17) . 1_455 ? PB7B Pb7A S19 63.1(17) . . ? S19 Pb7A S19 87.5(3) 1_455 . ? PB7B Pb7A S22 74.6(19) . 1_455 ? S19 Pb7A S22 79.6(2) 1_455 1_455 ? S19 Pb7A S22 137.0(5) . 1_455 ? PB7B Pb7A S22 74.6(19) . . ? S19 Pb7A S22 137.0(5) 1_455 . ? S19 Pb7A S22 79.6(2) . . ? S22 Pb7A S22 82.6(2) 1_455 . ? Pb7A PB7B S19 108.5(19) . 1_455 ? Pb7A PB7B S19 108.5(19) . . ? S19 PB7B S19 94.6(7) 1_455 . ? Pb7A PB7B S8 172(3) . 2_645 ? S19 PB7B S8 76.5(8) 1_455 2_645 ? S19 PB7B S8 76.5(8) . 2_645 ? Pb7A PB7B S22 97(2) . 1_455 ? S19 PB7B S22 84.0(3) 1_455 1_455 ? S19 PB7B S22 153.4(13) . 1_455 ? S8 PB7B S22 77.4(7) 2_645 1_455 ? Pb7A PB7B S22 97(2) . . ? S19 PB7B S22 153.4(13) 1_455 . ? S19 PB7B S22 84.0(3) . . ? S8 PB7B S22 77.4(7) 2_645 . ? S22 PB7B S22 85.6(5) 1_455 . ? Pb7A PB7B PB6B 138(3) . . ? S19 PB7B PB6B 50.3(5) 1_455 . ? S19 PB7B PB6B 50.3(5) . . ? S8 PB7B PB6B 50.1(6) 2_645 . ? S22 PB7B PB6B 113.4(8) 1_455 . ? S22 PB7B PB6B 113.4(8) . . ? S22 Pb8A S22 90.3(3) . 1_455 ? S22 Pb8A S8 78.6(2) . 2_645 ? S22 Pb8A S8 78.6(2) 1_455 2_645 ? S22 PB8B S22 93.8(5) . 1_455 ? S22 PB8B S25 151.1(8) . 1_455 ? S22 PB8B S25 85.8(2) 1_455 1_455 ? S22 PB8B S25 85.8(2) . . ? S22 PB8B S25 151.1(8) 1_455 . ? S25 PB8B S25 81.1(4) 1_455 . ? S15 Cu S19 101(3) . . ? S15 Cu S16 99(2) . . ? S19 Cu S16 118(2) . . ? S15 Cu S16 99(2) . 1_655 ? S19 Cu S16 118(2) . 1_655 ? S16 Cu S16 117(4) . 1_655 ? S15 Cu Pb5 76(2) . . ? S19 Cu Pb5 176(3) . . ? S16 Cu Pb5 63(2) . . ? S16 Cu Pb5 63(2) 1_655 . ? S15 Fe S19 93(3) . . ? S15 Fe S16 93(3) . . ? S19 Fe S16 120(3) . . ? S15 Fe S16 93(3) . 1_655 ? S19 Fe S16 120(3) . 1_655 ? S16 Fe S16 120(6) . 1_655 ? Cu1 Bi9 Cu2 177.0(14) . . ? Cu1 Bi9 S28 120.8(5) . 2_545 ? Cu2 Bi9 S28 60.8(6) . 2_545 ? Cu1 Bi9 S28 120.8(5) . 2_645 ? Cu2 Bi9 S28 60.8(6) . 2_645 ? S28 Bi9 S28 94.8(2) 2_545 2_645 ? Cu1 Bi9 S3 122.7(10) . . ? Cu2 Bi9 S3 54.3(11) . . ? S28 Bi9 S3 95.52(17) 2_545 . ? S28 Bi9 S3 95.52(17) 2_645 . ? Cu1 Bi9 S28 50.7(10) . 6_565 ? Cu2 Bi9 S28 132.3(11) . 6_565 ? S28 Bi9 S28 88.94(17) 2_545 6_565 ? S28 Bi9 S28 88.94(17) 2_645 6_565 ? S3 Bi9 S28 173.39(19) . 6_565 ? Cu1 Bi9 S1 55.1(5) . . ? Cu2 Bi9 S1 123.3(6) . . ? S28 Bi9 S1 175.86(17) 2_545 . ? S28 Bi9 S1 88.07(13) 2_645 . ? S3 Bi9 S1 87.15(16) . . ? S28 Bi9 S1 88.13(15) 6_565 . ? Cu1 Bi9 S1 55.1(5) . 1_455 ? Cu2 Bi9 S1 123.3(6) . 1_455 ? S28 Bi9 S1 88.07(13) 2_545 1_455 ? S28 Bi9 S1 175.86(17) 2_645 1_455 ? S3 Bi9 S1 87.15(16) . 1_455 ? S28 Bi9 S1 88.13(15) 6_565 1_455 ? S1 Bi9 S1 88.90(18) . 1_455 ? Bi9 Cu1 S28 106.2(12) . 6_565 ? Bi9 Cu1 S1 101.1(8) . . ? S28 Cu1 S1 115.9(5) 6_565 . ? Bi9 Cu1 S1 101.1(8) . 1_455 ? S28 Cu1 S1 115.9(5) 6_565 1_455 ? S1 Cu1 S1 113.8(8) . 1_455 ? Bi9 Cu1 Cu2 1.7(8) . . ? S28 Cu1 Cu2 107.9(10) 6_565 . ? S1 Cu1 Cu2 100.3(7) . . ? S1 Cu1 Cu2 100.3(7) 1_455 . ? Bi9 Cu2 S3 92.4(13) . . ? Bi9 Cu2 S28 85.7(9) . 2_545 ? S3 Cu2 S28 122.6(6) . 2_545 ? Bi9 Cu2 S28 85.7(9) . 2_645 ? S3 Cu2 S28 122.6(6) . 2_645 ? S28 Cu2 S28 114.4(12) 2_545 2_645 ? Bi9 Cu2 Cu1 1.3(6) . . ? S3 Cu2 Cu1 91.1(10) . . ? S28 Cu2 Cu1 86.4(8) 2_545 . ? S28 Cu2 Cu1 86.4(8) 2_645 . ? Cu1 S1 Cu1 113.8(8) . 1_655 ? Cu1 S1 Bi1 107.4(5) . . ? Cu1 S1 Bi1 107.4(5) 1_655 . ? Cu1 S1 Bi9 23.8(5) . . ? Cu1 S1 Bi9 105.0(5) 1_655 . ? Bi1 S1 Bi9 90.44(16) . . ? Cu1 S1 Bi9 105.0(5) . 1_655 ? Cu1 S1 Bi9 23.8(5) 1_655 1_655 ? Bi1 S1 Bi9 90.44(16) . 1_655 ? Bi9 S1 Bi9 88.90(18) . 1_655 ? Cu1 S1 Pb1 146.5(5) . 1_655 ? Cu1 S1 Pb1 75.8(4) 1_655 1_655 ? Bi1 S1 Pb1 99.14(17) . 1_655 ? Bi9 S1 Pb1 169.7(2) . 1_655 ? Bi9 S1 Pb1 94.71(3) 1_655 1_655 ? Cu1 S1 Pb1 75.8(4) . . ? Cu1 S1 Pb1 146.5(5) 1_655 . ? Bi1 S1 Pb1 99.14(17) . . ? Bi9 S1 Pb1 94.71(3) . . ? Bi9 S1 Pb1 169.7(2) 1_655 . ? Pb1 S1 Pb1 80.17(15) 1_655 . ? Bi2 S2 Pb1 103.68(16) . . ? Bi2 S2 Pb1 103.68(16) . 1_655 ? Pb1 S2 Pb1 87.28(17) . 1_655 ? Bi2 S2 ME2 100.23(17) . 1_655 ? Pb1 S2 ME2 155.9(2) . 1_655 ? Pb1 S2 ME2 90.22(5) 1_655 1_655 ? Bi2 S2 ME2 100.23(17) . . ? Pb1 S2 ME2 90.22(5) . . ? Pb1 S2 ME2 155.9(2) 1_655 . ? ME2 S2 ME2 82.36(15) 1_655 . ? Cu2 S3 Bi1 112.5(5) . . ? Cu2 S3 Bi1 112.5(5) . 1_455 ? Bi1 S3 Bi1 93.55(19) . 1_455 ? Cu2 S3 Bi9 33.3(7) . . ? Bi1 S3 Bi9 90.50(16) . . ? Bi1 S3 Bi9 90.50(16) 1_455 . ? Bi2 S4 Bi2 87.89(17) . 1_455 ? Bi2 S4 Bi1 171.8(3) . 1_455 ? Bi2 S4 Bi1 91.69(3) 1_455 1_455 ? Bi2 S4 Bi1 91.69(3) . . ? Bi2 S4 Bi1 171.8(3) 1_455 . ? Bi1 S4 Bi1 87.58(17) 1_455 . ? Bi2 S4 Pb1 93.27(16) . . ? Bi2 S4 Pb1 93.27(16) 1_455 . ? Bi1 S4 Pb1 94.89(16) 1_455 . ? Bi1 S4 Pb1 94.89(16) . . ? Bi2 S5 Bi2 92.7(2) 1_455 . ? Bi2 S5 Bi4 87.96(16) 1_455 . ? Bi2 S5 Bi4 87.96(16) . . ? Bi3 S6 Bi3 94.72(19) 1_655 . ? Bi3 S6 Bi1 89.19(15) 1_655 . ? Bi3 S6 Bi1 89.19(15) . . ? Bi3 S6 Pb3 95.62(15) 1_655 . ? Bi3 S6 Pb3 95.62(15) . . ? Bi1 S6 Pb3 172.9(2) . . ? Bi3 S7 Bi3 87.44(17) . 1_655 ? Bi3 S7 Bi4 177.8(3) . 1_655 ? Bi3 S7 Bi4 92.702(19) 1_655 1_655 ? Bi3 S7 Bi4 92.702(19) . . ? Bi3 S7 Bi4 177.8(3) 1_655 . ? Bi4 S7 Bi4 87.07(17) 1_655 . ? Bi4 S8 Bi4 94.7(2) . 1_655 ? Bi4 S8 PB7B 132.13(12) . 2_655 ? Bi4 S8 PB7B 132.13(12) 1_655 2_655 ? Bi4 S8 PB6B 93.9(3) . 2_655 ? Bi4 S8 PB6B 93.9(3) 1_655 2_655 ? PB7B S8 PB6B 76.2(5) 2_655 2_655 ? Bi4 S8 Pb8A 101.5(2) . 2_655 ? Bi4 S8 Pb8A 101.5(2) 1_655 2_655 ? PB7B S8 Pb8A 80.8(4) 2_655 2_655 ? PB6B S8 Pb8A 157.1(5) 2_655 2_655 ? Bi8 S9 Pb2 101.65(16) 2_645 1_455 ? Bi8 S9 Pb2 101.65(16) 2_645 . ? Pb2 S9 Pb2 87.35(17) 1_455 . ? Bi8 S9 Pb3 102.90(17) 2_645 . ? Pb2 S9 Pb3 155.2(2) 1_455 . ? Pb2 S9 Pb3 90.91(6) . . ? Bi8 S9 Pb3 102.90(17) 2_645 1_455 ? Pb2 S9 Pb3 90.91(6) 1_455 1_455 ? Pb2 S9 Pb3 155.2(2) . 1_455 ? Pb3 S9 Pb3 80.47(15) . 1_455 ? Bi3 S10 Pb3 99.20(17) . 1_455 ? Bi3 S10 Pb3 99.20(17) . . ? Pb3 S10 Pb3 82.34(16) 1_455 . ? Bi3 S10 Pb4 101.15(17) . . ? Pb3 S10 Pb4 159.6(2) 1_455 . ? Pb3 S10 Pb4 94.22(5) . . ? Bi3 S10 Pb4 101.15(17) . 1_455 ? Pb3 S10 Pb4 94.22(5) 1_455 1_455 ? Pb3 S10 Pb4 159.6(2) . 1_455 ? Pb4 S10 Pb4 82.03(15) . 1_455 ? Bi4 S11 Pb6A 100.2(3) . 2_655 ? Bi4 S11 Pb6A 100.2(3) . 2 ? Pb6A S11 Pb6A 87.5(3) 2_655 2 ? Bi4 S11 PB6B 92.9(3) . 2_655 ? Pb6A S11 PB6B 7.5(3) 2_655 2_655 ? Pb6A S11 PB6B 87.3(2) 2 2_655 ? Bi4 S11 PB6B 92.9(3) . 2 ? Pb6A S11 PB6B 87.3(2) 2_655 2 ? Pb6A S11 PB6B 7.5(3) 2 2 ? PB6B S11 PB6B 86.0(5) 2_655 2 ? Bi4 S11 Pb4 104.48(16) . 1_455 ? Pb6A S11 Pb4 155.3(4) 2_655 1_455 ? Pb6A S11 Pb4 88.85(17) 2 1_455 ? PB6B S11 Pb4 162.6(4) 2_655 1_455 ? PB6B S11 Pb4 92.2(2) 2 1_455 ? Bi4 S11 Pb4 104.48(16) . . ? Pb6A S11 Pb4 88.85(17) 2_655 . ? Pb6A S11 Pb4 155.3(4) 2 . ? PB6B S11 Pb4 92.2(2) 2_655 . ? PB6B S11 Pb4 162.6(4) 2 . ? Pb4 S11 Pb4 84.31(15) 1_455 . ? Bi5 S12 Pb5 102.43(16) . . ? Bi5 S12 Pb5 102.43(16) . 1_455 ? Pb5 S12 Pb5 83.47(15) . 1_455 ? Bi5 S12 Pb3 106.12(16) . 1_455 ? Pb5 S12 Pb3 151.5(2) . 1_455 ? Pb5 S12 Pb3 90.53(6) 1_455 1_455 ? Bi5 S12 Pb3 106.12(16) . . ? Pb5 S12 Pb3 90.53(6) . . ? Pb5 S12 Pb3 151.5(2) 1_455 . ? Pb3 S12 Pb3 81.52(14) 1_455 . ? Bi6 S13 Pb5 104.19(18) . 1_455 ? Bi6 S13 Pb5 104.19(18) . . ? Pb5 S13 Pb5 86.47(17) 1_455 . ? Bi6 S14 Bi6 97.89(19) 1_655 . ? Bi6 S14 Pb6A 130.91(10) 1_655 2_655 ? Bi6 S14 Pb6A 130.91(10) . 2_655 ? Fe S15 Cu 1(5) . . ? Fe S15 Bi5 125.5(11) . . ? Cu S15 Bi5 125.7(8) . . ? Fe S15 Bi5 125.5(12) . 1_655 ? Cu S15 Bi5 125.7(8) . 1_655 ? Bi5 S15 Bi5 98.0(2) . 1_655 ? Fe S16 Cu 7(4) 1_455 1_455 ? Fe S16 Fe 120(6) 1_455 . ? Cu S16 Fe 118.6(10) 1_455 . ? Fe S16 Cu 118.6(10) 1_455 . ? Cu S16 Cu 117(4) 1_455 . ? Fe S16 Cu 7(4) . . ? Fe S16 Bi7 98(2) 1_455 . ? Cu S16 Bi7 104.9(16) 1_455 . ? Fe S16 Bi7 98(2) . . ? Cu S16 Bi7 104.9(16) . . ? Fe S16 Pb5 151(3) 1_455 . ? Cu S16 Pb5 145.0(19) 1_455 . ? Fe S16 Pb5 76(3) . . ? Cu S16 Pb5 74(2) . . ? Bi7 S16 Pb5 103.88(16) . . ? Fe S16 Pb5 76(3) 1_455 1_455 ? Cu S16 Pb5 74(2) 1_455 1_455 ? Fe S16 Pb5 151(3) . 1_455 ? Cu S16 Pb5 145.0(19) . 1_455 ? Bi7 S16 Pb5 103.88(16) . 1_455 ? Pb5 S16 Pb5 80.16(16) . 1_455 ? Bi7 S17 Bi7 91.63(19) 1_655 . ? Bi7 S17 Bi6 176.28(18) 1_655 . ? Bi7 S17 Bi6 92.02(2) . . ? Bi7 S17 Bi6 92.02(2) 1_655 1_655 ? Bi7 S17 Bi6 176.28(18) . 1_655 ? Bi6 S17 Bi6 84.32(16) . 1_655 ? Bi8 S18 Bi8 94.3(2) 1_455 . ? Bi8 S18 Bi5 90.97(3) 1_455 2 ? Bi8 S18 Bi5 173.0(2) . 2 ? Bi8 S18 Bi5 173.0(2) 1_455 2_655 ? Bi8 S18 Bi5 90.97(3) . 2_655 ? Bi5 S18 Bi5 83.41(16) 2 2_655 ? Fe S19 Cu 7(4) . . ? Fe S19 PB7B 104.9(15) . 1_655 ? Cu S19 PB7B 109.3(12) . 1_655 ? Fe S19 PB7B 104.9(15) . . ? Cu S19 PB7B 109.3(12) . . ? PB7B S19 PB7B 94.6(7) 1_655 . ? Fe S19 PB6B 101.4(14) . . ? Cu S19 PB6B 96.7(12) . . ? PB7B S19 PB6B 153.7(7) 1_655 . ? PB7B S19 PB6B 79.9(6) . . ? Fe S19 PB6B 101.4(14) . 1_655 ? Cu S19 PB6B 96.7(12) . 1_655 ? PB7B S19 PB6B 79.9(6) 1_655 1_655 ? PB7B S19 PB6B 153.7(7) . 1_655 ? PB6B S19 PB6B 93.5(5) . 1_655 ? Fe S19 Pb7A 98.3(15) . 1_655 ? Cu S19 Pb7A 103.1(12) . 1_655 ? PB7B S19 Pb7A 8.4(5) 1_655 1_655 ? PB7B S19 Pb7A 91.6(5) . 1_655 ? PB6B S19 Pb7A 160.0(4) . 1_655 ? PB6B S19 Pb7A 86.1(3) 1_655 1_655 ? Fe S19 Pb7A 98.3(15) . . ? Cu S19 Pb7A 103.1(12) . . ? PB7B S19 Pb7A 91.6(5) 1_655 . ? PB7B S19 Pb7A 8.4(5) . . ? PB6B S19 Pb7A 86.1(3) . . ? PB6B S19 Pb7A 160.0(4) 1_655 . ? Pb7A S19 Pb7A 87.5(3) 1_655 . ? Fe S19 Pb6A 96.5(15) . . ? Cu S19 Pb6A 91.5(13) . . ? PB7B S19 Pb6A 157.7(7) 1_655 . ? PB7B S19 Pb6A 85.6(5) . . ? PB6B S19 Pb6A 6.7(3) . . ? PB6B S19 Pb6A 90.0(3) 1_655 . ? Pb7A S19 Pb6A 165.2(4) 1_655 . ? Pb7A S19 Pb6A 91.4(3) . . ? Fe S19 Pb6A 96.5(15) . 1_655 ? Cu S19 Pb6A 91.5(13) . 1_655 ? PB7B S19 Pb6A 85.6(5) 1_655 1_655 ? PB7B S19 Pb6A 157.7(7) . 1_655 ? PB6B S19 Pb6A 90.0(3) . 1_655 ? PB6B S19 Pb6A 6.7(3) 1_655 1_655 ? Pb7A S19 Pb6A 91.4(3) 1_655 1_655 ? Pb7A S19 Pb6A 165.2(4) . 1_655 ? Pb6A S19 Pb6A 85.9(4) . 1_655 ? ME3 S20 Bi7 93.96(17) . . ? ME3 S20 Bi7 93.96(17) . 1_655 ? Bi7 S20 Bi7 90.94(19) . 1_655 ? ME3 S21 ME3 88.45(17) 1_455 . ? ME3 S21 Bi8 170.8(2) 1_455 . ? ME3 S21 Bi8 91.61(3) . . ? ME3 S21 Bi8 91.61(3) 1_455 1_455 ? ME3 S21 Bi8 170.8(2) . 1_455 ? Bi8 S21 Bi8 86.84(17) . 1_455 ? ME3 S21 Pb2 98.30(15) 1_455 2_655 ? ME3 S21 Pb2 98.30(15) . 2_655 ? Bi8 S21 Pb2 90.83(15) . 2_655 ? Bi8 S21 Pb2 90.83(15) 1_455 2_655 ? PB8B S22 PB8B 93.8(5) 1_655 . ? PB8B S22 ME4 96.5(5) 1_655 . ? PB8B S22 ME4 96.5(5) . . ? PB8B S22 Pb8A 8.6(3) 1_655 1_655 ? PB8B S22 Pb8A 92.7(3) . 1_655 ? ME4 S22 Pb8A 105.0(3) . 1_655 ? PB8B S22 Pb8A 92.7(3) 1_655 . ? PB8B S22 Pb8A 8.6(3) . . ? ME4 S22 Pb8A 105.0(3) . . ? Pb8A S22 Pb8A 90.3(3) 1_655 . ? PB8B S22 PB7B 155.0(8) 1_655 . ? PB8B S22 PB7B 85.1(5) . . ? ME4 S22 PB7B 108.5(6) . . ? Pb8A S22 PB7B 146.4(7) 1_655 . ? Pb8A S22 PB7B 82.5(5) . . ? PB8B S22 PB7B 85.1(5) 1_655 1_655 ? PB8B S22 PB7B 155.0(8) . 1_655 ? ME4 S22 PB7B 108.5(6) . 1_655 ? Pb8A S22 PB7B 82.5(5) 1_655 1_655 ? Pb8A S22 PB7B 146.4(7) . 1_655 ? PB7B S22 PB7B 85.6(5) . 1_655 ? PB8B S22 Pb7A 162.0(5) 1_655 . ? PB8B S22 Pb7A 89.3(3) . . ? ME4 S22 Pb7A 100.8(3) . . ? Pb8A S22 Pb7A 153.6(4) 1_655 . ? Pb8A S22 Pb7A 87.74(17) . . ? PB7B S22 Pb7A 8.4(5) . . ? PB7B S22 Pb7A 84.7(3) 1_655 . ? PB8B S22 Pb7A 89.3(3) 1_655 1_655 ? PB8B S22 Pb7A 162.0(5) . 1_655 ? ME4 S22 Pb7A 100.8(3) . 1_655 ? Pb8A S22 Pb7A 87.74(17) 1_655 1_655 ? Pb8A S22 Pb7A 153.6(4) . 1_655 ? PB7B S22 Pb7A 84.7(3) . 1_655 ? PB7B S22 Pb7A 8.4(5) 1_655 1_655 ? Pb7A S22 Pb7A 82.6(2) . 1_655 ? ME3 S23 ME3 92.40(18) . 1_455 ? ME3 S23 ME5 88.78(16) . . ? ME3 S23 ME5 88.78(16) 1_455 . ? ME3 S23 ME4 174.66(19) . 1_455 ? ME3 S23 ME4 92.39(2) 1_455 1_455 ? ME5 S23 ME4 88.95(15) . 1_455 ? ME3 S23 ME4 92.39(2) . . ? ME3 S23 ME4 174.66(19) 1_455 . ? ME5 S23 ME4 88.95(15) . . ? ME4 S23 ME4 82.73(15) 1_455 . ? ME3 S24 ME5 92.96(16) . 1_655 ? ME3 S24 ME5 92.96(16) . . ? ME5 S24 ME5 90.70(19) 1_655 . ? ME2 S25 ME2 93.7(2) 6_666 6_566 ? ME2 S25 ME2 96.91(17) 6_666 2_645 ? ME2 S25 ME2 96.91(17) 6_566 2_645 ? ME2 S25 PB8B 153.7(4) 6_666 . ? ME2 S25 PB8B 87.0(3) 6_566 . ? ME2 S25 PB8B 109.1(4) 2_645 . ? ME2 S25 PB8B 87.0(3) 6_666 1_655 ? ME2 S25 PB8B 153.7(4) 6_566 1_655 ? ME2 S25 PB8B 109.1(4) 2_645 1_655 ? PB8B S25 PB8B 81.1(4) . 1_655 ? ME4 S26 ME4 98.5(2) . 1_455 ? ME4 S26 ME2 130.28(11) . 6_566 ? ME4 S26 ME2 130.28(11) 1_455 6_566 ? ME4 S27 ME5 97.54(16) . . ? ME4 S27 ME5 97.54(16) . 1_655 ? ME5 S27 ME5 91.85(18) . 1_655 ? Cu1 S28 Cu2 122.1(6) 6_566 2 ? Cu1 S28 Cu2 122.1(6) 6_566 2_655 ? Cu2 S28 Cu2 114.4(12) 2 2_655 ? Cu1 S28 Bi9 106.4(4) 6_566 2_655 ? Cu2 S28 Bi9 113.8(6) 2 2_655 ? Cu2 S28 Bi9 33.5(7) 2_655 2_655 ? Cu1 S28 Bi9 106.4(4) 6_566 2 ? Cu2 S28 Bi9 33.5(7) 2 2 ? Cu2 S28 Bi9 113.8(6) 2_655 2 ? Bi9 S28 Bi9 94.8(2) 2_655 2 ? Cu1 S28 ME5 102.3(6) 6_566 . ? Cu2 S28 ME5 89.4(7) 2 . ? Cu2 S28 ME5 89.4(7) 2_655 . ? Bi9 S28 ME5 122.73(16) 2_655 . ? Bi9 S28 ME5 122.73(16) 2 . ? Cu1 S28 Bi9 23.2(5) 6_566 6_566 ? Cu2 S28 Bi9 116.6(6) 2 6_566 ? Cu2 S28 Bi9 116.6(6) 2_655 6_566 ? Bi9 S28 Bi9 91.06(17) 2_655 6_566 ? Bi9 S28 Bi9 91.06(17) 2 6_566 ? ME5 S28 Bi9 125.4(2) . 6_566 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 2.702 _refine_diff_density_min -2.264 _refine_diff_density_rms 0.458