# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1887 data_99141 #(Compound 1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H91 Bi4 O0.50 P Se13' _chemical_formula_weight 3061.99 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9032(7) _cell_length_b 23.4916(13) _cell_length_c 30.3394(11) _cell_angle_alpha 79.858(3) _cell_angle_beta 83.279(3) _cell_angle_gamma 78.716(2) _cell_volume 9530.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Needle fragment' _exptl_crystal_colour Red-orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5672 _exptl_absorpt_coefficient_mu 12.387 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius KappaCCD' _diffrn_measurement_method 'Phi frames plus omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35069 _diffrn_reflns_av_R_equivalents 0.123 _diffrn_reflns_av_sigmaI/netI 0.1384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 19.79 _reflns_number_total 17094 _reflns_number_gt 9413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DenzoSMN' _computing_data_reduction 'DenzoSMN' _computing_structure_solution 'SHELXTL Ver 5.10' _computing_structure_refinement 'SHELXTL Ver 5.10' _computing_molecular_graphics 'XP Version 5.10' _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^)+(0.1180P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17094 _refine_ls_number_parameters 1051 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.1531 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2208 _refine_ls_wR_factor_gt 0.1907 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.006 _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 0.90427(9) 0.71389(6) 0.18148(4) 0.0411(4) Uani 1 1 d . . . Bi2 Bi 0.66156(9) 0.60747(6) 0.16312(4) 0.0415(4) Uani 1 1 d . . . Bi3 Bi 0.62404(9) 0.55561(6) 0.31990(4) 0.0422(4) Uani 1 1 d . . . Bi4 Bi 0.86994(9) 0.65544(6) 0.33502(4) 0.0402(4) Uani 1 1 d . B . Se1 Se 0.7988(2) 0.67888(15) 0.10556(9) 0.0508(11) Uani 1 1 d . . . Se2 Se 0.5376(2) 0.54735(15) 0.23625(10) 0.0467(10) Uani 1 1 d . . . Se3 Se 0.7388(2) 0.58254(15) 0.39318(9) 0.0460(10) Uani 1 1 d . . . Se4 Se 0.9758(2) 0.73638(14) 0.26128(10) 0.0404(9) Uani 1 1 d . . . Se5 Se 0.7666(2) 0.63206(13) 0.24746(9) 0.0331(9) Uani 1 1 d . . . Se6 Se 1.0008(3) 0.78989(16) 0.12230(11) 0.0592(11) Uani 1 1 d . . . Se7 Se 0.7444(2) 0.79519(15) 0.19136(10) 0.0487(10) Uani 1 1 d . . . Se8 Se 0.5421(3) 0.60364(18) 0.09851(12) 0.0705(13) Uani 1 1 d . . . Se9 Se 0.5457(3) 0.70271(16) 0.18681(10) 0.0539(11) Uani 1 1 d . . . Se10 Se 0.4855(3) 0.50577(17) 0.37440(11) 0.0622(12) Uani 1 1 d . . . Se11 Se 0.5206(2) 0.66345(15) 0.31653(10) 0.0485(10) Uani 1 1 d . A . Se12 Se 0.9506(2) 0.68602(15) 0.40199(10) 0.0458(10) Uani 1 1 d . . . Se13 Se 0.7172(2) 0.74263(15) 0.33929(10) 0.0460(10) Uani 1 1 d . . . C1 C 0.887(2) 0.6115(13) 0.0881(9) 0.039(8) Uiso 1 1 d . . . C2 C 0.852(2) 0.5683(15) 0.0733(10) 0.055(10) Uiso 1 1 d . . . C3 C 0.915(3) 0.5174(15) 0.0615(10) 0.064(10) Uiso 1 1 d . . . C4 C 1.019(2) 0.5107(14) 0.0639(9) 0.052(9) Uiso 1 1 d . . . C5 C 1.050(2) 0.5573(16) 0.0790(10) 0.063(10) Uiso 1 1 d . . . C6 C 0.992(2) 0.6073(13) 0.0914(8) 0.035(8) Uiso 1 1 d . . . C7 C 0.610(2) 0.4730(13) 0.2288(9) 0.043(9) Uiso 1 1 d . . . C8 C 0.555(2) 0.4274(15) 0.2233(9) 0.055(9) Uiso 1 1 d . . . C9 C 0.604(3) 0.3722(16) 0.2179(10) 0.068(11) Uiso 1 1 d . . . C10 C 0.710(2) 0.3567(14) 0.2192(9) 0.050(9) Uiso 1 1 d . . . C11 C 0.760(2) 0.4011(14) 0.2239(9) 0.048(9) Uiso 1 1 d . . . C12 C 0.713(2) 0.4609(13) 0.2285(9) 0.042(8) Uiso 1 1 d . . . C13 C 0.823(2) 0.5057(14) 0.4032(9) 0.044(9) Uiso 1 1 d . . . C14 C 0.785(2) 0.4538(16) 0.4085(10) 0.063(10) Uiso 1 1 d . . . C15 C 0.852(3) 0.3978(17) 0.4143(11) 0.086(12) Uiso 1 1 d . . . C16 C 0.953(3) 0.3968(15) 0.4160(10) 0.058(10) Uiso 1 1 d . . . C17 C 0.989(3) 0.4450(17) 0.4139(11) 0.071(11) Uiso 1 1 d . . . C18 C 0.926(2) 0.5015(15) 0.4047(10) 0.059(10) Uiso 1 1 d . . . C19 C 1.092(2) 0.6780(13) 0.2577(8) 0.031(8) Uiso 1 1 d . . . C20 C 1.083(2) 0.6232(14) 0.2536(9) 0.042(9) Uiso 1 1 d . . . C21 C 1.164(2) 0.5767(15) 0.2508(10) 0.060(10) Uiso 1 1 d . . . C22 C 1.261(3) 0.5925(17) 0.2529(11) 0.074(11) Uiso 1 1 d . . . C23 C 1.272(2) 0.6458(15) 0.2559(9) 0.051(9) Uiso 1 1 d . . . C24 C 1.185(2) 0.6908(15) 0.2572(10) 0.059(10) Uiso 1 1 d . . . C25 C 0.8677(18) 0.5613(11) 0.2454(8) 0.024(7) Uiso 1 1 d . . . C26 C 0.887(2) 0.5224(13) 0.2846(9) 0.041(8) Uiso 1 1 d . . . C27 C 0.953(2) 0.4722(14) 0.2829(9) 0.054(10) Uiso 1 1 d . . . C28 C 1.012(2) 0.4605(14) 0.2412(10) 0.059(10) Uiso 1 1 d . . . C29 C 0.985(2) 0.5014(13) 0.2025(8) 0.039(8) Uiso 1 1 d . . . C30 C 0.916(2) 0.5517(13) 0.2038(9) 0.039(8) Uiso 1 1 d . . . C31 C 1.103(2) 0.7307(12) 0.1045(8) 0.033(8) Uiso 1 1 d . . . C32 C 1.125(2) 0.7256(15) 0.0585(10) 0.060(10) Uiso 1 1 d . . . C33 C 1.203(3) 0.6858(16) 0.0432(11) 0.070(11) Uiso 1 1 d . . . C34 C 1.256(2) 0.6461(15) 0.0733(10) 0.063(10) Uiso 1 1 d . . . C35 C 1.244(2) 0.6475(14) 0.1186(10) 0.054(10) Uiso 1 1 d . . . C36 C 1.167(2) 0.6922(14) 0.1347(9) 0.054(9) Uiso 1 1 d . . . C37 C 0.791(3) 0.8665(15) 0.1668(11) 0.066(11) Uiso 1 1 d . . . C38 C 0.725(4) 0.902(2) 0.1332(16) 0.142(19) Uiso 1 1 d . . . C39 C 0.756(4) 0.959(3) 0.1160(17) 0.16(2) Uiso 1 1 d . . . C40 C 0.837(4) 0.983(2) 0.1311(17) 0.15(2) Uiso 1 1 d . . . C41 C 0.880(3) 0.947(2) 0.1679(14) 0.107(15) Uiso 1 1 d . . . C42 C 0.859(2) 0.8901(16) 0.1848(10) 0.058(10) Uiso 1 1 d . . . C43 C 0.604(2) 0.5338(14) 0.0796(10) 0.051(9) Uiso 1 1 d . . . C44 C 0.625(4) 0.532(2) 0.0327(16) 0.127(17) Uiso 1 1 d . . . C45 C 0.670(5) 0.476(3) 0.021(2) 0.19(3) Uiso 1 1 d . . . C46 C 0.690(4) 0.425(2) 0.0490(18) 0.142(19) Uiso 1 1 d . . . C47 C 0.677(3) 0.431(2) 0.0935(15) 0.112(15) Uiso 1 1 d . . . C48 C 0.633(3) 0.483(2) 0.1071(13) 0.097(14) Uiso 1 1 d . . . C49 C 0.504(2) 0.7458(13) 0.1306(9) 0.044(9) Uiso 1 1 d . . . C50 C 0.414(3) 0.7389(15) 0.1174(10) 0.063(10) Uiso 1 1 d . . . C51 C 0.373(3) 0.7724(18) 0.0803(12) 0.093(13) Uiso 1 1 d . . . C52 C 0.431(3) 0.8131(16) 0.0549(11) 0.073(11) Uiso 1 1 d . . . C53 C 0.522(3) 0.8272(16) 0.0680(11) 0.074(11) Uiso 1 1 d . . . C54 C 0.560(2) 0.7898(15) 0.1084(10) 0.061(10) Uiso 1 1 d . . . C55 C 0.555(2) 0.4260(13) 0.3792(9) 0.041(8) Uiso 1 1 d . . . C56 C 0.545(3) 0.3928(19) 0.4216(12) 0.093(13) Uiso 1 1 d . . . C57 C 0.595(3) 0.334(2) 0.4225(14) 0.114(16) Uiso 1 1 d . . . C58 C 0.651(3) 0.3050(17) 0.3890(12) 0.085(12) Uiso 1 1 d . . . C59 C 0.657(3) 0.3421(16) 0.3488(11) 0.073(11) Uiso 1 1 d . . . C60 C 0.610(2) 0.4033(15) 0.3423(10) 0.059(10) Uiso 1 1 d . . . C61 C 0.439(2) 0.6614(13) 0.3730(9) 0.040(8) Uiso 1 1 d . . . C62 C 0.501(4) 0.667(2) 0.4077(16) 0.025(15) Uiso 0.50 1 d P A 1 C63 C 0.436(5) 0.680(3) 0.4500(19) 0.052(19) Uiso 0.50 1 d P A 1 C64 C 0.331(8) 0.673(4) 0.456(3) 0.06(3) Uiso 0.50 1 d P A 1 C65 C 0.293(5) 0.667(3) 0.419(2) 0.036(19) Uiso 0.50 1 d P A 1 C66 C 0.345(5) 0.661(3) 0.377(2) 0.03(2) Uiso 0.50 1 d P A 1 C62A C 0.452(6) 0.640(4) 0.417(3) 0.08(3) Uiso 0.50 1 d P A 2 C63A C 0.394(6) 0.635(4) 0.456(2) 0.07(2) Uiso 0.50 1 d P A 2 C64A C 0.302(10) 0.660(6) 0.451(5) 0.13(6) Uiso 0.50 1 d P A 2 C65A C 0.264(6) 0.697(4) 0.407(3) 0.08(3) Uiso 0.50 1 d P A 2 C66A C 0.337(6) 0.683(4) 0.365(3) 0.06(3) Uiso 0.50 1 d P A 2 C67 C 1.050(2) 0.6181(13) 0.4130(9) 0.039(8) Uiso 1 1 d . B 2 C68 C 1.124(2) 0.6031(14) 0.3776(9) 0.048(9) Uiso 1 1 d . B 2 C69 C 1.198(3) 0.5531(16) 0.3865(11) 0.071(11) Uiso 1 1 d . B 2 C70 C 1.209(3) 0.5211(16) 0.4316(11) 0.076(12) Uiso 1 1 d . B 2 C71 C 1.137(2) 0.5413(15) 0.4657(10) 0.057(10) Uiso 1 1 d . B 2 C72 C 1.062(2) 0.5879(15) 0.4569(10) 0.059(10) Uiso 1 1 d . B 2 C73 C 0.779(2) 0.8093(13) 0.3469(9) 0.043(9) Uiso 1 1 d . B 2 C74 C 0.804(2) 0.8448(14) 0.3054(9) 0.050(9) Uiso 1 1 d . B 2 C75 C 0.841(2) 0.8933(13) 0.3120(9) 0.042(8) Uiso 1 1 d . B 2 C76 C 0.852(2) 0.9096(15) 0.3531(10) 0.061(10) Uiso 1 1 d . B 2 C77 C 0.829(2) 0.8677(16) 0.3910(10) 0.063(10) Uiso 1 1 d . B 2 C78 C 0.789(2) 0.8185(13) 0.3899(9) 0.038(8) Uiso 1 1 d . B 2 Bi5 Bi 0.32231(8) 0.22677(5) 0.22634(4) 0.0389(4) Uani 1 1 d . C 2 Bi6 Bi 0.30173(9) 0.16621(6) 0.38207(4) 0.0401(4) Uani 1 1 d . C 2 Bi7 Bi 0.05880(9) 0.06191(6) 0.37234(4) 0.0429(4) Uani 1 1 d . C 2 Bi8 Bi 0.08428(9) 0.11561(6) 0.21694(4) 0.0405(4) Uani 1 1 d . C 2 Se14 Se 0.4146(2) 0.23946(15) 0.30194(9) 0.0415(9) Uani 1 1 d . C 2 Se15 Se 0.1811(2) 0.09349(14) 0.44331(10) 0.0450(10) Uani 1 1 d . C 2 Se16 Se -0.0155(2) 0.03889(14) 0.29102(10) 0.0417(9) Uani 1 1 d . C 2 Se17 Se 0.2049(2) 0.19303(15) 0.15449(9) 0.0447(10) Uani 1 1 d . C 2 Se18 Se 0.1874(2) 0.14720(14) 0.29729(9) 0.0348(9) Uani 1 1 d . C 2 Se19 Se 0.4514(2) 0.27927(15) 0.16367(10) 0.0488(10) Uani 1 1 d . C 2 Se20 Se 0.4426(2) 0.12418(15) 0.22875(10) 0.0477(10) Uani 1 1 d . C 2 Se21 Se 0.4396(2) 0.16918(16) 0.43625(10) 0.0546(11) Uani 1 1 d . C 2 Se22 Se 0.4040(2) 0.07286(15) 0.35034(9) 0.0480(10) Uani 1 1 d . C 2 Se23 Se -0.0454(2) -0.00835(15) 0.43115(10) 0.0513(10) Uani 1 1 d . C 2 Se24 Se 0.2136(2) -0.02363(15) 0.36654(10) 0.0465(10) Uani 1 1 d . C 2 Se25 Se 0.0120(3) 0.07595(17) 0.15024(11) 0.0633(11) Uani 1 1 d . C 2 Se26 Se 0.2429(2) 0.03167(15) 0.22014(11) 0.0501(10) Uani 1 1 d . C 2 C79 C 0.3334(16) 0.3144(10) 0.3113(6) 0.004(6) Uiso 1 1 d . C 2 C80 C 0.382(3) 0.3615(16) 0.3094(10) 0.071(11) Uiso 1 1 d . C 2 C81 C 0.330(3) 0.4172(16) 0.3170(10) 0.066(10) Uiso 1 1 d . C 2 C82 C 0.222(2) 0.4217(15) 0.3263(9) 0.055(10) Uiso 1 1 d . C 2 C83 C 0.176(2) 0.3762(15) 0.3281(9) 0.049(9) Uiso 1 1 d . C 2 C84 C 0.231(2) 0.3210(12) 0.3193(8) 0.031(8) Uiso 1 1 d . C 2 C85 C 0.093(2) 0.1597(13) 0.4642(8) 0.033(8) Uiso 1 1 d . C 2 C86 C 0.131(2) 0.2022(14) 0.4751(9) 0.043(9) Uiso 1 1 d . C 2 C87 C 0.069(2) 0.2531(15) 0.4905(10) 0.061(10) Uiso 1 1 d . C 2 C88 C -0.033(2) 0.2548(14) 0.4954(9) 0.051(9) Uiso 1 1 d . C 2 C89 C -0.073(2) 0.2101(14) 0.4840(9) 0.045(9) Uiso 1 1 d . C 2 C90 C -0.011(2) 0.1615(14) 0.4692(9) 0.051(9) Uiso 1 1 d . C 2 C91 C -0.134(2) 0.0979(13) 0.2911(8) 0.035(8) Uiso 1 1 d . C 2 C92 C -0.224(2) 0.0785(14) 0.2861(9) 0.050(9) Uiso 1 1 d . C 2 C93 C -0.310(3) 0.1264(16) 0.2857(10) 0.065(10) Uiso 1 1 d . C 2 C94 C -0.307(3) 0.1816(18) 0.2891(11) 0.084(12) Uiso 1 1 d . C 2 C95 C -0.211(2) 0.2001(14) 0.2924(9) 0.054(9) Uiso 1 1 d . C 2 C96 C -0.128(2) 0.1554(14) 0.2945(9) 0.045(9) Uiso 1 1 d . C 2 C97 C 0.120(2) 0.2653(13) 0.1502(9) 0.040(8) Uiso 1 1 d . C 2 C98 C 0.156(2) 0.3174(13) 0.1465(8) 0.038(8) Uiso 1 1 d . C 2 C99 C 0.097(2) 0.3721(14) 0.1430(9) 0.050(9) Uiso 1 1 d . C 2 C100 C -0.010(2) 0.3790(14) 0.1470(9) 0.053(9) Uiso 1 1 d . C 2 C101 C -0.046(2) 0.3272(15) 0.1497(9) 0.055(10) Uiso 1 1 d . C 2 C102 C 0.016(2) 0.2723(13) 0.1510(8) 0.035(8) Uiso 1 1 d . C 2 C103 C 0.0888(18) 0.2139(11) 0.3053(8) 0.024(7) Uiso 1 1 d . C 2 C104 C 0.054(2) 0.2561(12) 0.2670(8) 0.036(8) Uiso 1 1 d . C 2 C105 C -0.018(2) 0.3073(14) 0.2751(10) 0.059(10) Uiso 1 1 d . C 2 C106 C -0.065(2) 0.3142(14) 0.3184(9) 0.051(9) Uiso 1 1 d . C 2 C107 C -0.025(2) 0.2711(14) 0.3549(9) 0.053(9) Uiso 1 1 d . C 2 C108 C 0.043(2) 0.2227(13) 0.3491(9) 0.040(8) Uiso 1 1 d . C 2 C109 C 0.385(2) 0.3592(14) 0.1620(10) 0.057(10) Uiso 1 1 d . C 2 C110 C 0.411(3) 0.396(2) 0.1212(14) 0.111(15) Uiso 1 1 d . C 2 C111 C 0.368(4) 0.461(2) 0.1203(16) 0.143(19) Uiso 1 1 d . C 2 C112 C 0.300(3) 0.4812(18) 0.1522(13) 0.091(13) Uiso 1 1 d . C 2 C113 C 0.287(2) 0.4418(16) 0.1932(10) 0.067(11) Uiso 1 1 d . C 2 C114 C 0.327(2) 0.3816(15) 0.1972(9) 0.053(9) Uiso 1 1 d . C 2 C115 C 0.491(2) 0.1207(12) 0.1664(8) 0.033(8) Uiso 1 1 d . C 2 C116 C 0.440(2) 0.0976(15) 0.1405(10) 0.058(10) Uiso 1 1 d . C 2 C117 C 0.483(3) 0.0913(15) 0.0967(10) 0.066(11) Uiso 1 1 d . C 2 C118 C 0.577(3) 0.1073(15) 0.0801(10) 0.063(10) Uiso 1 1 d . C 2 C119 C 0.625(3) 0.1328(15) 0.1109(11) 0.068(11) Uiso 1 1 d . C 2 C120 C 0.584(3) 0.1394(16) 0.1548(11) 0.074(11) Uiso 1 1 d . C 2 C121 C 0.379(2) 0.2397(14) 0.4579(10) 0.051(9) Uiso 1 1 d . C 2 C122 C 0.357(3) 0.288(2) 0.4254(14) 0.113(15) Uiso 1 1 d . C 2 C123 C 0.313(3) 0.339(2) 0.4421(14) 0.109(15) Uiso 1 1 d . C 2 C124 C 0.292(3) 0.3463(17) 0.4923(12) 0.081(12) Uiso 1 1 d . C 2 C125 C 0.315(3) 0.2939(18) 0.5180(11) 0.082(12) Uiso 1 1 d . C 2 C126 C 0.360(2) 0.2406(15) 0.5055(10) 0.060(10) Uiso 1 1 d . C 2 C127 C 0.479(2) 0.0264(13) 0.4000(9) 0.038(8) Uiso 1 1 d . C 2 C128 C 0.580(2) 0.0310(14) 0.3927(9) 0.052(9) Uiso 1 1 d . C 2 C129 C 0.638(2) -0.0092(15) 0.4262(10) 0.060(10) Uiso 1 1 d . C 2 C130 C 0.594(2) -0.0476(14) 0.4614(10) 0.058(10) Uiso 1 1 d . C 2 C131 C 0.495(2) -0.0486(13) 0.4639(9) 0.045(9) Uiso 1 1 d . C 2 C132 C 0.437(2) -0.0078(13) 0.4315(9) 0.039(8) Uiso 1 1 d . C 2 C133 C -0.1520(19) 0.0551(12) 0.4452(8) 0.027(7) Uiso 1 1 d . C 2 C134 C -0.175(2) 0.0571(13) 0.4887(9) 0.037(8) Uiso 1 1 d . C 2 C135 C -0.253(2) 0.1023(14) 0.5008(9) 0.048(9) Uiso 1 1 d . C 2 C136 C -0.308(2) 0.1433(15) 0.4683(10) 0.062(10) Uiso 1 1 d . C 2 C137 C -0.277(2) 0.1378(13) 0.4214(9) 0.039(8) Uiso 1 1 d . C 2 C138 C -0.203(2) 0.0923(15) 0.4109(10) 0.059(10) Uiso 1 1 d . C 2 C139 C 0.152(2) -0.0875(13) 0.3607(9) 0.039(8) Uiso 1 1 d . C 2 C140 C 0.123(2) -0.1260(13) 0.3967(9) 0.042(8) Uiso 1 1 d . C 2 C141 C 0.084(2) -0.1750(13) 0.3906(8) 0.034(8) Uiso 1 1 d . C 2 C142 C 0.079(2) -0.1871(14) 0.3467(10) 0.058(10) Uiso 1 1 d . C 2 C143 C 0.113(2) -0.1478(13) 0.3098(8) 0.037(8) Uiso 1 1 d . C 2 C144 C 0.146(2) -0.0989(13) 0.3162(9) 0.040(8) Uiso 1 1 d . C 2 C145 C -0.0866(19) 0.1431(12) 0.1378(8) 0.027(7) Uiso 1 1 d . C 2 C146 C -0.157(2) 0.1626(14) 0.1699(9) 0.051(9) Uiso 1 1 d . C 2 C147 C -0.229(3) 0.2136(16) 0.1579(11) 0.071(11) Uiso 1 1 d . C 2 C148 C -0.233(3) 0.2467(17) 0.1150(12) 0.080(12) Uiso 1 1 d . C 2 C149 C -0.158(3) 0.2235(17) 0.0837(11) 0.078(12) Uiso 1 1 d . C 2 C150 C -0.083(2) 0.1708(16) 0.0924(10) 0.067(11) Uiso 1 1 d . C 2 C151 C 0.216(2) -0.0231(14) 0.1894(9) 0.049(9) Uiso 1 1 d . C 2 C152 C 0.291(3) -0.0458(18) 0.1541(12) 0.082(12) Uiso 1 1 d . C 2 C153 C 0.285(3) -0.090(2) 0.1341(14) 0.110(15) Uiso 1 1 d . C 2 C154 C 0.210(3) -0.1219(19) 0.1461(13) 0.097(14) Uiso 1 1 d . C 2 C155 C 0.129(3) -0.1037(17) 0.1770(11) 0.079(12) Uiso 1 1 d . C 2 C156 C 0.134(2) -0.0563(14) 0.1980(9) 0.045(9) Uiso 1 1 d . C 2 P1 P 0.2734(11) 0.2402(7) 0.0169(4) 0.123(5) Uiso 1 1 d D D 2 P2 P 0.4778(15) 0.8937(10) 0.3042(7) 0.189(8) Uiso 1 1 d D E 2 C157 C 0.391(3) 0.248(3) 0.037(2) 0.21(3) Uiso 1 1 d D D 2 C158 C 0.428(3) 0.302(2) 0.0187(19) 0.19(3) Uiso 1 1 d D D 2 C159 C 0.530(3) 0.2947(18) 0.0290(12) 0.096(14) Uiso 1 1 d D D 2 C160 C 0.233(5) 0.1684(19) 0.033(2) 0.23(3) Uiso 1 1 d D D 2 C161 C 0.201(6) 0.174(4) -0.012(2) 0.29(4) Uiso 1 1 d D D 2 C162 C 0.169(6) 0.118(4) 0.000(2) 0.26(4) Uiso 1 1 d D D 2 C163 C 0.174(2) 0.3013(15) 0.0294(13) 0.106(15) Uiso 1 1 d D D 2 C164 C 0.072(2) 0.3014(15) 0.0221(11) 0.080(12) Uiso 1 1 d D D 2 C165 C -0.008(3) 0.3509(16) 0.0291(11) 0.086(12) Uiso 1 1 d D D 2 C166 C 0.492(5) 0.882(3) 0.3652(12) 0.21(3) Uiso 1 1 d D E 2 C167 C 0.437(5) 0.834(3) 0.376(2) 0.21(3) Uiso 1 1 d D E 2 C168 C 0.431(6) 0.820(3) 0.424(2) 0.25(3) Uiso 1 1 d D E 2 C169 C 0.511(6) 0.966(2) 0.278(2) 0.26(4) Uiso 1 1 d D E 2 C170 C 0.570(5) 0.963(3) 0.235(2) 0.27(4) Uiso 1 1 d D E 2 C171 C 0.642(4) 0.999(3) 0.2384(18) 0.17(2) Uiso 1 1 d D E 2 C172 C 0.494(5) 0.832(2) 0.2726(18) 0.19(3) Uiso 1 1 d D E 2 C173 C 0.401(6) 0.849(3) 0.253(4) 0.42(7) Uiso 1 1 d D E 2 C174 C 0.355(3) 0.803(2) 0.2428(14) 0.112(15) Uiso 1 1 d D E 2 O1S O 0.170(6) 0.895(4) -0.001(3) 0.40(5) Uiso 1 1 d D F 2 C1S C 0.218(5) 0.938(4) 0.005(3) 0.22(3) Uiso 1 1 d D F 2 C2S C 0.156(8) 0.984(5) 0.038(4) 0.48(8) Uiso 1 1 d D F 2 C3S C 0.068(5) 0.943(3) 0.047(2) 0.22(3) Uiso 1 1 d D F 2 C4S C 0.074(6) 0.895(3) 0.012(2) 0.21(3) Uiso 1 1 d D F 2 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 0.0314(8) 0.0432(9) 0.0457(8) 0.0020(7) -0.0045(6) -0.0069(7) Bi2 0.0396(9) 0.0441(10) 0.0406(8) -0.0036(6) -0.0152(6) -0.0031(7) Bi3 0.0305(8) 0.0460(10) 0.0477(8) -0.0042(7) 0.0002(6) -0.0061(7) Bi4 0.0317(8) 0.0458(10) 0.0466(8) -0.0123(7) -0.0140(6) -0.0046(7) Se1 0.059(3) 0.059(3) 0.0314(18) 0.0018(17) -0.0113(16) -0.007(2) Se2 0.026(2) 0.048(2) 0.064(2) -0.0047(18) -0.0086(16) -0.0042(18) Se3 0.043(2) 0.050(3) 0.0415(19) -0.0028(17) -0.0028(16) -0.0038(19) Se4 0.031(2) 0.044(2) 0.049(2) -0.0088(17) -0.0095(15) -0.0062(17) Se5 0.0248(19) 0.039(2) 0.0357(18) -0.0025(16) -0.0088(14) -0.0060(16) Se6 0.057(3) 0.056(3) 0.061(2) 0.0031(19) 0.0115(19) -0.021(2) Se7 0.032(2) 0.049(3) 0.066(2) -0.0052(19) -0.0111(17) -0.0074(18) Se8 0.056(3) 0.086(3) 0.075(2) -0.029(2) -0.037(2) 0.008(2) Se9 0.059(3) 0.055(3) 0.043(2) -0.0004(18) -0.0099(17) -0.001(2) Se10 0.041(2) 0.069(3) 0.074(2) -0.008(2) 0.0128(19) -0.018(2) Se11 0.044(2) 0.047(3) 0.053(2) -0.0070(18) -0.0050(17) -0.0046(19) Se12 0.041(2) 0.055(3) 0.048(2) -0.0120(17) -0.0176(16) -0.0116(19) Se13 0.030(2) 0.046(2) 0.063(2) -0.0084(18) -0.0082(16) -0.0091(18) Bi5 0.0301(8) 0.0428(9) 0.0417(8) -0.0012(6) -0.0012(6) -0.0076(7) Bi6 0.0357(8) 0.0436(9) 0.0428(8) -0.0028(6) -0.0199(6) -0.0049(7) Bi7 0.0362(8) 0.0400(9) 0.0509(8) 0.0022(7) -0.0076(6) -0.0091(7) Bi8 0.0306(8) 0.0480(10) 0.0448(8) -0.0066(7) -0.0145(6) -0.0059(7) Se14 0.027(2) 0.055(3) 0.0464(19) -0.0090(17) -0.0101(15) -0.0089(18) Se15 0.047(2) 0.043(2) 0.0427(19) 0.0043(17) -0.0101(16) -0.0093(19) Se16 0.031(2) 0.044(2) 0.050(2) -0.0002(17) -0.0135(16) -0.0071(18) Se17 0.045(2) 0.049(2) 0.0398(19) -0.0029(17) -0.0073(16) -0.0107(19) Se18 0.0271(19) 0.044(2) 0.0345(18) -0.0026(16) -0.0099(14) -0.0078(17) Se19 0.039(2) 0.052(3) 0.054(2) -0.0041(18) 0.0070(17) -0.0144(19) Se20 0.039(2) 0.054(3) 0.044(2) 0.0015(17) -0.0056(16) -0.0004(19) Se21 0.040(2) 0.075(3) 0.051(2) -0.0006(19) -0.0275(17) -0.010(2) Se22 0.055(2) 0.048(2) 0.0391(19) 0.0014(17) -0.0169(16) -0.0028(19) Se23 0.050(2) 0.054(3) 0.051(2) 0.0073(18) -0.0104(17) -0.023(2) Se24 0.034(2) 0.045(2) 0.063(2) -0.0050(18) -0.0172(17) -0.0078(18) Se25 0.068(3) 0.064(3) 0.069(2) -0.015(2) -0.037(2) -0.016(2) Se26 0.034(2) 0.052(3) 0.067(2) -0.0093(19) -0.0143(17) -0.0085(19) _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 Se7 2.657(3) . ? Bi1 Se6 2.731(3) . ? Bi1 Se4 2.890(3) . ? Bi1 Se1 3.172(4) . ? Bi1 Se5 3.248(3) . ? Bi2 Se9 2.646(4) . ? Bi2 Se8 2.737(4) . ? Bi2 Se2 2.974(3) . ? Bi2 Se1 2.991(4) . ? Bi3 Se11 2.649(3) . ? Bi3 Se10 2.696(3) . ? Bi3 Se2 2.984(4) . ? Bi3 Se3 3.100(4) . ? Bi4 Se13 2.655(3) . ? Bi4 Se12 2.696(3) . ? Bi4 Se3 2.962(3) . ? Bi4 Se4 3.101(3) . ? Se1 C1 1.92(3) . ? Se2 C7 1.87(3) . ? Se3 C13 1.95(3) . ? Se4 C19 1.91(3) . ? Se5 C25 1.96(2) . ? Se6 C31 1.89(3) . ? Se7 C37 1.91(4) . ? Se8 C43 1.85(3) . ? Se9 C49 1.91(3) . ? Se10 C55 1.92(3) . ? Se11 C61 1.94(3) . ? Se12 C67 1.90(3) . ? Se13 C73 1.98(3) . ? C1 C2 1.37(4) . ? C1 C6 1.46(4) . ? C2 C3 1.41(4) . ? C3 C4 1.43(4) . ? C4 C5 1.41(4) . ? C5 C6 1.37(4) . ? C7 C12 1.41(4) . ? C7 C8 1.48(4) . ? C8 C9 1.37(4) . ? C9 C10 1.45(4) . ? C10 C11 1.39(4) . ? C11 C12 1.45(4) . ? C13 C14 1.41(4) . ? C13 C18 1.42(4) . ? C14 C15 1.45(4) . ? C15 C16 1.41(5) . ? C16 C17 1.31(4) . ? C17 C18 1.44(4) . ? C19 C20 1.35(4) . ? C19 C24 1.38(4) . ? C20 C21 1.42(4) . ? C21 C22 1.48(5) . ? C22 C23 1.31(4) . ? C23 C24 1.44(4) . ? C25 C26 1.38(3) . ? C25 C30 1.39(3) . ? C26 C27 1.35(4) . ? C27 C28 1.46(4) . ? C28 C29 1.42(4) . ? C29 C30 1.37(3) . ? C31 C32 1.41(4) . ? C31 C36 1.42(4) . ? C32 C33 1.38(4) . ? C33 C34 1.36(4) . ? C34 C35 1.37(4) . ? C35 C36 1.45(4) . ? C37 C42 1.39(5) . ? C37 C38 1.49(5) . ? C38 C39 1.48(7) . ? C39 C40 1.50(7) . ? C40 C41 1.40(6) . ? C41 C42 1.41(5) . ? C43 C48 1.34(4) . ? C43 C44 1.43(5) . ? C44 C45 1.43(7) . ? C45 C46 1.34(7) . ? C46 C47 1.37(5) . ? C47 C48 1.36(5) . ? C49 C50 1.40(4) . ? C49 C54 1.44(4) . ? C50 C51 1.37(4) . ? C51 C52 1.43(5) . ? C52 C53 1.48(5) . ? C53 C54 1.46(4) . ? C55 C56 1.39(4) . ? C55 C60 1.40(4) . ? C56 C57 1.42(5) . ? C57 C58 1.40(5) . ? C58 C59 1.37(4) . ? C59 C60 1.45(4) . ? C61 C66 1.31(7) . ? C61 C62A 1.37(8) . ? C61 C66A 1.45(8) . ? C61 C62 1.48(6) . ? C62 C63 1.53(8) . ? C63 C64 1.48(12) . ? C64 C65 1.33(13) . ? C65 C66 1.41(8) . ? C62A C63A 1.34(9) . ? C63A C64A 1.31(15) . ? C64A C65A 1.54(15) . ? C65A C66A 1.59(10) . ? C67 C72 1.41(3) . ? C67 C68 1.44(3) . ? C68 C69 1.41(4) . ? C69 C70 1.45(4) . ? C70 C71 1.43(4) . ? C71 C72 1.37(4) . ? C73 C78 1.39(4) . ? C73 C74 1.43(4) . ? C74 C75 1.39(4) . ? C75 C76 1.40(4) . ? C76 C77 1.42(4) . ? C77 C78 1.38(4) . ? Bi5 Se20 2.646(3) . ? Bi5 Se19 2.757(3) . ? Bi5 Se14 2.841(3) . ? Bi5 Se17 3.161(4) . ? Bi5 Se18 3.264(3) . ? Bi6 Se22 2.638(4) . ? Bi6 Se21 2.685(3) . ? Bi6 Se15 2.908(3) . ? Bi6 Se14 3.166(3) . ? Bi7 Se24 2.654(3) . ? Bi7 Se23 2.702(3) . ? Bi7 Se16 2.955(3) . ? Bi7 Se15 3.161(4) . ? Bi8 Se26 2.653(3) . ? Bi8 Se25 2.735(4) . ? Bi8 Se17 2.991(3) . ? Bi8 Se16 3.007(3) . ? Bi8 Se18 3.228(3) . ? Se14 C79 1.94(2) . ? Se15 C85 1.93(3) . ? Se16 C91 1.93(3) . ? Se17 C97 1.86(3) . ? Se18 C103 1.90(2) . ? Se19 C109 1.92(3) . ? Se20 C115 1.95(2) . ? Se21 C121 1.90(3) . ? Se22 C127 1.98(3) . ? Se23 C133 1.95(3) . ? Se24 C139 1.91(3) . ? Se25 C145 1.89(2) . ? Se26 C151 1.83(3) . ? C79 C84 1.40(3) . ? C79 C80 1.40(4) . ? C80 C81 1.41(4) . ? C81 C82 1.48(4) . ? C82 C83 1.34(4) . ? C83 C84 1.42(4) . ? C85 C86 1.33(4) . ? C85 C90 1.42(4) . ? C86 C87 1.45(4) . ? C87 C88 1.39(4) . ? C88 C89 1.39(4) . ? C89 C90 1.40(4) . ? C91 C96 1.39(4) . ? C91 C92 1.44(4) . ? C92 C93 1.48(4) . ? C93 C94 1.33(5) . ? C94 C95 1.50(5) . ? C95 C96 1.40(4) . ? C97 C98 1.39(4) . ? C97 C102 1.43(4) . ? C98 C99 1.38(4) . ? C99 C100 1.46(4) . ? C100 C101 1.39(4) . ? C101 C102 1.40(4) . ? C103 C108 1.44(3) . ? C103 C104 1.45(3) . ? C104 C105 1.44(4) . ? C105 C106 1.42(4) . ? C106 C107 1.44(4) . ? C107 C108 1.36(4) . ? C109 C114 1.38(4) . ? C109 C110 1.43(4) . ? C110 C111 1.52(6) . ? C111 C112 1.35(5) . ? C112 C113 1.43(4) . ? C113 C114 1.41(4) . ? C115 C116 1.36(4) . ? C115 C120 1.43(4) . ? C116 C117 1.41(4) . ? C117 C118 1.43(4) . ? C118 C119 1.48(5) . ? C119 C120 1.41(4) . ? C121 C122 1.37(4) . ? C121 C126 1.44(4) . ? C122 C123 1.39(5) . ? C123 C124 1.55(5) . ? C124 C125 1.34(4) . ? C125 C126 1.38(4) . ? C127 C132 1.30(3) . ? C127 C128 1.41(4) . ? C128 C129 1.47(4) . ? C129 C130 1.43(4) . ? C130 C131 1.38(4) . ? C131 C132 1.44(4) . ? C133 C134 1.33(3) . ? C133 C138 1.40(4) . ? C134 C135 1.43(4) . ? C135 C136 1.43(4) . ? C136 C137 1.46(4) . ? C137 C138 1.38(4) . ? C139 C140 1.37(3) . ? C139 C144 1.44(4) . ? C140 C141 1.42(4) . ? C141 C142 1.42(4) . ? C142 C143 1.42(4) . ? C143 C144 1.37(4) . ? C145 C146 1.37(3) . ? C145 C150 1.42(4) . ? C146 C147 1.42(4) . ? C147 C148 1.39(4) . ? C148 C149 1.42(4) . ? C149 C150 1.46(4) . ? C151 C156 1.47(4) . ? C151 C152 1.50(4) . ? C152 C153 1.31(5) . ? C153 C154 1.39(5) . ? C154 C155 1.42(5) . ? C155 C156 1.40(4) . ? P1 C163 1.85(3) . ? P1 C160 1.85(3) . ? P1 C157 1.85(3) . ? P1 C161 2.33(8) . ? P2 C172 1.85(3) . ? P2 C166 1.85(3) . ? P2 C169 1.85(3) . ? C157 C158 1.45(2) . ? C158 C159 1.46(2) . ? C160 C161 1.46(2) . ? C161 C162 1.45(2) . ? C163 C164 1.47(2) . ? C164 C165 1.46(2) . ? C166 C167 1.45(2) . ? C167 C168 1.45(2) . ? C169 C170 1.45(2) . ? C170 C171 1.45(2) . ? C172 C173 1.45(2) . ? C173 C174 1.45(2) . ? O1S C4S 1.35(7) . ? O1S C1S 1.35(7) . ? C1S C2S 1.66(6) . ? C2S C3S 1.66(6) . ? C3S C4S 1.66(6) . ? 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 Se7 Bi1 Se6 93.02(11) . . ? Se7 Bi1 Se4 90.65(10) . . ? Se6 Bi1 Se4 95.94(11) . . ? Se7 Bi1 Se1 86.35(10) . . ? Se6 Bi1 Se1 93.63(11) . . ? Se4 Bi1 Se1 170.11(9) . . ? Se7 Bi1 Se5 81.43(9) . . ? Se6 Bi1 Se5 173.54(10) . . ? Se4 Bi1 Se5 87.48(8) . . ? Se1 Bi1 Se5 82.77(8) . . ? Se9 Bi2 Se8 91.49(11) . . ? Se9 Bi2 Se2 82.45(10) . . ? Se8 Bi2 Se2 93.19(11) . . ? Se9 Bi2 Se1 91.85(11) . . ? Se8 Bi2 Se1 97.90(11) . . ? Se2 Bi2 Se1 167.67(11) . . ? Se11 Bi3 Se10 93.90(11) . . ? Se11 Bi3 Se2 88.04(10) . . ? Se10 Bi3 Se2 93.56(11) . . ? Se11 Bi3 Se3 88.05(10) . . ? Se10 Bi3 Se3 98.31(11) . . ? Se2 Bi3 Se3 167.73(10) . . ? Se13 Bi4 Se12 91.88(11) . . ? Se13 Bi4 Se3 84.85(10) . . ? Se12 Bi4 Se3 96.57(10) . . ? Se13 Bi4 Se4 89.36(9) . . ? Se12 Bi4 Se4 93.09(10) . . ? Se3 Bi4 Se4 168.88(9) . . ? C1 Se1 Bi2 93.8(9) . . ? C1 Se1 Bi1 103.9(9) . . ? Bi2 Se1 Bi1 99.62(8) . . ? C7 Se2 Bi2 92.2(9) . . ? C7 Se2 Bi3 96.1(9) . . ? Bi2 Se2 Bi3 103.90(11) . . ? C13 Se3 Bi4 102.6(9) . . ? C13 Se3 Bi3 96.5(10) . . ? Bi4 Se3 Bi3 99.08(9) . . ? C19 Se4 Bi1 93.8(8) . . ? C19 Se4 Bi4 92.7(8) . . ? Bi1 Se4 Bi4 100.72(11) . . ? C25 Se5 Bi1 92.3(7) . . ? C31 Se6 Bi1 94.6(8) . . ? C37 Se7 Bi1 102.5(10) . . ? C43 Se8 Bi2 99.6(10) . . ? C49 Se9 Bi2 102.8(9) . . ? C55 Se10 Bi3 97.0(9) . . ? C61 Se11 Bi3 104.4(9) . . ? C67 Se12 Bi4 98.7(9) . . ? C73 Se13 Bi4 103.0(8) . . ? C2 C1 C6 121(3) . . ? C2 C1 Se1 121(2) . . ? C6 C1 Se1 118(2) . . ? C1 C2 C3 122(3) . . ? C2 C3 C4 120(3) . . ? C5 C4 C3 115(3) . . ? C6 C5 C4 128(3) . . ? C5 C6 C1 115(3) . . ? C12 C7 C8 121(3) . . ? C12 C7 Se2 121(3) . . ? C8 C7 Se2 117(2) . . ? C9 C8 C7 120(3) . . ? C8 C9 C10 121(3) . . ? C11 C10 C9 117(3) . . ? C10 C11 C12 125(3) . . ? C7 C12 C11 116(3) . . ? C14 C13 C18 119(3) . . ? C14 C13 Se3 121(2) . . ? C18 C13 Se3 120(3) . . ? C13 C14 C15 118(3) . . ? C16 C15 C14 120(4) . . ? C17 C16 C15 122(3) . . ? C16 C17 C18 120(4) . . ? C13 C18 C17 120(3) . . ? C20 C19 C24 119(3) . . ? C20 C19 Se4 119(2) . . ? C24 C19 Se4 122(2) . . ? C19 C20 C21 123(3) . . ? C20 C21 C22 115(3) . . ? C23 C22 C21 123(3) . . ? C22 C23 C24 119(3) . . ? C19 C24 C23 121(3) . . ? C26 C25 C30 123(2) . . ? C26 C25 Se5 119.5(19) . . ? C30 C25 Se5 117.9(18) . . ? C27 C26 C25 120(3) . . ? C26 C27 C28 121(3) . . ? C29 C28 C27 115(3) . . ? C30 C29 C28 123(3) . . ? C29 C30 C25 118(2) . . ? C32 C31 C36 116(3) . . ? C32 C31 Se6 120(2) . . ? C36 C31 Se6 124(2) . . ? C33 C32 C31 123(3) . . ? C34 C33 C32 120(3) . . ? C33 C34 C35 123(3) . . ? C34 C35 C36 117(3) . . ? C31 C36 C35 121(3) . . ? C42 C37 C38 122(4) . . ? C42 C37 Se7 126(3) . . ? C38 C37 Se7 109(3) . . ? C39 C38 C37 110(5) . . ? C38 C39 C40 127(5) . . ? C41 C40 C39 113(5) . . ? C40 C41 C42 123(5) . . ? C37 C42 C41 123(3) . . ? C48 C43 C44 116(4) . . ? C48 C43 Se8 125(3) . . ? C44 C43 Se8 119(3) . . ? C43 C44 C45 116(4) . . ? C46 C45 C44 127(6) . . ? C45 C46 C47 114(6) . . ? C48 C47 C46 122(4) . . ? C43 C48 C47 125(4) . . ? C50 C49 C54 124(3) . . ? C50 C49 Se9 118(2) . . ? C54 C49 Se9 117(2) . . ? C51 C50 C49 122(3) . . ? C50 C51 C52 115(4) . . ? C51 C52 C53 127(3) . . ? C54 C53 C52 114(3) . . ? C49 C54 C53 117(3) . . ? C56 C55 C60 123(3) . . ? C56 C55 Se10 115(2) . . ? C60 C55 Se10 122(2) . . ? C55 C56 C57 112(3) . . ? C58 C57 C56 132(4) . . ? C59 C58 C57 112(4) . . ? C58 C59 C60 124(3) . . ? C55 C60 C59 118(3) . . ? C66 C61 C62A 95(5) . . ? C66 C61 C66A 24(4) . . ? C62A C61 C66A 113(5) . . ? C66 C61 C62 128(4) . . ? C62A C61 C62 42(4) . . ? C66A C61 C62 134(4) . . ? C66 C61 Se11 124(4) . . ? C62A C61 Se11 136(4) . . ? C66A C61 Se11 110(3) . . ? C62 C61 Se11 107(3) . . ? C61 C62 C63 109(4) . . ? C64 C63 C62 122(6) . . ? C65 C64 C63 116(7) . . ? C64 C65 C66 127(7) . . ? C61 C66 C65 117(6) . . ? C63A C62A C61 136(7) . . ? C64A C63A C62A 113(9) . . ? C63A C64A C65A 125(10) . . ? C64A C65A C66A 111(9) . . ? C61 C66A C65A 116(6) . . ? C72 C67 C68 119(3) . . ? C72 C67 Se12 121(2) . . ? C68 C67 Se12 120(2) . . ? C69 C68 C67 119(3) . . ? C68 C69 C70 122(3) . . ? C71 C70 C69 116(3) . . ? C72 C71 C70 123(3) . . ? C71 C72 C67 121(3) . . ? C78 C73 C74 127(3) . . ? C78 C73 Se13 119(2) . . ? C74 C73 Se13 114(2) . . ? C75 C74 C73 112(3) . . ? C74 C75 C76 127(3) . . ? C75 C76 C77 113(3) . . ? C78 C77 C76 126(3) . . ? C77 C78 C73 114(3) . . ? Se20 Bi5 Se19 90.68(10) . . ? Se20 Bi5 Se14 85.60(10) . . ? Se19 Bi5 Se14 95.00(10) . . ? Se20 Bi5 Se17 89.97(10) . . ? Se19 Bi5 Se17 94.85(10) . . ? Se14 Bi5 Se17 169.24(10) . . ? Se20 Bi5 Se18 81.57(9) . . ? Se19 Bi5 Se18 171.99(10) . . ? Se14 Bi5 Se18 86.46(8) . . ? Se17 Bi5 Se18 83.19(8) . . ? Se22 Bi6 Se21 93.27(11) . . ? Se22 Bi6 Se15 90.83(10) . . ? Se21 Bi6 Se15 99.73(10) . . ? Se22 Bi6 Se14 85.41(9) . . ? Se21 Bi6 Se14 89.85(10) . . ? Se15 Bi6 Se14 169.90(10) . . ? Se24 Bi7 Se23 92.74(11) . . ? Se24 Bi7 Se16 91.70(10) . . ? Se23 Bi7 Se16 95.58(10) . . ? Se24 Bi7 Se15 82.08(10) . . ? Se23 Bi7 Se15 96.79(10) . . ? Se16 Bi7 Se15 166.39(9) . . ? Se26 Bi8 Se25 93.45(12) . . ? Se26 Bi8 Se17 87.95(10) . . ? Se25 Bi8 Se17 95.05(11) . . ? Se26 Bi8 Se16 88.39(10) . . ? Se25 Bi8 Se16 93.70(11) . . ? Se17 Bi8 Se16 170.71(10) . . ? Se26 Bi8 Se18 79.82(10) . . ? Se25 Bi8 Se18 173.04(10) . . ? Se17 Bi8 Se18 86.54(9) . . ? Se16 Bi8 Se18 84.40(8) . . ? C79 Se14 Bi5 95.9(7) . . ? C79 Se14 Bi6 94.1(6) . . ? Bi5 Se14 Bi6 102.22(10) . . ? C85 Se15 Bi6 94.1(8) . . ? C85 Se15 Bi7 101.9(9) . . ? Bi6 Se15 Bi7 98.69(9) . . ? C91 Se16 Bi7 97.2(9) . . ? C91 Se16 Bi8 91.1(8) . . ? Bi7 Se16 Bi8 102.54(11) . . ? C97 Se17 Bi8 101.7(9) . . ? C97 Se17 Bi5 91.8(10) . . ? Bi8 Se17 Bi5 98.45(8) . . ? C103 Se18 Bi8 93.6(8) . . ? C103 Se18 Bi5 91.9(7) . . ? Bi8 Se18 Bi5 91.75(7) . . ? C109 Se19 Bi5 98.2(9) . . ? C115 Se20 Bi5 104.5(8) . . ? C121 Se21 Bi6 97.5(10) . . ? C127 Se22 Bi6 105.8(8) . . ? C133 Se23 Bi7 95.1(7) . . ? C139 Se24 Bi7 101.4(8) . . ? C145 Se25 Bi8 95.3(8) . . ? C151 Se26 Bi8 105.0(9) . . ? C84 C79 C80 121(2) . . ? C84 C79 Se14 122(2) . . ? C80 C79 Se14 117(2) . . ? C79 C80 C81 121(3) . . ? C80 C81 C82 116(3) . . ? C83 C82 C81 123(3) . . ? C82 C83 C84 120(3) . . ? C79 C84 C83 119(3) . . ? C86 C85 C90 121(3) . . ? C86 C85 Se15 118(2) . . ? C90 C85 Se15 121(2) . . ? C85 C86 C87 121(3) . . ? C88 C87 C86 118(3) . . ? C87 C88 C89 121(3) . . ? C88 C89 C90 119(3) . . ? C89 C90 C85 120(3) . . ? C96 C91 C92 124(3) . . ? C96 C91 Se16 119(2) . . ? C92 C91 Se16 116(2) . . ? C91 C92 C93 113(3) . . ? C94 C93 C92 124(4) . . ? C93 C94 C95 121(4) . . ? C96 C95 C94 116(3) . . ? C91 C96 C95 121(3) . . ? C98 C97 C102 115(3) . . ? C98 C97 Se17 121(2) . . ? C102 C97 Se17 124(2) . . ? C99 C98 C97 124(3) . . ? C98 C99 C100 121(3) . . ? C101 C100 C99 115(3) . . ? C100 C101 C102 122(3) . . ? C101 C102 C97 123(3) . . ? C108 C103 C104 118(2) . . ? C108 C103 Se18 121.2(18) . . ? C104 C103 Se18 120.9(18) . . ? C105 C104 C103 119(2) . . ? C106 C105 C104 123(3) . . ? C105 C106 C107 115(3) . . ? C108 C107 C106 124(3) . . ? C107 C108 C103 121(2) . . ? C114 C109 C110 122(3) . . ? C114 C109 Se19 125(2) . . ? C110 C109 Se19 112(3) . . ? C109 C110 C111 114(4) . . ? C112 C111 C110 123(4) . . ? C111 C112 C113 117(4) . . ? C114 C113 C112 122(3) . . ? C109 C114 C113 120(3) . . ? C116 C115 C120 128(3) . . ? C116 C115 Se20 119(2) . . ? C120 C115 Se20 113(2) . . ? C115 C116 C117 116(3) . . ? C116 C117 C118 123(3) . . ? C117 C118 C119 117(3) . . ? C120 C119 C118 122(3) . . ? C119 C120 C115 114(3) . . ? C122 C121 C126 124(3) . . ? C122 C121 Se21 115(3) . . ? C126 C121 Se21 120(2) . . ? C121 C122 C123 114(4) . . ? C122 C123 C124 126(4) . . ? C125 C124 C123 109(4) . . ? C124 C125 C126 129(3) . . ? C125 C126 C121 116(3) . . ? C132 C127 C128 128(3) . . ? C132 C127 Se22 120(2) . . ? C128 C127 Se22 112(2) . . ? C127 C128 C129 112(3) . . ? C130 C129 C128 121(3) . . ? C131 C130 C129 120(3) . . ? C130 C131 C132 118(3) . . ? C127 C132 C131 121(3) . . ? C134 C133 C138 124(3) . . ? C134 C133 Se23 115.2(19) . . ? C138 C133 Se23 121(2) . . ? C133 C134 C135 117(2) . . ? C136 C135 C134 123(3) . . ? C135 C136 C137 116(3) . . ? C138 C137 C136 120(3) . . ? C137 C138 C133 120(3) . . ? C140 C139 C144 119(3) . . ? C140 C139 Se24 123(2) . . ? C144 C139 Se24 118(2) . . ? C139 C140 C141 121(3) . . ? C140 C141 C142 121(3) . . ? C141 C142 C143 117(3) . . ? C144 C143 C142 121(3) . . ? C143 C144 C139 121(2) . . ? C146 C145 C150 123(3) . . ? C146 C145 Se25 123(2) . . ? C150 C145 Se25 114(2) . . ? C145 C146 C147 119(3) . . ? C148 C147 C146 125(3) . . ? C147 C148 C149 112(3) . . ? C148 C149 C150 127(3) . . ? C145 C150 C149 114(3) . . ? C156 C151 C152 111(3) . . ? C156 C151 Se26 129(2) . . ? C152 C151 Se26 119(3) . . ? C153 C152 C151 124(4) . . ? C152 C153 C154 121(4) . . ? C153 C154 C155 121(4) . . ? C156 C155 C154 117(4) . . ? C155 C156 C151 124(3) . . ? C163 P1 C160 111(3) . . ? C163 P1 C157 111(2) . . ? C160 P1 C157 118(3) . . ? C163 P1 C161 107(3) . . ? C160 P1 C161 38.6(17) . . ? C157 P1 C161 142(3) . . ? C172 P2 C166 122(3) . . ? C172 P2 C169 122(3) . . ? C166 P2 C169 109(4) . . ? C158 C157 P1 117(4) . . ? C157 C158 C159 109(4) . . ? C161 C160 P1 89(4) . . ? C162 C161 C160 91(6) . . ? C162 C161 P1 143(6) . . ? C160 C161 P1 53(3) . . ? C164 C163 P1 121(3) . . ? C165 C164 C163 122(3) . . ? C167 C166 P2 94(4) . . ? C168 C167 C166 105(5) . . ? C170 C169 P2 113(5) . . ? C171 C170 C169 102(5) . . ? C173 C172 P2 96(4) . . ? C174 C173 C172 117(6) . . ? C4S O1S C1S 124(9) . . ? O1S C1S C2S 114(7) . . ? C1S C2S C3S 88(6) . . ? C4S C3S C2S 116(6) . . ? O1S C4S C3S 93(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 19.79 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.247 #(Bi) _refine_diff_density_min -2.416 _refine_diff_density_rms 0.281 #===END data_99156 #(Compound 2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H80 Bi6 Br2 Se16' _chemical_formula_weight 3910.66 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5193(7) _cell_length_b 14.9695(16) _cell_length_c 16.6252(18) _cell_angle_alpha 66.260(4) _cell_angle_beta 83.972(6) _cell_angle_gamma 81.496(6) _cell_volume 2592.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Red/orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 16.578 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.0943 _exptl_absorpt_correction_T_max 0.4362 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius KappaCCD' _diffrn_measurement_method 'Phi frames plus omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11311 _diffrn_reflns_av_R_equivalents 0.092 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 21.12 _reflns_number_total 5576 _reflns_number_gt 4211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZOSMN' _computing_data_reduction 'DENZOSMN' _computing_structure_solution 'SHELXTL Ver. 5.10' _computing_structure_refinement 'SHELXTL Ver 5.10' _computing_molecular_graphics 'XP (SHELXTL Version 5.1)' _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^)+(0.0556P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5576 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Bi1 Bi 0.31749(5) 0.21910(5) 0.19811(4) 0.0224(2) Uani 1 1 d . . . Bi2 Bi 0.31311(5) 0.46345(5) 0.27123(4) 0.0218(2) Uani 1 1 d . . . Bi3 Bi 0.41541(5) 0.67199(5) 0.00161(4) 0.0196(2) Uani 1 1 d . . . Se1 Se 0.33582(16) 0.02600(13) 0.29458(12) 0.0330(5) Uani 1 1 d . . . Se2 Se 0.46890(13) 0.16211(12) 0.05593(11) 0.0222(4) Uani 1 1 d . . . Se3 Se 0.52950(13) 0.26288(13) 0.21750(11) 0.0234(4) Uani 1 1 d . . . Se4 Se 0.09783(14) 0.54246(14) 0.22087(12) 0.0302(5) Uani 1 1 d . . . Se5 Se 0.27453(15) 0.48263(14) 0.42455(12) 0.0340(5) Uani 1 1 d . . . Se6 Se 0.21075(14) 0.78644(14) -0.02239(13) 0.0330(5) Uani 1 1 d . . . Se7 Se 0.26762(13) 0.25158(12) 0.35452(11) 0.0228(4) Uani 1 1 d . . . Se8 Se 0.39882(12) 0.66062(12) 0.17307(11) 0.0190(4) Uani 1 1 d . . . Br1 Br 0.33348(14) 0.45184(13) 0.07396(12) 0.0282(5) Uani 1 1 d . . . C1 C 0.2533(13) 0.0078(12) 0.2079(11) 0.022(4) Uiso 1 1 d . . . C2 C 0.3095(15) -0.0524(13) 0.1686(12) 0.033(5) Uiso 1 1 d . . . H2 H 0.3846 -0.0868 0.1867 0.039 Uiso 1 1 calc R . . C3 C 0.2563(15) -0.0633(13) 0.1016(12) 0.036(5) Uiso 1 1 d . . . H3 H 0.2956 -0.1044 0.0737 0.043 Uiso 1 1 calc R . . C4 C 0.1481(16) -0.0147(14) 0.0765(14) 0.047(5) Uiso 1 1 d . . . H4 H 0.1119 -0.0215 0.0307 0.056 Uiso 1 1 calc R . . C5 C 0.0915(17) 0.0438(15) 0.1174(13) 0.047(5) Uiso 1 1 d . . . H5 H 0.0156 0.0771 0.1003 0.056 Uiso 1 1 calc R . . C6 C 0.1446(14) 0.0548(13) 0.1843(12) 0.034(5) Uiso 1 1 d . . . H6 H 0.1047 0.0950 0.2130 0.041 Uiso 1 1 calc R . . C7 C 0.3680(13) 0.1752(12) -0.0342(11) 0.024(4) Uiso 1 1 d . . . C8 C 0.3995(15) 0.1152(13) -0.0793(12) 0.033(5) Uiso 1 1 d . . . H8 H 0.4708 0.0723 -0.0690 0.039 Uiso 1 1 calc R . . C9 C 0.3232(15) 0.1199(14) -0.1404(13) 0.044(5) Uiso 1 1 d . . . H9 H 0.3426 0.0798 -0.1731 0.053 Uiso 1 1 calc R . . C10 C 0.2198(17) 0.1819(15) -0.1545(14) 0.054(6) Uiso 1 1 d . . . H10 H 0.1687 0.1841 -0.1967 0.065 Uiso 1 1 calc R . . C11 C 0.1910(17) 0.2378(15) -0.1105(13) 0.048(6) Uiso 1 1 d . . . H11 H 0.1190 0.2799 -0.1214 0.057 Uiso 1 1 calc R . . C12 C 0.2627(13) 0.2376(12) -0.0481(11) 0.027(4) Uiso 1 1 d . . . H12 H 0.2409 0.2783 -0.0162 0.033 Uiso 1 1 calc R . . C13 C 0.5988(12) 0.1377(11) 0.2972(10) 0.017(4) Uiso 1 1 d . . . C14 C 0.5907(16) 0.1163(14) 0.3887(13) 0.044(5) Uiso 1 1 d . . . H14 H 0.5465 0.1609 0.4110 0.052 Uiso 1 1 calc R . . C15 C 0.6497(16) 0.0274(15) 0.4457(15) 0.053(6) Uiso 1 1 d . . . H15 H 0.6455 0.0120 0.5071 0.063 Uiso 1 1 calc R . . C16 C 0.7096(16) -0.0337(15) 0.4154(14) 0.049(6) Uiso 1 1 d . . . H16 H 0.7466 -0.0939 0.4557 0.058 Uiso 1 1 calc R . . C17 C 0.7217(16) -0.0143(15) 0.3262(13) 0.046(5) Uiso 1 1 d . . . H17 H 0.7694 -0.0587 0.3053 0.056 Uiso 1 1 calc R . . C18 C 0.6615(14) 0.0727(13) 0.2675(13) 0.038(5) Uiso 1 1 d . . . H18 H 0.6652 0.0857 0.2065 0.046 Uiso 1 1 calc R . . C19 C 0.0614(13) 0.6269(12) 0.2831(11) 0.024(4) Uiso 1 1 d . . . C20 C 0.0905(13) 0.7197(12) 0.2468(12) 0.026(4) Uiso 1 1 d . . . H20 H 0.1331 0.7399 0.1915 0.032 Uiso 1 1 calc R . . C21 C 0.0621(15) 0.7866(14) 0.2851(13) 0.041(5) Uiso 1 1 d . . . H21 H 0.0849 0.8510 0.2574 0.049 Uiso 1 1 calc R . . C22 C -0.0002(16) 0.7578(15) 0.3647(14) 0.047(5) Uiso 1 1 d . . . H22 H -0.0216 0.8024 0.3927 0.056 Uiso 1 1 calc R . . C23 C -0.0326(16) 0.6601(14) 0.4052(13) 0.044(5) Uiso 1 1 d . . . H23 H -0.0762 0.6395 0.4601 0.052 Uiso 1 1 calc R . . C24 C 0.0002(14) 0.5961(13) 0.3634(11) 0.030(4) Uiso 1 1 d . . . H24 H -0.0196 0.5307 0.3902 0.036 Uiso 1 1 calc R . . C25 C 0.3972(13) 0.3837(12) 0.4807(11) 0.022(4) Uiso 1 1 d . . . C26 C 0.3773(16) 0.2925(13) 0.5431(12) 0.036(5) Uiso 1 1 d . . . H26 H 0.2988 0.2766 0.5562 0.044 Uiso 1 1 calc R . . C27 C 0.4657(16) 0.2240(15) 0.5867(13) 0.047(5) Uiso 1 1 d . . . H27 H 0.4476 0.1617 0.6287 0.057 Uiso 1 1 calc R . . C28 C 0.5813(16) 0.2443(15) 0.5706(13) 0.045(5) Uiso 1 1 d . . . H28 H 0.6433 0.1965 0.6000 0.054 Uiso 1 1 calc R . . C29 C 0.6028(18) 0.3352(16) 0.5109(14) 0.058(6) Uiso 1 1 d . . . H29 H 0.6814 0.3510 0.5012 0.069 Uiso 1 1 calc R . . C30 C 0.5153(16) 0.4058(16) 0.4637(14) 0.050(6) Uiso 1 1 d . . . H30 H 0.5341 0.4675 0.4210 0.060 Uiso 1 1 calc R . . C31 C 0.1214(13) 0.7247(12) -0.0717(11) 0.024(4) Uiso 1 1 d . . . C32 C 0.0436(16) 0.6636(14) -0.0211(14) 0.049(6) Uiso 1 1 d . . . H32 H 0.0399 0.6471 0.0405 0.059 Uiso 1 1 calc R . . C33 C -0.0329(16) 0.6227(14) -0.0548(13) 0.045(5) Uiso 1 1 d . . . H33 H -0.0883 0.5806 -0.0183 0.054 Uiso 1 1 calc R . . C34 C -0.0209(15) 0.6486(13) -0.1456(12) 0.036(5) Uiso 1 1 d . . . H34 H -0.0697 0.6223 -0.1711 0.043 Uiso 1 1 calc R . . C35 C 0.0542(14) 0.7076(13) -0.1977(13) 0.035(5) Uiso 1 1 d . . . H35 H 0.0582 0.7234 -0.2592 0.042 Uiso 1 1 calc R . . C36 C 0.1298(14) 0.7476(13) -0.1613(12) 0.032(5) Uiso 1 1 d . . . H36 H 0.1852 0.7894 -0.1982 0.038 Uiso 1 1 calc R . . C37 C 0.1063(13) 0.2306(12) 0.3865(11) 0.024(4) Uiso 1 1 d . . . C38 C 0.0709(17) 0.1407(15) 0.4026(14) 0.051(6) Uiso 1 1 d . . . H38 H 0.1257 0.0898 0.3960 0.062 Uiso 1 1 calc R . . C39 C -0.0453(18) 0.1253(16) 0.4283(14) 0.057(6) Uiso 1 1 d . . . H39 H -0.0710 0.0649 0.4357 0.068 Uiso 1 1 calc R . . C40 C -0.1246(18) 0.1967(15) 0.4435(14) 0.051(6) Uiso 1 1 d . . . H40 H -0.2033 0.1850 0.4638 0.062 Uiso 1 1 calc R . . C41 C -0.0874(16) 0.2818(14) 0.4288(13) 0.043(5) Uiso 1 1 d . . . H41 H -0.1418 0.3314 0.4381 0.052 Uiso 1 1 calc R . . C42 C 0.0294(14) 0.3024(13) 0.3999(11) 0.031(5) Uiso 1 1 d . . . H42 H 0.0534 0.3641 0.3901 0.037 Uiso 1 1 calc R . . C43 C 0.5522(13) 0.5963(11) 0.2083(11) 0.019(4) Uiso 1 1 d . . . C44 C 0.6100(14) 0.5331(13) 0.1772(12) 0.034(5) Uiso 1 1 d . . . H44 H 0.5741 0.5185 0.1358 0.040 Uiso 1 1 calc R . . C45 C 0.7241(18) 0.4863(16) 0.2037(14) 0.056(6) Uiso 1 1 d . . . H45 H 0.7654 0.4410 0.1810 0.067 Uiso 1 1 calc R . . C46 C 0.7723(19) 0.5102(16) 0.2650(15) 0.061(6) Uiso 1 1 d . . . H46 H 0.8486 0.4800 0.2841 0.074 Uiso 1 1 calc R . . C47 C 0.7173(16) 0.5726(14) 0.2977(14) 0.048(6) Uiso 1 1 d . . . H47 H 0.7534 0.5868 0.3393 0.057 Uiso 1 1 calc R . . C48 C 0.6038(14) 0.6182(13) 0.2700(12) 0.034(5) Uiso 1 1 d . . . H48 H 0.5626 0.6634 0.2930 0.040 Uiso 1 1 calc R . . 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 0.0159(4) 0.0237(4) 0.0264(4) -0.0067(4) -0.0063(3) -0.0044(3) Bi2 0.0128(4) 0.0293(4) 0.0225(4) -0.0093(4) -0.0021(3) -0.0013(3) Bi3 0.0103(4) 0.0250(4) 0.0226(4) -0.0076(3) -0.0045(3) -0.0020(3) Se1 0.0423(12) 0.0252(11) 0.0271(12) -0.0035(10) -0.0093(9) -0.0056(9) Se2 0.0164(9) 0.0263(11) 0.0240(11) -0.0077(9) -0.0056(7) -0.0056(7) Se3 0.0147(9) 0.0309(11) 0.0254(11) -0.0100(9) -0.0034(7) -0.0067(8) Se4 0.0200(10) 0.0405(12) 0.0325(12) -0.0160(10) -0.0118(8) 0.0011(8) Se5 0.0305(10) 0.0453(13) 0.0269(12) -0.0171(10) -0.0090(8) 0.0076(9) Se6 0.0196(10) 0.0432(13) 0.0467(14) -0.0284(11) -0.0199(9) 0.0092(8) Se7 0.0195(9) 0.0259(11) 0.0217(11) -0.0061(9) -0.0035(7) -0.0060(8) Se8 0.0085(9) 0.0250(10) 0.0232(11) -0.0088(9) -0.0051(7) 0.0005(7) Br1 0.0228(10) 0.0296(11) 0.0323(12) -0.0108(10) -0.0032(8) -0.0057(8) _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 Se1 2.6703(19) . ? Bi1 Se3 2.7030(16) . ? Bi1 Se7 2.8196(18) . ? Bi1 Se2 3.1104(18) . ? Bi2 Se4 2.6497(17) . ? Bi2 Se5 2.6629(19) . ? Bi2 Se8 2.9991(18) . ? Bi2 Se7 3.0090(18) . ? Bi3 Se6 2.6655(17) . ? Bi3 Se2 2.7671(18) 2_665 ? Bi3 Se8 2.7741(18) . ? Se1 C1 1.932(15) . ? Se2 C7 1.923(16) . ? Se2 Bi3 2.7671(18) 2_665 ? Se3 C13 1.919(15) . ? Se4 C19 1.910(16) . ? Se5 C25 1.899(15) . ? Se6 C31 1.912(16) . ? Se7 C37 1.914(16) . ? Se8 C43 1.911(14) . ? C1 C6 1.36(2) . ? C1 C2 1.37(2) . ? C2 C3 1.40(2) . ? C3 C4 1.36(2) . ? C4 C5 1.37(2) . ? C5 C6 1.40(2) . ? C7 C8 1.37(2) . ? C7 C12 1.40(2) . ? C8 C9 1.39(2) . ? C9 C10 1.38(2) . ? C10 C11 1.31(2) . ? C11 C12 1.39(2) . ? C13 C18 1.35(2) . ? C13 C14 1.42(2) . ? C14 C15 1.41(3) . ? C15 C16 1.29(2) . ? C16 C17 1.39(3) . ? C17 C18 1.41(2) . ? C19 C20 1.35(2) . ? C19 C24 1.38(2) . ? C20 C21 1.37(2) . ? C21 C22 1.37(3) . ? C22 C23 1.43(3) . ? C23 C24 1.38(2) . ? C25 C26 1.38(2) . ? C25 C30 1.42(2) . ? C26 C27 1.36(2) . ? C27 C28 1.38(2) . ? C28 C29 1.36(3) . ? C29 C30 1.39(3) . ? C31 C32 1.35(2) . ? C31 C36 1.38(2) . ? C32 C33 1.42(2) . ? C33 C34 1.40(3) . ? C34 C35 1.32(2) . ? C35 C36 1.43(2) . ? C37 C42 1.36(2) . ? C37 C38 1.38(2) . ? C38 C39 1.39(3) . ? C39 C40 1.39(3) . ? C40 C41 1.32(2) . ? C41 C42 1.42(2) . ? C43 C44 1.32(2) . ? C43 C48 1.40(2) . ? C44 C45 1.42(2) . ? C45 C46 1.40(3) . ? C46 C47 1.32(3) . ? C47 C48 1.41(2) . ? 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 Se1 Bi1 Se3 101.34(6) . . ? Se1 Bi1 Se7 88.84(6) . . ? Se3 Bi1 Se7 80.41(5) . . ? Se1 Bi1 Se2 85.08(5) . . ? Se3 Bi1 Se2 79.60(5) . . ? Se7 Bi1 Se2 157.50(5) . . ? Se4 Bi2 Se5 93.11(6) . . ? Se4 Bi2 Se8 89.53(5) . . ? Se5 Bi2 Se8 95.19(6) . . ? Se4 Bi2 Se7 98.12(5) . . ? Se5 Bi2 Se7 91.87(6) . . ? Se8 Bi2 Se7 169.30(5) . . ? Se6 Bi3 Se2 89.31(6) . 2_665 ? Se6 Bi3 Se8 87.46(5) . . ? Se2 Bi3 Se8 91.30(5) 2_665 . ? C1 Se1 Bi1 89.8(5) . . ? C7 Se2 Bi3 108.5(5) . 2_665 ? C7 Se2 Bi1 108.4(5) . . ? Bi3 Se2 Bi1 92.65(5) 2_665 . ? C13 Se3 Bi1 101.3(4) . . ? C19 Se4 Bi2 101.0(5) . . ? C25 Se5 Bi2 94.6(5) . . ? C31 Se6 Bi3 102.0(5) . . ? C37 Se7 Bi1 105.3(5) . . ? C37 Se7 Bi2 115.2(5) . . ? Bi1 Se7 Bi2 94.63(5) . . ? C43 Se8 Bi3 99.2(5) . . ? C43 Se8 Bi2 86.7(5) . . ? Bi3 Se8 Bi2 101.26(5) . . ? C6 C1 C2 120.4(16) . . ? C6 C1 Se1 121.8(12) . . ? C2 C1 Se1 117.8(12) . . ? C1 C2 C3 120.0(16) . . ? C4 C3 C2 119.8(17) . . ? C3 C4 C5 119.8(19) . . ? C4 C5 C6 120.4(19) . . ? C1 C6 C5 119.6(17) . . ? C8 C7 C12 121.6(15) . . ? C8 C7 Se2 117.2(12) . . ? C12 C7 Se2 120.9(12) . . ? C7 C8 C9 117.4(16) . . ? C10 C9 C8 120.9(19) . . ? C11 C10 C9 121(2) . . ? C10 C11 C12 121.9(19) . . ? C11 C12 C7 117.4(16) . . ? C18 C13 C14 119.4(16) . . ? C18 C13 Se3 121.3(13) . . ? C14 C13 Se3 119.1(12) . . ? C15 C14 C13 118.5(18) . . ? C16 C15 C14 121(2) . . ? C15 C16 C17 122(2) . . ? C16 C17 C18 118.4(19) . . ? C13 C18 C17 120.5(18) . . ? C20 C19 C24 118.9(16) . . ? C20 C19 Se4 120.3(13) . . ? C24 C19 Se4 120.7(13) . . ? C19 C20 C21 123.8(18) . . ? C22 C21 C20 118.2(19) . . ? C21 C22 C23 119.7(19) . . ? C24 C23 C22 119.2(19) . . ? C19 C24 C23 120.2(17) . . ? C26 C25 C30 117.2(15) . . ? C26 C25 Se5 123.2(12) . . ? C30 C25 Se5 119.4(14) . . ? C27 C26 C25 122.7(17) . . ? C26 C27 C28 121(2) . . ? C29 C28 C27 117.6(19) . . ? C28 C29 C30 123(2) . . ? C29 C30 C25 119(2) . . ? C32 C31 C36 118.8(17) . . ? C32 C31 Se6 120.7(14) . . ? C36 C31 Se6 120.3(13) . . ? C31 C32 C33 124(2) . . ? C34 C33 C32 115.1(19) . . ? C35 C34 C33 123.6(18) . . ? C34 C35 C36 119.6(18) . . ? C31 C36 C35 119.3(17) . . ? C42 C37 C38 120.5(16) . . ? C42 C37 Se7 119.4(13) . . ? C38 C37 Se7 119.9(13) . . ? C37 C38 C39 119.5(18) . . ? C38 C39 C40 121(2) . . ? C41 C40 C39 118(2) . . ? C40 C41 C42 123.2(18) . . ? C37 C42 C41 117.7(17) . . ? C44 C43 C48 119.6(15) . . ? C44 C43 Se8 122.8(12) . . ? C48 C43 Se8 117.6(12) . . ? C43 C44 C45 122.1(18) . . ? C46 C45 C44 116(2) . . ? C47 C46 C45 123(2) . . ? C46 C47 C48 119(2) . . ? C43 C48 C47 119.5(16) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 21.12 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.733 _refine_diff_density_min -3.025 _refine_diff_density_rms 0.285