# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Burford, Neil' _publ_contact_author_email neil.burford@dal.ca _publ_section_title ; Title: Bismuthenium-pnictonium Dications [R\^aBiPnR3]2+ (Pn = As, Sb) containing Carbenoid Bismuth Centers and Rare Bi-Sb Bonds ; loop_ _publ_author_name E.Conrad N.Burford R.McDonald M.Ferguson # Attachment 'C100H84As4Bi4Cl8F12O12S4.CIF.txt' data_dal08f3 _database_code_depnum_ccdc_archive 'CCDC 755446' #TrackingRef 'C100H84As4Bi4Cl8F12O12S4.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H84 As4 Bi4 Cl8 F12 O12 S4' _chemical_formula_weight 3253.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 11.4407(9) _cell_length_b 15.4984(13) _cell_length_c 18.1472(15) _cell_angle_alpha 67.5168(9) _cell_angle_beta 74.1484(9) _cell_angle_gamma 76.2140(10) _cell_volume 2827.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.54 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.552 _exptl_crystal_size_mid 0.291 _exptl_crystal_size_min 0.228 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 7.704 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1027 _exptl_absorpt_correction_T_max 0.2947 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24994 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12865 _reflns_number_gt 11607 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0435P)^2^+9.6797P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12865 _refine_ls_number_parameters 650 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _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 0.476149(14) 0.669097(11) 0.479127(10) 0.02254(5) Uani 1 1 d . . . Bi2 Bi 0.410328(15) 0.562582(11) 0.759704(10) 0.02438(5) Uani 1 1 d . . . As1 As 0.31019(4) 0.82375(3) 0.39643(3) 0.02491(9) Uani 1 1 d . . . As2 As 0.21191(4) 0.68741(3) 0.82309(3) 0.02575(10) Uani 1 1 d . . . Cl1 Cl 0.61921(10) 0.78319(7) 0.45312(7) 0.0278(2) Uani 1 1 d . . . Cl2 Cl 0.34149(10) 0.71933(7) 0.60097(6) 0.0284(2) Uani 1 1 d . . . Cl3 Cl 0.56094(10) 0.63740(8) 0.78725(7) 0.0296(2) Uani 1 1 d . . . Cl4 Cl 0.36959(11) 0.43786(7) 0.89924(6) 0.0296(2) Uani 1 1 d . . . S1 S 0.68929(10) 0.56074(8) 0.35125(7) 0.0267(2) Uani 1 1 d . . . S2 S 0.64484(10) 0.46043(8) 0.63995(7) 0.0254(2) Uani 1 1 d . . . F11 F 0.9029(4) 0.4741(3) 0.3833(3) 0.0703(12) Uani 1 1 d . . . F12 F 0.8373(4) 0.5964(3) 0.4179(3) 0.0736(13) Uani 1 1 d . . . F13 F 0.9069(3) 0.6093(4) 0.2925(3) 0.0760(13) Uani 1 1 d . . . F21 F 0.8759(3) 0.4759(3) 0.5733(2) 0.0600(10) Uani 1 1 d . . . F22 F 0.8455(3) 0.3728(3) 0.6920(2) 0.0573(10) Uani 1 1 d . . . F23 F 0.8066(3) 0.5202(3) 0.6774(3) 0.0717(13) Uani 1 1 d . . . O11 O 0.6289(3) 0.6567(2) 0.3421(2) 0.0340(7) Uani 1 1 d . . . O12 O 0.7111(4) 0.5342(3) 0.2806(2) 0.0461(10) Uani 1 1 d . . . O13 O 0.6365(4) 0.4944(3) 0.4270(2) 0.0448(9) Uani 1 1 d . . . O21 O 0.5825(3) 0.4348(3) 0.7243(2) 0.0385(8) Uani 1 1 d . . . O22 O 0.6065(4) 0.5585(2) 0.5935(2) 0.0405(9) Uani 1 1 d . . . O23 O 0.6548(3) 0.3920(2) 0.6027(2) 0.0330(7) Uani 1 1 d . . . C10 C 0.8437(5) 0.5603(5) 0.3614(4) 0.0435(13) Uani 1 1 d . . . C11 C 0.3088(5) 0.8312(3) 0.2874(3) 0.0294(9) Uani 1 1 d . . . C12 C 0.4170(5) 0.8033(4) 0.2407(3) 0.0399(12) Uani 1 1 d . . . H12 H 0.4909 0.7840 0.2609 0.048 Uiso 1 1 calc R . . C13 C 0.4183(6) 0.8036(4) 0.1644(4) 0.0484(14) Uani 1 1 d . . . H13 H 0.4929 0.7841 0.1321 0.058 Uiso 1 1 calc R . . C14 C 0.3102(7) 0.8324(4) 0.1351(4) 0.0505(15) Uani 1 1 d . . . H14 H 0.3109 0.8329 0.0825 0.061 Uiso 1 1 calc R . . C15 C 0.2037(7) 0.8599(5) 0.1813(4) 0.0546(16) Uani 1 1 d . . . H15 H 0.1302 0.8799 0.1607 0.066 Uiso 1 1 calc R . . C16 C 0.2011(5) 0.8590(4) 0.2585(3) 0.0419(12) Uani 1 1 d . . . H16 H 0.1260 0.8774 0.2910 0.050 Uiso 1 1 calc R . . C20 C 0.8027(4) 0.4576(4) 0.6461(4) 0.0365(11) Uani 1 1 d . . . C21 C 0.3369(4) 0.9467(3) 0.3869(3) 0.0285(9) Uani 1 1 d . . . C22 C 0.3408(6) 1.0198(4) 0.3128(3) 0.0438(13) Uani 1 1 d . . . H22 H 0.3282 1.0102 0.2670 0.053 Uiso 1 1 calc R . . C23 C 0.3632(6) 1.1070(4) 0.3057(4) 0.0498(15) Uani 1 1 d . . . H23 H 0.3645 1.1575 0.2552 0.060 Uiso 1 1 calc R . . C24 C 0.3837(5) 1.1205(4) 0.3717(4) 0.0399(12) Uani 1 1 d . . . H24 H 0.4014 1.1798 0.3660 0.048 Uiso 1 1 calc R . . C25 C 0.3786(5) 1.0484(4) 0.4458(3) 0.0351(11) Uani 1 1 d . . . H25 H 0.3907 1.0586 0.4914 0.042 Uiso 1 1 calc R . . C26 C 0.3556(5) 0.9605(3) 0.4539(3) 0.0332(10) Uani 1 1 d . . . H26 H 0.3529 0.9104 0.5047 0.040 Uiso 1 1 calc R . . C31 C 0.1438(4) 0.8109(3) 0.4563(3) 0.0279(9) Uani 1 1 d . . . C32 C 0.0795(5) 0.8659(4) 0.5045(3) 0.0369(11) Uani 1 1 d . . . H32 H 0.1162 0.9131 0.5074 0.044 Uiso 1 1 calc R . . C33 C -0.0381(5) 0.8510(4) 0.5478(4) 0.0449(13) Uani 1 1 d . . . H33 H -0.0822 0.8888 0.5801 0.054 Uiso 1 1 calc R . . C34 C -0.0922(5) 0.7823(4) 0.5448(4) 0.0425(13) Uani 1 1 d . . . H34 H -0.1725 0.7723 0.5756 0.051 Uiso 1 1 calc R . . C35 C -0.0296(5) 0.7280(4) 0.4971(4) 0.0507(15) Uani 1 1 d . . . H35 H -0.0672 0.6813 0.4941 0.061 Uiso 1 1 calc R . . C36 C 0.0889(5) 0.7421(4) 0.4535(4) 0.0439(13) Uani 1 1 d . . . H36 H 0.1326 0.7040 0.4213 0.053 Uiso 1 1 calc R . . C41 C 0.0648(4) 0.6434(3) 0.8291(3) 0.0308(10) Uani 1 1 d . . . C42 C 0.0360(5) 0.6520(4) 0.7564(4) 0.0403(12) Uani 1 1 d . . . H42 H 0.0857 0.6825 0.7057 0.048 Uiso 1 1 calc R . . C43 C -0.0655(6) 0.6160(4) 0.7583(4) 0.0462(13) Uani 1 1 d . . . H43 H -0.0865 0.6237 0.7087 0.055 Uiso 1 1 calc R . . C44 C -0.1358(6) 0.5690(5) 0.8316(4) 0.0535(16) Uani 1 1 d . . . H44 H -0.2043 0.5437 0.8327 0.064 Uiso 1 1 calc R . . C45 C -0.1059(6) 0.5590(5) 0.9039(4) 0.0592(18) Uani 1 1 d . . . H45 H -0.1537 0.5262 0.9545 0.071 Uiso 1 1 calc R . . C46 C -0.0066(5) 0.5968(5) 0.9028(4) 0.0487(15) Uani 1 1 d . . . H46 H 0.0125 0.5906 0.9525 0.058 Uiso 1 1 calc R . . C51 C 0.2025(5) 0.6872(4) 0.9314(3) 0.0344(10) Uani 1 1 d . . . C52 C 0.1017(7) 0.7384(5) 0.9672(4) 0.0561(17) Uani 1 1 d . . . H52 H 0.0391 0.7753 0.9380 0.067 Uiso 1 1 calc R . . C53 C 0.0931(9) 0.7353(6) 1.0458(4) 0.072(2) Uani 1 1 d . . . H53 H 0.0239 0.7697 1.0706 0.087 Uiso 1 1 calc R . . C54 C 0.1833(7) 0.6832(5) 1.0875(4) 0.0571(18) Uani 1 1 d . . . H54 H 0.1755 0.6803 1.1419 0.069 Uiso 1 1 calc R . . C55 C 0.2862(7) 0.6343(5) 1.0516(4) 0.0511(15) Uani 1 1 d . . . H55 H 0.3503 0.6001 1.0802 0.061 Uiso 1 1 calc R . . C56 C 0.2948(5) 0.6358(4) 0.9730(3) 0.0401(12) Uani 1 1 d . . . H56 H 0.3642 0.6014 0.9483 0.048 Uiso 1 1 calc R . . C61 C 0.1934(5) 0.8196(3) 0.7550(3) 0.0309(10) Uani 1 1 d . . . C62 C 0.2950(5) 0.8656(4) 0.7311(4) 0.0422(13) Uani 1 1 d . . . H62 H 0.3689 0.8333 0.7496 0.051 Uiso 1 1 calc R . . C63 C 0.2876(7) 0.9589(4) 0.6801(4) 0.0561(17) Uani 1 1 d . . . H63 H 0.3564 0.9909 0.6643 0.067 Uiso 1 1 calc R . . C64 C 0.1820(7) 1.0055(4) 0.6522(4) 0.0569(18) Uani 1 1 d . . . H64 H 0.1781 1.0694 0.6168 0.068 Uiso 1 1 calc R . . C65 C 0.0808(7) 0.9596(4) 0.6757(4) 0.0545(17) Uani 1 1 d . . . H65 H 0.0077 0.9920 0.6562 0.065 Uiso 1 1 calc R . . C66 C 0.0858(6) 0.8668(4) 0.7273(4) 0.0444(13) Uani 1 1 d . . . H66 H 0.0162 0.8356 0.7438 0.053 Uiso 1 1 calc R . . C1S C 0.7687(8) 0.8220(7) 0.1653(4) 0.097(4) Uani 1 1 d D . . H1S H 0.7385 0.7642 0.1978 0.116 Uiso 1 1 calc R . . C2S C 0.7728(9) 0.8563(6) 0.0836(4) 0.087(3) Uani 1 1 d D . . H2S H 0.7434 0.8236 0.0592 0.104 Uiso 1 1 calc R . . C3S C 0.8194(9) 0.9379(6) 0.0372(5) 0.087(3) Uani 1 1 d D . . H3S H 0.8258 0.9602 -0.0202 0.104 Uiso 1 1 calc R . . C4S C 0.8569(9) 0.9880(7) 0.0716(5) 0.086(3) Uani 1 1 d D . . H4S H 0.8862 1.0462 0.0392 0.103 Uiso 1 1 calc R . . C5S C 0.8516(11) 0.9529(8) 0.1534(5) 0.116(4) Uani 1 1 d D . . H5S H 0.8788 0.9866 0.1781 0.139 Uiso 1 1 calc R . . C6S C 0.8079(11) 0.8703(8) 0.2005(6) 0.122(5) Uani 1 1 d D . . H6S H 0.8047 0.8466 0.2576 0.146 Uiso 1 1 calc R . . C7S C 0.3851(8) 0.0655(5) 0.0998(5) 0.077(2) Uani 1 1 d D . . H7S H 0.3717 0.0054 0.1040 0.092 Uiso 1 1 calc R . . C8S C 0.5016(8) 0.0807(8) 0.0898(6) 0.110(4) Uani 1 1 d D . . H8S H 0.5683 0.0306 0.0898 0.132 Uiso 1 1 calc R . . C9S C 0.5228(12) 0.1677(8) 0.0799(7) 0.132(6) Uani 1 1 d D . . H9S H 0.6035 0.1791 0.0739 0.159 Uiso 1 1 calc R . . C10S C 0.4250(13) 0.2379(7) 0.0788(6) 0.133(7) Uani 1 1 d D . . H10S H 0.4393 0.2999 0.0683 0.160 Uiso 1 1 calc R . . C11S C 0.3074(13) 0.2227(7) 0.0921(8) 0.153(7) Uani 1 1 d D . . H11S H 0.2406 0.2724 0.0932 0.184 Uiso 1 1 calc R . . C12S C 0.2875(10) 0.1348(7) 0.1037(8) 0.118(4) Uani 1 1 d D . . H12S H 0.2062 0.1221 0.1145 0.141 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 0.02313(8) 0.02107(8) 0.02551(9) -0.01062(6) -0.00491(6) -0.00262(6) Bi2 0.02615(9) 0.02315(8) 0.02410(9) -0.00853(6) -0.00683(6) -0.00135(6) As1 0.0271(2) 0.0228(2) 0.0267(2) -0.01137(17) -0.00717(17) -0.00033(16) As2 0.0249(2) 0.0261(2) 0.0265(2) -0.01025(17) -0.00466(17) -0.00259(16) Cl1 0.0253(5) 0.0214(5) 0.0457(6) -0.0189(4) -0.0068(4) -0.0078(4) Cl2 0.0359(6) 0.0250(5) 0.0189(5) -0.0086(4) -0.0042(4) 0.0056(4) Cl3 0.0219(5) 0.0308(5) 0.0435(6) -0.0170(5) -0.0107(4) -0.0056(4) Cl4 0.0451(6) 0.0214(5) 0.0153(4) -0.0006(4) -0.0051(4) -0.0032(4) S1 0.0213(5) 0.0319(6) 0.0300(6) -0.0135(4) -0.0032(4) -0.0066(4) S2 0.0208(5) 0.0238(5) 0.0360(6) -0.0135(4) -0.0106(4) -0.0004(4) F11 0.046(2) 0.074(3) 0.099(3) -0.044(3) -0.035(2) 0.0249(19) F12 0.055(2) 0.102(3) 0.105(3) -0.073(3) -0.043(2) 0.008(2) F13 0.0354(19) 0.102(3) 0.088(3) -0.025(3) 0.004(2) -0.035(2) F21 0.0352(18) 0.081(3) 0.066(2) -0.032(2) 0.0074(16) -0.0231(18) F22 0.0429(19) 0.066(2) 0.065(2) -0.0246(19) -0.0337(18) 0.0169(17) F23 0.042(2) 0.095(3) 0.123(4) -0.083(3) -0.024(2) -0.006(2) O11 0.0292(17) 0.0334(18) 0.0372(19) -0.0112(15) -0.0058(14) -0.0031(14) O12 0.038(2) 0.071(3) 0.045(2) -0.037(2) -0.0050(17) -0.0096(19) O13 0.045(2) 0.0338(19) 0.045(2) -0.0085(17) 0.0037(17) -0.0103(16) O21 0.0346(19) 0.0362(19) 0.041(2) -0.0173(16) 0.0019(15) -0.0027(15) O22 0.049(2) 0.0262(17) 0.052(2) -0.0119(16) -0.0278(18) 0.0028(15) O23 0.0317(17) 0.0335(18) 0.042(2) -0.0191(15) -0.0140(15) -0.0021(14) C10 0.025(2) 0.060(4) 0.056(3) -0.030(3) -0.012(2) -0.004(2) C11 0.039(3) 0.024(2) 0.028(2) -0.0106(18) -0.0108(19) -0.0012(18) C12 0.047(3) 0.037(3) 0.029(2) -0.010(2) -0.008(2) 0.004(2) C13 0.067(4) 0.040(3) 0.034(3) -0.018(2) 0.000(3) -0.005(3) C14 0.080(5) 0.049(3) 0.032(3) -0.016(2) -0.009(3) -0.025(3) C15 0.060(4) 0.070(4) 0.045(3) -0.015(3) -0.025(3) -0.019(3) C16 0.037(3) 0.052(3) 0.040(3) -0.018(3) -0.012(2) -0.002(2) C20 0.025(2) 0.048(3) 0.051(3) -0.031(3) -0.011(2) -0.004(2) C21 0.029(2) 0.023(2) 0.033(2) -0.0116(18) -0.0040(18) -0.0025(17) C22 0.065(4) 0.039(3) 0.030(3) -0.015(2) -0.004(2) -0.015(3) C23 0.072(4) 0.035(3) 0.035(3) -0.006(2) 0.002(3) -0.020(3) C24 0.037(3) 0.033(3) 0.049(3) -0.020(2) 0.007(2) -0.013(2) C25 0.034(3) 0.032(2) 0.045(3) -0.020(2) -0.009(2) -0.0021(19) C26 0.039(3) 0.026(2) 0.035(3) -0.0130(19) -0.010(2) -0.0003(19) C31 0.026(2) 0.027(2) 0.031(2) -0.0117(18) -0.0077(18) 0.0010(17) C32 0.038(3) 0.039(3) 0.039(3) -0.022(2) -0.007(2) -0.003(2) C33 0.038(3) 0.050(3) 0.048(3) -0.028(3) 0.000(2) 0.001(2) C34 0.028(2) 0.043(3) 0.048(3) -0.013(2) -0.003(2) 0.000(2) C35 0.035(3) 0.047(3) 0.076(4) -0.032(3) -0.001(3) -0.009(2) C36 0.032(3) 0.043(3) 0.063(4) -0.033(3) 0.003(2) -0.006(2) C41 0.024(2) 0.029(2) 0.040(3) -0.012(2) -0.0057(19) -0.0040(17) C42 0.040(3) 0.046(3) 0.041(3) -0.020(2) -0.005(2) -0.013(2) C43 0.045(3) 0.049(3) 0.054(3) -0.019(3) -0.017(3) -0.013(3) C44 0.039(3) 0.050(3) 0.070(4) -0.006(3) -0.021(3) -0.017(3) C45 0.038(3) 0.070(4) 0.054(4) 0.006(3) -0.010(3) -0.026(3) C46 0.035(3) 0.066(4) 0.036(3) -0.002(3) -0.012(2) -0.014(3) C51 0.043(3) 0.031(2) 0.030(2) -0.012(2) -0.007(2) -0.008(2) C52 0.069(4) 0.057(4) 0.041(3) -0.028(3) -0.009(3) 0.009(3) C53 0.100(6) 0.069(5) 0.044(4) -0.031(4) -0.001(4) -0.002(4) C54 0.093(5) 0.058(4) 0.032(3) -0.020(3) -0.008(3) -0.030(4) C55 0.074(4) 0.051(3) 0.038(3) -0.008(3) -0.021(3) -0.027(3) C56 0.048(3) 0.045(3) 0.036(3) -0.014(2) -0.013(2) -0.017(2) C61 0.038(3) 0.026(2) 0.027(2) -0.0097(18) -0.0069(19) 0.0003(18) C62 0.040(3) 0.032(3) 0.044(3) -0.011(2) 0.001(2) -0.003(2) C63 0.064(4) 0.032(3) 0.053(4) -0.008(3) 0.011(3) -0.009(3) C64 0.085(5) 0.031(3) 0.041(3) -0.008(2) -0.006(3) 0.002(3) C65 0.075(4) 0.039(3) 0.051(4) -0.018(3) -0.031(3) 0.015(3) C66 0.049(3) 0.037(3) 0.053(3) -0.020(3) -0.025(3) 0.006(2) C1S 0.066(5) 0.096(7) 0.070(6) 0.013(5) 0.010(4) -0.005(5) C2S 0.082(6) 0.087(6) 0.071(6) 0.001(5) -0.013(5) -0.026(5) C3S 0.104(7) 0.089(6) 0.056(5) -0.002(4) -0.016(5) -0.032(5) C4S 0.089(6) 0.091(7) 0.073(6) -0.028(5) 0.000(5) -0.024(5) C5S 0.110(9) 0.162(13) 0.083(7) -0.072(8) -0.002(6) -0.002(8) C6S 0.103(9) 0.181(14) 0.048(5) -0.023(7) -0.003(5) -0.001(9) C7S 0.114(7) 0.049(4) 0.074(5) -0.017(4) -0.021(5) -0.026(5) C8S 0.115(9) 0.122(10) 0.079(7) -0.051(7) 0.027(6) -0.022(7) C9S 0.181(14) 0.157(13) 0.067(6) -0.032(8) 0.037(8) -0.123(12) C10S 0.31(2) 0.062(6) 0.057(5) 0.002(5) -0.067(10) -0.079(10) C11S 0.25(2) 0.086(9) 0.145(13) -0.045(9) -0.135(14) 0.046(11) C12S 0.139(11) 0.110(9) 0.141(11) -0.060(8) -0.082(9) 0.004(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 Cl1 2.5193(10) . ? Bi1 Cl2 2.5986(10) . ? Bi1 O11 2.665(3) . ? Bi1 O22 2.687(4) . ? Bi1 O13 2.835(4) 2_666 ? Bi1 As1 2.8703(5) . ? Bi1 O23 2.883(3) 2_666 ? Bi2 Cl4 2.5311(10) . ? Bi2 Cl3 2.5357(10) . ? Bi2 O21 2.576(3) . ? Bi2 O12 2.666(4) 2_666 ? Bi2 As2 2.8985(5) . ? Bi2 Cl2 3.1297(10) . ? As1 C31 1.931(5) . ? As1 C21 1.937(5) . ? As1 C11 1.941(5) . ? As2 C41 1.923(5) . ? As2 C51 1.938(5) . ? As2 C61 1.941(5) . ? S1 O12 1.432(4) . ? S1 O13 1.440(4) . ? S1 O11 1.450(4) . ? S1 C10 1.823(5) . ? S2 O23 1.430(3) . ? S2 O21 1.443(4) . ? S2 O22 1.455(4) . ? S2 C20 1.829(5) . ? F11 C10 1.309(7) . ? F12 C10 1.322(7) . ? F13 C10 1.306(7) . ? F21 C20 1.324(7) . ? F22 C20 1.319(7) . ? F23 C20 1.312(6) . ? O12 Bi2 2.666(4) 2_666 ? C11 C12 1.375(7) . ? C11 C16 1.381(7) . ? C12 C13 1.379(8) . ? C13 C14 1.388(10) . ? C14 C15 1.356(10) . ? C15 C16 1.387(8) . ? C21 C22 1.386(7) . ? C21 C26 1.390(7) . ? C22 C23 1.386(8) . ? C23 C24 1.379(9) . ? C24 C25 1.379(8) . ? C25 C26 1.393(7) . ? C31 C36 1.383(7) . ? C31 C32 1.397(7) . ? C32 C33 1.383(8) . ? C33 C34 1.377(8) . ? C34 C35 1.379(8) . ? C35 C36 1.392(8) . ? C41 C46 1.386(7) . ? C41 C42 1.396(8) . ? C42 C43 1.391(8) . ? C43 C44 1.378(9) . ? C44 C45 1.388(10) . ? C45 C46 1.389(8) . ? C51 C56 1.376(8) . ? C51 C52 1.390(8) . ? C52 C53 1.384(9) . ? C53 C54 1.362(11) . ? C54 C55 1.385(10) . ? C55 C56 1.393(8) . ? C61 C66 1.389(7) . ? C61 C62 1.390(8) . ? C62 C63 1.384(8) . ? C63 C64 1.370(10) . ? C64 C65 1.385(11) . ? C65 C66 1.381(8) . ? C1S C2S 1.361(3) . ? C1S C6S 1.361(4) . ? C2S C3S 1.361(3) . ? C3S C4S 1.361(3) . ? C4S C5S 1.361(4) . ? C5S C6S 1.361(4) . ? C7S C12S 1.361(4) . ? C7S C8S 1.361(4) . ? C8S C9S 1.362(4) . ? C9S C10S 1.361(4) . ? C10S C11S 1.361(4) . ? C11S C12S 1.361(4) . ? 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 Cl1 Bi1 Cl2 89.93(4) . . ? Cl1 Bi1 O11 78.19(8) . . ? Cl2 Bi1 O11 166.87(8) . . ? Cl1 Bi1 O22 82.90(9) . . ? Cl2 Bi1 O22 81.29(9) . . ? O11 Bi1 O22 102.50(12) . . ? Cl1 Bi1 O13 153.41(9) . 2_666 ? Cl2 Bi1 O13 79.51(9) . 2_666 ? O11 Bi1 O13 113.62(11) . 2_666 ? O22 Bi1 O13 71.47(12) . 2_666 ? Cl1 Bi1 As1 89.21(3) . . ? Cl2 Bi1 As1 79.92(3) . . ? O11 Bi1 As1 94.18(7) . . ? O22 Bi1 As1 159.61(8) . . ? O13 Bi1 As1 112.49(9) 2_666 . ? Cl1 Bi1 O23 142.08(8) . 2_666 ? Cl2 Bi1 O23 114.98(8) . 2_666 ? O11 Bi1 O23 73.02(11) . 2_666 ? O22 Bi1 O23 126.86(10) . 2_666 ? O13 Bi1 O23 63.54(12) 2_666 2_666 ? As1 Bi1 O23 69.16(7) . 2_666 ? Cl4 Bi2 Cl3 97.34(4) . . ? Cl4 Bi2 O21 84.75(9) . . ? Cl3 Bi2 O21 91.66(9) . . ? Cl4 Bi2 O12 83.87(10) . 2_666 ? Cl3 Bi2 O12 169.45(9) . 2_666 ? O21 Bi2 O12 77.98(12) . 2_666 ? Cl4 Bi2 As2 87.12(3) . . ? Cl3 Bi2 As2 88.56(3) . . ? O21 Bi2 As2 171.83(8) . . ? O12 Bi2 As2 101.98(9) 2_666 . ? Cl4 Bi2 Cl2 155.81(4) . . ? Cl3 Bi2 Cl2 100.73(4) . . ? O21 Bi2 Cl2 110.52(9) . . ? O12 Bi2 Cl2 81.32(10) 2_666 . ? As2 Bi2 Cl2 77.44(2) . . ? C31 As1 C21 106.19(19) . . ? C31 As1 C11 105.0(2) . . ? C21 As1 C11 106.3(2) . . ? C31 As1 Bi1 109.36(14) . . ? C21 As1 Bi1 114.12(14) . . ? C11 As1 Bi1 115.15(14) . . ? C41 As2 C51 105.6(2) . . ? C41 As2 C61 105.4(2) . . ? C51 As2 C61 105.5(2) . . ? C41 As2 Bi2 104.59(14) . . ? C51 As2 Bi2 118.16(16) . . ? C61 As2 Bi2 116.41(14) . . ? Bi1 Cl2 Bi2 106.94(3) . . ? O12 S1 O13 115.8(3) . . ? O12 S1 O11 115.3(2) . . ? O13 S1 O11 111.6(2) . . ? O12 S1 C10 103.2(3) . . ? O13 S1 C10 105.1(3) . . ? O11 S1 C10 104.1(2) . . ? O23 S2 O21 114.8(2) . . ? O23 S2 O22 116.7(2) . . ? O21 S2 O22 112.4(2) . . ? O23 S2 C20 104.3(2) . . ? O21 S2 C20 102.5(2) . . ? O22 S2 C20 104.0(2) . . ? S1 O11 Bi1 111.91(19) . . ? S1 O12 Bi2 131.7(2) . 2_666 ? S2 O21 Bi2 114.9(2) . . ? S2 O22 Bi1 143.1(2) . . ? F13 C10 F11 108.0(5) . . ? F13 C10 F12 109.2(5) . . ? F11 C10 F12 107.9(5) . . ? F13 C10 S1 111.0(4) . . ? F11 C10 S1 110.8(4) . . ? F12 C10 S1 109.9(4) . . ? C12 C11 C16 120.3(5) . . ? C12 C11 As1 118.4(4) . . ? C16 C11 As1 121.3(4) . . ? C11 C12 C13 119.9(6) . . ? C12 C13 C14 119.7(6) . . ? C15 C14 C13 120.2(6) . . ? C14 C15 C16 120.6(6) . . ? C11 C16 C15 119.3(6) . . ? F23 C20 F22 109.3(5) . . ? F23 C20 F21 108.7(5) . . ? F22 C20 F21 107.5(4) . . ? F23 C20 S2 110.3(4) . . ? F22 C20 S2 109.8(4) . . ? F21 C20 S2 111.1(4) . . ? C22 C21 C26 120.3(5) . . ? C22 C21 As1 119.9(4) . . ? C26 C21 As1 119.8(4) . . ? C21 C22 C23 119.7(5) . . ? C24 C23 C22 120.2(5) . . ? C25 C24 C23 120.3(5) . . ? C24 C25 C26 120.1(5) . . ? C21 C26 C25 119.4(5) . . ? C36 C31 C32 119.3(5) . . ? C36 C31 As1 118.3(4) . . ? C32 C31 As1 122.3(4) . . ? C33 C32 C31 119.3(5) . . ? C34 C33 C32 121.1(5) . . ? C33 C34 C35 120.0(5) . . ? C34 C35 C36 119.4(6) . . ? C31 C36 C35 120.9(5) . . ? C46 C41 C42 119.5(5) . . ? C46 C41 As2 122.2(4) . . ? C42 C41 As2 118.1(4) . . ? C43 C42 C41 119.9(5) . . ? C44 C43 C42 120.4(6) . . ? C43 C44 C45 119.6(6) . . ? C44 C45 C46 120.4(6) . . ? C41 C46 C45 120.1(6) . . ? C56 C51 C52 120.1(5) . . ? C56 C51 As2 120.1(4) . . ? C52 C51 As2 119.7(4) . . ? C53 C52 C51 119.6(7) . . ? C54 C53 C52 120.4(7) . . ? C53 C54 C55 120.6(6) . . ? C54 C55 C56 119.5(6) . . ? C51 C56 C55 119.8(6) . . ? C66 C61 C62 120.1(5) . . ? C66 C61 As2 122.5(4) . . ? C62 C61 As2 117.3(4) . . ? C63 C62 C61 119.4(6) . . ? C64 C63 C62 120.6(7) . . ? C63 C64 C65 120.0(6) . . ? C66 C65 C64 120.3(6) . . ? C65 C66 C61 119.6(6) . . ? C2S C1S C6S 120.2(9) . . ? C1S C2S C3S 119.5(8) . . ? C4S C3S C2S 121.0(8) . . ? C3S C4S C5S 118.6(9) . . ? C6S C5S C4S 121.1(10) . . ? C5S C6S C1S 119.5(10) . . ? C12S C7S C8S 121.1(9) . . ? C7S C8S C9S 120.1(10) . . ? C10S C9S C8S 118.1(10) . . ? C9S C10S C11S 122.4(11) . . ? C12S C11S C10S 118.7(11) . . ? C7S C12S C11S 119.4(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Bi1 As1 C31 -137.46(15) . . . . ? Cl2 Bi1 As1 C31 -47.38(15) . . . . ? O11 Bi1 As1 C31 144.44(17) . . . . ? O22 Bi1 As1 C31 -70.5(3) . . . . ? O13 Bi1 As1 C31 26.73(17) 2_666 . . . ? O23 Bi1 As1 C31 74.39(17) 2_666 . . . ? Cl1 Bi1 As1 C21 -18.69(16) . . . . ? Cl2 Bi1 As1 C21 71.38(16) . . . . ? O11 Bi1 As1 C21 -96.79(17) . . . . ? O22 Bi1 As1 C21 48.2(3) . . . . ? O13 Bi1 As1 C21 145.50(18) 2_666 . . . ? O23 Bi1 As1 C21 -166.84(17) 2_666 . . . ? Cl1 Bi1 As1 C11 104.63(17) . . . . ? Cl2 Bi1 As1 C11 -165.29(17) . . . . ? O11 Bi1 As1 C11 26.53(18) . . . . ? O22 Bi1 As1 C11 171.6(3) . . . . ? O13 Bi1 As1 C11 -91.18(19) 2_666 . . . ? O23 Bi1 As1 C11 -43.52(18) 2_666 . . . ? Cl4 Bi2 As2 C41 -74.58(16) . . . . ? Cl3 Bi2 As2 C41 -172.00(16) . . . . ? O21 Bi2 As2 C41 -80.3(6) . . . . ? O12 Bi2 As2 C41 8.52(19) 2_666 . . . ? Cl2 Bi2 As2 C41 86.67(16) . . . . ? Cl4 Bi2 As2 C51 42.46(18) . . . . ? Cl3 Bi2 As2 C51 -54.96(18) . . . . ? O21 Bi2 As2 C51 36.7(6) . . . . ? O12 Bi2 As2 C51 125.6(2) 2_666 . . . ? Cl2 Bi2 As2 C51 -156.29(17) . . . . ? Cl4 Bi2 As2 C61 169.57(17) . . . . ? Cl3 Bi2 As2 C61 72.15(17) . . . . ? O21 Bi2 As2 C61 163.8(6) . . . . ? O12 Bi2 As2 C61 -107.3(2) 2_666 . . . ? Cl2 Bi2 As2 C61 -29.18(17) . . . . ? Cl1 Bi1 Cl2 Bi2 -100.79(4) . . . . ? O11 Bi1 Cl2 Bi2 -125.9(3) . . . . ? O22 Bi1 Cl2 Bi2 -17.96(9) . . . . ? O13 Bi1 Cl2 Bi2 54.66(9) 2_666 . . . ? As1 Bi1 Cl2 Bi2 170.01(4) . . . . ? O23 Bi1 Cl2 Bi2 108.78(8) 2_666 . . . ? Cl4 Bi2 Cl2 Bi1 -124.48(7) . . . . ? Cl3 Bi2 Cl2 Bi1 97.89(4) . . . . ? O21 Bi2 Cl2 Bi1 2.01(10) . . . . ? O12 Bi2 Cl2 Bi1 -71.62(9) 2_666 . . . ? As2 Bi2 Cl2 Bi1 -176.04(4) . . . . ? O12 S1 O11 Bi1 144.7(2) . . . . ? O13 S1 O11 Bi1 9.8(3) . . . . ? C10 S1 O11 Bi1 -103.1(2) . . . . ? Cl1 Bi1 O11 S1 122.5(2) . . . . ? Cl2 Bi1 O11 S1 148.1(2) . . . . ? O22 Bi1 O11 S1 42.6(2) . . . . ? O13 Bi1 O11 S1 -32.4(2) 2_666 . . . ? As1 Bi1 O11 S1 -149.21(18) . . . . ? O23 Bi1 O11 S1 -82.5(2) 2_666 . . . ? O13 S1 O12 Bi2 33.8(4) . . . 2_666 ? O11 S1 O12 Bi2 -99.2(3) . . . 2_666 ? C10 S1 O12 Bi2 148.0(3) . . . 2_666 ? O23 S2 O21 Bi2 -130.0(2) . . . . ? O22 S2 O21 Bi2 6.5(3) . . . . ? C20 S2 O21 Bi2 117.7(2) . . . . ? Cl4 Bi2 O21 S2 174.6(2) . . . . ? Cl3 Bi2 O21 S2 -88.2(2) . . . . ? O12 Bi2 O21 S2 89.8(2) 2_666 . . . ? As2 Bi2 O21 S2 -179.6(4) . . . . ? Cl2 Bi2 O21 S2 13.9(2) . . . . ? O23 S2 O22 Bi1 27.7(5) . . . . ? O21 S2 O22 Bi1 -107.9(4) . . . . ? C20 S2 O22 Bi1 141.9(4) . . . . ? Cl1 Bi1 O22 S2 -154.4(4) . . . . ? Cl2 Bi1 O22 S2 114.6(4) . . . . ? O11 Bi1 O22 S2 -78.2(4) . . . . ? O13 Bi1 O22 S2 32.8(4) 2_666 . . . ? As1 Bi1 O22 S2 137.7(3) . . . . ? O23 Bi1 O22 S2 -0.2(5) 2_666 . . . ? O12 S1 C10 F13 50.4(5) . . . . ? O13 S1 C10 F13 172.2(4) . . . . ? O11 S1 C10 F13 -70.3(5) . . . . ? O12 S1 C10 F11 -69.5(5) . . . . ? O13 S1 C10 F11 52.2(5) . . . . ? O11 S1 C10 F11 169.7(4) . . . . ? O12 S1 C10 F12 171.3(5) . . . . ? O13 S1 C10 F12 -66.9(5) . . . . ? O11 S1 C10 F12 50.6(5) . . . . ? C31 As1 C11 C12 -154.4(4) . . . . ? C21 As1 C11 C12 93.3(4) . . . . ? Bi1 As1 C11 C12 -34.1(4) . . . . ? C31 As1 C11 C16 22.3(5) . . . . ? C21 As1 C11 C16 -90.0(5) . . . . ? Bi1 As1 C11 C16 142.6(4) . . . . ? C16 C11 C12 C13 0.3(8) . . . . ? As1 C11 C12 C13 177.0(4) . . . . ? C11 C12 C13 C14 0.3(9) . . . . ? C12 C13 C14 C15 -0.3(9) . . . . ? C13 C14 C15 C16 -0.4(10) . . . . ? C12 C11 C16 C15 -1.0(9) . . . . ? As1 C11 C16 C15 -177.5(5) . . . . ? C14 C15 C16 C11 1.0(10) . . . . ? O23 S2 C20 F23 178.1(4) . . . . ? O21 S2 C20 F23 -62.0(5) . . . . ? O22 S2 C20 F23 55.3(5) . . . . ? O23 S2 C20 F22 -61.3(4) . . . . ? O21 S2 C20 F22 58.6(4) . . . . ? O22 S2 C20 F22 175.9(4) . . . . ? O23 S2 C20 F21 57.4(4) . . . . ? O21 S2 C20 F21 177.4(4) . . . . ? O22 S2 C20 F21 -65.4(4) . . . . ? C31 As1 C21 C22 -106.4(4) . . . . ? C11 As1 C21 C22 5.0(5) . . . . ? Bi1 As1 C21 C22 133.0(4) . . . . ? C31 As1 C21 C26 75.5(4) . . . . ? C11 As1 C21 C26 -173.1(4) . . . . ? Bi1 As1 C21 C26 -45.1(4) . . . . ? C26 C21 C22 C23 -0.2(9) . . . . ? As1 C21 C22 C23 -178.3(5) . . . . ? C21 C22 C23 C24 1.1(10) . . . . ? C22 C23 C24 C25 -1.9(9) . . . . ? C23 C24 C25 C26 1.6(8) . . . . ? C22 C21 C26 C25 -0.1(8) . . . . ? As1 C21 C26 C25 178.0(4) . . . . ? C24 C25 C26 C21 -0.6(8) . . . . ? C21 As1 C31 C36 163.0(4) . . . . ? C11 As1 C31 C36 50.6(5) . . . . ? Bi1 As1 C31 C36 -73.5(4) . . . . ? C21 As1 C31 C32 -19.6(5) . . . . ? C11 As1 C31 C32 -132.0(4) . . . . ? Bi1 As1 C31 C32 103.9(4) . . . . ? C36 C31 C32 C33 -0.6(8) . . . . ? As1 C31 C32 C33 -178.0(4) . . . . ? C31 C32 C33 C34 0.7(9) . . . . ? C32 C33 C34 C35 -1.0(9) . . . . ? C33 C34 C35 C36 1.2(10) . . . . ? C32 C31 C36 C35 0.8(9) . . . . ? As1 C31 C36 C35 178.3(5) . . . . ? C34 C35 C36 C31 -1.1(10) . . . . ? C51 As2 C41 C46 -16.7(5) . . . . ? C61 As2 C41 C46 -128.1(5) . . . . ? Bi2 As2 C41 C46 108.7(5) . . . . ? C51 As2 C41 C42 168.9(4) . . . . ? C61 As2 C41 C42 57.5(4) . . . . ? Bi2 As2 C41 C42 -65.8(4) . . . . ? C46 C41 C42 C43 1.6(8) . . . . ? As2 C41 C42 C43 176.2(4) . . . . ? C41 C42 C43 C44 -2.1(9) . . . . ? C42 C43 C44 C45 0.9(10) . . . . ? C43 C44 C45 C46 0.6(11) . . . . ? C42 C41 C46 C45 0.0(9) . . . . ? As2 C41 C46 C45 -174.4(5) . . . . ? C44 C45 C46 C41 -1.1(11) . . . . ? C41 As2 C51 C56 122.7(4) . . . . ? C61 As2 C51 C56 -126.0(4) . . . . ? Bi2 As2 C51 C56 6.2(5) . . . . ? C41 As2 C51 C52 -56.7(5) . . . . ? C61 As2 C51 C52 54.7(5) . . . . ? Bi2 As2 C51 C52 -173.2(4) . . . . ? C56 C51 C52 C53 -1.8(10) . . . . ? As2 C51 C52 C53 177.6(6) . . . . ? C51 C52 C53 C54 0.6(12) . . . . ? C52 C53 C54 C55 1.5(12) . . . . ? C53 C54 C55 C56 -2.5(10) . . . . ? C52 C51 C56 C55 0.8(9) . . . . ? As2 C51 C56 C55 -178.6(4) . . . . ? C54 C55 C56 C51 1.3(9) . . . . ? C41 As2 C61 C66 6.0(5) . . . . ? C51 As2 C61 C66 -105.5(5) . . . . ? Bi2 As2 C61 C66 121.4(4) . . . . ? C41 As2 C61 C62 -171.2(4) . . . . ? C51 As2 C61 C62 77.3(4) . . . . ? Bi2 As2 C61 C62 -55.8(4) . . . . ? C66 C61 C62 C63 0.5(8) . . . . ? As2 C61 C62 C63 177.7(5) . . . . ? C61 C62 C63 C64 -1.0(10) . . . . ? C62 C63 C64 C65 0.7(10) . . . . ? C63 C64 C65 C66 0.1(10) . . . . ? C64 C65 C66 C61 -0.6(9) . . . . ? C62 C61 C66 C65 0.3(8) . . . . ? As2 C61 C66 C65 -176.8(4) . . . . ? C6S C1S C2S C3S 1.8(16) . . . . ? C1S C2S C3S C4S -3.0(16) . . . . ? C2S C3S C4S C5S 2.6(16) . . . . ? C3S C4S C5S C6S -1.1(17) . . . . ? C4S C5S C6S C1S -0.1(19) . . . . ? C2S C1S C6S C5S -0.3(18) . . . . ? C12S C7S C8S C9S -3.1(17) . . . . ? C7S C8S C9S C10S -1.2(17) . . . . ? C8S C9S C10S C11S 4.1(18) . . . . ? C9S C10S C11S C12S -2.7(19) . . . . ? C8S C7S C12S C11S 4.5(18) . . . . ? C10S C11S C12S C7S -1.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.590 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.137 # Attachment 'C25H23AlBiCl6Sb.CIF.txt' data_dal09d1 _database_code_depnum_ccdc_archive 'CCDC 755447' #TrackingRef 'C25H23AlBiCl6Sb.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 Bi Cl2 Sb, C7 H8, Al Cl4' _chemical_formula_sum 'C25 H23 Al Bi Cl6 Sb' _chemical_formula_weight 893.84 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0275(10) _cell_length_b 11.0904(11) _cell_length_c 15.4057(16) _cell_angle_alpha 92.5010(10) _cell_angle_beta 106.0140(10) _cell_angle_gamma 112.4710(10) _cell_volume 1500.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 7.335 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1310 _exptl_absorpt_correction_T_max 0.6431 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13108 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6781 _reflns_number_gt 6142 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0393P)^2^+5.0667P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6781 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Bi Bi 0.25170(2) 0.298238(16) 0.329348(12) 0.02219(6) Uani 1 1 d . . . Sb Sb 0.38973(3) 0.40738(3) 0.18328(2) 0.02180(8) Uani 1 1 d . . . Cl1 Cl 0.01131(15) 0.27214(14) 0.21136(10) 0.0368(3) Uani 1 1 d . . . Cl2 Cl 0.3233(2) 0.53089(13) 0.39531(11) 0.0474(4) Uani 1 1 d . . . C11 C 0.2887(5) 0.5279(5) 0.1140(4) 0.0248(10) Uani 1 1 d . . . C12 C 0.2383(6) 0.5064(5) 0.0186(4) 0.0303(11) Uani 1 1 d . . . H12 H 0.2477 0.4379 -0.0151 0.036 Uiso 1 1 calc R . . C13 C 0.1739(6) 0.5866(5) -0.0267(4) 0.0314(11) Uani 1 1 d . . . H13 H 0.1385 0.5725 -0.0917 0.038 Uiso 1 1 calc R . . C14 C 0.1610(6) 0.6865(5) 0.0224(4) 0.0352(12) Uani 1 1 d . . . H14 H 0.1177 0.7415 -0.0087 0.042 Uiso 1 1 calc R . . C15 C 0.2109(7) 0.7062(6) 0.1164(4) 0.0393(13) Uani 1 1 d . . . H15 H 0.2015 0.7749 0.1498 0.047 Uiso 1 1 calc R . . C16 C 0.2745(7) 0.6277(5) 0.1634(4) 0.0351(12) Uani 1 1 d . . . H16 H 0.3081 0.6419 0.2285 0.042 Uiso 1 1 calc R . . C21 C 0.3472(6) 0.2596(5) 0.0759(3) 0.0239(10) Uani 1 1 d . . . C22 C 0.4654(6) 0.2409(5) 0.0554(4) 0.0309(11) Uani 1 1 d . . . H22 H 0.5681 0.2971 0.0887 0.037 Uiso 1 1 calc R . . C23 C 0.4327(6) 0.1396(6) -0.0139(4) 0.0378(13) Uani 1 1 d . . . H23 H 0.5133 0.1273 -0.0285 0.045 Uiso 1 1 calc R . . C24 C 0.2838(7) 0.0569(6) -0.0617(4) 0.0348(12) Uani 1 1 d . . . H24 H 0.2624 -0.0132 -0.1082 0.042 Uiso 1 1 calc R . . C25 C 0.1651(6) 0.0754(5) -0.0424(4) 0.0321(11) Uani 1 1 d . . . H25 H 0.0626 0.0187 -0.0759 0.039 Uiso 1 1 calc R . . C26 C 0.1970(6) 0.1774(5) 0.0264(3) 0.0271(10) Uani 1 1 d . . . H26 H 0.1162 0.1909 0.0395 0.032 Uiso 1 1 calc R . . C31 C 0.6266(5) 0.5241(5) 0.2202(3) 0.0246(10) Uani 1 1 d . . . C32 C 0.6776(6) 0.6543(5) 0.2043(4) 0.0334(12) Uani 1 1 d . . . H32 H 0.6068 0.6910 0.1789 0.040 Uiso 1 1 calc R . . C33 C 0.8330(7) 0.7299(6) 0.2259(4) 0.0435(15) Uani 1 1 d . . . H33 H 0.8683 0.8187 0.2153 0.052 Uiso 1 1 calc R . . C34 C 0.9362(7) 0.6775(6) 0.2626(4) 0.0406(14) Uani 1 1 d . . . H34 H 1.0421 0.7300 0.2768 0.049 Uiso 1 1 calc R . . C35 C 0.8859(6) 0.5480(6) 0.2789(4) 0.0373(13) Uani 1 1 d . . . H35 H 0.9574 0.5121 0.3043 0.045 Uiso 1 1 calc R . . C36 C 0.7317(6) 0.4712(5) 0.2582(4) 0.0312(11) Uani 1 1 d . . . H36 H 0.6973 0.3828 0.2697 0.037 Uiso 1 1 calc R . . Cl3 Cl 0.22113(14) 0.03534(12) 0.22111(9) 0.0292(3) Uani 1 1 d . . . Cl4 Cl 0.38631(18) -0.11843(13) 0.37911(10) 0.0398(3) Uani 1 1 d . . . Cl5 Cl 0.54208(14) 0.23356(13) 0.39435(9) 0.0320(3) Uani 1 1 d . . . Cl6 Cl 0.5774(2) 0.0385(2) 0.22889(13) 0.0603(5) Uani 1 1 d . . . Al Al 0.43630(17) 0.04279(15) 0.30715(11) 0.0269(3) Uani 1 1 d . . . C1S C 0.0487(6) 0.2283(6) 0.4611(4) 0.0361(13) Uani 1 1 d . . . C2S C 0.1907(6) 0.2750(6) 0.5278(4) 0.0337(12) Uani 1 1 d . . . H2S H 0.2281 0.3581 0.5659 0.040 Uiso 1 1 calc R . . C3S C 0.2793(7) 0.2023(6) 0.5397(4) 0.0361(12) Uani 1 1 d . . . H3S H 0.3755 0.2357 0.5861 0.043 Uiso 1 1 calc R . . C4S C 0.2278(7) 0.0820(6) 0.4844(4) 0.0365(13) Uani 1 1 d . . . H4S H 0.2880 0.0323 0.4925 0.044 Uiso 1 1 calc R . . C5S C 0.0876(7) 0.0348(6) 0.4172(4) 0.0389(13) Uani 1 1 d . . . H5S H 0.0514 -0.0480 0.3789 0.047 Uiso 1 1 calc R . . C6S C -0.0013(6) 0.1072(6) 0.4050(4) 0.0405(14) Uani 1 1 d . . . H6S H -0.0968 0.0739 0.3579 0.049 Uiso 1 1 calc R . . C7S C -0.0475(9) 0.3042(9) 0.4518(6) 0.064(2) Uani 1 1 d . . . H7SA H -0.1110 0.2876 0.3878 0.077 Uiso 1 1 calc R . . H7SB H 0.0179 0.3989 0.4708 0.077 Uiso 1 1 calc R . . H7SC H -0.1127 0.2759 0.4907 0.077 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 Bi 0.02321(10) 0.01837(9) 0.02496(10) 0.00467(6) 0.00870(7) 0.00764(7) Sb 0.02219(16) 0.01821(14) 0.02465(17) 0.00427(12) 0.00898(13) 0.00678(12) Cl1 0.0277(6) 0.0433(7) 0.0368(7) 0.0107(6) 0.0057(5) 0.0145(6) Cl2 0.0734(11) 0.0211(6) 0.0415(8) -0.0004(6) 0.0218(8) 0.0113(7) C11 0.024(2) 0.020(2) 0.030(3) 0.0057(19) 0.010(2) 0.0068(19) C12 0.030(3) 0.030(3) 0.032(3) 0.008(2) 0.012(2) 0.012(2) C13 0.027(3) 0.037(3) 0.027(3) 0.013(2) 0.008(2) 0.009(2) C14 0.030(3) 0.030(3) 0.049(3) 0.013(2) 0.011(2) 0.016(2) C15 0.050(4) 0.028(3) 0.045(3) 0.005(2) 0.013(3) 0.023(3) C16 0.045(3) 0.030(3) 0.031(3) 0.002(2) 0.010(2) 0.018(2) C21 0.026(2) 0.019(2) 0.029(3) 0.0063(19) 0.013(2) 0.0080(19) C22 0.026(3) 0.026(2) 0.037(3) 0.001(2) 0.014(2) 0.006(2) C23 0.032(3) 0.039(3) 0.045(3) -0.002(3) 0.019(3) 0.013(2) C24 0.041(3) 0.032(3) 0.032(3) -0.002(2) 0.015(2) 0.013(2) C25 0.028(3) 0.027(3) 0.032(3) 0.000(2) 0.008(2) 0.004(2) C26 0.024(2) 0.029(2) 0.026(3) 0.005(2) 0.008(2) 0.009(2) C31 0.020(2) 0.026(2) 0.023(2) 0.0025(19) 0.0050(18) 0.0043(19) C32 0.029(3) 0.025(3) 0.036(3) 0.009(2) 0.005(2) 0.005(2) C33 0.039(3) 0.032(3) 0.041(3) 0.011(3) 0.008(3) -0.004(2) C34 0.029(3) 0.043(3) 0.036(3) 0.000(3) 0.011(2) 0.000(2) C35 0.025(3) 0.044(3) 0.039(3) 0.004(3) 0.009(2) 0.011(2) C36 0.027(3) 0.030(3) 0.036(3) 0.005(2) 0.012(2) 0.010(2) Cl3 0.0291(6) 0.0252(6) 0.0294(6) 0.0032(5) 0.0016(5) 0.0125(5) Cl4 0.0497(8) 0.0303(6) 0.0402(8) 0.0098(6) 0.0056(6) 0.0227(6) Cl5 0.0249(6) 0.0301(6) 0.0340(7) 0.0011(5) 0.0056(5) 0.0069(5) Cl6 0.0462(9) 0.0909(14) 0.0510(10) -0.0040(9) 0.0247(8) 0.0308(9) Al 0.0249(7) 0.0303(8) 0.0277(8) 0.0035(6) 0.0076(6) 0.0141(6) C1S 0.030(3) 0.050(3) 0.036(3) 0.017(3) 0.019(2) 0.017(3) C2S 0.036(3) 0.035(3) 0.032(3) 0.005(2) 0.014(2) 0.015(2) C3S 0.032(3) 0.044(3) 0.034(3) 0.011(3) 0.013(2) 0.015(3) C4S 0.040(3) 0.039(3) 0.042(3) 0.017(3) 0.025(3) 0.019(3) C5S 0.048(3) 0.026(3) 0.039(3) 0.007(2) 0.025(3) 0.003(2) C6S 0.023(3) 0.056(4) 0.029(3) 0.014(3) 0.008(2) 0.001(3) C7S 0.059(5) 0.093(6) 0.070(5) 0.033(5) 0.029(4) 0.054(5) _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 Bi Cl2 2.4817(14) . ? Bi Cl1 2.4903(13) . ? Bi Sb 3.0199(4) . ? Sb C21 2.109(5) . ? Sb C31 2.117(5) . ? Sb C11 2.125(5) . ? C11 C16 1.389(7) . ? C11 C12 1.393(7) . ? C12 C13 1.394(7) . ? C13 C14 1.381(8) . ? C14 C15 1.372(9) . ? C15 C16 1.383(8) . ? C21 C26 1.392(7) . ? C21 C22 1.392(7) . ? C22 C23 1.389(8) . ? C23 C24 1.379(8) . ? C24 C25 1.387(8) . ? C25 C26 1.392(7) . ? C31 C32 1.394(7) . ? C31 C36 1.399(7) . ? C32 C33 1.390(8) . ? C33 C34 1.377(9) . ? C34 C35 1.389(9) . ? C35 C36 1.384(7) . ? Cl3 Al 2.1669(19) . ? Cl4 Al 2.115(2) . ? Cl5 Al 2.158(2) . ? Cl6 Al 2.108(2) . ? C1S C2S 1.391(8) . ? C1S C6S 1.396(9) . ? C1S C7S 1.488(9) . ? C2S C3S 1.394(8) . ? C3S C4S 1.380(9) . ? C4S C5S 1.381(9) . ? C5S C6S 1.395(9) . ? 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 Cl2 Bi Cl1 95.70(6) . . ? Cl2 Bi Sb 87.02(4) . . ? Cl1 Bi Sb 82.84(3) . . ? C21 Sb C31 104.15(19) . . ? C21 Sb C11 102.60(19) . . ? C31 Sb C11 104.30(18) . . ? C21 Sb Bi 113.19(12) . . ? C31 Sb Bi 119.46(13) . . ? C11 Sb Bi 111.43(13) . . ? C16 C11 C12 120.5(5) . . ? C16 C11 Sb 120.3(4) . . ? C12 C11 Sb 119.1(4) . . ? C11 C12 C13 119.0(5) . . ? C14 C13 C12 120.4(5) . . ? C15 C14 C13 119.7(5) . . ? C14 C15 C16 121.3(5) . . ? C15 C16 C11 119.0(5) . . ? C26 C21 C22 119.8(5) . . ? C26 C21 Sb 118.7(4) . . ? C22 C21 Sb 121.5(4) . . ? C23 C22 C21 119.8(5) . . ? C24 C23 C22 120.2(5) . . ? C23 C24 C25 120.5(5) . . ? C24 C25 C26 119.6(5) . . ? C21 C26 C25 120.1(5) . . ? C32 C31 C36 119.9(5) . . ? C32 C31 Sb 119.1(4) . . ? C36 C31 Sb 120.9(4) . . ? C33 C32 C31 119.3(5) . . ? C34 C33 C32 120.8(5) . . ? C33 C34 C35 120.1(5) . . ? C36 C35 C34 120.0(6) . . ? C35 C36 C31 119.9(5) . . ? Cl6 Al Cl4 112.33(10) . . ? Cl6 Al Cl5 107.95(9) . . ? Cl4 Al Cl5 113.66(9) . . ? Cl6 Al Cl3 111.21(10) . . ? Cl4 Al Cl3 107.18(9) . . ? Cl5 Al Cl3 104.25(8) . . ? C2S C1S C6S 117.8(5) . . ? C2S C1S C7S 120.7(6) . . ? C6S C1S C7S 121.4(6) . . ? C1S C2S C3S 121.3(6) . . ? C4S C3S C2S 120.3(6) . . ? C3S C4S C5S 119.2(6) . . ? C4S C5S C6S 120.8(6) . . ? C5S C6S C1S 120.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Bi Sb C21 -171.23(15) . . . . ? Cl1 Bi Sb C21 -75.11(15) . . . . ? Cl2 Bi Sb C31 65.56(16) . . . . ? Cl1 Bi Sb C31 161.69(16) . . . . ? Cl2 Bi Sb C11 -56.20(15) . . . . ? Cl1 Bi Sb C11 39.93(15) . . . . ? C21 Sb C11 C16 171.3(4) . . . . ? C31 Sb C11 C16 -80.3(4) . . . . ? Bi Sb C11 C16 49.9(4) . . . . ? C21 Sb C11 C12 -9.3(4) . . . . ? C31 Sb C11 C12 99.1(4) . . . . ? Bi Sb C11 C12 -130.7(4) . . . . ? C16 C11 C12 C13 0.2(8) . . . . ? Sb C11 C12 C13 -179.2(4) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C12 C13 C14 C15 -0.5(8) . . . . ? C13 C14 C15 C16 0.1(9) . . . . ? C14 C15 C16 C11 0.4(9) . . . . ? C12 C11 C16 C15 -0.6(8) . . . . ? Sb C11 C16 C15 178.8(4) . . . . ? C31 Sb C21 C26 -170.4(4) . . . . ? C11 Sb C21 C26 -61.9(4) . . . . ? Bi Sb C21 C26 58.3(4) . . . . ? C31 Sb C21 C22 11.3(4) . . . . ? C11 Sb C21 C22 119.8(4) . . . . ? Bi Sb C21 C22 -120.0(4) . . . . ? C26 C21 C22 C23 -0.4(8) . . . . ? Sb C21 C22 C23 177.9(4) . . . . ? C21 C22 C23 C24 -0.7(9) . . . . ? C22 C23 C24 C25 1.2(9) . . . . ? C23 C24 C25 C26 -0.6(9) . . . . ? C22 C21 C26 C25 1.0(7) . . . . ? Sb C21 C26 C25 -177.3(4) . . . . ? C24 C25 C26 C21 -0.5(8) . . . . ? C21 Sb C31 C32 113.2(4) . . . . ? C11 Sb C31 C32 6.0(5) . . . . ? Bi Sb C31 C32 -119.3(4) . . . . ? C21 Sb C31 C36 -65.2(5) . . . . ? C11 Sb C31 C36 -172.5(4) . . . . ? Bi Sb C31 C36 62.3(5) . . . . ? C36 C31 C32 C33 0.4(9) . . . . ? Sb C31 C32 C33 -178.1(4) . . . . ? C31 C32 C33 C34 0.1(10) . . . . ? C32 C33 C34 C35 -0.3(10) . . . . ? C33 C34 C35 C36 0.1(9) . . . . ? C34 C35 C36 C31 0.4(9) . . . . ? C32 C31 C36 C35 -0.7(8) . . . . ? Sb C31 C36 C35 177.8(4) . . . . ? C6S C1S C2S C3S -1.4(8) . . . . ? C7S C1S C2S C3S 177.3(6) . . . . ? C1S C2S C3S C4S 0.7(8) . . . . ? C2S C3S C4S C5S 0.0(8) . . . . ? C3S C4S C5S C6S 0.1(8) . . . . ? C4S C5S C6S C1S -0.8(8) . . . . ? C2S C1S C6S C5S 1.5(8) . . . . ? C7S C1S C6S C5S -177.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.552 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.147 # Attachment 'C52H40As2Bi2F12O12S4.CIF.txt' data_dal0958 _database_code_depnum_ccdc_archive 'CCDC 755448' #TrackingRef 'C52H40As2Bi2F12O12S4.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 As2 Bi2 F12 O12 S4' _chemical_formula_weight 1780.88 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' As As 0.0499 2.0058 '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 10.9929(6) _cell_length_b 14.9895(9) _cell_length_c 18.7965(11) _cell_angle_alpha 77.2400(10) _cell_angle_beta 81.0850(10) _cell_angle_gamma 88.2030(10) _cell_volume 2984.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9748 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.71 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 7.225 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0791 _exptl_absorpt_correction_T_max 0.2236 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26194 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13503 _reflns_number_gt 12538 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0283P)^2^+3.3066P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13503 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _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 0.400984(9) 0.637092(7) 0.212244(6) 0.02263(3) Uani 1 1 d . . . Bi2 Bi 0.083845(9) 0.345582(7) 0.267953(5) 0.02077(3) Uani 1 1 d . . . As1 As 0.44426(2) 0.807821(18) 0.109290(15) 0.02049(6) Uani 1 1 d . . . As2 As 0.04925(2) 0.183933(18) 0.380808(15) 0.02037(6) Uani 1 1 d . . . S1 S 0.14786(7) 0.57427(5) 0.15666(5) 0.03065(16) Uani 1 1 d . . . S2 S 0.36227(7) 0.39486(5) 0.30326(5) 0.03079(16) Uani 1 1 d . . . S3 S 0.51051(8) 0.74157(6) 0.32709(4) 0.03496(17) Uani 1 1 d . . . S4 S -0.05822(8) 0.22486(5) 0.17655(4) 0.03043(16) Uani 1 1 d . . . F11 F -0.0670(2) 0.6323(2) 0.20858(17) 0.0667(7) Uani 1 1 d . . . F12 F 0.0147(3) 0.7128(2) 0.10580(15) 0.0847(10) Uani 1 1 d . . . F13 F 0.0825(2) 0.72127(16) 0.20400(14) 0.0569(6) Uani 1 1 d . . . F21 F 0.5761(2) 0.32124(19) 0.3130(3) 0.1063(15) Uani 1 1 d . . . F22 F 0.4277(2) 0.22646(16) 0.3341(2) 0.0975(13) Uani 1 1 d . . . F23 F 0.4570(4) 0.3031(3) 0.4133(2) 0.1123(14) Uani 1 1 d . . . F31 F 0.3956(3) 0.7265(2) 0.46078(12) 0.0684(8) Uani 1 1 d . . . F32 F 0.5070(3) 0.6099(2) 0.44527(15) 0.0962(13) Uani 1 1 d . . . F33 F 0.3349(3) 0.63122(18) 0.40310(15) 0.0662(7) Uani 1 1 d . . . F41 F 0.0270(4) 0.22010(19) 0.04142(13) 0.0866(11) Uani 1 1 d . . . F42 F -0.1004(4) 0.3289(2) 0.05306(17) 0.1185(17) Uani 1 1 d . . . F43 F 0.0847(5) 0.3349(2) 0.07566(18) 0.1179(17) Uani 1 1 d . . . O11 O 0.2609(2) 0.62446(16) 0.12052(13) 0.0353(5) Uani 1 1 d . . . O12 O 0.1579(2) 0.52764(17) 0.23131(16) 0.0492(7) Uani 1 1 d . . . O13 O 0.0957(2) 0.5225(2) 0.11380(19) 0.0588(8) Uani 1 1 d . . . O21 O 0.23943(19) 0.36541(15) 0.34373(12) 0.0295(5) Uani 1 1 d . . . O22 O 0.4061(2) 0.47743(16) 0.31675(15) 0.0408(6) Uani 1 1 d . . . O23 O 0.3763(3) 0.3905(2) 0.22656(16) 0.0614(8) Uani 1 1 d . . . O31 O 0.5447(2) 0.67176(16) 0.28213(12) 0.0328(5) Uani 1 1 d . . . O32 O 0.4138(3) 0.80000(17) 0.30011(13) 0.0436(6) Uani 1 1 d . . . O33 O 0.6128(3) 0.7813(3) 0.34555(19) 0.0683(9) Uani 1 1 d . . . O41 O -0.0802(2) 0.30215(15) 0.21427(12) 0.0306(5) Uani 1 1 d . . . O42 O 0.0473(3) 0.17302(17) 0.19744(13) 0.0430(6) Uani 1 1 d . . . O43 O -0.1659(3) 0.1757(2) 0.1762(2) 0.0668(9) Uani 1 1 d . . . C1 C 0.0376(3) 0.6656(2) 0.16868(19) 0.0361(7) Uani 1 1 d . . . C2 C 0.4612(4) 0.3067(3) 0.3438(3) 0.0612(14) Uani 1 1 d . . . C3 C 0.4334(4) 0.6714(3) 0.4145(2) 0.0515(11) Uani 1 1 d . . . C4 C -0.0086(6) 0.2810(3) 0.0807(2) 0.0644(15) Uani 1 1 d . . . C11 C 0.5565(3) 0.58083(19) 0.14406(17) 0.0261(6) Uani 1 1 d . . . C12 C 0.6646(3) 0.5549(2) 0.1719(2) 0.0377(7) Uani 1 1 d . . . H12 H 0.6725 0.5593 0.2207 0.045 Uiso 1 1 calc R . . C13 C 0.7617(3) 0.5224(3) 0.1279(2) 0.0460(9) Uani 1 1 d . . . H13 H 0.8359 0.5038 0.1469 0.055 Uiso 1 1 calc R . . C14 C 0.7510(3) 0.5169(2) 0.0568(2) 0.0435(9) Uani 1 1 d . . . H14 H 0.8180 0.4954 0.0267 0.052 Uiso 1 1 calc R . . C15 C 0.6426(4) 0.5426(3) 0.0294(2) 0.0430(8) Uani 1 1 d . . . H15 H 0.6356 0.5392 -0.0197 0.052 Uiso 1 1 calc R . . C16 C 0.5441(3) 0.5734(2) 0.07302(19) 0.0357(7) Uani 1 1 d . . . H16 H 0.4688 0.5893 0.0546 0.043 Uiso 1 1 calc R . . C21 C -0.0575(3) 0.41137(18) 0.33861(16) 0.0233(5) Uani 1 1 d . . . C22 C -0.0214(4) 0.4486(3) 0.3931(2) 0.0540(12) Uani 1 1 d . . . H22 H 0.0620 0.4448 0.4012 0.065 Uiso 1 1 calc R . . C23 C -0.1079(4) 0.4915(4) 0.4357(3) 0.0687(16) Uani 1 1 d . . . H23 H -0.0836 0.5168 0.4734 0.082 Uiso 1 1 calc R . . C24 C -0.2288(4) 0.4979(3) 0.4242(2) 0.0468(9) Uani 1 1 d . . . H24 H -0.2876 0.5269 0.4542 0.056 Uiso 1 1 calc R . . C25 C -0.2640(3) 0.4625(3) 0.3695(2) 0.0394(8) Uani 1 1 d . . . H25 H -0.3472 0.4676 0.3611 0.047 Uiso 1 1 calc R . . C26 C -0.1784(3) 0.4191(2) 0.32614(19) 0.0330(7) Uani 1 1 d . . . H26 H -0.2030 0.3948 0.2880 0.040 Uiso 1 1 calc R . . C31 C 0.4942(3) 0.7984(2) 0.00803(16) 0.0248(6) Uani 1 1 d . . . C32 C 0.4143(3) 0.7583(2) -0.02690(18) 0.0345(7) Uani 1 1 d . . . H32 H 0.3346 0.7387 -0.0019 0.041 Uiso 1 1 calc R . . C33 C 0.4521(4) 0.7474(3) -0.0980(2) 0.0436(8) Uani 1 1 d . . . H33 H 0.3983 0.7202 -0.1222 0.052 Uiso 1 1 calc R . . C34 C 0.5692(4) 0.7764(3) -0.1345(2) 0.0466(9) Uani 1 1 d . . . H34 H 0.5951 0.7686 -0.1833 0.056 Uiso 1 1 calc R . . C35 C 0.6470(3) 0.8161(3) -0.09988(19) 0.0426(8) Uani 1 1 d . . . H35 H 0.7266 0.8360 -0.1250 0.051 Uiso 1 1 calc R . . C36 C 0.6102(3) 0.8274(2) -0.02837(18) 0.0320(7) Uani 1 1 d . . . H36 H 0.6642 0.8550 -0.0046 0.038 Uiso 1 1 calc R . . C41 C 0.5743(3) 0.87460(19) 0.13260(15) 0.0227(5) Uani 1 1 d . . . C42 C 0.6850(3) 0.8299(2) 0.14407(18) 0.0314(6) Uani 1 1 d . . . H42 H 0.6960 0.7684 0.1389 0.038 Uiso 1 1 calc R . . C43 C 0.7792(3) 0.8754(2) 0.1631(2) 0.0373(7) Uani 1 1 d . . . H43 H 0.8554 0.8456 0.1700 0.045 Uiso 1 1 calc R . . C44 C 0.7609(3) 0.9647(2) 0.17200(18) 0.0349(7) Uani 1 1 d . . . H44 H 0.8244 0.9957 0.1859 0.042 Uiso 1 1 calc R . . C45 C 0.6507(3) 1.0088(2) 0.16076(17) 0.0312(6) Uani 1 1 d . . . H45 H 0.6393 1.0699 0.1667 0.037 Uiso 1 1 calc R . . C46 C 0.5567(3) 0.9643(2) 0.14082(16) 0.0255(6) Uani 1 1 d . . . H46 H 0.4813 0.9947 0.1329 0.031 Uiso 1 1 calc R . . C51 C 0.3018(3) 0.88649(19) 0.10849(16) 0.0238(5) Uani 1 1 d . . . C52 C 0.2621(3) 0.9282(2) 0.04277(18) 0.0324(7) Uani 1 1 d . . . H52 H 0.3052 0.9185 -0.0027 0.039 Uiso 1 1 calc R . . C53 C 0.1588(3) 0.9844(2) 0.0436(2) 0.0386(8) Uani 1 1 d . . . H53 H 0.1312 1.0130 -0.0014 0.046 Uiso 1 1 calc R . . C54 C 0.0965(3) 0.9985(2) 0.1099(2) 0.0370(7) Uani 1 1 d . . . H54 H 0.0264 1.0372 0.1104 0.044 Uiso 1 1 calc R . . C55 C 0.1356(3) 0.9570(2) 0.1750(2) 0.0381(8) Uani 1 1 d . . . H55 H 0.0922 0.9671 0.2203 0.046 Uiso 1 1 calc R . . C56 C 0.2383(3) 0.9001(2) 0.17542(18) 0.0311(6) Uani 1 1 d . . . H56 H 0.2647 0.8709 0.2207 0.037 Uiso 1 1 calc R . . C61 C 0.0177(3) 0.2070(2) 0.47923(16) 0.0265(6) Uani 1 1 d . . . C62 C -0.0936(3) 0.1832(2) 0.52368(18) 0.0357(7) Uani 1 1 d . . . H62 H -0.1553 0.1541 0.5065 0.043 Uiso 1 1 calc R . . C63 C -0.1151(4) 0.2019(3) 0.5938(2) 0.0526(11) Uani 1 1 d . . . H63 H -0.1917 0.1860 0.6246 0.063 Uiso 1 1 calc R . . C64 C -0.0251(5) 0.2436(3) 0.6182(2) 0.0572(12) Uani 1 1 d . . . H64 H -0.0402 0.2568 0.6660 0.069 Uiso 1 1 calc R . . C65 C 0.0869(5) 0.2666(3) 0.5743(2) 0.0535(11) Uani 1 1 d . . . H65 H 0.1488 0.2947 0.5921 0.064 Uiso 1 1 calc R . . C66 C 0.1093(4) 0.2487(2) 0.50394(19) 0.0383(8) Uani 1 1 d . . . H66 H 0.1860 0.2647 0.4732 0.046 Uiso 1 1 calc R . . C71 C 0.1898(2) 0.10353(19) 0.37944(15) 0.0221(5) Uani 1 1 d . . . C72 C 0.2348(3) 0.0637(2) 0.44404(18) 0.0331(7) Uani 1 1 d . . . H72 H 0.1989 0.0776 0.4896 0.040 Uiso 1 1 calc R . . C73 C 0.3334(3) 0.0028(3) 0.4415(2) 0.0412(8) Uani 1 1 d . . . H73 H 0.3653 -0.0246 0.4853 0.049 Uiso 1 1 calc R . . C74 C 0.3846(3) -0.0176(2) 0.3750(2) 0.0395(8) Uani 1 1 d . . . H74 H 0.4510 -0.0595 0.3734 0.047 Uiso 1 1 calc R . . C75 C 0.3398(3) 0.0224(3) 0.3110(2) 0.0415(8) Uani 1 1 d . . . H75 H 0.3756 0.0081 0.2656 0.050 Uiso 1 1 calc R . . C76 C 0.2425(3) 0.0838(2) 0.31256(18) 0.0329(7) Uani 1 1 d . . . H76 H 0.2122 0.1119 0.2683 0.039 Uiso 1 1 calc R . . C81 C -0.0865(3) 0.11103(19) 0.37115(15) 0.0232(5) Uani 1 1 d . . . C82 C -0.0664(3) 0.0211(2) 0.36390(16) 0.0264(6) Uani 1 1 d . . . H82 H 0.0126 -0.0058 0.3670 0.032 Uiso 1 1 calc R . . C83 C -0.1627(3) -0.0289(2) 0.35215(18) 0.0346(7) Uani 1 1 d . . . H83 H -0.1496 -0.0901 0.3468 0.042 Uiso 1 1 calc R . . C84 C -0.2778(3) 0.0105(3) 0.3483(2) 0.0403(8) Uani 1 1 d . . . H84 H -0.3435 -0.0242 0.3406 0.048 Uiso 1 1 calc R . . C85 C -0.2977(3) 0.0989(3) 0.3553(2) 0.0421(8) Uani 1 1 d . . . H85 H -0.3770 0.1253 0.3523 0.051 Uiso 1 1 calc R . . C86 C -0.2024(3) 0.1504(2) 0.36700(19) 0.0335(7) Uani 1 1 d . . . H86 H -0.2162 0.2117 0.3721 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 0.02030(5) 0.02055(6) 0.02579(6) -0.00444(4) -0.00021(4) -0.00167(4) Bi2 0.01994(5) 0.01873(6) 0.02366(6) -0.00447(4) -0.00295(4) -0.00322(4) As1 0.01982(13) 0.01919(13) 0.02217(13) -0.00585(10) 0.00003(10) -0.00208(10) As2 0.02038(13) 0.01846(13) 0.02159(13) -0.00488(10) -0.00015(10) -0.00120(10) S1 0.0215(3) 0.0234(4) 0.0474(5) -0.0079(3) -0.0059(3) -0.0025(3) S2 0.0226(3) 0.0274(4) 0.0434(4) -0.0075(3) -0.0080(3) -0.0036(3) S3 0.0390(4) 0.0397(4) 0.0305(4) -0.0166(3) -0.0062(3) 0.0033(3) S4 0.0414(4) 0.0247(4) 0.0290(4) -0.0103(3) -0.0103(3) -0.0012(3) F11 0.0297(11) 0.0809(19) 0.095(2) -0.0390(16) 0.0022(12) 0.0019(11) F12 0.111(2) 0.088(2) 0.0541(16) -0.0073(15) -0.0338(16) 0.0588(19) F13 0.0628(15) 0.0496(13) 0.0672(16) -0.0375(12) -0.0010(12) -0.0040(11) F21 0.0252(12) 0.0466(15) 0.250(5) -0.029(2) -0.0325(19) 0.0015(10) F22 0.0491(15) 0.0283(13) 0.220(4) -0.0206(18) -0.046(2) -0.0007(11) F23 0.120(3) 0.107(3) 0.109(3) 0.023(2) -0.082(3) 0.004(2) F31 0.0776(18) 0.099(2) 0.0315(11) -0.0261(13) -0.0059(11) 0.0329(16) F32 0.106(3) 0.113(3) 0.0477(15) 0.0124(16) -0.0038(16) 0.070(2) F33 0.0703(18) 0.0613(16) 0.0554(15) -0.0050(12) 0.0159(13) -0.0051(13) F41 0.172(3) 0.0582(16) 0.0308(12) -0.0182(11) -0.0156(16) 0.0399(19) F42 0.216(5) 0.091(2) 0.0556(18) -0.0165(16) -0.059(2) 0.091(3) F43 0.201(5) 0.065(2) 0.064(2) -0.0076(16) 0.055(2) -0.051(3) O11 0.0281(11) 0.0373(13) 0.0386(12) -0.0080(10) 0.0015(9) -0.0088(9) O12 0.0382(13) 0.0371(14) 0.0616(17) 0.0166(12) -0.0122(12) -0.0093(11) O13 0.0349(14) 0.0613(18) 0.097(2) -0.0540(18) -0.0091(14) -0.0016(12) O21 0.0234(10) 0.0316(11) 0.0320(11) -0.0014(9) -0.0070(9) -0.0037(8) O22 0.0383(13) 0.0271(12) 0.0580(16) -0.0065(11) -0.0133(12) -0.0062(10) O23 0.0447(16) 0.093(2) 0.0503(17) -0.0288(16) 0.0043(13) -0.0235(15) O31 0.0298(11) 0.0388(13) 0.0339(12) -0.0168(10) -0.0057(9) 0.0062(9) O32 0.0613(16) 0.0337(13) 0.0345(13) -0.0086(10) -0.0052(12) 0.0157(12) O33 0.0569(19) 0.097(3) 0.069(2) -0.0537(19) -0.0099(16) -0.0140(17) O41 0.0313(11) 0.0319(12) 0.0349(12) -0.0172(9) -0.0107(9) 0.0026(9) O42 0.0592(16) 0.0396(14) 0.0318(12) -0.0100(10) -0.0118(11) 0.0182(12) O43 0.066(2) 0.066(2) 0.084(2) -0.0403(18) -0.0201(17) -0.0218(16) C1 0.0343(17) 0.0399(19) 0.0369(17) -0.0131(14) -0.0090(14) 0.0075(14) C2 0.0347(19) 0.032(2) 0.119(4) -0.003(2) -0.039(2) -0.0004(15) C3 0.058(2) 0.064(3) 0.0285(17) -0.0062(17) -0.0044(17) 0.031(2) C4 0.131(5) 0.033(2) 0.0279(18) -0.0047(15) -0.016(2) 0.023(3) C11 0.0258(14) 0.0209(14) 0.0304(15) -0.0068(11) 0.0014(11) -0.0022(11) C12 0.0322(16) 0.0418(19) 0.0417(18) -0.0146(15) -0.0068(14) 0.0074(14) C13 0.0308(17) 0.051(2) 0.059(2) -0.0196(19) -0.0063(16) 0.0117(16) C14 0.0407(19) 0.0366(19) 0.051(2) -0.0175(16) 0.0113(16) 0.0020(15) C15 0.053(2) 0.041(2) 0.0371(18) -0.0184(15) -0.0012(16) 0.0065(16) C16 0.0392(18) 0.0323(17) 0.0384(18) -0.0142(14) -0.0058(14) 0.0046(14) C21 0.0253(14) 0.0172(13) 0.0286(14) -0.0069(11) -0.0059(11) 0.0008(10) C22 0.042(2) 0.071(3) 0.074(3) -0.055(2) -0.036(2) 0.0284(19) C23 0.063(3) 0.096(4) 0.080(3) -0.071(3) -0.046(2) 0.047(3) C24 0.044(2) 0.054(2) 0.049(2) -0.0272(18) -0.0084(17) 0.0196(17) C25 0.0239(15) 0.045(2) 0.053(2) -0.0202(17) -0.0054(14) 0.0027(14) C26 0.0259(15) 0.0403(18) 0.0373(17) -0.0169(14) -0.0054(13) -0.0028(13) C31 0.0274(14) 0.0235(14) 0.0235(13) -0.0079(11) 0.0004(11) 0.0000(11) C32 0.0404(18) 0.0332(17) 0.0318(16) -0.0102(13) -0.0062(14) -0.0051(13) C33 0.059(2) 0.042(2) 0.0344(18) -0.0154(15) -0.0084(16) -0.0042(17) C34 0.064(3) 0.047(2) 0.0298(17) -0.0184(16) 0.0024(17) 0.0039(18) C35 0.0400(19) 0.051(2) 0.0336(18) -0.0129(16) 0.0106(15) 0.0014(16) C36 0.0307(15) 0.0345(17) 0.0300(15) -0.0107(13) 0.0028(12) -0.0018(13) C41 0.0222(13) 0.0234(14) 0.0221(13) -0.0061(11) -0.0001(10) -0.0038(10) C42 0.0275(15) 0.0253(15) 0.0419(18) -0.0084(13) -0.0054(13) -0.0005(12) C43 0.0266(15) 0.0397(19) 0.047(2) -0.0108(15) -0.0086(14) 0.0004(13) C44 0.0317(16) 0.0393(18) 0.0369(17) -0.0125(14) -0.0074(13) -0.0102(13) C45 0.0374(17) 0.0276(16) 0.0305(15) -0.0111(12) -0.0020(13) -0.0067(12) C46 0.0287(14) 0.0228(14) 0.0247(14) -0.0065(11) -0.0014(11) -0.0003(11) C51 0.0209(13) 0.0212(13) 0.0286(14) -0.0058(11) -0.0008(11) -0.0021(10) C52 0.0275(15) 0.0374(18) 0.0291(15) -0.0030(13) -0.0015(12) 0.0025(13) C53 0.0333(17) 0.0385(19) 0.0406(18) -0.0002(15) -0.0089(14) 0.0074(14) C54 0.0247(15) 0.0319(17) 0.055(2) -0.0129(15) -0.0050(14) 0.0045(12) C55 0.0330(17) 0.0393(19) 0.0441(19) -0.0198(15) 0.0018(14) 0.0050(14) C56 0.0303(15) 0.0344(17) 0.0304(15) -0.0116(13) -0.0039(12) 0.0024(13) C61 0.0353(16) 0.0218(14) 0.0232(13) -0.0067(11) -0.0047(12) 0.0043(11) C62 0.0335(16) 0.0420(19) 0.0293(16) -0.0081(14) 0.0017(13) 0.0083(14) C63 0.053(2) 0.070(3) 0.0323(19) -0.0154(18) 0.0046(17) 0.020(2) C64 0.082(3) 0.062(3) 0.0320(19) -0.0228(19) -0.005(2) 0.018(2) C65 0.085(3) 0.046(2) 0.037(2) -0.0180(17) -0.019(2) -0.002(2) C66 0.050(2) 0.0358(18) 0.0297(16) -0.0086(14) -0.0030(15) -0.0090(15) C71 0.0193(12) 0.0202(13) 0.0265(14) -0.0064(11) -0.0003(10) -0.0025(10) C72 0.0315(16) 0.0325(17) 0.0312(16) -0.0015(13) -0.0001(13) 0.0028(13) C73 0.0331(17) 0.0389(19) 0.046(2) 0.0018(15) -0.0068(15) 0.0060(14) C74 0.0227(15) 0.0307(17) 0.066(2) -0.0142(16) -0.0036(15) 0.0028(12) C75 0.0288(16) 0.051(2) 0.051(2) -0.0320(18) 0.0020(15) 0.0036(15) C76 0.0286(15) 0.0415(18) 0.0312(16) -0.0153(14) -0.0023(12) 0.0003(13) C81 0.0233(13) 0.0229(14) 0.0220(13) -0.0028(10) -0.0018(10) -0.0039(10) C82 0.0284(14) 0.0243(14) 0.0258(14) -0.0049(11) -0.0024(11) -0.0025(11) C83 0.0410(18) 0.0293(16) 0.0346(17) -0.0080(13) -0.0057(14) -0.0079(13) C84 0.0344(17) 0.045(2) 0.0411(19) -0.0066(16) -0.0052(15) -0.0157(15) C85 0.0248(15) 0.045(2) 0.055(2) -0.0071(17) -0.0087(15) 0.0004(14) C86 0.0261(15) 0.0300(16) 0.0426(18) -0.0041(13) -0.0057(13) 0.0019(12) _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 C11 2.232(3) . ? Bi1 O31 2.342(2) . ? Bi1 O11 2.523(2) . ? Bi1 O22 2.746(2) . ? Bi1 As1 2.8502(3) . ? Bi2 C21 2.235(3) . ? Bi2 O41 2.371(2) . ? Bi2 O21 2.453(2) . ? Bi2 O12 2.778(3) . ? Bi2 As2 2.8377(3) . ? As1 C41 1.927(3) . ? As1 C51 1.931(3) . ? As1 C31 1.932(3) . ? As2 C71 1.930(3) . ? As2 C81 1.931(3) . ? As2 C61 1.933(3) . ? S1 O13 1.424(3) . ? S1 O12 1.442(3) . ? S1 O11 1.464(2) . ? S1 C1 1.828(3) . ? S2 O22 1.429(2) . ? S2 O23 1.442(3) . ? S2 O21 1.472(2) . ? S2 C2 1.798(4) . ? S3 O33 1.412(3) . ? S3 O32 1.438(3) . ? S3 O31 1.489(2) . ? S3 C3 1.840(4) . ? S4 O43 1.415(3) . ? S4 O42 1.433(3) . ? S4 O41 1.482(2) . ? S4 C4 1.818(4) . ? F11 C1 1.318(4) . ? F12 C1 1.293(4) . ? F13 C1 1.324(4) . ? F21 C2 1.308(5) . ? F22 C2 1.327(5) . ? F23 C2 1.289(7) . ? F31 C3 1.340(5) . ? F32 C3 1.305(4) . ? F33 C3 1.323(6) . ? F41 C4 1.311(5) . ? F42 C4 1.325(6) . ? F43 C4 1.303(7) . ? C11 C12 1.383(4) . ? C11 C16 1.392(5) . ? C12 C13 1.390(5) . ? C13 C14 1.381(6) . ? C14 C15 1.381(6) . ? C15 C16 1.386(5) . ? C21 C26 1.382(4) . ? C21 C22 1.382(4) . ? C22 C23 1.383(5) . ? C23 C24 1.376(6) . ? C24 C25 1.364(5) . ? C25 C26 1.390(5) . ? C31 C36 1.384(4) . ? C31 C32 1.396(4) . ? C32 C33 1.381(5) . ? C33 C34 1.395(6) . ? C34 C35 1.373(6) . ? C35 C36 1.388(5) . ? C41 C46 1.390(4) . ? C41 C42 1.394(4) . ? C42 C43 1.390(5) . ? C43 C44 1.391(5) . ? C44 C45 1.384(5) . ? C45 C46 1.388(4) . ? C51 C52 1.384(4) . ? C51 C56 1.394(4) . ? C52 C53 1.393(4) . ? C53 C54 1.383(5) . ? C54 C55 1.370(5) . ? C55 C56 1.394(4) . ? C61 C62 1.379(4) . ? C61 C66 1.390(5) . ? C62 C63 1.390(5) . ? C63 C64 1.374(7) . ? C64 C65 1.380(7) . ? C65 C66 1.390(5) . ? C71 C72 1.387(4) . ? C71 C76 1.390(4) . ? C72 C73 1.397(5) . ? C73 C74 1.383(5) . ? C74 C75 1.376(5) . ? C75 C76 1.389(5) . ? C81 C86 1.392(4) . ? C81 C82 1.392(4) . ? C82 C83 1.387(4) . ? C83 C84 1.385(5) . ? C84 C85 1.368(5) . ? C85 C86 1.392(5) . ? 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 C11 Bi1 O31 87.74(9) . . ? C11 Bi1 O11 90.08(9) . . ? O31 Bi1 O11 169.92(8) . . ? C11 Bi1 O22 87.31(9) . . ? O31 Bi1 O22 78.05(8) . . ? O11 Bi1 O22 111.69(7) . . ? C11 Bi1 As1 87.40(8) . . ? O31 Bi1 As1 91.57(6) . . ? O11 Bi1 As1 78.50(5) . . ? O22 Bi1 As1 168.52(5) . . ? C21 Bi2 O41 87.22(9) . . ? C21 Bi2 O21 90.30(9) . . ? O41 Bi2 O21 168.72(8) . . ? C21 Bi2 O12 77.08(9) . . ? O41 Bi2 O12 118.70(8) . . ? O21 Bi2 O12 71.29(7) . . ? C21 Bi2 As2 87.40(7) . . ? O41 Bi2 As2 90.26(6) . . ? O21 Bi2 As2 78.63(5) . . ? O12 Bi2 As2 145.81(6) . . ? C41 As1 C51 106.55(12) . . ? C41 As1 C31 105.56(12) . . ? C51 As1 C31 105.63(12) . . ? C41 As1 Bi1 110.76(8) . . ? C51 As1 Bi1 113.00(8) . . ? C31 As1 Bi1 114.72(9) . . ? C71 As2 C81 104.99(12) . . ? C71 As2 C61 105.85(12) . . ? C81 As2 C61 106.79(13) . . ? C71 As2 Bi2 112.93(8) . . ? C81 As2 Bi2 112.10(8) . . ? C61 As2 Bi2 113.53(9) . . ? O13 S1 O12 115.85(19) . . ? O13 S1 O11 115.73(17) . . ? O12 S1 O11 111.40(14) . . ? O13 S1 C1 105.52(16) . . ? O12 S1 C1 103.43(17) . . ? O11 S1 C1 103.01(16) . . ? O22 S2 O23 114.88(18) . . ? O22 S2 O21 114.61(15) . . ? O23 S2 O21 112.90(15) . . ? O22 S2 C2 104.95(17) . . ? O23 S2 C2 104.9(2) . . ? O21 S2 C2 102.93(18) . . ? O33 S3 O32 119.0(2) . . ? O33 S3 O31 113.62(17) . . ? O32 S3 O31 111.32(14) . . ? O33 S3 C3 105.3(2) . . ? O32 S3 C3 103.32(17) . . ? O31 S3 C3 101.94(17) . . ? O43 S4 O42 117.48(19) . . ? O43 S4 O41 114.11(17) . . ? O42 S4 O41 111.05(14) . . ? O43 S4 C4 105.3(2) . . ? O42 S4 C4 103.8(2) . . ? O41 S4 C4 103.34(16) . . ? S1 O11 Bi1 111.55(13) . . ? S1 O12 Bi2 114.72(16) . . ? S2 O21 Bi2 115.93(12) . . ? S2 O22 Bi1 119.28(14) . . ? S3 O31 Bi1 118.01(12) . . ? S4 O41 Bi2 117.36(12) . . ? F12 C1 F11 108.6(3) . . ? F12 C1 F13 108.5(3) . . ? F11 C1 F13 107.3(3) . . ? F12 C1 S1 111.3(2) . . ? F11 C1 S1 111.2(3) . . ? F13 C1 S1 109.7(2) . . ? F23 C2 F21 107.2(4) . . ? F23 C2 F22 109.6(4) . . ? F21 C2 F22 107.8(4) . . ? F23 C2 S2 111.2(4) . . ? F21 C2 S2 111.4(3) . . ? F22 C2 S2 109.6(3) . . ? F32 C3 F33 109.9(4) . . ? F32 C3 F31 108.7(3) . . ? F33 C3 F31 107.8(3) . . ? F32 C3 S3 111.8(3) . . ? F33 C3 S3 110.1(3) . . ? F31 C3 S3 108.5(3) . . ? F43 C4 F41 107.7(5) . . ? F43 C4 F42 109.8(4) . . ? F41 C4 F42 108.7(4) . . ? F43 C4 S4 110.2(3) . . ? F41 C4 S4 110.2(3) . . ? F42 C4 S4 110.2(4) . . ? C12 C11 C16 120.4(3) . . ? C12 C11 Bi1 120.2(2) . . ? C16 C11 Bi1 119.4(2) . . ? C11 C12 C13 119.4(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C11 119.4(3) . . ? C26 C21 C22 119.9(3) . . ? C26 C21 Bi2 120.9(2) . . ? C22 C21 Bi2 119.1(2) . . ? C21 C22 C23 119.3(3) . . ? C24 C23 C22 120.9(3) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C26 120.2(3) . . ? C21 C26 C25 119.9(3) . . ? C36 C31 C32 120.4(3) . . ? C36 C31 As1 120.2(2) . . ? C32 C31 As1 119.4(2) . . ? C33 C32 C31 119.5(3) . . ? C32 C33 C34 120.1(3) . . ? C35 C34 C33 120.1(3) . . ? C34 C35 C36 120.4(3) . . ? C31 C36 C35 119.6(3) . . ? C46 C41 C42 120.5(3) . . ? C46 C41 As1 120.9(2) . . ? C42 C41 As1 118.5(2) . . ? C43 C42 C41 119.9(3) . . ? C42 C43 C44 119.4(3) . . ? C45 C44 C43 120.4(3) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 119.2(3) . . ? C52 C51 C56 120.3(3) . . ? C52 C51 As1 120.8(2) . . ? C56 C51 As1 118.9(2) . . ? C51 C52 C53 119.8(3) . . ? C54 C53 C52 119.9(3) . . ? C55 C54 C53 120.3(3) . . ? C54 C55 C56 120.7(3) . . ? C51 C56 C55 119.0(3) . . ? C62 C61 C66 120.8(3) . . ? C62 C61 As2 120.7(2) . . ? C66 C61 As2 118.6(2) . . ? C61 C62 C63 119.7(4) . . ? C64 C63 C62 119.7(4) . . ? C63 C64 C65 120.8(4) . . ? C64 C65 C66 120.0(4) . . ? C65 C66 C61 119.0(4) . . ? C72 C71 C76 120.5(3) . . ? C72 C71 As2 120.9(2) . . ? C76 C71 As2 118.5(2) . . ? C71 C72 C73 119.4(3) . . ? C74 C73 C72 119.9(3) . . ? C75 C74 C73 120.4(3) . . ? C74 C75 C76 120.4(3) . . ? C75 C76 C71 119.4(3) . . ? C86 C81 C82 120.3(3) . . ? C86 C81 As2 119.8(2) . . ? C82 C81 As2 119.8(2) . . ? C83 C82 C81 119.4(3) . . ? C84 C83 C82 120.0(3) . . ? C85 C84 C83 120.7(3) . . ? C84 C85 C86 120.3(3) . . ? C81 C86 C85 119.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Bi1 As1 C41 -83.56(12) . . . . ? O31 Bi1 As1 C41 4.11(10) . . . . ? O11 Bi1 As1 C41 -174.17(10) . . . . ? O22 Bi1 As1 C41 -20.9(3) . . . . ? C11 Bi1 As1 C51 156.99(12) . . . . ? O31 Bi1 As1 C51 -115.35(11) . . . . ? O11 Bi1 As1 C51 66.38(11) . . . . ? O22 Bi1 As1 C51 -140.4(3) . . . . ? C11 Bi1 As1 C31 35.81(12) . . . . ? O31 Bi1 As1 C31 123.47(11) . . . . ? O11 Bi1 As1 C31 -54.80(11) . . . . ? O22 Bi1 As1 C31 98.4(3) . . . . ? C21 Bi2 As2 C71 -156.11(12) . . . . ? O41 Bi2 As2 C71 116.69(10) . . . . ? O21 Bi2 As2 C71 -65.28(10) . . . . ? O12 Bi2 As2 C71 -93.82(13) . . . . ? C21 Bi2 As2 C81 85.54(12) . . . . ? O41 Bi2 As2 C81 -1.67(10) . . . . ? O21 Bi2 As2 C81 176.36(11) . . . . ? O12 Bi2 As2 C81 147.82(13) . . . . ? C21 Bi2 As2 C61 -35.59(12) . . . . ? O41 Bi2 As2 C61 -122.80(11) . . . . ? O21 Bi2 As2 C61 55.23(11) . . . . ? O12 Bi2 As2 C61 26.69(14) . . . . ? O13 S1 O11 Bi1 -148.30(16) . . . . ? O12 S1 O11 Bi1 -13.17(19) . . . . ? C1 S1 O11 Bi1 97.10(15) . . . . ? C11 Bi1 O11 S1 127.56(15) . . . . ? O31 Bi1 O11 S1 -155.0(3) . . . . ? O22 Bi1 O11 S1 40.43(15) . . . . ? As1 Bi1 O11 S1 -145.11(13) . . . . ? O13 S1 O12 Bi2 3.2(2) . . . . ? O11 S1 O12 Bi2 -131.85(13) . . . . ? C1 S1 O12 Bi2 118.15(16) . . . . ? C21 Bi2 O12 S1 -113.27(17) . . . . ? O41 Bi2 O12 S1 -33.78(19) . . . . ? O21 Bi2 O12 S1 151.95(17) . . . . ? As2 Bi2 O12 S1 -178.41(7) . . . . ? O22 S2 O21 Bi2 123.10(15) . . . . ? O23 S2 O21 Bi2 -11.0(2) . . . . ? C2 S2 O21 Bi2 -123.6(2) . . . . ? C21 Bi2 O21 S2 -138.63(14) . . . . ? O41 Bi2 O21 S2 144.2(3) . . . . ? O12 Bi2 O21 S2 -62.39(13) . . . . ? As2 Bi2 O21 S2 134.08(13) . . . . ? O23 S2 O22 Bi1 29.6(2) . . . . ? O21 S2 O22 Bi1 -103.61(16) . . . . ? C2 S2 O22 Bi1 144.2(2) . . . . ? C11 Bi1 O22 S2 -72.31(17) . . . . ? O31 Bi1 O22 S2 -160.57(17) . . . . ? O11 Bi1 O22 S2 16.71(18) . . . . ? As1 Bi1 O22 S2 -134.9(2) . . . . ? O33 S3 O31 Bi1 -158.73(19) . . . . ? O32 S3 O31 Bi1 -21.1(2) . . . . ? C3 S3 O31 Bi1 88.46(18) . . . . ? C11 Bi1 O31 S3 160.11(16) . . . . ? O11 Bi1 O31 S3 82.5(4) . . . . ? O22 Bi1 O31 S3 -112.17(16) . . . . ? As1 Bi1 O31 S3 72.77(14) . . . . ? O43 S4 O41 Bi2 152.27(18) . . . . ? O42 S4 O41 Bi2 16.7(2) . . . . ? C4 S4 O41 Bi2 -94.0(2) . . . . ? C21 Bi2 O41 S4 -159.07(16) . . . . ? O21 Bi2 O41 S4 -81.6(4) . . . . ? O12 Bi2 O41 S4 127.29(14) . . . . ? As2 Bi2 O41 S4 -71.69(14) . . . . ? O13 S1 C1 F12 -55.7(3) . . . . ? O12 S1 C1 F12 -177.8(3) . . . . ? O11 S1 C1 F12 66.1(3) . . . . ? O13 S1 C1 F11 65.6(3) . . . . ? O12 S1 C1 F11 -56.6(3) . . . . ? O11 S1 C1 F11 -172.7(2) . . . . ? O13 S1 C1 F13 -175.8(3) . . . . ? O12 S1 C1 F13 62.1(3) . . . . ? O11 S1 C1 F13 -54.1(3) . . . . ? O22 S2 C2 F23 58.7(4) . . . . ? O23 S2 C2 F23 -179.9(3) . . . . ? O21 S2 C2 F23 -61.6(3) . . . . ? O22 S2 C2 F21 -60.8(4) . . . . ? O23 S2 C2 F21 60.6(4) . . . . ? O21 S2 C2 F21 179.0(4) . . . . ? O22 S2 C2 F22 -180.0(4) . . . . ? O23 S2 C2 F22 -58.5(4) . . . . ? O21 S2 C2 F22 59.8(4) . . . . ? O33 S3 C3 F32 -57.9(4) . . . . ? O32 S3 C3 F32 176.5(3) . . . . ? O31 S3 C3 F32 60.9(4) . . . . ? O33 S3 C3 F33 179.7(3) . . . . ? O32 S3 C3 F33 54.1(3) . . . . ? O31 S3 C3 F33 -61.5(3) . . . . ? O33 S3 C3 F31 62.0(3) . . . . ? O32 S3 C3 F31 -63.6(3) . . . . ? O31 S3 C3 F31 -179.2(3) . . . . ? O43 S4 C4 F43 174.6(3) . . . . ? O42 S4 C4 F43 -61.4(4) . . . . ? O41 S4 C4 F43 54.6(4) . . . . ? O43 S4 C4 F41 -66.7(5) . . . . ? O42 S4 C4 F41 57.3(5) . . . . ? O41 S4 C4 F41 173.3(4) . . . . ? O43 S4 C4 F42 53.3(4) . . . . ? O42 S4 C4 F42 177.3(3) . . . . ? O41 S4 C4 F42 -66.7(4) . . . . ? O31 Bi1 C11 C12 20.7(3) . . . . ? O11 Bi1 C11 C12 -169.1(3) . . . . ? O22 Bi1 C11 C12 -57.4(3) . . . . ? As1 Bi1 C11 C12 112.4(3) . . . . ? O31 Bi1 C11 C16 -158.3(3) . . . . ? O11 Bi1 C11 C16 11.8(3) . . . . ? O22 Bi1 C11 C16 123.5(3) . . . . ? As1 Bi1 C11 C16 -66.6(2) . . . . ? C16 C11 C12 C13 0.8(5) . . . . ? Bi1 C11 C12 C13 -178.2(3) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C11 2.0(6) . . . . ? C12 C11 C16 C15 -2.1(5) . . . . ? Bi1 C11 C16 C15 176.9(3) . . . . ? O41 Bi2 C21 C26 -8.3(3) . . . . ? O21 Bi2 C21 C26 -177.3(3) . . . . ? O12 Bi2 C21 C26 112.0(3) . . . . ? As2 Bi2 C21 C26 -98.7(2) . . . . ? O41 Bi2 C21 C22 174.9(3) . . . . ? O21 Bi2 C21 C22 5.9(3) . . . . ? O12 Bi2 C21 C22 -64.8(3) . . . . ? As2 Bi2 C21 C22 84.5(3) . . . . ? C26 C21 C22 C23 1.5(6) . . . . ? Bi2 C21 C22 C23 178.4(4) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C22 C23 C24 C25 -0.7(8) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C22 C21 C26 C25 -1.5(5) . . . . ? Bi2 C21 C26 C25 -178.2(3) . . . . ? C24 C25 C26 C21 0.3(6) . . . . ? C41 As1 C31 C36 7.0(3) . . . . ? C51 As1 C31 C36 119.7(3) . . . . ? Bi1 As1 C31 C36 -115.2(2) . . . . ? C41 As1 C31 C32 -175.8(2) . . . . ? C51 As1 C31 C32 -63.1(3) . . . . ? Bi1 As1 C31 C32 62.0(3) . . . . ? C36 C31 C32 C33 0.3(5) . . . . ? As1 C31 C32 C33 -176.9(3) . . . . ? C31 C32 C33 C34 -0.1(6) . . . . ? C32 C33 C34 C35 -0.2(6) . . . . ? C33 C34 C35 C36 0.2(6) . . . . ? C32 C31 C36 C35 -0.3(5) . . . . ? As1 C31 C36 C35 176.8(3) . . . . ? C34 C35 C36 C31 0.0(5) . . . . ? C51 As1 C41 C46 -3.7(3) . . . . ? C31 As1 C41 C46 108.3(2) . . . . ? Bi1 As1 C41 C46 -127.0(2) . . . . ? C51 As1 C41 C42 173.7(2) . . . . ? C31 As1 C41 C42 -74.3(3) . . . . ? Bi1 As1 C41 C42 50.4(2) . . . . ? C46 C41 C42 C43 -0.7(5) . . . . ? As1 C41 C42 C43 -178.1(3) . . . . ? C41 C42 C43 C44 1.3(5) . . . . ? C42 C43 C44 C45 -1.1(5) . . . . ? C43 C44 C45 C46 0.3(5) . . . . ? C44 C45 C46 C41 0.3(5) . . . . ? C42 C41 C46 C45 -0.1(4) . . . . ? As1 C41 C46 C45 177.2(2) . . . . ? C41 As1 C51 C52 107.3(3) . . . . ? C31 As1 C51 C52 -4.7(3) . . . . ? Bi1 As1 C51 C52 -130.9(2) . . . . ? C41 As1 C51 C56 -73.4(3) . . . . ? C31 As1 C51 C56 174.7(2) . . . . ? Bi1 As1 C51 C56 48.5(3) . . . . ? C56 C51 C52 C53 0.4(5) . . . . ? As1 C51 C52 C53 179.8(3) . . . . ? C51 C52 C53 C54 0.2(5) . . . . ? C52 C53 C54 C55 -0.4(5) . . . . ? C53 C54 C55 C56 0.0(5) . . . . ? C52 C51 C56 C55 -0.8(5) . . . . ? As1 C51 C56 C55 179.9(3) . . . . ? C54 C55 C56 C51 0.6(5) . . . . ? C71 As2 C61 C62 -119.9(3) . . . . ? C81 As2 C61 C62 -8.4(3) . . . . ? Bi2 As2 C61 C62 115.7(2) . . . . ? C71 As2 C61 C66 60.6(3) . . . . ? C81 As2 C61 C66 172.1(2) . . . . ? Bi2 As2 C61 C66 -63.8(3) . . . . ? C66 C61 C62 C63 0.7(5) . . . . ? As2 C61 C62 C63 -178.8(3) . . . . ? C61 C62 C63 C64 -0.3(6) . . . . ? C62 C63 C64 C65 -0.5(7) . . . . ? C63 C64 C65 C66 0.8(7) . . . . ? C64 C65 C66 C61 -0.5(6) . . . . ? C62 C61 C66 C65 -0.3(5) . . . . ? As2 C61 C66 C65 179.2(3) . . . . ? C81 As2 C71 C72 -103.1(3) . . . . ? C61 As2 C71 C72 9.7(3) . . . . ? Bi2 As2 C71 C72 134.5(2) . . . . ? C81 As2 C71 C76 74.7(3) . . . . ? C61 As2 C71 C76 -172.6(2) . . . . ? Bi2 As2 C71 C76 -47.8(3) . . . . ? C76 C71 C72 C73 -0.4(5) . . . . ? As2 C71 C72 C73 177.3(3) . . . . ? C71 C72 C73 C74 -0.4(5) . . . . ? C72 C73 C74 C75 0.7(6) . . . . ? C73 C74 C75 C76 -0.1(6) . . . . ? C74 C75 C76 C71 -0.7(5) . . . . ? C72 C71 C76 C75 1.0(5) . . . . ? As2 C71 C76 C75 -176.8(3) . . . . ? C71 As2 C81 C86 -177.2(2) . . . . ? C61 As2 C81 C86 70.7(3) . . . . ? Bi2 As2 C81 C86 -54.3(3) . . . . ? C71 As2 C81 C82 -1.1(3) . . . . ? C61 As2 C81 C82 -113.2(2) . . . . ? Bi2 As2 C81 C82 121.8(2) . . . . ? C86 C81 C82 C83 0.3(4) . . . . ? As2 C81 C82 C83 -175.8(2) . . . . ? C81 C82 C83 C84 -0.5(5) . . . . ? C82 C83 C84 C85 0.5(5) . . . . ? C83 C84 C85 C86 -0.4(6) . . . . ? C82 C81 C86 C85 -0.1(5) . . . . ? As2 C81 C86 C85 176.0(3) . . . . ? C84 C85 C86 C81 0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.158 _refine_diff_density_min -1.552 _refine_diff_density_rms 0.114 # Attachment 'C24H21Al2BiCl9Sb.cif.txt' data_dal0932 _database_code_depnum_ccdc_archive 'CCDC 755449' #TrackingRef 'C24H21Al2BiCl9Sb.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 Al2 Bi Cl9 Sb, C6 H6' _chemical_formula_sum 'C24 H21 Al2 Bi Cl9 Sb' _chemical_formula_weight 1013.15 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.9027(4) _cell_length_b 10.6863(5) _cell_length_c 10.7459(5) _cell_angle_alpha 112.0241(5) _cell_angle_beta 106.9854(5) _cell_angle_gamma 101.5107(5) _cell_volume 849.52(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 478 _exptl_absorpt_coefficient_mu 6.741 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1526 _exptl_absorpt_correction_T_max 0.2605 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7690 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7690 _reflns_number_gt 7645 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0344P)^2^+0.3800P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #_refine_ls_abs_structure_Flack -0.0205(15) _refine_ls_number_reflns 7690 _refine_ls_number_parameters 334 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0189 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0488 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 Bi Bi 0.1000 0.1000 0.3000 0.02343(4) Uani 1 1 d . . . Sb Sb 0.05935(3) 0.13218(2) 0.57390(2) 0.02164(5) Uani 1 1 d . . . Cl1 Cl 0.34982(12) 0.04380(12) 0.39492(11) 0.0371(2) Uani 1 1 d . . . Cl2 Cl -0.06698(12) -0.19654(10) 0.18398(10) 0.03063(18) Uani 1 1 d . . . Cl3 Cl -0.31665(13) 0.00168(11) 0.20320(14) 0.0453(3) Uani 1 1 d . . . Cl4 Cl -0.47949(17) -0.35840(15) 0.13702(15) 0.0587(3) Uani 1 1 d . . . Cl5 Cl -0.40357(16) -0.28337(15) -0.13466(12) 0.0519(3) Uani 1 1 d . . . Cl6 Cl 0.31442(12) 0.38960(10) 0.48210(12) 0.0344(2) Uani 1 1 d . . . Cl7 Cl -0.09139(12) 0.34171(11) 0.31218(12) 0.0380(2) Uani 1 1 d . . . Cl8 Cl 0.16806(16) 0.65536(12) 0.64946(14) 0.0489(3) Uani 1 1 d . . . Cl9 Cl 0.20756(16) 0.61202(16) 0.32087(17) 0.0581(3) Uani 1 1 d . . . Al1 Al -0.33359(15) -0.21668(13) 0.09111(13) 0.0308(2) Uani 1 1 d . . . Al2 Al 0.14611(15) 0.51124(13) 0.44203(14) 0.0338(3) Uani 1 1 d . . . C11 C -0.0069(5) 0.3099(4) 0.6790(4) 0.0277(7) Uani 1 1 d . . . C12 C 0.0957(6) 0.4109(4) 0.8233(4) 0.0359(8) Uani 1 1 d . . . H12 H 0.1986 0.4034 0.8725 0.043 Uiso 1 1 calc R . . C13 C 0.0472(7) 0.5220(5) 0.8945(5) 0.0451(11) Uani 1 1 d . . . H13 H 0.1167 0.5914 0.9933 0.054 Uiso 1 1 calc R . . C14 C -0.1023(7) 0.5327(5) 0.8226(6) 0.0463(11) Uani 1 1 d . . . H14 H -0.1348 0.6098 0.8722 0.056 Uiso 1 1 calc R . . C15 C -0.2050(6) 0.4323(5) 0.6792(5) 0.0413(10) Uani 1 1 d . . . H15 H -0.3076 0.4405 0.6308 0.050 Uiso 1 1 calc R . . C16 C -0.1585(5) 0.3191(4) 0.6055(5) 0.0326(8) Uani 1 1 d . . . H16 H -0.2286 0.2494 0.5070 0.039 Uiso 1 1 calc R . . C21 C -0.1212(4) -0.0468(4) 0.5482(4) 0.0260(7) Uani 1 1 d . . . C22 C -0.2596(5) -0.0296(4) 0.5785(4) 0.0329(8) Uani 1 1 d . . . H22 H -0.2753 0.0607 0.6055 0.040 Uiso 1 1 calc R . . C23 C -0.3742(5) -0.1452(5) 0.5689(5) 0.0421(10) Uani 1 1 d . . . H23 H -0.4695 -0.1345 0.5885 0.051 Uiso 1 1 calc R . . C24 C -0.3506(6) -0.2754(5) 0.5312(5) 0.0429(10) Uani 1 1 d . . . H24 H -0.4289 -0.3534 0.5268 0.051 Uiso 1 1 calc R . . C25 C -0.2141(6) -0.2945(5) 0.4995(5) 0.0411(10) Uani 1 1 d . . . H25 H -0.1990 -0.3850 0.4732 0.049 Uiso 1 1 calc R . . C26 C -0.0992(5) -0.1797(4) 0.5066(5) 0.0323(8) Uani 1 1 d . . . H26 H -0.0065 -0.1919 0.4831 0.039 Uiso 1 1 calc R . . C31 C 0.2941(5) 0.1602(4) 0.7234(4) 0.0268(7) Uani 1 1 d . . . C32 C 0.4263(5) 0.2900(5) 0.7894(5) 0.0394(9) Uani 1 1 d . . . H32 H 0.4115 0.3669 0.7690 0.047 Uiso 1 1 calc R . . C33 C 0.5795(6) 0.3053(6) 0.8853(5) 0.0498(12) Uani 1 1 d . . . H33 H 0.6705 0.3936 0.9314 0.060 Uiso 1 1 calc R . . C34 C 0.6018(6) 0.1934(6) 0.9148(5) 0.0464(11) Uani 1 1 d . . . H34 H 0.7073 0.2058 0.9818 0.056 Uiso 1 1 calc R . . C35 C 0.4714(6) 0.0639(6) 0.8472(5) 0.0414(10) Uani 1 1 d . . . H35 H 0.4880 -0.0135 0.8659 0.050 Uiso 1 1 calc R . . C36 C 0.3156(5) 0.0466(5) 0.7519(4) 0.0323(8) Uani 1 1 d . . . H36 H 0.2249 -0.0418 0.7066 0.039 Uiso 1 1 calc R . . C1S C 0.2407(8) 0.2394(6) 0.0983(6) 0.0544(13) Uani 1 1 d . . . H1S H 0.3071 0.3389 0.1505 0.065 Uiso 1 1 calc R . . C2S C 0.3141(7) 0.1366(8) 0.1036(6) 0.0595(15) Uani 1 1 d . . . H2S H 0.4305 0.1656 0.1603 0.071 Uiso 1 1 calc R . . C3S C 0.2159(9) -0.0078(7) 0.0254(7) 0.0589(15) Uani 1 1 d . . . H3S H 0.2651 -0.0783 0.0284 0.071 Uiso 1 1 calc R . . C4S C 0.0475(9) -0.0497(6) -0.0565(6) 0.0626(16) Uani 1 1 d . . . H4S H -0.0194 -0.1490 -0.1114 0.075 Uiso 1 1 calc R . . C5S C -0.0240(7) 0.0534(8) -0.0589(6) 0.0590(15) Uani 1 1 d . . . H5S H -0.1408 0.0245 -0.1140 0.071 Uiso 1 1 calc R . . C6S C 0.0712(8) 0.1955(7) 0.0169(7) 0.0563(14) Uani 1 1 d . . . H6S H 0.0206 0.2652 0.0138 0.068 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 Bi 0.02269(6) 0.02573(6) 0.02296(6) 0.01247(5) 0.00832(4) 0.00956(4) Sb 0.02153(11) 0.02020(11) 0.02217(11) 0.00968(9) 0.00762(9) 0.00731(9) Cl1 0.0308(4) 0.0497(6) 0.0397(5) 0.0238(4) 0.0150(4) 0.0238(4) Cl2 0.0301(4) 0.0259(4) 0.0311(4) 0.0101(3) 0.0087(4) 0.0122(3) Cl3 0.0331(5) 0.0308(5) 0.0544(6) 0.0063(4) 0.0103(4) 0.0145(4) Cl4 0.0461(6) 0.0541(7) 0.0532(7) 0.0224(6) 0.0118(5) -0.0094(5) Cl5 0.0467(6) 0.0683(8) 0.0301(5) 0.0164(5) 0.0075(5) 0.0242(6) Cl6 0.0267(4) 0.0277(4) 0.0428(5) 0.0188(4) 0.0047(4) 0.0066(3) Cl7 0.0281(4) 0.0340(5) 0.0392(5) 0.0139(4) 0.0055(4) 0.0040(4) Cl8 0.0495(6) 0.0323(5) 0.0450(6) 0.0100(5) 0.0031(5) 0.0152(5) Cl9 0.0468(6) 0.0624(8) 0.0772(9) 0.0549(7) 0.0156(6) 0.0117(6) Al1 0.0277(5) 0.0262(5) 0.0271(5) 0.0058(4) 0.0067(4) 0.0066(4) Al2 0.0283(5) 0.0262(5) 0.0414(7) 0.0190(5) 0.0050(5) 0.0061(5) C11 0.0321(18) 0.0247(16) 0.0305(18) 0.0140(14) 0.0150(15) 0.0121(14) C12 0.042(2) 0.034(2) 0.0303(19) 0.0137(16) 0.0128(17) 0.0142(17) C13 0.063(3) 0.030(2) 0.034(2) 0.0067(18) 0.020(2) 0.014(2) C14 0.064(3) 0.037(2) 0.052(3) 0.019(2) 0.036(2) 0.029(2) C15 0.042(2) 0.044(2) 0.051(3) 0.024(2) 0.025(2) 0.027(2) C16 0.0348(19) 0.0309(19) 0.034(2) 0.0161(16) 0.0135(16) 0.0139(16) C21 0.0239(16) 0.0270(17) 0.0231(16) 0.0116(14) 0.0062(13) 0.0056(14) C22 0.0316(19) 0.0326(19) 0.0310(19) 0.0116(16) 0.0131(16) 0.0096(16) C23 0.030(2) 0.046(2) 0.044(2) 0.018(2) 0.0166(18) 0.0044(18) C24 0.032(2) 0.041(2) 0.048(3) 0.025(2) 0.0103(19) -0.0017(17) C25 0.036(2) 0.0291(19) 0.050(3) 0.0198(18) 0.0092(19) 0.0053(17) C26 0.0304(18) 0.0303(18) 0.036(2) 0.0170(16) 0.0113(16) 0.0099(15) C31 0.0243(17) 0.0340(19) 0.0242(17) 0.0151(15) 0.0100(14) 0.0107(15) C32 0.032(2) 0.037(2) 0.039(2) 0.0180(18) 0.0057(17) 0.0031(17) C33 0.027(2) 0.062(3) 0.041(2) 0.019(2) 0.0045(18) 0.002(2) C34 0.029(2) 0.073(3) 0.033(2) 0.022(2) 0.0077(17) 0.023(2) C35 0.043(2) 0.058(3) 0.039(2) 0.030(2) 0.0173(19) 0.031(2) C36 0.0339(19) 0.036(2) 0.0320(19) 0.0187(16) 0.0135(16) 0.0172(16) C1S 0.068(3) 0.055(3) 0.046(3) 0.025(2) 0.035(3) 0.012(3) C2S 0.043(3) 0.105(5) 0.049(3) 0.044(3) 0.027(2) 0.032(3) C3S 0.089(4) 0.077(4) 0.062(3) 0.048(3) 0.055(3) 0.058(4) C4S 0.096(5) 0.049(3) 0.037(3) 0.014(2) 0.037(3) 0.011(3) C5S 0.046(3) 0.096(5) 0.039(3) 0.039(3) 0.014(2) 0.020(3) C6S 0.070(4) 0.081(4) 0.061(3) 0.055(3) 0.041(3) 0.043(3) _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 Bi Cl1 2.4525(9) . ? Bi Cl2 2.8072(9) . ? Bi Cl6 2.8229(9) . ? Bi Sb 2.9707(3) . ? Sb C21 2.106(4) . ? Sb C11 2.112(4) . ? Sb C31 2.113(4) . ? Cl2 Al1 2.2197(15) . ? Cl3 Al1 2.1363(15) . ? Cl4 Al1 2.0913(18) . ? Cl5 Al1 2.1035(17) . ? Cl6 Al2 2.2226(15) . ? Cl7 Al2 2.1333(15) . ? Cl8 Al2 2.1047(19) . ? Cl9 Al2 2.0945(18) . ? C11 C12 1.388(6) . ? C11 C16 1.394(5) . ? C12 C13 1.378(6) . ? C13 C14 1.381(8) . ? C14 C15 1.381(7) . ? C15 C16 1.391(6) . ? C21 C22 1.392(5) . ? C21 C26 1.393(5) . ? C22 C23 1.385(6) . ? C23 C24 1.374(7) . ? C24 C25 1.387(7) . ? C25 C26 1.393(6) . ? C31 C32 1.391(6) . ? C31 C36 1.394(5) . ? C32 C33 1.383(6) . ? C33 C34 1.382(8) . ? C34 C35 1.380(7) . ? C35 C36 1.390(6) . ? C1S C6S 1.379(8) . ? C1S C2S 1.396(9) . ? C2S C3S 1.382(10) . ? C3S C4S 1.374(10) . ? C4S C5S 1.382(10) . ? C5S C6S 1.358(9) . ? 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 Cl1 Bi Cl2 83.85(3) . . ? Cl1 Bi Cl6 84.57(3) . . ? Cl2 Bi Cl6 164.66(3) . . ? Cl1 Bi Sb 85.89(2) . . ? Cl2 Bi Sb 86.86(2) . . ? Cl6 Bi Sb 82.30(2) . . ? C21 Sb C11 104.60(14) . . ? C21 Sb C31 108.00(14) . . ? C11 Sb C31 106.80(15) . . ? C21 Sb Bi 114.38(10) . . ? C11 Sb Bi 116.04(10) . . ? C31 Sb Bi 106.57(10) . . ? Al1 Cl2 Bi 102.09(5) . . ? Al2 Cl6 Bi 102.82(5) . . ? Cl4 Al1 Cl5 113.56(8) . . ? Cl4 Al1 Cl3 113.72(8) . . ? Cl5 Al1 Cl3 110.81(8) . . ? Cl4 Al1 Cl2 109.89(8) . . ? Cl5 Al1 Cl2 106.97(7) . . ? Cl3 Al1 Cl2 100.93(6) . . ? Cl9 Al2 Cl8 113.77(8) . . ? Cl9 Al2 Cl7 110.17(8) . . ? Cl8 Al2 Cl7 113.86(8) . . ? Cl9 Al2 Cl6 110.47(8) . . ? Cl8 Al2 Cl6 106.41(7) . . ? Cl7 Al2 Cl6 101.33(6) . . ? C12 C11 C16 120.9(4) . . ? C12 C11 Sb 119.6(3) . . ? C16 C11 Sb 119.4(3) . . ? C13 C12 C11 119.5(4) . . ? C12 C13 C14 120.1(4) . . ? C15 C14 C13 120.6(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 C11 118.7(4) . . ? C22 C21 C26 120.3(4) . . ? C22 C21 Sb 119.3(3) . . ? C26 C21 Sb 120.3(3) . . ? C23 C22 C21 119.5(4) . . ? C24 C23 C22 120.3(4) . . ? C23 C24 C25 120.9(4) . . ? C24 C25 C26 119.4(4) . . ? C21 C26 C25 119.6(4) . . ? C32 C31 C36 120.7(4) . . ? C32 C31 Sb 119.9(3) . . ? C36 C31 Sb 119.4(3) . . ? C33 C32 C31 119.0(4) . . ? C34 C33 C32 120.7(5) . . ? C35 C34 C33 120.3(4) . . ? C34 C35 C36 120.1(4) . . ? C35 C36 C31 119.3(4) . . ? C6S C1S C2S 119.5(6) . . ? C3S C2S C1S 119.4(5) . . ? C4S C3S C2S 120.3(5) . . ? C3S C4S C5S 119.7(6) . . ? C6S C5S C4S 120.6(6) . . ? C5S C6S C1S 120.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Bi Sb C21 -100.78(12) . . . . ? Cl2 Bi Sb C21 -16.73(11) . . . . ? Cl6 Bi Sb C21 174.15(11) . . . . ? Cl1 Bi Sb C11 137.24(12) . . . . ? Cl2 Bi Sb C11 -138.71(12) . . . . ? Cl6 Bi Sb C11 52.17(12) . . . . ? Cl1 Bi Sb C31 18.48(11) . . . . ? Cl2 Bi Sb C31 102.53(11) . . . . ? Cl6 Bi Sb C31 -66.58(11) . . . . ? Cl1 Bi Cl2 Al1 174.24(5) . . . . ? Cl6 Bi Cl2 Al1 133.05(10) . . . . ? Sb Bi Cl2 Al1 88.04(5) . . . . ? Cl1 Bi Cl6 Al2 179.70(6) . . . . ? Cl2 Bi Cl6 Al2 -139.17(10) . . . . ? Sb Bi Cl6 Al2 -93.72(5) . . . . ? Bi Cl2 Al1 Cl4 -138.54(6) . . . . ? Bi Cl2 Al1 Cl5 97.76(7) . . . . ? Bi Cl2 Al1 Cl3 -18.17(7) . . . . ? Bi Cl6 Al2 Cl9 -108.98(7) . . . . ? Bi Cl6 Al2 Cl8 127.07(6) . . . . ? Bi Cl6 Al2 Cl7 7.78(7) . . . . ? C21 Sb C11 C12 110.9(3) . . . . ? C31 Sb C11 C12 -3.5(3) . . . . ? Bi Sb C11 C12 -122.1(3) . . . . ? C21 Sb C11 C16 -65.1(3) . . . . ? C31 Sb C11 C16 -179.4(3) . . . . ? Bi Sb C11 C16 61.9(3) . . . . ? C16 C11 C12 C13 -0.2(6) . . . . ? Sb C11 C12 C13 -176.1(3) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 C11 -0.2(7) . . . . ? C12 C11 C16 C15 0.4(6) . . . . ? Sb C11 C16 C15 176.3(3) . . . . ? C11 Sb C21 C22 9.3(3) . . . . ? C31 Sb C21 C22 122.8(3) . . . . ? Bi Sb C21 C22 -118.7(3) . . . . ? C11 Sb C21 C26 -168.3(3) . . . . ? C31 Sb C21 C26 -54.8(3) . . . . ? Bi Sb C21 C26 63.6(3) . . . . ? C26 C21 C22 C23 0.9(6) . . . . ? Sb C21 C22 C23 -176.7(3) . . . . ? C21 C22 C23 C24 0.6(7) . . . . ? C22 C23 C24 C25 -1.2(7) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C22 C21 C26 C25 -1.9(6) . . . . ? Sb C21 C26 C25 175.7(3) . . . . ? C24 C25 C26 C21 1.3(7) . . . . ? C21 Sb C31 C32 -163.4(3) . . . . ? C11 Sb C31 C32 -51.4(4) . . . . ? Bi Sb C31 C32 73.3(3) . . . . ? C21 Sb C31 C36 18.2(3) . . . . ? C11 Sb C31 C36 130.3(3) . . . . ? Bi Sb C31 C36 -105.1(3) . . . . ? C36 C31 C32 C33 -0.7(7) . . . . ? Sb C31 C32 C33 -179.1(4) . . . . ? C31 C32 C33 C34 0.3(8) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C33 C34 C35 C36 -1.6(7) . . . . ? C34 C35 C36 C31 1.2(6) . . . . ? C32 C31 C36 C35 -0.1(6) . . . . ? Sb C31 C36 C35 178.3(3) . . . . ? C6S C1S C2S C3S 0.8(7) . . . . ? C1S C2S C3S C4S -0.1(7) . . . . ? C2S C3S C4S C5S -1.0(8) . . . . ? C3S C4S C5S C6S 1.2(8) . . . . ? C4S C5S C6S C1S -0.5(8) . . . . ? C2S C1S C6S C5S -0.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.579 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.074