# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tracy Hanna' _publ_contact_author_email T.HANNA@TCU.EDU _publ_section_title ; Synthesis, X-ray Structures, and Reactivity of Calix[5]arene Bismuth(III) and Antimony(III) Complexes ; loop_ _publ_author_name 'Tracy Hanna' 'Daniel Mendoza-Espinosa' # Attachment '1.CIF' data_tcu86m _database_code_depnum_ccdc_archive 'CCDC 716835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110 H134 Bi2 O10' _chemical_formula_sum 'C110 H134 Bi2 O10' _chemical_formula_weight 2034.13 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.586(5) _cell_length_b 18.566(3) _cell_length_c 26.834(5) _cell_angle_alpha 90.00 _cell_angle_beta 122.108(9) _cell_angle_gamma 90.00 _cell_volume 12063(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 2.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 0.587 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 34359 _diffrn_reflns_av_R_equivalents 0.1373 _diffrn_reflns_av_sigmaI/netI 0.1494 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10608 _reflns_number_gt 6055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10608 _refine_ls_number_parameters 554 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi -0.057734(14) 0.565005(19) -0.055492(14) 0.02812(13) Uani 1 1 d . . . O1 O -0.0404(3) 0.3399(3) -0.0862(3) 0.0379(17) Uani 1 1 d . . . H1A H -0.0512 0.3822 -0.0940 0.045 Uiso 1 1 d R . . O2 O 0.0154(3) 0.2894(3) 0.0280(3) 0.0371(16) Uani 1 1 d . . . H2A H 0.0000 0.2998 -0.0074 0.045 Uiso 1 1 d R . . O3 O 0.0845(3) 0.4006(3) 0.1420(3) 0.0350(16) Uani 1 1 d . . . O4 O 0.0924(2) 0.5379(3) 0.0916(2) 0.0308(15) Uani 1 1 d . . . O5 O 0.0163(2) 0.5185(3) -0.0430(2) 0.0305(15) Uani 1 1 d . . . C1 C -0.0079(4) 0.3247(5) -0.1087(4) 0.030(2) Uani 1 1 d . . . C2 C 0.0058(4) 0.3744(5) -0.1379(4) 0.032(2) Uani 1 1 d . . . C3 C 0.0419(4) 0.3502(5) -0.1548(4) 0.038(2) Uani 1 1 d . . . H3A H 0.0521 0.3831 -0.1740 0.045 Uiso 1 1 calc R . . C4 C 0.0637(4) 0.2811(6) -0.1451(4) 0.044(3) Uani 1 1 d . A . C5 C 0.0478(4) 0.2335(5) -0.1168(4) 0.043(3) Uani 1 1 d . . . H5A H 0.0620 0.1864 -0.1090 0.052 Uiso 1 1 calc R . . C6 C 0.0108(4) 0.2538(5) -0.0995(4) 0.034(2) Uani 1 1 d . . . C7 C 0.1026(4) 0.2568(5) -0.1657(4) 0.054(3) Uani 1 1 d D . . C8 C 0.1194(8) 0.3162(8) -0.1899(8) 0.071(6) Uiso 0.619(14) 1 d PD A 1 H8A H 0.1382 0.3532 -0.1602 0.107 Uiso 0.619(14) 1 calc PR A 1 H8B H 0.0869 0.3367 -0.2240 0.107 Uiso 0.619(14) 1 calc PR A 1 H8C H 0.1440 0.2976 -0.2014 0.107 Uiso 0.619(14) 1 calc PR A 1 C9 C 0.0738(7) 0.1980(9) -0.2139(7) 0.062(6) Uiso 0.619(14) 1 d PD A 1 H9A H 0.0737 0.1528 -0.1958 0.093 Uiso 0.619(14) 1 calc PR A 1 H9B H 0.0937 0.1919 -0.2337 0.093 Uiso 0.619(14) 1 calc PR A 1 H9C H 0.0361 0.2125 -0.2422 0.093 Uiso 0.619(14) 1 calc PR A 1 C10 C 0.1531(6) 0.2210(9) -0.1146(7) 0.068(6) Uiso 0.619(14) 1 d PD A 1 H10A H 0.1702 0.2535 -0.0812 0.102 Uiso 0.619(14) 1 calc PR A 1 H10B H 0.1793 0.2098 -0.1260 0.102 Uiso 0.619(14) 1 calc PR A 1 H10C H 0.1422 0.1770 -0.1040 0.102 Uiso 0.619(14) 1 calc PR A 1 C8A C 0.0796(11) 0.2815(14) -0.2293(8) 0.068(10) Uiso 0.381(14) 1 d PD A 2 H8AA H 0.0865 0.3326 -0.2296 0.102 Uiso 0.381(14) 1 calc PR A 2 H8AB H 0.0402 0.2725 -0.2528 0.102 Uiso 0.381(14) 1 calc PR A 2 H8AC H 0.0977 0.2550 -0.2456 0.102 Uiso 0.381(14) 1 calc PR A 2 C9A C 0.1178(12) 0.1796(9) -0.1600(12) 0.075(11) Uiso 0.381(14) 1 d PD A 2 H9AA H 0.1461 0.1692 -0.1194 0.112 Uiso 0.381(14) 1 calc PR A 2 H9AB H 0.1319 0.1689 -0.1851 0.112 Uiso 0.381(14) 1 calc PR A 2 H9AC H 0.0855 0.1502 -0.1717 0.112 Uiso 0.381(14) 1 calc PR A 2 C10A C 0.1547(9) 0.3020(13) -0.1280(10) 0.075(11) Uiso 0.381(14) 1 d PD A 2 H10D H 0.1454 0.3449 -0.1145 0.113 Uiso 0.381(14) 1 calc PR A 2 H10E H 0.1700 0.3158 -0.1513 0.113 Uiso 0.381(14) 1 calc PR A 2 H10F H 0.1817 0.2739 -0.0944 0.113 Uiso 0.381(14) 1 calc PR A 2 C12 C 0.0340(4) 0.1789(5) -0.0085(4) 0.037(2) Uani 1 1 d . . . C13 C 0.0631(4) 0.1144(5) 0.0060(5) 0.042(3) Uani 1 1 d . . . H13A H 0.0581 0.0843 -0.0246 0.050 Uiso 1 1 calc R . . C14 C 0.0993(4) 0.0923(5) 0.0640(4) 0.041(3) Uani 1 1 d . A . C15 C 0.1047(4) 0.1374(5) 0.1080(5) 0.043(3) Uani 1 1 d . . . H15A H 0.1283 0.1230 0.1473 0.051 Uiso 1 1 calc R . . C16 C 0.0772(4) 0.2026(6) 0.0970(4) 0.037(2) Uani 1 1 d . . . C17 C 0.0429(4) 0.2234(5) 0.0386(4) 0.031(2) Uani 1 1 d . . . C18 C 0.1287(5) 0.0180(6) 0.0777(4) 0.063(3) Uani 1 1 d D . . C19 C 0.1536(8) 0.0083(12) 0.0384(8) 0.076(7) Uiso 0.619(14) 1 d PD A 1 H19A H 0.1241 -0.0003 -0.0019 0.114 Uiso 0.619(14) 1 calc PR A 1 H19B H 0.1788 -0.0324 0.0526 0.114 Uiso 0.619(14) 1 calc PR A 1 H19C H 0.1735 0.0516 0.0403 0.114 Uiso 0.619(14) 1 calc PR A 1 C20 C 0.0858(7) -0.0429(10) 0.0619(9) 0.078(7) Uiso 0.619(14) 1 d PD A 1 H20A H 0.0520 -0.0315 0.0250 0.117 Uiso 0.619(14) 1 calc PR A 1 H20B H 0.0780 -0.0470 0.0928 0.117 Uiso 0.619(14) 1 calc PR A 1 H20C H 0.1006 -0.0881 0.0581 0.117 Uiso 0.619(14) 1 calc PR A 1 C21 C 0.1759(8) 0.0110(13) 0.1422(6) 0.096(8) Uiso 0.619(14) 1 d PD A 1 H21A H 0.1620 -0.0104 0.1648 0.144 Uiso 0.619(14) 1 calc PR A 1 H21B H 0.1909 0.0583 0.1579 0.144 Uiso 0.619(14) 1 calc PR A 1 H21C H 0.2048 -0.0193 0.1448 0.144 Uiso 0.619(14) 1 calc PR A 1 C19A C 0.1276(14) -0.021(2) 0.0257(11) 0.110(16) Uiso 0.381(14) 1 d PD A 2 H19D H 0.0896 -0.0273 -0.0065 0.165 Uiso 0.381(14) 1 calc PR A 2 H19E H 0.1451 -0.0679 0.0387 0.165 Uiso 0.381(14) 1 calc PR A 2 H19F H 0.1473 0.0075 0.0124 0.165 Uiso 0.381(14) 1 calc PR A 2 C20A C 0.1028(13) -0.0327(18) 0.1023(14) 0.103(14) Uiso 0.381(14) 1 d PD A 2 H20D H 0.0630 -0.0336 0.0754 0.154 Uiso 0.381(14) 1 calc PR A 2 H20E H 0.1116 -0.0153 0.1404 0.154 Uiso 0.381(14) 1 calc PR A 2 H20F H 0.1174 -0.0809 0.1063 0.154 Uiso 0.381(14) 1 calc PR A 2 C21A C 0.1912(7) 0.0290(15) 0.1270(9) 0.047(8) Uiso 0.381(14) 1 d PD A 2 H21D H 0.2026 0.0774 0.1244 0.071 Uiso 0.381(14) 1 calc PR A 2 H21E H 0.2136 -0.0057 0.1218 0.071 Uiso 0.381(14) 1 calc PR A 2 H21F H 0.1961 0.0221 0.1653 0.071 Uiso 0.381(14) 1 calc PR A 2 C22 C 0.0833(4) 0.2478(5) 0.1486(4) 0.033(2) Uani 1 1 d . . . H22A H 0.0513 0.2799 0.1334 0.040 Uiso 1 1 calc R . . H22B H 0.0829 0.2153 0.1771 0.040 Uiso 1 1 calc R . . C23 C 0.1357(4) 0.2931(5) 0.1802(4) 0.030(2) Uani 1 1 d . . . C24 C 0.1875(4) 0.2601(6) 0.2173(4) 0.040(3) Uani 1 1 d . . . H24A H 0.1887 0.2098 0.2212 0.048 Uiso 1 1 calc R . . C25 C 0.2369(4) 0.2979(5) 0.2483(4) 0.034(2) Uani 1 1 d . . . C26 C 0.2323(4) 0.3731(5) 0.2420(4) 0.030(2) Uani 1 1 d . . . H26A H 0.2646 0.4009 0.2627 0.036 Uiso 1 1 calc R . . C27 C 0.1826(4) 0.4083(5) 0.2067(4) 0.028(2) Uani 1 1 d . . . C28 C 0.1335(4) 0.3663(6) 0.1743(4) 0.035(2) Uani 1 1 d . . . C29 C 0.2916(4) 0.2604(5) 0.2873(4) 0.039(3) Uani 1 1 d . . . C30 C 0.2928(5) 0.1838(6) 0.2677(5) 0.061(3) Uani 1 1 d . . . H30A H 0.2876 0.1848 0.2290 0.091 Uiso 1 1 calc R . . H30B H 0.2634 0.1559 0.2663 0.091 Uiso 1 1 calc R . . H30C H 0.3281 0.1618 0.2954 0.091 Uiso 1 1 calc R . . C31 C 0.3048(5) 0.2598(7) 0.3515(5) 0.076(4) Uani 1 1 d . . . H31A H 0.3428 0.2449 0.3780 0.114 Uiso 1 1 calc R . . H31B H 0.2802 0.2264 0.3544 0.114 Uiso 1 1 calc R . . H31C H 0.2996 0.3078 0.3621 0.114 Uiso 1 1 calc R . . C32 C 0.3381(4) 0.3016(6) 0.2875(4) 0.053(3) Uani 1 1 d . . . H32A H 0.3287 0.3086 0.2474 0.080 Uiso 1 1 calc R . . H32B H 0.3721 0.2743 0.3092 0.080 Uiso 1 1 calc R . . H32C H 0.3430 0.3481 0.3062 0.080 Uiso 1 1 calc R . . C33 C 0.1815(4) 0.4906(5) 0.2030(4) 0.036(3) Uani 1 1 d . . . H33A H 0.2108 0.5097 0.2411 0.044 Uiso 1 1 calc R . . H33B H 0.1462 0.5077 0.1962 0.044 Uiso 1 1 calc R . . C34 C 0.1892(4) 0.5219(5) 0.1549(4) 0.032(2) Uani 1 1 d . . . C35 C 0.2418(4) 0.5272(5) 0.1641(4) 0.039(2) Uani 1 1 d . . . H35A H 0.2716 0.5056 0.1978 0.046 Uiso 1 1 calc R . . C36 C 0.2521(4) 0.5634(6) 0.1253(4) 0.045(3) Uani 1 1 d . . . C37 C 0.2057(4) 0.5922(5) 0.0751(4) 0.043(3) Uani 1 1 d . . . H37A H 0.2109 0.6160 0.0475 0.051 Uiso 1 1 calc R . . C38 C 0.1524(4) 0.5877(5) 0.0638(4) 0.029(2) Uani 1 1 d . . . C39 C 0.1455(4) 0.5485(5) 0.1043(4) 0.030(2) Uani 1 1 d . . . C40 C 0.3099(4) 0.5674(7) 0.1363(5) 0.056(3) Uani 1 1 d . . . C41 C 0.3350(7) 0.4972(9) 0.1440(10) 0.139(8) Uani 1 1 d . . . H41A H 0.3347 0.4716 0.1753 0.209 Uiso 1 1 calc R . . H41B H 0.3728 0.5030 0.1540 0.209 Uiso 1 1 calc R . . H41C H 0.3142 0.4700 0.1077 0.209 Uiso 1 1 calc R . . C42 C 0.3464(6) 0.6141(11) 0.1920(8) 0.134(7) Uani 1 1 d . . . H42A H 0.3520 0.5890 0.2264 0.201 Uiso 1 1 calc R . . H42B H 0.3282 0.6598 0.1879 0.201 Uiso 1 1 calc R . . H42C H 0.3819 0.6228 0.1963 0.201 Uiso 1 1 calc R . . C43 C 0.3112(6) 0.6030(12) 0.0863(8) 0.156(9) Uani 1 1 d . . . H43A H 0.2849 0.5796 0.0496 0.233 Uiso 1 1 calc R . . H43B H 0.3480 0.5988 0.0931 0.233 Uiso 1 1 calc R . . H43C H 0.3017 0.6535 0.0843 0.233 Uiso 1 1 calc R . . C44 C 0.1056(3) 0.6245(5) 0.0120(3) 0.027(2) Uani 1 1 d . . . H44A H 0.1168 0.6741 0.0110 0.033 Uiso 1 1 calc R . . H44B H 0.0745 0.6268 0.0177 0.033 Uiso 1 1 calc R . . C45 C 0.0854(4) 0.5901(5) -0.0478(4) 0.031(2) Uani 1 1 d . . . C46 C 0.1108(4) 0.6102(5) -0.0773(4) 0.037(2) Uani 1 1 d . . . H46A H 0.1391 0.6448 -0.0602 0.044 Uiso 1 1 calc R . . C47 C 0.0432(4) 0.5405(5) -0.0735(4) 0.028(2) Uani 1 1 d . . . C48 C 0.0266(4) 0.5084(5) -0.1275(4) 0.035(2) Uani 1 1 d . . . C49 C -0.0163(4) 0.4493(5) -0.1543(4) 0.033(2) Uani 1 1 d . . . H49A H -0.0430 0.4568 -0.1425 0.040 Uiso 1 1 calc R . . H49B H -0.0364 0.4537 -0.1973 0.040 Uiso 1 1 calc R . . C50 C 0.0539(4) 0.5310(5) -0.1552(4) 0.038(3) Uani 1 1 d . . . H50A H 0.0428 0.5108 -0.1920 0.046 Uiso 1 1 calc R . . C51 C 0.0956(4) 0.5804(5) -0.1324(4) 0.040(3) Uani 1 1 d . . . C52 C 0.1230(5) 0.6040(7) -0.1660(5) 0.056(3) Uani 1 1 d . . . C53 C 0.1453(7) 0.5370(8) -0.1802(7) 0.104(6) Uani 1 1 d . . . H53A H 0.1614 0.5510 -0.2027 0.155 Uiso 1 1 calc R . . H53B H 0.1152 0.5034 -0.2030 0.155 Uiso 1 1 calc R . . H53C H 0.1732 0.5141 -0.1438 0.155 Uiso 1 1 calc R . . C54 C 0.0801(6) 0.6389(10) -0.2242(6) 0.121(7) Uani 1 1 d . . . H54A H 0.0983 0.6593 -0.2428 0.181 Uiso 1 1 calc R . . H54B H 0.0611 0.6767 -0.2168 0.181 Uiso 1 1 calc R . . H54C H 0.0536 0.6029 -0.2498 0.181 Uiso 1 1 calc R . . C55 C 0.1695(8) 0.6555(10) -0.1321(7) 0.159(10) Uani 1 1 d . . . H55A H 0.1805 0.6754 -0.1578 0.238 Uiso 1 1 calc R . . H55B H 0.2005 0.6305 -0.0996 0.238 Uiso 1 1 calc R . . H55C H 0.1576 0.6941 -0.1170 0.238 Uiso 1 1 calc R . . C301 C -0.0073(4) 0.1968(5) -0.0715(4) 0.034(2) Uani 1 1 d . . . H11A H -0.0411 0.2138 -0.0744 0.040 Uiso 1 1 calc R . . H11Y H -0.0164 0.1525 -0.0947 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 0.0312(2) 0.0329(2) 0.02440(18) 0.00072(19) 0.01754(17) 0.0030(2) O1 0.046(4) 0.032(4) 0.045(4) 0.010(3) 0.031(4) 0.018(3) O2 0.041(4) 0.039(4) 0.026(3) 0.003(3) 0.014(3) 0.005(3) O3 0.033(4) 0.046(4) 0.028(4) -0.003(3) 0.018(3) -0.006(3) O4 0.021(4) 0.051(4) 0.017(3) 0.003(3) 0.008(3) -0.001(3) O5 0.027(4) 0.044(4) 0.022(3) 0.005(3) 0.014(3) 0.003(3) C1 0.036(6) 0.034(6) 0.022(5) 0.000(4) 0.017(5) 0.006(5) C2 0.041(6) 0.031(6) 0.025(5) -0.007(4) 0.018(5) -0.005(5) C3 0.037(7) 0.044(7) 0.033(6) 0.004(5) 0.019(5) 0.004(5) C4 0.046(7) 0.056(8) 0.037(6) -0.002(5) 0.027(6) 0.010(6) C5 0.057(8) 0.035(6) 0.037(6) 0.001(5) 0.024(6) 0.011(5) C6 0.035(6) 0.045(7) 0.025(5) -0.004(5) 0.017(5) 0.001(5) C7 0.054(8) 0.068(8) 0.055(7) 0.000(6) 0.039(7) 0.011(6) C12 0.033(6) 0.043(7) 0.035(6) 0.002(5) 0.018(5) -0.008(5) C13 0.052(7) 0.028(6) 0.049(7) -0.010(5) 0.029(6) -0.003(5) C14 0.049(7) 0.031(6) 0.035(6) 0.005(5) 0.017(6) 0.010(5) C15 0.049(7) 0.029(6) 0.040(6) 0.009(5) 0.017(6) -0.002(5) C16 0.023(6) 0.052(7) 0.033(6) 0.005(5) 0.013(5) -0.006(5) C17 0.034(6) 0.035(6) 0.018(5) 0.005(4) 0.009(5) -0.002(5) C18 0.093(10) 0.040(7) 0.035(6) 0.013(5) 0.022(7) 0.015(7) C22 0.044(7) 0.031(6) 0.023(5) 0.005(4) 0.017(5) -0.007(5) C23 0.045(7) 0.029(6) 0.019(5) -0.002(4) 0.019(5) 0.001(5) C24 0.051(8) 0.039(6) 0.032(6) 0.000(5) 0.023(6) 0.000(6) C25 0.036(7) 0.047(7) 0.023(5) 0.000(5) 0.018(5) 0.002(5) C26 0.026(6) 0.031(6) 0.028(5) -0.005(4) 0.011(5) -0.002(5) C27 0.035(6) 0.026(5) 0.031(5) 0.000(4) 0.024(5) 0.003(5) C28 0.034(7) 0.051(7) 0.026(5) 0.003(5) 0.021(5) 0.017(5) C29 0.042(7) 0.041(7) 0.034(6) 0.006(5) 0.021(6) 0.005(5) C30 0.044(8) 0.049(8) 0.078(9) 0.011(7) 0.024(7) 0.020(6) C31 0.075(10) 0.100(11) 0.054(8) 0.040(8) 0.036(8) 0.021(8) C32 0.041(7) 0.072(8) 0.040(6) 0.010(6) 0.018(6) 0.005(6) C33 0.033(6) 0.053(7) 0.025(5) -0.009(5) 0.017(5) 0.004(5) C34 0.040(7) 0.029(6) 0.034(6) -0.007(5) 0.026(5) 0.000(5) C35 0.028(6) 0.045(7) 0.039(6) -0.006(5) 0.016(5) 0.003(5) C36 0.039(7) 0.058(7) 0.046(6) -0.002(6) 0.029(6) -0.002(6) C37 0.056(8) 0.048(7) 0.038(6) -0.001(5) 0.034(6) -0.001(6) C38 0.022(6) 0.037(6) 0.029(5) -0.007(4) 0.015(5) -0.002(4) C39 0.031(6) 0.028(6) 0.040(6) -0.008(4) 0.026(5) 0.001(4) C40 0.033(7) 0.080(9) 0.052(7) -0.001(7) 0.021(6) -0.006(7) C41 0.094(14) 0.093(13) 0.29(3) 0.006(15) 0.142(17) 0.019(11) C42 0.083(13) 0.22(2) 0.135(15) -0.060(16) 0.081(13) -0.057(14) C43 0.053(11) 0.31(3) 0.114(14) 0.065(17) 0.050(11) -0.005(14) C44 0.021(5) 0.033(6) 0.024(5) 0.003(4) 0.009(5) 0.001(4) C45 0.031(6) 0.030(6) 0.034(5) -0.003(4) 0.018(5) -0.003(5) C46 0.043(7) 0.045(6) 0.028(5) -0.006(5) 0.023(5) -0.016(5) C47 0.029(6) 0.034(6) 0.028(5) 0.010(4) 0.021(5) 0.009(4) C48 0.045(7) 0.036(6) 0.029(5) -0.001(5) 0.024(5) 0.000(5) C49 0.034(6) 0.048(7) 0.015(4) 0.002(4) 0.011(5) 0.002(5) C50 0.054(7) 0.045(6) 0.026(5) -0.001(5) 0.028(6) -0.002(6) C51 0.044(7) 0.051(7) 0.032(5) -0.008(5) 0.025(5) -0.012(5) C52 0.068(9) 0.080(9) 0.047(7) -0.014(6) 0.049(7) -0.020(7) C53 0.137(15) 0.116(13) 0.130(13) -0.012(11) 0.119(13) -0.020(11) C54 0.127(14) 0.200(19) 0.070(10) 0.025(12) 0.076(11) -0.027(13) C55 0.21(2) 0.23(2) 0.119(13) -0.086(14) 0.142(15) -0.162(18) C301 0.037(6) 0.028(5) 0.028(5) -0.001(4) 0.012(5) 0.006(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 Bi1 O3 2.120(6) 5_565 ? Bi1 O4 2.134(6) 5_565 ? Bi1 O5 2.142(5) . ? Bi1 O5 2.733(5) 5_565 ? O1 C1 1.379(9) . ? O1 H1A 0.8300 . ? O2 C17 1.400(11) . ? O2 H2A 0.8300 . ? O3 C28 1.354(10) . ? O3 Bi1 2.120(6) 5_565 ? O4 C39 1.382(10) . ? O4 Bi1 2.134(6) 5_565 ? O5 C47 1.445(9) . ? O5 Bi1 2.733(5) 5_565 ? C1 C6 1.393(12) . ? C1 C2 1.396(11) . ? C2 C3 1.404(12) . ? C2 C49 1.493(12) . ? C3 C4 1.388(13) . ? C3 H3A 0.9400 . ? C4 C5 1.390(13) . ? C4 C7 1.548(12) . ? C5 C6 1.413(12) . ? C5 H5A 0.9400 . ? C6 C301 1.536(12) . ? C7 C8 1.483(13) . ? C7 C9A 1.482(15) . ? C7 C10 1.518(13) . ? C7 C8A 1.536(14) . ? C7 C9 1.552(13) . ? C7 C10A 1.532(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C8A H8AC 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C10A H10D 0.9700 . ? C10A H10E 0.9700 . ? C10A H10F 0.9700 . ? C12 C13 1.389(13) . ? C12 C17 1.417(12) . ? C12 C301 1.496(12) . ? C13 C14 1.397(14) . ? C13 H13A 0.9400 . ? C14 C15 1.386(13) . ? C14 C18 1.554(14) . ? C15 C16 1.389(13) . ? C15 H15A 0.9400 . ? C16 C17 1.391(12) . ? C16 C22 1.547(12) . ? C18 C21 1.534(14) . ? C18 C20 1.552(13) . ? C18 C19A 1.559(15) . ? C18 C19 1.563(13) . ? C18 C20A 1.547(15) . ? C18 C21A 1.573(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C19A H19D 0.9700 . ? C19A H19E 0.9700 . ? C19A H19F 0.9700 . ? C20A H20D 0.9700 . ? C20A H20E 0.9700 . ? C20A H20F 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22 C23 1.523(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C28 1.366(13) . ? C23 C24 1.411(13) . ? C24 C25 1.389(13) . ? C24 H24A 0.9400 . ? C25 C26 1.404(13) . ? C25 C29 1.510(13) . ? C26 C27 1.384(12) . ? C26 H26A 0.9400 . ? C27 C28 1.426(13) . ? C27 C33 1.532(13) . ? C29 C30 1.524(13) . ? C29 C32 1.531(13) . ? C29 C31 1.555(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.533(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C39 1.359(13) . ? C34 C35 1.392(12) . ? C35 C36 1.396(12) . ? C35 H35A 0.9400 . ? C36 C37 1.400(14) . ? C36 C40 1.519(13) . ? C37 C38 1.388(12) . ? C37 H37A 0.9400 . ? C38 C39 1.405(12) . ? C38 C44 1.488(12) . ? C40 C41 1.449(17) . ? C40 C43 1.513(17) . ? C40 C42 1.554(18) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 C45 1.525(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C47 1.377(12) . ? C45 C46 1.379(11) . ? C46 C51 1.414(12) . ? C46 H46A 0.9400 . ? C47 C48 1.397(12) . ? C48 C50 1.398(11) . ? C48 C49 1.514(13) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.363(13) . ? C50 H50A 0.9400 . ? C51 C52 1.540(12) . ? C52 C55 1.490(16) . ? C52 C54 1.526(18) . ? C52 C53 1.534(17) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C55 H55C 0.9700 . ? C301 H11A 0.9800 . ? C301 H11Y 0.9800 . ? 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 O3 Bi1 O4 87.9(2) 5_565 5_565 ? O3 Bi1 O5 92.5(2) 5_565 . ? O4 Bi1 O5 83.8(2) 5_565 . ? O3 Bi1 O5 161.6(2) 5_565 5_565 ? O4 Bi1 O5 77.82(19) 5_565 5_565 ? O5 Bi1 O5 74.72(19) . 5_565 ? C1 O1 H1A 109.1 . . ? C17 O2 H2A 109.6 . . ? C28 O3 Bi1 119.5(5) . 5_565 ? C39 O4 Bi1 115.0(5) . 5_565 ? C47 O5 Bi1 125.2(5) . . ? C47 O5 Bi1 128.3(5) . 5_565 ? Bi1 O5 Bi1 105.28(19) . 5_565 ? O1 C1 C6 113.6(7) . . ? O1 C1 C2 124.5(8) . . ? C6 C1 C2 121.8(8) . . ? C1 C2 C3 116.3(9) . . ? C1 C2 C49 125.5(8) . . ? C3 C2 C49 118.2(8) . . ? C4 C3 C2 124.7(9) . . ? C4 C3 H3A 117.6 . . ? C2 C3 H3A 117.6 . . ? C3 C4 C5 116.4(8) . . ? C3 C4 C7 122.5(9) . . ? C5 C4 C7 121.0(9) . . ? C4 C5 C6 122.0(9) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C1 C6 C5 118.6(8) . . ? C1 C6 C301 122.6(7) . . ? C5 C6 C301 118.8(8) . . ? C8 C7 C9A 128.2(16) . . ? C8 C7 C10 110.2(9) . . ? C9A C7 C10 52.9(11) . . ? C8 C7 C8A 48.6(10) . . ? C9A C7 C8A 109.5(11) . . ? C10 C7 C8A 140.6(14) . . ? C8 C7 C9 108.1(9) . . ? C9A C7 C9 53.3(11) . . ? C10 C7 C9 105.8(9) . . ? C8A C7 C9 64.0(11) . . ? C8 C7 C4 113.6(11) . . ? C9A C7 C4 118.1(14) . . ? C10 C7 C4 108.9(9) . . ? C8A C7 C4 110.2(13) . . ? C9 C7 C4 109.9(10) . . ? C8 C7 C10A 56.9(11) . . ? C9A C7 C10A 109.4(12) . . ? C10 C7 C10A 61.2(11) . . ? C8A C7 C10A 105.1(10) . . ? C9 C7 C10A 146.5(15) . . ? C4 C7 C10A 103.6(13) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8A H8AA 109.5 . . ? C7 C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7 C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7 C9A H9AA 109.5 . . ? C7 C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C7 C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C7 C10A H10D 109.5 . . ? C7 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C7 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C13 C12 C17 117.1(9) . . ? C13 C12 C301 120.3(9) . . ? C17 C12 C301 122.5(9) . . ? C12 C13 C14 123.0(9) . . ? C12 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? C15 C14 C13 116.9(9) . . ? C15 C14 C18 122.2(9) . . ? C13 C14 C18 120.8(9) . . ? C14 C15 C16 123.5(9) . . ? C14 C15 H15A 118.2 . . ? C16 C15 H15A 118.2 . . ? C15 C16 C17 117.4(9) . . ? C15 C16 C22 120.2(8) . . ? C17 C16 C22 122.3(9) . . ? C16 C17 O2 117.1(8) . . ? C16 C17 C12 121.9(9) . . ? O2 C17 C12 121.0(8) . . ? C21 C18 C20 109.8(10) . . ? C21 C18 C14 112.5(13) . . ? C20 C18 C14 109.4(11) . . ? C21 C18 C19A 124.0(19) . . ? C20 C18 C19A 77.2(13) . . ? C14 C18 C19A 116.8(17) . . ? C21 C18 C19 107.9(10) . . ? C20 C18 C19 108.0(10) . . ? C14 C18 C19 109.0(10) . . ? C19A C18 C19 31.1(12) . . ? C21 C18 C20A 78.5(13) . . ? C20 C18 C20A 35.3(12) . . ? C14 C18 C20A 108.6(17) . . ? C19A C18 C20A 108.2(12) . . ? C19 C18 C20A 135.3(17) . . ? C21 C18 C21A 30.3(10) . . ? C20 C18 C21A 134.7(14) . . ? C14 C18 C21A 108.3(13) . . ? C19A C18 C21A 106.8(12) . . ? C19 C18 C21A 82.0(11) . . ? C20A C18 C21A 107.9(12) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21A H21D 109.5 . . ? C18 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C18 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C23 C22 C16 114.0(7) . . ? C23 C22 H22A 108.8 . . ? C16 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C16 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 118.6(9) . . ? C28 C23 C22 120.9(9) . . ? C24 C23 C22 120.5(8) . . ? C25 C24 C23 123.8(10) . . ? C25 C24 H24A 118.1 . . ? C23 C24 H24A 118.1 . . ? C24 C25 C26 115.4(9) . . ? C24 C25 C29 122.1(9) . . ? C26 C25 C29 122.5(9) . . ? C27 C26 C25 123.3(9) . . ? C27 C26 H26A 118.4 . . ? C25 C26 H26A 118.4 . . ? C26 C27 C28 118.6(8) . . ? C26 C27 C33 119.5(9) . . ? C28 C27 C33 121.9(9) . . ? O3 C28 C23 120.7(10) . . ? O3 C28 C27 118.7(9) . . ? C23 C28 C27 120.3(9) . . ? C25 C29 C30 113.3(9) . . ? C25 C29 C32 110.4(8) . . ? C30 C29 C32 106.8(8) . . ? C25 C29 C31 108.9(8) . . ? C30 C29 C31 109.7(9) . . ? C32 C29 C31 107.4(9) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 C34 115.3(7) . . ? C27 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? C27 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C39 C34 C35 118.9(8) . . ? C39 C34 C33 120.8(8) . . ? C35 C34 C33 120.2(9) . . ? C34 C35 C36 122.5(10) . . ? C34 C35 H35A 118.7 . . ? C36 C35 H35A 118.7 . . ? C35 C36 C37 115.8(9) . . ? C35 C36 C40 121.1(10) . . ? C37 C36 C40 123.0(9) . . ? C38 C37 C36 123.7(9) . . ? C38 C37 H37A 118.2 . . ? C36 C37 H37A 118.2 . . ? C37 C38 C39 116.8(9) . . ? C37 C38 C44 120.8(8) . . ? C39 C38 C44 122.3(8) . . ? C34 C39 O4 120.0(8) . . ? C34 C39 C38 121.9(8) . . ? O4 C39 C38 118.0(8) . . ? C41 C40 C43 106.0(13) . . ? C41 C40 C36 112.9(11) . . ? C43 C40 C36 112.7(10) . . ? C41 C40 C42 109.7(13) . . ? C43 C40 C42 106.7(13) . . ? C36 C40 C42 108.7(9) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C38 C44 C45 116.2(7) . . ? C38 C44 H44A 108.2 . . ? C45 C44 H44A 108.2 . . ? C38 C44 H44B 108.2 . . ? C45 C44 H44B 108.2 . . ? H44A C44 H44B 107.4 . . ? C47 C45 C46 118.8(8) . . ? C47 C45 C44 123.3(7) . . ? C46 C45 C44 117.9(8) . . ? C45 C46 C51 122.1(9) . . ? C45 C46 H46A 119.0 . . ? C51 C46 H46A 119.0 . . ? C45 C47 C48 121.9(7) . . ? C45 C47 O5 119.5(7) . . ? C48 C47 O5 118.6(8) . . ? C47 C48 C50 116.6(9) . . ? C47 C48 C49 122.9(7) . . ? C50 C48 C49 120.4(8) . . ? C2 C49 C48 115.1(8) . . ? C2 C49 H49A 108.5 . . ? C48 C49 H49A 108.5 . . ? C2 C49 H49B 108.5 . . ? C48 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C51 C50 C48 124.3(8) . . ? C51 C50 H50A 117.8 . . ? C48 C50 H50A 117.8 . . ? C50 C51 C46 116.3(8) . . ? C50 C51 C52 121.6(8) . . ? C46 C51 C52 122.1(9) . . ? C55 C52 C54 108.8(13) . . ? C55 C52 C53 108.7(12) . . ? C54 C52 C53 107.8(11) . . ? C55 C52 C51 113.1(8) . . ? C54 C52 C51 109.6(9) . . ? C53 C52 C51 108.8(10) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C12 C301 C6 115.9(8) . . ? C12 C301 H11A 108.3 . . ? C6 C301 H11A 108.3 . . ? C12 C301 H11Y 108.3 . . ? C6 C301 H11Y 108.3 . . ? H11A C301 H11Y 107.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.229 _refine_diff_density_min -2.346 _refine_diff_density_rms 0.167 # Attachment 'CCDC-716836.CIF' data_tcu164m _database_code_depnum_ccdc_archive 'CCDC 716836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H146 Bi2 O10' _chemical_formula_sum 'C124 H146 Bi2 O10' _chemical_formula_weight 2214.37 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 12.142(2) _cell_length_b 14.819(3) _cell_length_c 18.082(4) _cell_angle_alpha 86.083(3) _cell_angle_beta 74.457(4) _cell_angle_gamma 69.430(3) _cell_volume 2933.5(10) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 3.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6252 _exptl_absorpt_correction_T_max 0.6926 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 15173 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.29 _reflns_number_total 8360 _reflns_number_gt 6876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. Disorder for the tert-butyl groups was due to 2-fold axis, and was modeled using partial occupancies and isotropic displacement parameters. Carbon atoms 52, 53 and 54 refined better with isotropic displacement parameters, otherwise non-positive definite alerts are observed. ; _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^)+(0.1379P)^2^+9.1948P] 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 8360 _refine_ls_number_parameters 596 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.015 _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 0.40216(4) 0.55409(3) 0.40544(2) 0.0267(2) Uani 1 1 d . . . O1 O 0.3750(7) 0.6952(5) 0.3635(4) 0.0236(17) Uani 1 1 d . . . C1 C 0.3763(10) 0.7298(7) 0.2903(6) 0.019(2) Uani 1 1 d . . . O2 O 0.2205(6) 0.5730(5) 0.4119(4) 0.0197(16) Uani 1 1 d . . . C2 C 0.4788(10) 0.7500(7) 0.2487(6) 0.020(2) Uani 1 1 d . . . O3 O 0.3826(7) 0.3878(5) 0.4785(4) 0.0205(16) Uani 1 1 d . . . H3A H 0.3451 0.3804 0.5228 0.031 Uiso 1 1 calc R . . C3 C 0.4807(11) 0.7898(7) 0.1758(6) 0.024(2) Uani 1 1 d . . . H3B H 0.5497 0.8042 0.1480 0.029 Uiso 1 1 calc R . . O4 O 0.6369(6) 0.3961(5) 0.4805(4) 0.0174(15) Uani 1 1 d . . . C4 C 0.3831(11) 0.8085(7) 0.1435(6) 0.024(3) Uani 1 1 d . . . O5 O 0.7394(6) 0.6261(5) 0.3769(4) 0.0175(15) Uani 1 1 d . . . C5 C 0.2842(10) 0.7870(7) 0.1859(6) 0.021(2) Uani 1 1 d . . . H5A H 0.2175 0.7994 0.1649 0.025 Uiso 1 1 calc R . . C6 C 0.2773(10) 0.7473(7) 0.2592(6) 0.020(2) Uani 1 1 d . . . C7 C 0.3877(12) 0.8488(9) 0.0611(6) 0.031(3) Uani 1 1 d . . . C8 C 0.5122(17) 0.8601(14) 0.0224(8) 0.066(5) Uani 1 1 d . . . H8A H 0.5122 0.8849 -0.0286 0.099 Uiso 1 1 calc R . . H8B H 0.5767 0.7978 0.0187 0.099 Uiso 1 1 calc R . . H8C H 0.5258 0.9046 0.0529 0.099 Uiso 1 1 calc R . . C9 C 0.294(2) 0.9467(12) 0.0662(10) 0.081(6) Uani 1 1 d . . . H9A H 0.2139 0.9432 0.0898 0.121 Uiso 1 1 calc R . . H9B H 0.2965 0.9719 0.0151 0.121 Uiso 1 1 calc R . . H9C H 0.3105 0.9891 0.0971 0.121 Uiso 1 1 calc R . . C10 C 0.367(2) 0.7819(16) 0.0119(9) 0.087(7) Uani 1 1 d . . . H10A H 0.2890 0.7742 0.0356 0.130 Uiso 1 1 calc R . . H10B H 0.4314 0.7197 0.0069 0.130 Uiso 1 1 calc R . . H10C H 0.3663 0.8088 -0.0385 0.130 Uiso 1 1 calc R . . C11 C 0.1660(10) 0.7228(8) 0.3033(7) 0.027(3) Uani 1 1 d . . . H11A H 0.1533 0.7335 0.3583 0.032 Uiso 1 1 calc R . . H11B H 0.0942 0.7670 0.2885 0.032 Uiso 1 1 calc R . . C12 C 0.1759(9) 0.6205(7) 0.2899(6) 0.018(2) Uani 1 1 d . . . C13 C 0.1564(10) 0.5963(8) 0.2238(6) 0.023(2) Uani 1 1 d . . . H13A H 0.1438 0.6428 0.1860 0.028 Uiso 1 1 calc R . . C14 C 0.1546(11) 0.5041(9) 0.2106(7) 0.030(3) Uani 1 1 d . A . C15 C 0.1714(10) 0.4376(8) 0.2693(6) 0.025(3) Uani 1 1 d . . . H15A H 0.1670 0.3766 0.2631 0.030 Uiso 1 1 calc R . . C16 C 0.1942(10) 0.4589(8) 0.3361(6) 0.023(2) Uani 1 1 d . . . C17 C 0.1991(9) 0.5506(7) 0.3459(6) 0.019(2) Uani 1 1 d . . . C18 C 0.1380(12) 0.4751(9) 0.1357(7) 0.043(3) Uani 1 1 d DU . . C19 C 0.138(3) 0.5539(18) 0.0735(15) 0.069(9) Uiso 0.63(3) 1 d PDU A 1 H19A H 0.0631 0.6090 0.0886 0.103 Uiso 0.63(3) 1 calc PR A 1 H19B H 0.1433 0.5276 0.0245 0.103 Uiso 0.63(3) 1 calc PR A 1 H19C H 0.2072 0.5742 0.0689 0.103 Uiso 0.63(3) 1 calc PR A 1 C20 C 0.022(2) 0.454(2) 0.1494(15) 0.058(8) Uiso 0.63(3) 1 d PDU A 1 H20A H -0.0440 0.5024 0.1842 0.086 Uiso 0.63(3) 1 calc PR A 1 H20B H 0.0325 0.3908 0.1720 0.086 Uiso 0.63(3) 1 calc PR A 1 H20C H 0.0014 0.4538 0.1010 0.086 Uiso 0.63(3) 1 calc PR A 1 C21 C 0.265(3) 0.418(3) 0.0822(19) 0.072(9) Uiso 0.63(3) 1 d PU A 1 H21A H 0.2980 0.3554 0.1040 0.108 Uiso 0.63(3) 1 calc PR A 1 H21B H 0.3194 0.4533 0.0773 0.108 Uiso 0.63(3) 1 calc PR A 1 H21C H 0.2557 0.4080 0.0319 0.108 Uiso 0.63(3) 1 calc PR A 1 C19A C 0.066(5) 0.559(3) 0.093(3) 0.070(14) Uiso 0.37(3) 1 d PDU A 2 H19D H -0.0122 0.5942 0.1268 0.105 Uiso 0.37(3) 1 calc PR A 2 H19E H 0.0545 0.5340 0.0485 0.105 Uiso 0.37(3) 1 calc PR A 2 H19F H 0.1120 0.6025 0.0757 0.105 Uiso 0.37(3) 1 calc PR A 2 C20A C 0.092(5) 0.388(3) 0.145(3) 0.068(14) Uiso 0.37(3) 1 d PDU A 2 H20D H 0.0091 0.4082 0.1775 0.102 Uiso 0.37(3) 1 calc PR A 2 H20E H 0.1441 0.3361 0.1689 0.102 Uiso 0.37(3) 1 calc PR A 2 H20F H 0.0940 0.3670 0.0952 0.102 Uiso 0.37(3) 1 calc PR A 2 C21A C 0.249(3) 0.382(2) 0.103(2) 0.036(9) Uiso 0.37(3) 1 d PDU A 2 H21D H 0.2335 0.3260 0.1285 0.054 Uiso 0.37(3) 1 calc PR A 2 H21E H 0.3219 0.3864 0.1113 0.054 Uiso 0.37(3) 1 calc PR A 2 H21F H 0.2587 0.3752 0.0481 0.054 Uiso 0.37(3) 1 calc PR A 2 C22 C 0.2083(10) 0.3853(7) 0.3990(6) 0.021(2) Uani 1 1 d . . . H22A H 0.1885 0.4201 0.4477 0.025 Uiso 1 1 calc R . . H22B H 0.1479 0.3541 0.4035 0.025 Uiso 1 1 calc R . . C23 C 0.3303(9) 0.3085(7) 0.3888(6) 0.016(2) Uani 1 1 d . . . C24 C 0.3672(10) 0.2309(8) 0.3364(6) 0.024(2) Uani 1 1 d . . . H24A H 0.3158 0.2314 0.3055 0.029 Uiso 1 1 calc R . . C25 C 0.4760(10) 0.1533(7) 0.3281(6) 0.022(2) Uani 1 1 d . . . C26 C 0.5470(10) 0.1514(7) 0.3781(6) 0.020(2) Uani 1 1 d . . . H26A H 0.6186 0.0981 0.3757 0.024 Uiso 1 1 calc R . . C27 C 0.5143(9) 0.2270(7) 0.4319(6) 0.017(2) Uani 1 1 d . . . C28 C 0.4098(9) 0.3068(7) 0.4332(6) 0.015(2) Uani 1 1 d . . . C29 C 0.5129(11) 0.0687(8) 0.2713(7) 0.031(3) Uani 1 1 d . . . C30 C 0.4578(14) 0.1010(10) 0.2021(7) 0.043(3) Uani 1 1 d . . . H30A H 0.3696 0.1259 0.2200 0.065 Uiso 1 1 calc R . . H30B H 0.4830 0.0463 0.1671 0.065 Uiso 1 1 calc R . . H30C H 0.4862 0.1510 0.1756 0.065 Uiso 1 1 calc R . . C31 C 0.4669(17) -0.0089(9) 0.3127(9) 0.059(5) Uani 1 1 d . . . H31A H 0.5020 -0.0302 0.3559 0.088 Uiso 1 1 calc R . . H31B H 0.4906 -0.0631 0.2775 0.088 Uiso 1 1 calc R . . H31C H 0.3788 0.0170 0.3311 0.088 Uiso 1 1 calc R . . C32 C 0.6496(14) 0.0291(14) 0.2386(11) 0.082(7) Uani 1 1 d . . . H32A H 0.6887 0.0071 0.2801 0.123 Uiso 1 1 calc R . . H32B H 0.6769 0.0792 0.2114 0.123 Uiso 1 1 calc R . . H32C H 0.6709 -0.0246 0.2034 0.123 Uiso 1 1 calc R . . C33 C 0.5908(10) 0.2163(7) 0.4891(6) 0.020(2) Uani 1 1 d . . . H33A H 0.5464 0.2664 0.5296 0.024 Uiso 1 1 calc R . . H33B H 0.6018 0.1536 0.5133 0.024 Uiso 1 1 calc R . . C34 C 0.7139(9) 0.2237(7) 0.4523(6) 0.018(2) Uani 1 1 d . . . C35 C 0.8099(10) 0.1435(7) 0.4157(6) 0.023(2) Uani 1 1 d . . . H35A H 0.7987 0.0836 0.4203 0.027 Uiso 1 1 calc R . . C36 C 0.9236(11) 0.1473(8) 0.3720(6) 0.026(3) Uani 1 1 d . . . C37 C 0.9346(10) 0.2402(7) 0.3670(6) 0.021(2) Uani 1 1 d . . . H37A H 1.0075 0.2472 0.3374 0.025 Uiso 1 1 calc R . . C38 C 0.8402(9) 0.3209(7) 0.4048(6) 0.019(2) Uani 1 1 d . . . C39 C 0.7323(9) 0.3132(7) 0.4477(6) 0.016(2) Uani 1 1 d . . . C40 C 1.0238(11) 0.0574(8) 0.3303(7) 0.028(3) Uani 1 1 d . . . C41 C 0.9753(14) 0.0144(11) 0.2756(9) 0.053(4) Uani 1 1 d . . . H41A H 0.9035 0.0006 0.3046 0.080 Uiso 1 1 calc R . . H41B H 1.0377 -0.0447 0.2515 0.080 Uiso 1 1 calc R . . H41C H 0.9541 0.0604 0.2364 0.080 Uiso 1 1 calc R . . C42 C 1.0613(12) -0.0194(8) 0.3882(8) 0.040(3) Uani 1 1 d . . . H42A H 1.0921 0.0052 0.4236 0.060 Uiso 1 1 calc R . . H42B H 1.1244 -0.0765 0.3613 0.060 Uiso 1 1 calc R . . H42C H 0.9912 -0.0359 0.4165 0.060 Uiso 1 1 calc R . . C43 C 1.1353(12) 0.0787(10) 0.2849(9) 0.048(4) Uani 1 1 d . . . H43A H 1.1664 0.1051 0.3192 0.071 Uiso 1 1 calc R . . H43B H 1.1139 0.1251 0.2460 0.071 Uiso 1 1 calc R . . H43C H 1.1974 0.0197 0.2604 0.071 Uiso 1 1 calc R . . C44 C 0.8494(9) 0.4198(7) 0.3858(6) 0.018(2) Uani 1 1 d . . . H44A H 0.8185 0.4601 0.4328 0.021 Uiso 1 1 calc R . . H44B H 0.9348 0.4135 0.3636 0.021 Uiso 1 1 calc R . . C45 C 0.7758(9) 0.4667(7) 0.3292(6) 0.017(2) Uani 1 1 d . . . C46 C 0.7514(10) 0.4118(8) 0.2800(6) 0.022(2) Uani 1 1 d . . . H46A H 0.7847 0.3443 0.2811 0.026 Uiso 1 1 calc R . . C47 C 0.6791(10) 0.4534(8) 0.2286(6) 0.025(3) Uani 1 1 d . . . C48 C 0.6298(10) 0.5548(8) 0.2276(6) 0.024(2) Uani 1 1 d . . . H48A H 0.5825 0.5838 0.1932 0.029 Uiso 1 1 calc R . . C49 C 0.6498(9) 0.6137(7) 0.2767(6) 0.017(2) Uani 1 1 d . . . C50 C 0.7249(10) 0.5671(7) 0.3256(6) 0.018(2) Uani 1 1 d . . . C51 C 0.6522(11) 0.3898(9) 0.1754(6) 0.029(3) Uani 1 1 d . . . C52 C 0.771(3) 0.314(2) 0.1276(17) 0.140(11) Uiso 1 1 d . . . H52A H 0.8322 0.3442 0.1090 0.210 Uiso 1 1 calc R . . H52B H 0.7541 0.2913 0.0844 0.210 Uiso 1 1 calc R . . H52C H 0.7999 0.2608 0.1596 0.210 Uiso 1 1 calc R . . C53 C 0.527(3) 0.385(2) 0.2111(16) 0.129(9) Uiso 1 1 d . . . H53A H 0.4659 0.4488 0.2147 0.193 Uiso 1 1 calc R . . H53B H 0.5230 0.3587 0.2621 0.193 Uiso 1 1 calc R . . H53C H 0.5102 0.3432 0.1794 0.193 Uiso 1 1 calc R . . C54 C 0.607(2) 0.4447(18) 0.1070(14) 0.125(10) Uiso 1 1 d . . . H54A H 0.6733 0.4583 0.0705 0.188 Uiso 1 1 calc R . . H54B H 0.5410 0.5048 0.1258 0.188 Uiso 1 1 calc R . . H54C H 0.5772 0.4053 0.0821 0.188 Uiso 1 1 calc R . . C55 C 0.5887(10) 0.7214(7) 0.2789(6) 0.019(2) Uani 1 1 d . . . H55A H 0.5649 0.7459 0.3319 0.023 Uiso 1 1 calc R . . H55B H 0.6465 0.7506 0.2481 0.023 Uiso 1 1 calc R . . C56 C 0.8489(11) 0.6545(8) 0.3506(7) 0.027(3) Uani 1 1 d . . . H56A H 0.8596 0.6742 0.2970 0.033 Uiso 1 1 calc R . . H56B H 0.9221 0.6007 0.3547 0.033 Uiso 1 1 calc R . . C57 C 0.8261(10) 0.7382(7) 0.4031(6) 0.022(2) Uani 1 1 d . . . C58 C 0.9100(10) 0.7333(8) 0.4433(6) 0.026(3) Uani 1 1 d . . . H58A H 0.9804 0.6782 0.4385 0.031 Uiso 1 1 calc R . . C59 C 0.8897(11) 0.8107(9) 0.4912(7) 0.031(3) Uani 1 1 d . . . H59A H 0.9471 0.8075 0.5182 0.037 Uiso 1 1 calc R . . C60 C 0.7864(12) 0.8918(8) 0.4993(7) 0.031(3) Uani 1 1 d . . . H60A H 0.7730 0.9433 0.5321 0.037 Uiso 1 1 calc R . . C61 C 0.7031(12) 0.8967(8) 0.4589(8) 0.035(3) Uani 1 1 d . . . H61A H 0.6321 0.9513 0.4644 0.042 Uiso 1 1 calc R . . C62 C 0.7247(12) 0.8199(8) 0.4097(7) 0.035(3) Uani 1 1 d . . . H62A H 0.6692 0.8242 0.3809 0.042 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 0.0321(3) 0.0222(3) 0.0268(3) -0.00093(18) -0.0107(2) -0.00813(19) O1 0.043(5) 0.021(4) 0.015(4) 0.001(3) -0.011(3) -0.018(4) C1 0.034(7) 0.009(5) 0.016(5) -0.002(4) -0.009(5) -0.005(5) O2 0.027(4) 0.013(3) 0.024(4) 0.001(3) -0.015(3) -0.006(3) C2 0.028(6) 0.014(5) 0.019(6) -0.001(4) -0.008(5) -0.008(5) O3 0.029(4) 0.015(4) 0.017(4) -0.005(3) -0.003(3) -0.009(3) C3 0.037(7) 0.020(6) 0.021(6) 0.000(5) -0.009(5) -0.016(5) O4 0.016(4) 0.010(3) 0.024(4) -0.004(3) -0.009(3) 0.001(3) C4 0.037(7) 0.016(5) 0.019(6) 0.001(5) -0.013(5) -0.005(5) O5 0.020(4) 0.019(4) 0.017(4) 0.001(3) -0.006(3) -0.011(3) C5 0.028(6) 0.015(5) 0.024(6) 0.000(4) -0.017(5) -0.003(5) C6 0.021(6) 0.016(5) 0.023(6) 0.001(4) -0.008(5) -0.006(4) C7 0.041(7) 0.037(7) 0.020(6) 0.008(5) -0.015(5) -0.015(6) C8 0.090(13) 0.101(14) 0.032(8) 0.026(9) -0.029(8) -0.059(11) C9 0.120(17) 0.056(10) 0.056(11) 0.025(9) -0.032(11) -0.016(11) C10 0.15(2) 0.120(17) 0.032(9) 0.006(10) -0.031(11) -0.098(16) C11 0.023(6) 0.019(6) 0.038(7) 0.007(5) -0.013(5) -0.005(5) C12 0.009(5) 0.018(5) 0.024(6) -0.006(5) -0.003(4) -0.001(4) C13 0.025(6) 0.024(6) 0.020(6) 0.001(5) -0.006(5) -0.008(5) C14 0.024(6) 0.035(7) 0.030(7) -0.005(5) -0.007(5) -0.007(5) C15 0.020(6) 0.025(6) 0.030(6) -0.011(5) -0.005(5) -0.008(5) C16 0.017(6) 0.022(6) 0.031(6) 0.000(5) -0.006(5) -0.007(5) C17 0.012(5) 0.013(5) 0.027(6) -0.006(4) -0.004(5) 0.002(4) C18 0.062(9) 0.046(8) 0.028(7) -0.009(6) -0.024(7) -0.016(7) C22 0.022(6) 0.015(5) 0.027(6) -0.001(4) -0.009(5) -0.006(5) C23 0.020(6) 0.009(5) 0.019(5) 0.001(4) -0.004(4) -0.004(4) C24 0.027(6) 0.028(6) 0.027(6) 0.001(5) -0.013(5) -0.015(5) C25 0.028(6) 0.013(5) 0.026(6) -0.006(5) -0.008(5) -0.007(5) C26 0.020(6) 0.012(5) 0.024(6) -0.004(4) -0.005(5) -0.001(4) C27 0.021(6) 0.017(5) 0.020(5) 0.002(4) -0.008(5) -0.012(5) C28 0.014(5) 0.014(5) 0.019(5) 0.005(4) -0.003(4) -0.010(4) C29 0.032(7) 0.025(6) 0.036(7) -0.019(5) -0.015(6) -0.002(5) C30 0.059(9) 0.042(8) 0.029(7) -0.017(6) -0.016(7) -0.011(7) C31 0.099(13) 0.024(7) 0.069(11) -0.008(7) -0.049(10) -0.017(8) C32 0.034(9) 0.102(14) 0.092(13) -0.078(12) -0.016(9) 0.013(9) C33 0.028(6) 0.019(5) 0.018(5) 0.001(4) -0.011(5) -0.009(5) C34 0.023(6) 0.019(5) 0.013(5) 0.000(4) -0.009(4) -0.006(5) C35 0.032(7) 0.013(5) 0.027(6) -0.001(5) -0.010(5) -0.009(5) C36 0.032(7) 0.022(6) 0.025(6) -0.002(5) -0.013(5) -0.007(5) C37 0.019(6) 0.018(5) 0.027(6) -0.001(5) -0.010(5) -0.005(5) C38 0.019(6) 0.013(5) 0.026(6) 0.002(4) -0.010(5) -0.003(4) C39 0.022(6) 0.014(5) 0.014(5) 0.000(4) -0.010(4) -0.003(4) C40 0.026(6) 0.020(6) 0.036(7) -0.013(5) -0.008(5) 0.000(5) C41 0.046(9) 0.052(9) 0.060(10) -0.035(8) -0.018(7) -0.004(7) C42 0.036(8) 0.017(6) 0.064(9) -0.009(6) -0.018(7) 0.000(5) C43 0.032(8) 0.041(8) 0.057(9) -0.019(7) 0.004(7) -0.005(6) C44 0.018(6) 0.011(5) 0.022(6) 0.001(4) -0.004(5) -0.004(4) C45 0.016(5) 0.021(5) 0.018(5) 0.002(4) -0.005(4) -0.011(4) C46 0.026(6) 0.018(5) 0.023(6) 0.001(5) -0.005(5) -0.009(5) C47 0.027(6) 0.025(6) 0.025(6) -0.012(5) -0.004(5) -0.014(5) C48 0.027(6) 0.029(6) 0.021(6) -0.002(5) -0.012(5) -0.009(5) C49 0.022(6) 0.016(5) 0.014(5) -0.002(4) -0.001(4) -0.009(4) C50 0.026(6) 0.021(5) 0.014(5) -0.001(4) -0.005(5) -0.017(5) C51 0.030(7) 0.035(7) 0.023(6) -0.013(5) -0.009(5) -0.011(5) C55 0.028(6) 0.017(5) 0.019(5) 0.007(4) -0.012(5) -0.011(5) C56 0.029(7) 0.030(6) 0.030(6) 0.000(5) -0.009(5) -0.019(5) C57 0.026(6) 0.018(5) 0.027(6) 0.003(5) -0.006(5) -0.015(5) C58 0.020(6) 0.028(6) 0.028(6) 0.001(5) -0.003(5) -0.008(5) C59 0.039(7) 0.044(7) 0.028(6) 0.010(6) -0.023(6) -0.027(6) C60 0.051(8) 0.022(6) 0.031(7) 0.000(5) -0.013(6) -0.024(6) C61 0.041(8) 0.019(6) 0.050(8) -0.001(6) -0.020(6) -0.009(6) C62 0.050(8) 0.025(6) 0.044(8) -0.002(6) -0.030(7) -0.017(6) _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 O2 2.096(7) . ? Bi1 O4 2.112(7) 2_666 ? Bi1 O1 2.119(7) . ? O1 C1 1.384(12) . ? C1 C2 1.390(15) . ? C1 C6 1.398(15) . ? O2 C17 1.372(12) . ? C2 C3 1.406(15) . ? C2 C55 1.490(15) . ? O3 C28 1.389(12) . ? O3 H3A 0.8300 . ? C3 C4 1.393(16) . ? C3 H3B 0.9400 . ? O4 C39 1.391(12) . ? O4 Bi1 2.112(7) 2_666 ? C4 C5 1.368(16) . ? C4 C7 1.561(15) . ? O5 C50 1.401(12) . ? O5 C56 1.483(13) . ? C5 C6 1.407(15) . ? C5 H5A 0.9400 . ? C6 C11 1.523(15) . ? C7 C9 1.49(2) . ? C7 C10 1.502(19) . ? C7 C8 1.55(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.510(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.372(15) . ? C12 C17 1.407(15) . ? C13 C14 1.412(16) . ? C13 H13A 0.9400 . ? C14 C15 1.403(17) . ? C14 C18 1.532(16) . ? C15 C16 1.390(15) . ? C15 H15A 0.9400 . ? C16 C17 1.405(15) . ? C16 C22 1.522(15) . ? C18 C20 1.509(17) . ? C18 C19A 1.544(19) . ? C18 C20A 1.553(19) . ? C18 C21 1.56(3) . ? C18 C19 1.564(17) . ? C18 C21A 1.565(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C19A H19D 0.9700 . ? C19A H19E 0.9700 . ? C19A H19F 0.9700 . ? C20A H20D 0.9700 . ? C20A H20E 0.9700 . ? C20A H20F 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22 C23 1.490(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C28 1.406(14) . ? C23 C24 1.408(15) . ? C24 C25 1.393(16) . ? C24 H24A 0.9400 . ? C25 C26 1.399(15) . ? C25 C29 1.537(14) . ? C26 C27 1.411(14) . ? C26 H26A 0.9400 . ? C27 C28 1.393(15) . ? C27 C33 1.532(14) . ? C29 C32 1.512(19) . ? C29 C31 1.52(2) . ? C29 C30 1.545(17) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.504(15) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.389(15) . ? C34 C39 1.413(14) . ? C35 C36 1.413(17) . ? C35 H35A 0.9400 . ? C36 C37 1.423(15) . ? C36 C40 1.527(15) . ? C37 C38 1.393(15) . ? C37 H37A 0.9400 . ? C38 C39 1.371(15) . ? C38 C44 1.517(14) . ? C40 C43 1.510(18) . ? C40 C42 1.525(18) . ? C40 C41 1.547(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 C45 1.511(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.396(14) . ? C45 C50 1.400(14) . ? C46 C47 1.413(16) . ? C46 H46A 0.9400 . ? C47 C48 1.409(16) . ? C47 C51 1.558(14) . ? C48 C49 1.407(14) . ? C48 H48A 0.9400 . ? C49 C50 1.413(15) . ? C49 C55 1.503(14) . ? C51 C53 1.52(3) . ? C51 C52 1.55(3) . ? C51 C54 1.55(3) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.515(15) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C62 1.374(17) . ? C57 C58 1.383(16) . ? C58 C59 1.395(16) . ? C58 H58A 0.9400 . ? C59 C60 1.381(18) . ? C59 H59A 0.9400 . ? C60 C61 1.378(17) . ? C60 H60A 0.9400 . ? C61 C62 1.400(17) . ? C61 H61A 0.9400 . ? C62 H62A 0.9400 . ? 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 O2 Bi1 O4 94.1(3) . 2_666 ? O2 Bi1 O1 89.9(3) . . ? O4 Bi1 O1 91.6(3) 2_666 . ? C1 O1 Bi1 130.9(6) . . ? O1 C1 C2 117.8(9) . . ? O1 C1 C6 121.9(10) . . ? C2 C1 C6 120.3(10) . . ? C17 O2 Bi1 115.6(6) . . ? C1 C2 C3 119.3(10) . . ? C1 C2 C55 119.7(9) . . ? C3 C2 C55 120.8(10) . . ? C28 O3 H3A 109.5 . . ? C4 C3 C2 121.7(10) . . ? C4 C3 H3B 119.2 . . ? C2 C3 H3B 119.2 . . ? C39 O4 Bi1 124.5(6) . 2_666 ? C5 C4 C3 117.3(10) . . ? C5 C4 C7 121.1(10) . . ? C3 C4 C7 121.5(10) . . ? C50 O5 C56 115.7(7) . . ? C4 C5 C6 123.4(10) . . ? C4 C5 H5A 118.3 . . ? C6 C5 H5A 118.3 . . ? C1 C6 C5 118.0(10) . . ? C1 C6 C11 120.7(9) . . ? C5 C6 C11 121.3(10) . . ? C9 C7 C10 110.9(15) . . ? C9 C7 C8 106.5(13) . . ? C10 C7 C8 108.7(13) . . ? C9 C7 C4 109.3(11) . . ? C10 C7 C4 110.0(11) . . ? C8 C7 C4 111.5(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C6 114.0(9) . . ? C12 C11 H11A 108.8 . . ? C6 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C6 C11 H11B 108.8 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C17 119.4(9) . . ? C13 C12 C11 119.6(10) . . ? C17 C12 C11 120.9(9) . . ? C12 C13 C14 122.4(10) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 116.9(10) . . ? C15 C14 C18 120.4(10) . . ? C13 C14 C18 122.7(11) . . ? C16 C15 C14 122.2(10) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C15 C16 C17 119.0(10) . . ? C15 C16 C22 120.2(9) . . ? C17 C16 C22 120.7(10) . . ? O2 C17 C16 119.6(9) . . ? O2 C17 C12 120.3(9) . . ? C16 C17 C12 120.0(10) . . ? C20 C18 C14 111.3(14) . . ? C20 C18 C19A 80(2) . . ? C14 C18 C19A 115(2) . . ? C20 C18 C20A 39.3(19) . . ? C14 C18 C20A 113(2) . . ? C19A C18 C20A 113(3) . . ? C20 C18 C21 127.1(19) . . ? C14 C18 C21 109.5(15) . . ? C19A C18 C21 111(3) . . ? C20A C18 C21 94(3) . . ? C20 C18 C19 108.8(17) . . ? C14 C18 C19 112.7(14) . . ? C19A C18 C19 31(2) . . ? C20A C18 C19 133(2) . . ? C21 C18 C19 84(2) . . ? C20 C18 C21A 109(2) . . ? C14 C18 C21A 107.3(16) . . ? C19A C18 C21A 129(3) . . ? C20A C18 C21A 71(3) . . ? C21 C18 C21A 25.2(15) . . ? C19 C18 C21A 108(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C19A H19D 109.4 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.4 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21A H21D 109.5 . . ? C18 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C18 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C23 C22 C16 116.7(9) . . ? C23 C22 H22A 108.1 . . ? C16 C22 H22A 108.1 . . ? C23 C22 H22B 108.1 . . ? C16 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C28 C23 C24 117.2(9) . . ? C28 C23 C22 122.4(9) . . ? C24 C23 C22 120.3(9) . . ? C25 C24 C23 123.2(10) . . ? C25 C24 H24A 118.4 . . ? C23 C24 H24A 118.4 . . ? C24 C25 C26 117.2(9) . . ? C24 C25 C29 122.1(10) . . ? C26 C25 C29 120.6(10) . . ? C25 C26 C27 122.0(10) . . ? C25 C26 H26A 119.0 . . ? C27 C26 H26A 119.0 . . ? C28 C27 C26 118.4(9) . . ? C28 C27 C33 122.5(9) . . ? C26 C27 C33 119.1(9) . . ? O3 C28 C27 120.2(9) . . ? O3 C28 C23 118.2(9) . . ? C27 C28 C23 121.6(9) . . ? C32 C29 C31 110.7(13) . . ? C32 C29 C25 110.9(10) . . ? C31 C29 C25 108.8(10) . . ? C32 C29 C30 106.3(12) . . ? C31 C29 C30 108.9(10) . . ? C25 C29 C30 111.3(10) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C27 112.9(8) . . ? C34 C33 H33A 109.0 . . ? C27 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C27 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C39 118.2(9) . . ? C35 C34 C33 120.1(9) . . ? C39 C34 C33 121.4(9) . . ? C34 C35 C36 123.5(10) . . ? C34 C35 H35A 118.3 . . ? C36 C35 H35A 118.3 . . ? C35 C36 C37 115.5(10) . . ? C35 C36 C40 121.0(10) . . ? C37 C36 C40 123.4(10) . . ? C38 C37 C36 121.7(10) . . ? C38 C37 H37A 119.1 . . ? C36 C37 H37A 119.1 . . ? C39 C38 C37 120.5(9) . . ? C39 C38 C44 119.8(9) . . ? C37 C38 C44 118.7(9) . . ? C38 C39 O4 119.2(9) . . ? C38 C39 C34 120.5(9) . . ? O4 C39 C34 120.1(9) . . ? C43 C40 C42 108.4(11) . . ? C43 C40 C36 112.0(10) . . ? C42 C40 C36 110.0(10) . . ? C43 C40 C41 109.3(11) . . ? C42 C40 C41 107.3(10) . . ? C36 C40 C41 109.8(10) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C38 109.6(8) . . ? C45 C44 H44A 109.7 . . ? C38 C44 H44A 109.7 . . ? C45 C44 H44B 109.7 . . ? C38 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? C46 C45 C50 116.8(9) . . ? C46 C45 C44 121.5(9) . . ? C50 C45 C44 121.7(9) . . ? C45 C46 C47 122.9(10) . . ? C45 C46 H46A 118.6 . . ? C47 C46 H46A 118.6 . . ? C48 C47 C46 117.9(9) . . ? C48 C47 C51 120.7(10) . . ? C46 C47 C51 121.4(10) . . ? C49 C48 C47 121.7(10) . . ? C49 C48 H48A 119.2 . . ? C47 C48 H48A 119.2 . . ? C48 C49 C50 117.2(9) . . ? C48 C49 C55 120.8(9) . . ? C50 C49 C55 122.0(9) . . ? C45 C50 O5 119.5(9) . . ? C45 C50 C49 123.5(9) . . ? O5 C50 C49 116.7(9) . . ? C53 C51 C52 131.3(17) . . ? C53 C51 C54 89.6(15) . . ? C52 C51 C54 97.4(16) . . ? C53 C51 C47 108.9(13) . . ? C52 C51 C47 111.9(14) . . ? C54 C51 C47 113.6(13) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C2 C55 C49 111.5(8) . . ? C2 C55 H55A 109.3 . . ? C49 C55 H55A 109.3 . . ? C2 C55 H55B 109.3 . . ? C49 C55 H55B 109.3 . . ? H55A C55 H55B 108.0 . . ? O5 C56 C57 105.5(8) . . ? O5 C56 H56A 110.6 . . ? C57 C56 H56A 110.6 . . ? O5 C56 H56B 110.6 . . ? C57 C56 H56B 110.6 . . ? H56A C56 H56B 108.8 . . ? C62 C57 C58 119.6(10) . . ? C62 C57 C56 120.9(10) . . ? C58 C57 C56 119.5(10) . . ? C57 C58 C59 119.6(11) . . ? C57 C58 H58A 120.2 . . ? C59 C58 H58A 120.2 . . ? C60 C59 C58 120.8(11) . . ? C60 C59 H59A 119.6 . . ? C58 C59 H59A 119.6 . . ? C61 C60 C59 119.4(11) . . ? C61 C60 H60A 120.3 . . ? C59 C60 H60A 120.3 . . ? C60 C61 C62 119.7(12) . . ? C60 C61 H61A 120.2 . . ? C62 C61 H61A 120.2 . . ? C57 C62 C61 120.8(11) . . ? C57 C62 H62A 119.6 . . ? C61 C62 H62A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.008 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.265 # Attachment 'CCDC-716837.CIF' data_tcu140m _database_code_depnum_ccdc_archive 'CCDC 716837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 O6 Sb2' _chemical_formula_sum 'C62 H72 O6 Sb2' _chemical_formula_weight 1156.72 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' Sb Sb -0.5866 1.5461 '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 14.411(4) _cell_length_b 16.183(4) _cell_length_c 16.211(4) _cell_angle_alpha 94.706(5) _cell_angle_beta 109.515(5) _cell_angle_gamma 105.495(5) _cell_volume 3372.4(16) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8701 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 18324 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.34 _reflns_number_total 9667 _reflns_number_gt 6397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. Disorder for the tert-butyl groups was due to 2-fold axis, and was modeled using partial occupancies and isotropic displacement parameters. The larger solvent void problem could not be fixed by the SQUEEZE program since no large residual (1.94) map density was available. ; _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^)+(0.1317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9667 _refine_ls_number_parameters 624 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.1993 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.009 _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 Sb1 Sb 0.45231(5) 0.37070(4) -0.00783(4) 0.0305(2) Uani 1 1 d . . . O1 O 0.5586(4) 0.4017(4) 0.1142(4) 0.0294(14) Uani 1 1 d . . . C1 C 0.6356(7) 0.3620(6) 0.1427(5) 0.026(2) Uani 1 1 d . . . Sb2 Sb 0.50912(5) 0.22659(4) -0.14954(4) 0.0354(2) Uani 1 1 d . . . O2 O 0.5418(5) 0.4630(4) -0.0503(4) 0.0315(15) Uani 1 1 d . . . C2 C 0.6239(7) 0.2992(6) 0.1948(6) 0.033(2) Uani 1 1 d . . . O3 O 0.4030(5) 0.2778(4) -0.2172(4) 0.0348(16) Uani 1 1 d . . . C3 C 0.7042(8) 0.2667(7) 0.2298(6) 0.037(2) Uani 1 1 d . . . H3A H 0.6960 0.2243 0.2654 0.044 Uiso 1 1 calc R . . O4 O 0.4033(5) 0.1115(4) -0.1719(4) 0.0392(16) Uani 1 1 d . . . C4 C 0.7969(8) 0.2922(7) 0.2160(6) 0.037(2) Uani 1 1 d . A . O5 O 0.4803(5) 0.1223(4) 0.0884(4) 0.0384(16) Uani 1 1 d . . . C5 C 0.8037(7) 0.3542(6) 0.1623(6) 0.033(2) Uani 1 1 d . . . H5A H 0.8652 0.3733 0.1511 0.039 Uiso 1 1 calc R . . O6 O 0.5006(5) 0.2766(4) -0.0412(4) 0.0379(16) Uani 1 1 d . . . C6 C 0.7262(7) 0.3895(6) 0.1245(6) 0.029(2) Uani 1 1 d . . . C7 C 0.8891(8) 0.2591(7) 0.2623(7) 0.049(3) Uani 1 1 d D . . C8 C 0.857(2) 0.1618(11) 0.2343(17) 0.085(10) Uiso 0.478(11) 1 d PD A 1 H8A H 0.7915 0.1419 0.1845 0.127 Uiso 0.478(11) 1 calc PR A 1 H8B H 0.8509 0.1340 0.2837 0.127 Uiso 0.478(11) 1 calc PR A 1 H8C H 0.9097 0.1466 0.2165 0.127 Uiso 0.478(11) 1 calc PR A 1 C8A C 0.862(2) 0.1859(15) 0.3138(17) 0.097(10) Uiso 0.522(11) 1 d PD A 2 H8AA H 0.7963 0.1431 0.2773 0.145 Uiso 0.522(11) 1 calc PR A 2 H8AB H 0.8582 0.2107 0.3685 0.145 Uiso 0.522(11) 1 calc PR A 2 H8AC H 0.9160 0.1578 0.3280 0.145 Uiso 0.522(11) 1 calc PR A 2 C9 C 0.9224(19) 0.2837(15) 0.3641(11) 0.060(7) Uiso 0.478(11) 1 d PD A 1 H9A H 0.8736 0.2444 0.3835 0.090 Uiso 0.478(11) 1 calc PR A 1 H9B H 0.9234 0.3432 0.3798 0.090 Uiso 0.478(11) 1 calc PR A 1 H9C H 0.9911 0.2792 0.3931 0.090 Uiso 0.478(11) 1 calc PR A 1 C9A C 0.983(2) 0.3319(17) 0.3299(18) 0.137(15) Uiso 0.522(11) 1 d PD A 2 H9AA H 1.0232 0.3644 0.2988 0.205 Uiso 0.522(11) 1 calc PR A 2 H9AB H 1.0260 0.3063 0.3731 0.205 Uiso 0.522(11) 1 calc PR A 2 H9AC H 0.9591 0.3709 0.3603 0.205 Uiso 0.522(11) 1 calc PR A 2 C10 C 0.9828(17) 0.3025(15) 0.2387(16) 0.067(8) Uiso 0.478(11) 1 d PD A 1 H10A H 0.9714 0.2761 0.1788 0.101 Uiso 0.478(11) 1 calc PR A 1 H10B H 1.0445 0.2945 0.2805 0.101 Uiso 0.478(11) 1 calc PR A 1 H10C H 0.9917 0.3644 0.2418 0.101 Uiso 0.478(11) 1 calc PR A 1 C10A C 0.924(2) 0.2212(17) 0.1920(16) 0.099(10) Uiso 0.522(11) 1 d PD A 2 H10D H 0.8654 0.1777 0.1464 0.149 Uiso 0.522(11) 1 calc PR A 2 H10E H 0.9767 0.1945 0.2204 0.149 Uiso 0.522(11) 1 calc PR A 2 H10F H 0.9534 0.2678 0.1651 0.149 Uiso 0.522(11) 1 calc PR A 2 C11 C 0.7407(7) 0.4631(6) 0.0713(6) 0.032(2) Uani 1 1 d . . . H11A H 0.7041 0.5025 0.0845 0.039 Uiso 1 1 calc R . . H11B H 0.8147 0.4965 0.0946 0.039 Uiso 1 1 calc R . . C12 C 0.7055(7) 0.4398(6) -0.0297(6) 0.030(2) Uani 1 1 d . . . C13 C 0.7738(7) 0.4204(6) -0.0666(6) 0.037(2) Uani 1 1 d . . . H13A H 0.8376 0.4169 -0.0286 0.044 Uiso 1 1 calc R . . C14 C 0.7491(7) 0.4060(6) -0.1604(6) 0.035(2) Uani 1 1 d . A . C15 C 0.6561(8) 0.4149(6) -0.2135(7) 0.037(2) Uani 1 1 d . . . H15A H 0.6392 0.4076 -0.2755 0.044 Uiso 1 1 calc R . . C16 C 0.5854(7) 0.4345(6) -0.1781(6) 0.031(2) Uani 1 1 d . . . C17 C 0.6103(7) 0.4445(6) -0.0856(6) 0.028(2) Uani 1 1 d . . . C18 C 0.8241(8) 0.3862(7) -0.2016(6) 0.051(3) Uani 1 1 d D . . C19 C 0.9338(14) 0.4515(13) -0.1454(13) 0.055(7) Uiso 0.478(11) 1 d PD A 1 H19A H 0.9267 0.5036 -0.1175 0.083 Uiso 0.478(11) 1 calc PR A 1 H19B H 0.9721 0.4671 -0.1839 0.083 Uiso 0.478(11) 1 calc PR A 1 H19C H 0.9708 0.4243 -0.0997 0.083 Uiso 0.478(11) 1 calc PR A 1 C19A C 0.9211(15) 0.3783(15) -0.1410(14) 0.076(8) Uiso 0.522(11) 1 d PD A 2 H19D H 0.9124 0.3175 -0.1365 0.114 Uiso 0.522(11) 1 calc PR A 2 H19E H 0.9397 0.4125 -0.0826 0.114 Uiso 0.522(11) 1 calc PR A 2 H19F H 0.9756 0.3997 -0.1637 0.114 Uiso 0.522(11) 1 calc PR A 2 C20 C 0.798(2) 0.3948(17) -0.2954(11) 0.078(9) Uiso 0.478(11) 1 d PD A 1 H20A H 0.7269 0.3604 -0.3296 0.117 Uiso 0.478(11) 1 calc PR A 1 H20B H 0.8436 0.3740 -0.3187 0.117 Uiso 0.478(11) 1 calc PR A 1 H20C H 0.8077 0.4557 -0.3000 0.117 Uiso 0.478(11) 1 calc PR A 1 C20A C 0.8417(16) 0.4482(12) -0.2645(12) 0.048(6) Uiso 0.522(11) 1 d PD A 2 H20D H 0.7828 0.4295 -0.3206 0.072 Uiso 0.522(11) 1 calc PR A 2 H20E H 0.9040 0.4479 -0.2752 0.072 Uiso 0.522(11) 1 calc PR A 2 H20F H 0.8496 0.5068 -0.2379 0.072 Uiso 0.522(11) 1 calc PR A 2 C21 C 0.831(2) 0.2981(12) -0.1860(18) 0.091(10) Uiso 0.478(11) 1 d PD A 1 H21A H 0.7643 0.2543 -0.2199 0.137 Uiso 0.478(11) 1 calc PR A 1 H21B H 0.8484 0.2965 -0.1231 0.137 Uiso 0.478(11) 1 calc PR A 1 H21C H 0.8836 0.2860 -0.2050 0.137 Uiso 0.478(11) 1 calc PR A 1 C21A C 0.7588(17) 0.2969(11) -0.2645(14) 0.069(7) Uiso 0.522(11) 1 d PD A 2 H21D H 0.6858 0.2918 -0.2838 0.104 Uiso 0.522(11) 1 calc PR A 2 H21E H 0.7713 0.2502 -0.2331 0.104 Uiso 0.522(11) 1 calc PR A 2 H21F H 0.7783 0.2930 -0.3161 0.104 Uiso 0.522(11) 1 calc PR A 2 C22 C 0.4849(7) 0.4464(6) -0.2404(6) 0.034(2) Uani 1 1 d . . . H22A H 0.4398 0.4501 -0.2073 0.040 Uiso 1 1 calc R . . H22B H 0.5013 0.5010 -0.2624 0.040 Uiso 1 1 calc R . . C23 C 0.4283(7) 0.3701(6) -0.3191(6) 0.033(2) Uani 1 1 d . . . C24 C 0.4143(7) 0.3821(7) -0.4059(6) 0.036(2) Uani 1 1 d . . . H24A H 0.4372 0.4389 -0.4162 0.043 Uiso 1 1 calc R . . C25 C 0.3665(8) 0.3113(7) -0.4793(6) 0.042(3) Uani 1 1 d . . . C26 C 0.3335(8) 0.2302(7) -0.4601(6) 0.045(3) Uani 1 1 d . . . H26A H 0.3013 0.1818 -0.5073 0.054 Uiso 1 1 calc R . . C27 C 0.3455(8) 0.2158(7) -0.3731(7) 0.043(3) Uani 1 1 d . . . C28 C 0.3905(8) 0.2873(7) -0.3043(6) 0.037(2) Uani 1 1 d . . . C29 C 0.3568(10) 0.3249(8) -0.5725(7) 0.057(3) Uani 1 1 d . . . C30 C 0.4692(15) 0.3549(13) -0.5735(11) 0.130(8) Uani 1 1 d . . . H30A H 0.4657 0.3644 -0.6326 0.195 Uiso 1 1 calc R . . H30B H 0.5016 0.3101 -0.5578 0.195 Uiso 1 1 calc R . . H30C H 0.5097 0.4088 -0.5307 0.195 Uiso 1 1 calc R . . C31 C 0.3030(17) 0.2463(10) -0.6407(8) 0.131(9) Uani 1 1 d . . . H31A H 0.2320 0.2235 -0.6442 0.197 Uiso 1 1 calc R . . H31B H 0.3378 0.2028 -0.6256 0.197 Uiso 1 1 calc R . . H31C H 0.3031 0.2600 -0.6978 0.197 Uiso 1 1 calc R . . C32 C 0.3147(18) 0.3974(12) -0.5965(9) 0.131(8) Uani 1 1 d . . . H32A H 0.2445 0.3827 -0.5973 0.196 Uiso 1 1 calc R . . H32B H 0.3141 0.4066 -0.6550 0.196 Uiso 1 1 calc R . . H32C H 0.3578 0.4503 -0.5529 0.196 Uiso 1 1 calc R . . C33 C 0.3127(9) 0.1229(7) -0.3582(7) 0.051(3) Uani 1 1 d . . . H33A H 0.3754 0.1059 -0.3331 0.062 Uiso 1 1 calc R . . H33B H 0.2712 0.0847 -0.4165 0.062 Uiso 1 1 calc R . . C34 C 0.2502(9) 0.1043(6) -0.2972(7) 0.043(3) Uani 1 1 d . . . C35 C 0.1426(8) 0.0874(7) -0.3319(7) 0.048(3) Uani 1 1 d . . . H35A H 0.1108 0.0949 -0.3905 0.057 Uiso 1 1 calc R . . C36 C 0.0833(9) 0.0608(8) -0.2843(8) 0.055(3) Uani 1 1 d . A . C37 C 0.1303(8) 0.0474(7) -0.1993(7) 0.046(3) Uani 1 1 d . . . H37A H 0.0890 0.0261 -0.1667 0.056 Uiso 1 1 calc R . . C38 C 0.2369(8) 0.0647(6) -0.1606(6) 0.039(2) Uani 1 1 d . . . C39 C 0.2969(8) 0.0955(6) -0.2084(6) 0.038(2) Uani 1 1 d . . . C40 C -0.0350(10) 0.0470(8) -0.3241(8) 0.072(4) Uani 1 1 d D . . C41 C -0.081(6) 0.117(3) -0.365(3) 0.46(8) Uiso 0.478(11) 1 d PD A 1 H41A H -0.0451 0.1725 -0.3244 0.696 Uiso 0.478(11) 1 calc PR A 1 H41B H -0.1540 0.0999 -0.3744 0.696 Uiso 0.478(11) 1 calc PR A 1 H41C H -0.0722 0.1213 -0.4213 0.696 Uiso 0.478(11) 1 calc PR A 1 C42 C -0.083(3) -0.036(2) -0.399(2) 0.132(15) Uiso 0.478(11) 1 d PD A 1 H42A H -0.0864 -0.0874 -0.3723 0.198 Uiso 0.478(11) 1 calc PR A 1 H42B H -0.0406 -0.0332 -0.4346 0.198 Uiso 0.478(11) 1 calc PR A 1 H42C H -0.1526 -0.0381 -0.4365 0.198 Uiso 0.478(11) 1 calc PR A 1 C43 C -0.085(4) 0.020(3) -0.254(3) 0.21(3) Uiso 0.478(11) 1 d PD A 1 H43A H -0.0381 -0.0010 -0.2082 0.321 Uiso 0.478(11) 1 calc PR A 1 H43B H -0.1503 -0.0259 -0.2831 0.321 Uiso 0.478(11) 1 calc PR A 1 H43C H -0.0957 0.0703 -0.2266 0.321 Uiso 0.478(11) 1 calc PR A 1 C41A C -0.0707(19) 0.0701(13) -0.4197(12) 0.066(7) Uiso 0.522(11) 1 d PD A 2 H41D H -0.1061 0.0167 -0.4640 0.098 Uiso 0.522(11) 1 calc PR A 2 H41E H -0.0105 0.1036 -0.4305 0.098 Uiso 0.522(11) 1 calc PR A 2 H41F H -0.1174 0.1043 -0.4237 0.098 Uiso 0.522(11) 1 calc PR A 2 C42A C -0.0954(18) -0.0481(11) -0.3341(14) 0.065(7) Uiso 0.522(11) 1 d PD A 2 H42D H -0.0736 -0.0663 -0.2771 0.097 Uiso 0.522(11) 1 calc PR A 2 H42E H -0.0823 -0.0837 -0.3774 0.097 Uiso 0.522(11) 1 calc PR A 2 H42F H -0.1689 -0.0550 -0.3542 0.097 Uiso 0.522(11) 1 calc PR A 2 C43A C -0.0650(17) 0.1060(12) -0.2667(12) 0.052(6) Uiso 0.522(11) 1 d PD A 2 H43D H -0.0428 0.0955 -0.2062 0.079 Uiso 0.522(11) 1 calc PR A 2 H43E H -0.1396 0.0936 -0.2904 0.079 Uiso 0.522(11) 1 calc PR A 2 H43F H -0.0317 0.1665 -0.2669 0.079 Uiso 0.522(11) 1 calc PR A 2 C44 C 0.2882(8) 0.0512(6) -0.0656(6) 0.038(2) Uani 1 1 d . . . H44A H 0.3535 0.0401 -0.0599 0.046 Uiso 1 1 calc R . . H44B H 0.2428 -0.0007 -0.0555 0.046 Uiso 1 1 calc R . . C45 C 0.3108(8) 0.1290(6) 0.0069(6) 0.033(2) Uani 1 1 d . . . C46 C 0.2363(7) 0.1695(6) 0.0011(6) 0.034(2) Uani 1 1 d . . . H46A H 0.1735 0.1484 -0.0484 0.041 Uiso 1 1 calc R . . C47 C 0.2480(7) 0.2387(6) 0.0634(6) 0.032(2) Uani 1 1 d . . . C48 C 0.3450(7) 0.2715(6) 0.1326(6) 0.033(2) Uani 1 1 d . . . H48A H 0.3582 0.3210 0.1746 0.039 Uiso 1 1 calc R . . C49 C 0.4229(7) 0.2334(6) 0.1415(6) 0.031(2) Uani 1 1 d . . . C50 C 0.4042(7) 0.1611(6) 0.0803(6) 0.031(2) Uani 1 1 d . . . C51 C 0.1609(8) 0.2775(7) 0.0540(7) 0.044(3) Uani 1 1 d . . . C52 C 0.0656(9) 0.2066(9) 0.0492(11) 0.080(5) Uani 1 1 d . . . H52A H 0.0808 0.1826 0.1032 0.120 Uiso 1 1 calc R . . H52B H 0.0453 0.1608 -0.0018 0.120 Uiso 1 1 calc R . . H52C H 0.0095 0.2310 0.0429 0.120 Uiso 1 1 calc R . . C53 C 0.1384(11) 0.3168(10) -0.0310(9) 0.076(4) Uani 1 1 d . . . H53A H 0.0826 0.3416 -0.0374 0.114 Uiso 1 1 calc R . . H53B H 0.1183 0.2715 -0.0824 0.114 Uiso 1 1 calc R . . H53C H 0.2002 0.3623 -0.0269 0.114 Uiso 1 1 calc R . . C54 C 0.1852(9) 0.3525(8) 0.1281(8) 0.063(4) Uani 1 1 d . . . H54A H 0.2000 0.3325 0.1845 0.095 Uiso 1 1 calc R . . H54B H 0.1261 0.3738 0.1167 0.095 Uiso 1 1 calc R . . H54C H 0.2451 0.3992 0.1307 0.095 Uiso 1 1 calc R . . C55 C 0.5271(7) 0.2737(6) 0.2184(6) 0.032(2) Uani 1 1 d . . . H55A H 0.5352 0.2322 0.2590 0.038 Uiso 1 1 calc R . . H55B H 0.5245 0.3261 0.2513 0.038 Uiso 1 1 calc R . . C56 C 0.4831(9) 0.0589(8) 0.1468(8) 0.053(3) Uani 1 1 d . . . H56A H 0.5494 0.0468 0.1616 0.063 Uiso 1 1 calc R . . H56B H 0.4798 0.0841 0.2024 0.063 Uiso 1 1 calc R . . C57 C 0.3994(9) -0.0225(8) 0.1081(8) 0.054(3) Uani 1 1 d . . . C58 C 0.3998(9) -0.0845(8) 0.0431(7) 0.054(3) Uani 1 1 d . . . H58A H 0.4577 -0.0717 0.0261 0.065 Uiso 1 1 calc R . . C59 C 0.3248(12) -0.1607(8) 0.0027(8) 0.069(4) Uani 1 1 d . . . H59A H 0.3291 -0.1998 -0.0410 0.083 Uiso 1 1 calc R . . C60 C 0.2369(11) -0.1792(9) 0.0303(9) 0.072(4) Uani 1 1 d . . . H60A H 0.1810 -0.2307 0.0024 0.086 Uiso 1 1 calc R . . C61 C 0.2341(11) -0.1227(10) 0.0964(11) 0.081(4) Uani 1 1 d . . . H61A H 0.1782 -0.1380 0.1158 0.097 Uiso 1 1 calc R . . C62 C 0.3108(11) -0.0443(9) 0.1350(9) 0.069(4) Uani 1 1 d . . . H62A H 0.3060 -0.0051 0.1783 0.083 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 Sb1 0.0203(4) 0.0400(4) 0.0289(4) 0.0093(3) 0.0080(3) 0.0062(3) O1 0.025(3) 0.036(4) 0.024(3) 0.006(3) 0.006(3) 0.010(3) C1 0.022(5) 0.034(5) 0.015(4) 0.002(4) -0.001(4) 0.009(4) Sb2 0.0316(4) 0.0357(4) 0.0401(4) 0.0076(3) 0.0168(3) 0.0077(3) O2 0.031(4) 0.038(4) 0.028(3) 0.004(3) 0.014(3) 0.010(3) C2 0.025(5) 0.046(6) 0.025(5) 0.008(4) 0.006(4) 0.013(5) O3 0.041(4) 0.038(4) 0.025(3) 0.009(3) 0.011(3) 0.011(3) C3 0.044(6) 0.044(6) 0.025(5) 0.011(4) 0.013(5) 0.015(5) O4 0.039(4) 0.035(4) 0.044(4) 0.006(3) 0.017(3) 0.010(3) C4 0.037(6) 0.043(6) 0.032(5) 0.002(5) 0.013(5) 0.017(5) O5 0.033(4) 0.040(4) 0.046(4) 0.009(3) 0.017(3) 0.013(3) C5 0.027(5) 0.047(6) 0.023(5) 0.000(4) 0.008(4) 0.015(5) O6 0.038(4) 0.035(4) 0.032(4) 0.007(3) 0.007(3) 0.008(3) C6 0.020(5) 0.037(5) 0.022(5) 0.004(4) 0.001(4) 0.007(4) C7 0.042(7) 0.058(7) 0.058(7) 0.015(6) 0.021(6) 0.027(6) C11 0.016(5) 0.041(6) 0.032(5) 0.010(4) 0.003(4) 0.002(4) C12 0.024(5) 0.034(5) 0.028(5) 0.003(4) 0.009(4) 0.001(4) C13 0.028(5) 0.045(6) 0.041(6) 0.013(5) 0.016(5) 0.012(5) C14 0.028(5) 0.042(6) 0.040(6) 0.010(5) 0.017(5) 0.012(5) C15 0.037(6) 0.039(6) 0.037(6) 0.012(5) 0.019(5) 0.008(5) C16 0.025(5) 0.031(5) 0.034(5) 0.006(4) 0.011(4) 0.004(4) C17 0.027(5) 0.032(5) 0.025(5) 0.004(4) 0.012(4) 0.006(4) C18 0.048(7) 0.068(8) 0.052(7) 0.012(6) 0.028(6) 0.030(6) C22 0.029(5) 0.044(6) 0.032(5) 0.012(5) 0.014(4) 0.013(5) C23 0.029(5) 0.041(6) 0.031(5) 0.009(4) 0.014(4) 0.012(5) C24 0.027(5) 0.044(6) 0.032(5) 0.008(5) 0.007(4) 0.007(5) C25 0.041(6) 0.044(6) 0.031(5) -0.001(5) 0.013(5) 0.001(5) C26 0.044(6) 0.046(7) 0.028(5) -0.004(5) 0.007(5) -0.001(5) C27 0.042(6) 0.040(6) 0.039(6) 0.006(5) 0.015(5) -0.001(5) C28 0.038(6) 0.043(6) 0.029(5) 0.001(5) 0.015(5) 0.011(5) C29 0.077(9) 0.057(8) 0.032(6) 0.008(6) 0.024(6) 0.007(7) C30 0.153(19) 0.141(17) 0.081(11) 0.018(11) 0.074(13) -0.017(14) C31 0.22(2) 0.079(11) 0.037(8) -0.004(7) 0.047(11) -0.038(12) C32 0.23(2) 0.112(14) 0.043(8) 0.034(9) 0.036(12) 0.054(16) C33 0.061(8) 0.042(6) 0.043(6) 0.003(5) 0.017(6) 0.008(6) C34 0.056(7) 0.030(6) 0.038(6) -0.001(5) 0.021(6) 0.003(5) C35 0.042(7) 0.042(6) 0.035(6) -0.009(5) 0.000(5) -0.001(5) C36 0.040(7) 0.052(7) 0.050(7) -0.008(6) 0.004(6) 0.003(6) C37 0.038(6) 0.040(6) 0.046(7) -0.016(5) 0.013(5) -0.003(5) C38 0.040(6) 0.036(6) 0.037(6) -0.002(5) 0.016(5) 0.007(5) C39 0.033(6) 0.033(6) 0.038(6) -0.005(5) 0.011(5) 0.003(5) C40 0.040(7) 0.076(9) 0.072(9) -0.005(7) 0.005(7) 0.001(7) C44 0.036(6) 0.034(6) 0.043(6) 0.009(5) 0.015(5) 0.005(5) C45 0.038(6) 0.032(5) 0.035(5) 0.004(4) 0.020(5) 0.012(5) C46 0.025(5) 0.037(6) 0.032(5) 0.004(5) 0.006(4) 0.003(4) C47 0.026(5) 0.041(6) 0.027(5) 0.005(4) 0.015(4) 0.000(4) C48 0.035(6) 0.035(6) 0.037(5) 0.008(4) 0.023(5) 0.010(5) C49 0.025(5) 0.035(6) 0.034(5) 0.011(4) 0.014(4) 0.008(4) C50 0.031(5) 0.036(6) 0.035(5) 0.009(4) 0.020(5) 0.013(5) C51 0.034(6) 0.055(7) 0.039(6) 0.003(5) 0.008(5) 0.016(5) C52 0.040(7) 0.076(9) 0.117(12) -0.022(9) 0.037(8) 0.006(7) C53 0.074(10) 0.099(11) 0.071(9) 0.019(8) 0.022(8) 0.056(9) C54 0.053(8) 0.066(8) 0.074(8) -0.013(7) 0.022(7) 0.034(7) C55 0.037(6) 0.036(5) 0.026(5) 0.009(4) 0.014(4) 0.014(5) C56 0.037(7) 0.062(8) 0.058(7) 0.011(6) 0.012(6) 0.020(6) C57 0.058(8) 0.067(8) 0.056(7) 0.023(6) 0.029(6) 0.037(7) C58 0.045(7) 0.071(9) 0.048(7) 0.012(6) 0.016(6) 0.022(7) C59 0.092(11) 0.041(7) 0.040(7) 0.006(6) -0.004(7) 0.005(7) C60 0.060(9) 0.070(9) 0.075(9) 0.015(8) 0.019(8) 0.012(7) C61 0.061(9) 0.092(11) 0.099(11) 0.017(10) 0.046(9) 0.019(9) C62 0.071(9) 0.075(10) 0.080(9) 0.018(8) 0.042(8) 0.034(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 Sb1 O6 1.944(7) . ? Sb1 O1 1.979(6) . ? Sb1 O2 2.025(6) . ? O1 C1 1.394(10) . ? C1 C2 1.385(13) . ? C1 C6 1.400(12) . ? Sb2 O6 1.928(6) . ? Sb2 O4 1.982(6) . ? Sb2 O3 1.983(6) . ? O2 C17 1.379(10) . ? C2 C3 1.369(13) . ? C2 C55 1.529(13) . ? O3 C28 1.389(11) . ? C3 C4 1.388(13) . ? C3 H3A 0.9400 . ? O4 C39 1.388(12) . ? C4 C5 1.387(13) . ? C4 C7 1.548(14) . ? O5 C50 1.377(11) . ? O5 C56 1.452(13) . ? C5 C6 1.375(12) . ? C5 H5A 0.9400 . ? C6 C11 1.536(12) . ? C7 C8 1.501(16) . ? C7 C10 1.531(16) . ? C7 C9A 1.538(17) . ? C7 C10A 1.539(16) . ? C7 C9 1.540(15) . ? C7 C8A 1.543(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C8A H8AC 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C10A H10D 0.9700 . ? C10A H10E 0.9700 . ? C10A H10F 0.9700 . ? C11 C12 1.524(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C17 1.395(13) . ? C12 C13 1.397(13) . ? C13 C14 1.425(13) . ? C13 H13A 0.9400 . ? C14 C15 1.382(14) . ? C14 C18 1.533(13) . ? C15 C16 1.416(13) . ? C15 H15A 0.9400 . ? C16 C17 1.403(12) . ? C16 C22 1.536(13) . ? C18 C19A 1.461(15) . ? C18 C20 1.468(15) . ? C18 C21 1.491(15) . ? C18 C20A 1.522(14) . ? C18 C21A 1.550(15) . ? C18 C19 1.559(15) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19A H19D 0.9700 . ? C19A H19E 0.9700 . ? C19A H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20A H20D 0.9700 . ? C20A H20E 0.9700 . ? C20A H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22 C23 1.525(13) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C28 1.378(14) . ? C23 C24 1.390(13) . ? C24 C25 1.418(13) . ? C24 H24A 0.9400 . ? C25 C26 1.370(14) . ? C25 C29 1.510(14) . ? C26 C27 1.410(14) . ? C26 H26A 0.9400 . ? C27 C28 1.380(13) . ? C27 C33 1.517(14) . ? C29 C31 1.453(17) . ? C29 C32 1.48(2) . ? C29 C30 1.57(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.541(14) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.400(15) . ? C34 C39 1.409(14) . ? C35 C36 1.346(15) . ? C35 H35A 0.9400 . ? C36 C37 1.382(16) . ? C36 C40 1.553(17) . ? C37 C38 1.389(14) . ? C37 H37A 0.9400 . ? C38 C39 1.369(13) . ? C38 C44 1.532(14) . ? C40 C42A 1.517(16) . ? C40 C43A 1.519(15) . ? C40 C41 1.538(19) . ? C40 C42 1.555(18) . ? C40 C43 1.568(19) . ? C40 C41A 1.572(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C41A H41D 0.9700 . ? C41A H41E 0.9700 . ? C41A H41F 0.9700 . ? C42A H42D 0.9700 . ? C42A H42E 0.9700 . ? C42A H42F 0.9700 . ? C43A H43D 0.9700 . ? C43A H43E 0.9700 . ? C43A H43F 0.9700 . ? C44 C45 1.535(13) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.382(13) . ? C45 C50 1.398(13) . ? C46 C47 1.380(13) . ? C46 H46A 0.9400 . ? C47 C48 1.398(13) . ? C47 C51 1.517(14) . ? C48 C49 1.392(13) . ? C48 H48A 0.9400 . ? C49 C50 1.374(13) . ? C49 C55 1.525(13) . ? C51 C52 1.509(16) . ? C51 C54 1.514(15) . ? C51 C53 1.539(16) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.447(16) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.396(16) . ? C57 C62 1.450(17) . ? C58 C59 1.342(16) . ? C58 H58A 0.9400 . ? C59 C60 1.445(19) . ? C59 H59A 0.9400 . ? C60 C61 1.369(19) . ? C60 H60A 0.9400 . ? C61 C62 1.372(19) . ? C61 H61A 0.9400 . ? C62 H62A 0.9400 . ? 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 O6 Sb1 O1 92.3(3) . . ? O6 Sb1 O2 95.6(3) . . ? O1 Sb1 O2 91.9(2) . . ? C1 O1 Sb1 123.4(5) . . ? C2 C1 O1 118.6(8) . . ? C2 C1 C6 120.7(8) . . ? O1 C1 C6 120.6(8) . . ? O6 Sb2 O4 97.8(3) . . ? O6 Sb2 O3 88.6(3) . . ? O4 Sb2 O3 91.8(3) . . ? C17 O2 Sb1 121.5(5) . . ? C3 C2 C1 118.3(9) . . ? C3 C2 C55 121.6(8) . . ? C1 C2 C55 119.9(8) . . ? C28 O3 Sb2 120.0(6) . . ? C2 C3 C4 124.1(9) . . ? C2 C3 H3A 117.9 . . ? C4 C3 H3A 117.9 . . ? C39 O4 Sb2 125.1(6) . . ? C5 C4 C3 115.1(9) . . ? C5 C4 C7 122.1(9) . . ? C3 C4 C7 122.7(9) . . ? C50 O5 C56 114.6(7) . . ? C6 C5 C4 124.1(9) . . ? C6 C5 H5A 117.9 . . ? C4 C5 H5A 117.9 . . ? Sb2 O6 Sb1 134.9(3) . . ? C5 C6 C1 117.7(8) . . ? C5 C6 C11 122.1(8) . . ? C1 C6 C11 120.0(8) . . ? C8 C7 C10 109.6(11) . . ? C8 C7 C9A 137(2) . . ? C10 C7 C9A 59.1(12) . . ? C8 C7 C10A 60.9(12) . . ? C10 C7 C10A 52.3(12) . . ? C9A C7 C10A 107.8(12) . . ? C8 C7 C9 110.1(11) . . ? C10 C7 C9 107.4(10) . . ? C9A C7 C9 50.3(12) . . ? C10A C7 C9 140.7(17) . . ? C8 C7 C8A 50.1(12) . . ? C10 C7 C8A 135.4(17) . . ? C9A C7 C8A 106.3(12) . . ? C10A C7 C8A 106.7(11) . . ? C9 C7 C8A 61.8(12) . . ? C8 C7 C4 109.7(14) . . ? C10 C7 C4 110.9(13) . . ? C9A C7 C4 112.6(16) . . ? C10A C7 C4 109.7(14) . . ? C9 C7 C4 109.2(12) . . ? C8A C7 C4 113.5(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8A H8AA 109.5 . . ? C7 C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7 C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C9A H9AA 109.5 . . ? C7 C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C7 C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C10A H10D 109.5 . . ? C7 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C7 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C12 C11 C6 119.1(8) . . ? C12 C11 H11A 107.5 . . ? C6 C11 H11A 107.5 . . ? C12 C11 H11B 107.5 . . ? C6 C11 H11B 107.5 . . ? H11A C11 H11B 107.0 . . ? C17 C12 C13 119.6(8) . . ? C17 C12 C11 121.2(8) . . ? C13 C12 C11 119.0(8) . . ? C12 C13 C14 121.6(9) . . ? C12 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 117.3(9) . . ? C15 C14 C18 120.6(8) . . ? C13 C14 C18 122.1(9) . . ? C14 C15 C16 122.4(9) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C17 C16 C15 118.7(9) . . ? C17 C16 C22 121.4(8) . . ? C15 C16 C22 119.9(8) . . ? O2 C17 C12 120.3(7) . . ? O2 C17 C16 119.4(8) . . ? C12 C17 C16 120.3(8) . . ? C19A C18 C20 127.0(17) . . ? C19A C18 C21 60.7(12) . . ? C20 C18 C21 113.3(12) . . ? C19A C18 C20A 112.2(11) . . ? C20 C18 C20A 35.2(10) . . ? C21 C18 C20A 139.4(16) . . ? C19A C18 C14 117.3(13) . . ? C20 C18 C14 114.5(14) . . ? C21 C18 C14 107.0(14) . . ? C20A C18 C14 110.6(11) . . ? C19A C18 C21A 109.0(11) . . ? C20 C18 C21A 69.0(11) . . ? C21 C18 C21A 52.3(11) . . ? C20A C18 C21A 104.0(9) . . ? C14 C18 C21A 102.5(12) . . ? C19A C18 C19 45.0(10) . . ? C20 C18 C19 108.9(11) . . ? C21 C18 C19 105.7(11) . . ? C20A C18 C19 77.6(10) . . ? C14 C18 C19 107.0(11) . . ? C21A C18 C19 147.8(14) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C21A H21D 109.5 . . ? C18 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C18 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C23 C22 C16 110.6(8) . . ? C23 C22 H22A 109.5 . . ? C16 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C28 C23 C24 119.0(9) . . ? C28 C23 C22 119.6(8) . . ? C24 C23 C22 121.4(9) . . ? C23 C24 C25 122.1(9) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C26 C25 C24 116.1(9) . . ? C26 C25 C29 122.4(9) . . ? C24 C25 C29 121.4(9) . . ? C25 C26 C27 123.2(9) . . ? C25 C26 H26A 118.4 . . ? C27 C26 H26A 118.4 . . ? C28 C27 C26 118.2(9) . . ? C28 C27 C33 122.8(9) . . ? C26 C27 C33 119.0(9) . . ? C23 C28 C27 121.2(9) . . ? C23 C28 O3 117.7(8) . . ? C27 C28 O3 121.1(9) . . ? C31 C29 C32 112.2(14) . . ? C31 C29 C25 114.6(10) . . ? C32 C29 C25 112.0(11) . . ? C31 C29 C30 104.5(13) . . ? C32 C29 C30 105.3(14) . . ? C25 C29 C30 107.3(11) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 C34 117.3(9) . . ? C27 C33 H33A 108.0 . . ? C34 C33 H33A 108.0 . . ? C27 C33 H33B 108.0 . . ? C34 C33 H33B 108.0 . . ? H33A C33 H33B 107.2 . . ? C35 C34 C39 117.9(10) . . ? C35 C34 C33 120.1(10) . . ? C39 C34 C33 121.7(10) . . ? C36 C35 C34 122.3(10) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? C35 C36 C37 118.5(11) . . ? C35 C36 C40 120.4(11) . . ? C37 C36 C40 121.1(11) . . ? C36 C37 C38 121.9(11) . . ? C36 C37 H37A 119.1 . . ? C38 C37 H37A 119.1 . . ? C39 C38 C37 118.9(10) . . ? C39 C38 C44 119.8(9) . . ? C37 C38 C44 121.3(9) . . ? C38 C39 O4 120.0(9) . . ? C38 C39 C34 120.3(9) . . ? O4 C39 C34 119.5(9) . . ? C42A C40 C43A 110.9(11) . . ? C42A C40 C41 126(3) . . ? C43A C40 C41 61(2) . . ? C42A C40 C36 110.2(13) . . ? C43A C40 C36 110.8(12) . . ? C41 C40 C36 123(3) . . ? C42A C40 C42 43.8(15) . . ? C43A C40 C42 141.4(19) . . ? C41 C40 C42 106.0(16) . . ? C36 C40 C42 106.4(18) . . ? C42A C40 C43 61.2(17) . . ? C43A C40 C43 53.6(19) . . ? C41 C40 C43 106.1(16) . . ? C36 C40 C43 110(2) . . ? C42 C40 C43 103.8(14) . . ? C42A C40 C41A 106.4(10) . . ? C43A C40 C41A 106.1(11) . . ? C41 C40 C41A 45(2) . . ? C36 C40 C41A 112.4(13) . . ? C42 C40 C41A 67.9(16) . . ? C43 C40 C41A 137(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C41A H41D 109.5 . . ? C40 C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40 C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40 C42A H42D 109.5 . . ? C40 C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40 C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C40 C43A H43D 109.5 . . ? C40 C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C40 C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C38 C44 C45 113.8(8) . . ? C38 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C38 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C46 C45 C50 117.6(8) . . ? C46 C45 C44 119.6(9) . . ? C50 C45 C44 122.7(8) . . ? C47 C46 C45 124.2(9) . . ? C47 C46 H46A 117.9 . . ? C45 C46 H46A 117.9 . . ? C46 C47 C48 115.8(9) . . ? C46 C47 C51 121.0(8) . . ? C48 C47 C51 123.2(8) . . ? C49 C48 C47 122.3(9) . . ? C49 C48 H48A 118.9 . . ? C47 C48 H48A 118.9 . . ? C50 C49 C48 119.2(9) . . ? C50 C49 C55 121.8(8) . . ? C48 C49 C55 119.0(8) . . ? C49 C50 O5 119.9(8) . . ? C49 C50 C45 120.7(9) . . ? O5 C50 C45 119.3(8) . . ? C52 C51 C54 108.8(10) . . ? C52 C51 C47 109.1(9) . . ? C54 C51 C47 114.8(9) . . ? C52 C51 C53 110.4(11) . . ? C54 C51 C53 104.6(10) . . ? C47 C51 C53 109.2(9) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 C2 117.3(7) . . ? C49 C55 H55A 108.0 . . ? C2 C55 H55A 108.0 . . ? C49 C55 H55B 108.0 . . ? C2 C55 H55B 108.0 . . ? H55A C55 H55B 107.2 . . ? C57 C56 O5 113.3(9) . . ? C57 C56 H56A 108.9 . . ? O5 C56 H56A 108.9 . . ? C57 C56 H56B 108.9 . . ? O5 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C58 C57 C56 121.8(11) . . ? C58 C57 C62 116.4(12) . . ? C56 C57 C62 121.8(11) . . ? C59 C58 C57 125.6(13) . . ? C59 C58 H58A 117.2 . . ? C57 C58 H58A 117.2 . . ? C58 C59 C60 116.2(13) . . ? C58 C59 H59A 121.9 . . ? C60 C59 H59A 121.9 . . ? C61 C60 C59 120.8(13) . . ? C61 C60 H60A 119.6 . . ? C59 C60 H60A 119.6 . . ? C60 C61 C62 121.6(13) . . ? C60 C61 H61A 119.2 . . ? C62 C61 H61A 119.2 . . ? C61 C62 C57 119.2(13) . . ? C61 C62 H62A 120.4 . . ? C57 C62 H62A 120.4 . . ? 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 O6 Sb1 O1 C1 4.4(6) . . . . ? O2 Sb1 O1 C1 -91.3(6) . . . . ? Sb1 O1 C1 C2 -102.3(8) . . . . ? Sb1 O1 C1 C6 82.3(9) . . . . ? O6 Sb1 O2 C17 -2.0(6) . . . . ? O1 Sb1 O2 C17 90.5(6) . . . . ? O1 C1 C2 C3 -173.7(8) . . . . ? C6 C1 C2 C3 1.6(13) . . . . ? O1 C1 C2 C55 1.2(12) . . . . ? C6 C1 C2 C55 176.5(8) . . . . ? O6 Sb2 O3 C28 161.7(7) . . . . ? O4 Sb2 O3 C28 -100.6(7) . . . . ? C1 C2 C3 C4 -0.4(15) . . . . ? C55 C2 C3 C4 -175.2(9) . . . . ? O6 Sb2 O4 C39 78.7(7) . . . . ? O3 Sb2 O4 C39 -10.1(7) . . . . ? C2 C3 C4 C5 -0.5(14) . . . . ? C2 C3 C4 C7 175.3(9) . . . . ? C3 C4 C5 C6 0.1(14) . . . . ? C7 C4 C5 C6 -175.7(9) . . . . ? O4 Sb2 O6 Sb1 -111.9(5) . . . . ? O3 Sb2 O6 Sb1 -20.3(5) . . . . ? O1 Sb1 O6 Sb2 -146.4(5) . . . . ? O2 Sb1 O6 Sb2 -54.2(5) . . . . ? C4 C5 C6 C1 1.1(14) . . . . ? C4 C5 C6 C11 175.2(8) . . . . ? C2 C1 C6 C5 -2.0(13) . . . . ? O1 C1 C6 C5 173.2(7) . . . . ? C2 C1 C6 C11 -176.3(8) . . . . ? O1 C1 C6 C11 -1.0(12) . . . . ? C5 C4 C7 C8 -122.2(13) . . . . ? C3 C4 C7 C8 62.3(14) . . . . ? C5 C4 C7 C10 -1.1(14) . . . . ? C3 C4 C7 C10 -176.6(12) . . . . ? C5 C4 C7 C9A 63.0(15) . . . . ? C3 C4 C7 C9A -112.5(15) . . . . ? C5 C4 C7 C10A -57.1(15) . . . . ? C3 C4 C7 C10A 127.4(14) . . . . ? C5 C4 C7 C9 117.0(12) . . . . ? C3 C4 C7 C9 -58.5(14) . . . . ? C5 C4 C7 C8A -176.2(13) . . . . ? C3 C4 C7 C8A 8.2(15) . . . . ? C5 C6 C11 C12 94.5(10) . . . . ? C1 C6 C11 C12 -91.5(11) . . . . ? C6 C11 C12 C17 98.7(11) . . . . ? C6 C11 C12 C13 -86.7(11) . . . . ? C17 C12 C13 C14 0.5(14) . . . . ? C11 C12 C13 C14 -174.2(9) . . . . ? C12 C13 C14 C15 2.2(14) . . . . ? C12 C13 C14 C18 178.9(9) . . . . ? C13 C14 C15 C16 -2.1(14) . . . . ? C18 C14 C15 C16 -178.9(9) . . . . ? C14 C15 C16 C17 -0.6(14) . . . . ? C14 C15 C16 C22 178.1(9) . . . . ? Sb1 O2 C17 C12 -78.2(9) . . . . ? Sb1 O2 C17 C16 104.7(8) . . . . ? C13 C12 C17 O2 179.6(8) . . . . ? C11 C12 C17 O2 -5.9(13) . . . . ? C13 C12 C17 C16 -3.3(14) . . . . ? C11 C12 C17 C16 171.2(8) . . . . ? C15 C16 C17 O2 -179.5(8) . . . . ? C22 C16 C17 O2 1.8(13) . . . . ? C15 C16 C17 C12 3.4(13) . . . . ? C22 C16 C17 C12 -175.3(8) . . . . ? C15 C14 C18 C19A 179.6(12) . . . . ? C13 C14 C18 C19A 3.0(16) . . . . ? C15 C14 C18 C20 11.2(16) . . . . ? C13 C14 C18 C20 -165.4(13) . . . . ? C15 C14 C18 C21 -115.2(13) . . . . ? C13 C14 C18 C21 68.2(14) . . . . ? C15 C14 C18 C20A 49.2(13) . . . . ? C13 C14 C18 C20A -127.4(11) . . . . ? C15 C14 C18 C21A -61.2(13) . . . . ? C13 C14 C18 C21A 122.2(11) . . . . ? C15 C14 C18 C19 132.0(12) . . . . ? C13 C14 C18 C19 -44.6(13) . . . . ? C17 C16 C22 C23 -131.3(9) . . . . ? C15 C16 C22 C23 50.0(11) . . . . ? C16 C22 C23 C28 64.1(11) . . . . ? C16 C22 C23 C24 -115.5(10) . . . . ? C28 C23 C24 C25 -2.9(15) . . . . ? C22 C23 C24 C25 176.7(9) . . . . ? C23 C24 C25 C26 0.9(15) . . . . ? C23 C24 C25 C29 -176.9(10) . . . . ? C24 C25 C26 C27 -0.2(17) . . . . ? C29 C25 C26 C27 177.5(11) . . . . ? C25 C26 C27 C28 1.6(18) . . . . ? C25 C26 C27 C33 -175.9(11) . . . . ? C24 C23 C28 C27 4.3(15) . . . . ? C22 C23 C28 C27 -175.3(9) . . . . ? C24 C23 C28 O3 -178.2(8) . . . . ? C22 C23 C28 O3 2.2(14) . . . . ? C26 C27 C28 C23 -3.6(16) . . . . ? C33 C27 C28 C23 173.8(10) . . . . ? C26 C27 C28 O3 178.9(9) . . . . ? C33 C27 C28 O3 -3.7(16) . . . . ? Sb2 O3 C28 C23 -105.1(9) . . . . ? Sb2 O3 C28 C27 72.4(11) . . . . ? C26 C25 C29 C31 4(2) . . . . ? C24 C25 C29 C31 -178.0(14) . . . . ? C26 C25 C29 C32 133.7(14) . . . . ? C24 C25 C29 C32 -48.7(17) . . . . ? C26 C25 C29 C30 -111.2(14) . . . . ? C24 C25 C29 C30 66.4(15) . . . . ? C28 C27 C33 C34 47.1(16) . . . . ? C26 C27 C33 C34 -135.5(11) . . . . ? C27 C33 C34 C35 84.2(13) . . . . ? C27 C33 C34 C39 -102.0(12) . . . . ? C39 C34 C35 C36 -2.1(16) . . . . ? C33 C34 C35 C36 172.0(10) . . . . ? C34 C35 C36 C37 -1.9(17) . . . . ? C34 C35 C36 C40 177.2(10) . . . . ? C35 C36 C37 C38 3.2(17) . . . . ? C40 C36 C37 C38 -175.9(10) . . . . ? C36 C37 C38 C39 -0.2(16) . . . . ? C36 C37 C38 C44 178.8(10) . . . . ? C37 C38 C39 O4 -178.7(9) . . . . ? C44 C38 C39 O4 2.3(14) . . . . ? C37 C38 C39 C34 -3.9(15) . . . . ? C44 C38 C39 C34 177.0(9) . . . . ? Sb2 O4 C39 C38 -119.5(9) . . . . ? Sb2 O4 C39 C34 65.8(11) . . . . ? C35 C34 C39 C38 5.1(15) . . . . ? C33 C34 C39 C38 -168.9(9) . . . . ? C35 C34 C39 O4 179.8(9) . . . . ? C33 C34 C39 O4 5.9(14) . . . . ? C35 C36 C40 C42A 116.7(13) . . . . ? C37 C36 C40 C42A -64.2(15) . . . . ? C35 C36 C40 C43A -120.2(13) . . . . ? C37 C36 C40 C43A 58.9(15) . . . . ? C35 C36 C40 C41 -52(3) . . . . ? C37 C36 C40 C41 127(3) . . . . ? C35 C36 C40 C42 71(2) . . . . ? C37 C36 C40 C42 -110.3(19) . . . . ? C35 C36 C40 C43 -178(2) . . . . ? C37 C36 C40 C43 1(2) . . . . ? C35 C36 C40 C41A -1.7(16) . . . . ? C37 C36 C40 C41A 177.3(12) . . . . ? C39 C38 C44 C45 94.7(11) . . . . ? C37 C38 C44 C45 -84.4(12) . . . . ? C38 C44 C45 C46 44.4(12) . . . . ? C38 C44 C45 C50 -136.4(9) . . . . ? C50 C45 C46 C47 -0.5(14) . . . . ? C44 C45 C46 C47 178.7(9) . . . . ? C45 C46 C47 C48 4.2(14) . . . . ? C45 C46 C47 C51 -177.8(9) . . . . ? C46 C47 C48 C49 -3.9(13) . . . . ? C51 C47 C48 C49 178.1(9) . . . . ? C47 C48 C49 C50 0.1(14) . . . . ? C47 C48 C49 C55 179.4(8) . . . . ? C48 C49 C50 O5 -179.7(8) . . . . ? C55 C49 C50 O5 1.0(13) . . . . ? C48 C49 C50 C45 3.9(13) . . . . ? C55 C49 C50 C45 -175.4(8) . . . . ? C56 O5 C50 C49 85.7(10) . . . . ? C56 O5 C50 C45 -97.8(10) . . . . ? C46 C45 C50 C49 -3.7(13) . . . . ? C44 C45 C50 C49 177.1(9) . . . . ? C46 C45 C50 O5 179.9(8) . . . . ? C44 C45 C50 O5 0.7(13) . . . . ? C46 C47 C51 C52 57.1(13) . . . . ? C48 C47 C51 C52 -125.0(11) . . . . ? C46 C47 C51 C54 179.4(10) . . . . ? C48 C47 C51 C54 -2.7(14) . . . . ? C46 C47 C51 C53 -63.6(13) . . . . ? C48 C47 C51 C53 114.3(11) . . . . ? C50 C49 C55 C2 54.6(12) . . . . ? C48 C49 C55 C2 -124.7(9) . . . . ? C3 C2 C55 C49 -123.2(10) . . . . ? C1 C2 C55 C49 62.1(12) . . . . ? C50 O5 C56 C57 74.0(11) . . . . ? O5 C56 C57 C58 76.2(13) . . . . ? O5 C56 C57 C62 -104.0(13) . . . . ? C56 C57 C58 C59 -178.8(12) . . . . ? C62 C57 C58 C59 1.4(18) . . . . ? C57 C58 C59 C60 -0.4(18) . . . . ? C58 C59 C60 C61 -2(2) . . . . ? C59 C60 C61 C62 4(2) . . . . ? C60 C61 C62 C57 -3(2) . . . . ? C58 C57 C62 C61 0.2(18) . . . . ? C56 C57 C62 C61 -179.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.950 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.216 # Attachment '5.CIF' data_tcu155m _database_code_depnum_ccdc_archive 'CCDC 716838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C140 H112 Bi4 O12' _chemical_formula_sum 'C140 H112 Bi4 O12' _chemical_formula_weight 2822.30 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n n a' _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 34.222(7) _cell_length_b 19.487(4) _cell_length_c 19.805(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13208(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5512 _exptl_absorpt_coefficient_mu 5.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.403 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 66832 _diffrn_reflns_av_R_equivalents 0.1882 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.30 _reflns_number_total 9516 _reflns_number_gt 5664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1258P)^2^+135.4524P] 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 9516 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2388 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Bi2 Bi 0.61899(2) 0.59944(4) 0.19562(4) 0.0307(2) Uani 1 1 d . . . Bi1 Bi 0.64239(2) 0.78133(4) 0.16562(4) 0.0320(2) Uani 1 1 d . . . O5 O 0.6667(3) 0.5950(6) 0.1227(6) 0.029(3) Uani 1 1 d . . . C55 C 0.5966(5) 0.4980(10) 0.3350(10) 0.034(5) Uani 1 1 d . . . H55A H 0.5926 0.4519 0.3535 0.041 Uiso 1 1 calc R . . H55B H 0.5994 0.4942 0.2859 0.041 Uiso 1 1 calc R . . O4 O 0.7102(3) 0.7683(6) 0.1898(6) 0.033(3) Uani 1 1 d . . . O1 O 0.5957(3) 0.6961(6) 0.1331(6) 0.030(3) Uani 1 1 d . . . O3 O 0.6635(4) 0.5436(6) 0.2545(6) 0.036(3) Uani 1 1 d . . . O2 O 0.5913(3) 0.6434(6) 0.3027(6) 0.029(3) Uani 1 1 d . . . C42 C 0.6652(5) 0.5487(9) 0.3221(11) 0.032(5) Uani 1 1 d . . . C56 C 0.5606(5) 0.5451(10) 0.3526(9) 0.028(4) Uani 1 1 d . . . C2 C 0.5293(5) 0.7240(9) 0.1015(9) 0.029(4) Uani 1 1 d . . . C4 C 0.4995(5) 0.6665(10) 0.0045(11) 0.038(5) Uani 1 1 d . . . C15 C 0.6403(7) 0.6431(10) 0.0183(9) 0.042(5) Uani 1 1 d . . . C63 C 0.4497(5) 0.4462(11) 0.4044(10) 0.038(5) Uani 1 1 d . . . C45 C 0.6706(6) 0.5588(11) 0.4647(11) 0.047(6) Uani 1 1 d . . . C60 C 0.5265(5) 0.6550(10) 0.3520(9) 0.029(4) Uani 1 1 d . . . C14 C 0.6031(6) 0.6022(9) 0.0241(10) 0.036(5) Uani 1 1 d . . . H14A H 0.5999 0.5744 -0.0167 0.043 Uiso 1 1 calc R . . H14B H 0.6054 0.5708 0.0626 0.043 Uiso 1 1 calc R . . C43 C 0.7000(5) 0.5731(9) 0.3529(10) 0.032(5) Uani 1 1 d . . . C29 C 0.7613(5) 0.7337(8) 0.1156(9) 0.026(4) Uani 1 1 d . . . C33 C 0.7588(5) 0.8491(10) 0.1571(9) 0.033(5) Uani 1 1 d . . . C34 C 0.7444(6) 0.7846(11) 0.1545(9) 0.038(5) Uani 1 1 d . . . C31 C 0.8115(6) 0.8148(10) 0.0837(10) 0.037(5) Uani 1 1 d . . . C59 C 0.4948(5) 0.6195(9) 0.3808(9) 0.030(5) Uani 1 1 d . . . H59A H 0.4722 0.6452 0.3906 0.036 Uiso 1 1 calc R . . C70 C 0.7354(5) 0.5944(10) 0.3090(11) 0.039(5) Uani 1 1 d . . . H70A H 0.7523 0.5545 0.3015 0.047 Uiso 1 1 calc R . . H70B H 0.7261 0.6105 0.2649 0.047 Uiso 1 1 calc R . . C6 C 0.5674(6) 0.6463(9) 0.0334(10) 0.032(5) Uani 1 1 d . . . C5 C 0.5359(6) 0.6359(10) -0.0088(10) 0.038(5) Uani 1 1 d . . . H5A H 0.5388 0.6079 -0.0471 0.045 Uiso 1 1 calc R . . C40 C 0.9291(7) 0.8096(14) 0.1703(13) 0.067(8) Uani 1 1 d . . . H40A H 0.9321 0.8026 0.2170 0.080 Uiso 1 1 calc R . . C20 C 0.6707(5) 0.6378(10) 0.0676(10) 0.033(5) Uani 1 1 d . . . C49 C 0.6770(7) 0.4931(14) 0.5743(11) 0.055(7) Uani 1 1 d . . . C1 C 0.5645(5) 0.6915(9) 0.0884(10) 0.032(5) Uani 1 1 d . . . C48 C 0.6740(7) 0.5627(13) 0.5420(11) 0.054(6) Uani 1 1 d . . . H48A H 0.6972 0.5898 0.5539 0.065 Uiso 1 1 calc R . . H48B H 0.6511 0.5866 0.5601 0.065 Uiso 1 1 calc R . . C62 C 0.4594(6) 0.5176(10) 0.4294(11) 0.044(6) Uani 1 1 d . . . H62A H 0.4365 0.5469 0.4227 0.053 Uiso 1 1 calc R . . H62B H 0.4644 0.5152 0.4780 0.053 Uiso 1 1 calc R . . C36 C 0.8873(5) 0.8266(9) 0.0738(11) 0.036(5) Uani 1 1 d . . . C58 C 0.4936(5) 0.5505(9) 0.3961(9) 0.029(4) Uani 1 1 d . . . C57 C 0.5278(5) 0.5117(10) 0.3819(9) 0.031(5) Uani 1 1 d . . . H57A H 0.5286 0.4645 0.3917 0.038 Uiso 1 1 calc R . . C30 C 0.7949(5) 0.7499(12) 0.0811(10) 0.039(5) Uani 1 1 d . . . H30A H 0.8070 0.7158 0.0548 0.047 Uiso 1 1 calc R . . C41 C 0.8932(7) 0.8109(11) 0.1426(13) 0.058(7) Uani 1 1 d . . . H41A H 0.8715 0.8010 0.1699 0.069 Uiso 1 1 calc R . . C16 C 0.6490(6) 0.6806(10) -0.0399(10) 0.044(5) Uani 1 1 d . . . H16A H 0.6297 0.6823 -0.0736 0.052 Uiso 1 1 calc R . . C35 C 0.8463(5) 0.8318(12) 0.0414(10) 0.046(6) Uani 1 1 d . . . H35A H 0.8431 0.8788 0.0249 0.055 Uiso 1 1 calc R . . H35B H 0.8460 0.8015 0.0019 0.055 Uiso 1 1 calc R . . C64 C 0.4439(5) 0.3927(10) 0.4497(13) 0.047(6) Uani 1 1 d . . . H64A H 0.4477 0.4004 0.4961 0.056 Uiso 1 1 calc R . . C23 C 0.6750(11) 0.6646(16) -0.2127(16) 0.098(11) Uani 1 1 d . . . H23A H 0.6491 0.6801 -0.2085 0.117 Uiso 1 1 calc R . . C3 C 0.4977(5) 0.7116(10) 0.0578(10) 0.038(5) Uani 1 1 d . . . H3A H 0.4742 0.7353 0.0654 0.046 Uiso 1 1 calc R . . C44 C 0.7021(6) 0.5784(10) 0.4243(11) 0.041(5) Uani 1 1 d . . . H44A H 0.7249 0.5953 0.4446 0.049 Uiso 1 1 calc R . . O6 O 0.6459(3) 0.6915(5) 0.2297(6) 0.026(3) Uani 1 1 d . . . C61 C 0.5610(6) 0.6141(9) 0.3367(10) 0.031(5) Uani 1 1 d . . . C47 C 0.6326(6) 0.5297(8) 0.3650(9) 0.031(5) Uani 1 1 d . . . C28 C 0.7398(5) 0.6639(10) 0.1057(10) 0.041(5) Uani 1 1 d . . . H28A H 0.7583 0.6297 0.0886 0.049 Uiso 1 1 calc R . . H28B H 0.7300 0.6477 0.1494 0.049 Uiso 1 1 calc R . . C69 C 0.5249(6) 0.7297(9) 0.3364(9) 0.031(5) Uani 1 1 d . . . H69A H 0.5000 0.7400 0.3145 0.038 Uiso 1 1 calc R . . H69B H 0.5458 0.7406 0.3043 0.038 Uiso 1 1 calc R . . C17 C 0.6829(6) 0.7148(10) -0.0519(10) 0.041(5) Uani 1 1 d . . . C19 C 0.7062(5) 0.6709(9) 0.0570(9) 0.030(4) Uani 1 1 d . . . C18 C 0.7111(6) 0.7115(11) -0.0030(10) 0.042(5) Uani 1 1 d . . . H18A H 0.7343 0.7366 -0.0088 0.050 Uiso 1 1 calc R . . C68 C 0.4438(6) 0.4314(12) 0.3372(11) 0.047(6) Uani 1 1 d . . . H68A H 0.4467 0.4664 0.3049 0.057 Uiso 1 1 calc R . . C32 C 0.7929(5) 0.8616(12) 0.1231(11) 0.047(6) Uani 1 1 d . . . H32A H 0.8042 0.9053 0.1273 0.056 Uiso 1 1 calc R . . C22 C 0.7004(9) 0.6954(15) -0.1725(13) 0.066(7) Uani 1 1 d . . . C21 C 0.6911(7) 0.7475(12) -0.1202(11) 0.056(6) Uani 1 1 d . . . H21A H 0.6681 0.7739 -0.1345 0.067 Uiso 1 1 calc R . . H21B H 0.7131 0.7795 -0.1158 0.067 Uiso 1 1 calc R . . C11 C 0.4800(8) 0.4979(14) -0.1974(13) 0.069(8) Uani 1 1 d . . . H11A H 0.4841 0.4653 -0.2316 0.083 Uiso 1 1 calc R . . C8 C 0.4683(6) 0.5977(11) -0.0947(11) 0.042(5) Uani 1 1 d . . . C9 C 0.4730(7) 0.6150(12) -0.1630(12) 0.051(6) Uani 1 1 d . . . H9A H 0.4723 0.6617 -0.1751 0.061 Uiso 1 1 calc R . . C46 C 0.6381(6) 0.5335(12) 0.4329(12) 0.052(6) Uani 1 1 d . . . H46A H 0.6177 0.5173 0.4605 0.062 Uiso 1 1 calc R . . C39 C 0.9614(8) 0.8186(12) 0.1299(18) 0.078(9) Uani 1 1 d . . . H39A H 0.9867 0.8156 0.1483 0.093 Uiso 1 1 calc R . . C38 C 0.9564(6) 0.8319(13) 0.0628(14) 0.059(7) Uani 1 1 d . . . H38A H 0.9782 0.8395 0.0349 0.070 Uiso 1 1 calc R . . C12 C 0.4752(6) 0.4793(14) -0.1291(14) 0.063(7) Uani 1 1 d . . . H12A H 0.4756 0.4329 -0.1162 0.075 Uiso 1 1 calc R . . C13 C 0.4700(6) 0.5305(12) -0.0811(11) 0.049(6) Uani 1 1 d . . . H13A H 0.4675 0.5169 -0.0358 0.059 Uiso 1 1 calc R . . C65 C 0.4324(7) 0.3270(11) 0.4275(14) 0.057(7) Uani 1 1 d . . . H65A H 0.4283 0.2917 0.4589 0.069 Uiso 1 1 calc R . . C67 C 0.4334(7) 0.3650(15) 0.3156(14) 0.065(7) Uani 1 1 d . . . H67A H 0.4307 0.3557 0.2693 0.078 Uiso 1 1 calc R . . C7 C 0.4632(6) 0.6529(12) -0.0398(12) 0.057(7) Uani 1 1 d . . . H7A H 0.4416 0.6393 -0.0103 0.068 Uiso 1 1 calc R . . H7B H 0.4557 0.6960 -0.0618 0.068 Uiso 1 1 calc R . . C37 C 0.9205(5) 0.8342(10) 0.0372(11) 0.040(5) Uani 1 1 d . . . H37A H 0.9179 0.8416 -0.0095 0.047 Uiso 1 1 calc R . . C10 C 0.4782(8) 0.5694(14) -0.2109(12) 0.065(7) Uani 1 1 d . . . H10A H 0.4810 0.5846 -0.2557 0.077 Uiso 1 1 calc R . . C50 C 0.7062(8) 0.4500(13) 0.5574(13) 0.061(7) Uani 1 1 d . . . H50A H 0.7240 0.4643 0.5241 0.073 Uiso 1 1 calc R . . C66 C 0.4274(7) 0.3149(13) 0.3609(16) 0.064(7) Uani 1 1 d . . . H66A H 0.4196 0.2711 0.3462 0.077 Uiso 1 1 calc R . . C54 C 0.6502(9) 0.475(2) 0.6263(13) 0.095(11) Uani 1 1 d . . . H54A H 0.6310 0.5053 0.6417 0.114 Uiso 1 1 calc R . . C51 C 0.7114(11) 0.388(2) 0.5849(18) 0.109(14) Uani 1 1 d . . . H51A H 0.7318 0.3599 0.5700 0.130 Uiso 1 1 calc R . . C24 C 0.6804(13) 0.616(2) -0.2574(17) 0.103(11) Uani 1 1 d . . . H24A H 0.6600 0.5985 -0.2842 0.123 Uiso 1 1 calc R . . C25 C 0.7177(17) 0.593(2) -0.2619(18) 0.121(15) Uani 1 1 d . . . H25A H 0.7232 0.5564 -0.2918 0.145 Uiso 1 1 calc R . . C27 C 0.7368(11) 0.675(2) -0.1790(14) 0.104(12) Uani 1 1 d . . . H27A H 0.7567 0.6962 -0.1537 0.125 Uiso 1 1 calc R . . C53 C 0.6539(13) 0.407(2) 0.6541(16) 0.118(14) Uani 1 1 d . . . H53A H 0.6353 0.3888 0.6843 0.141 Uiso 1 1 calc R . . C52 C 0.6877(16) 0.3678(19) 0.633(2) 0.131(18) Uani 1 1 d . . . H52A H 0.6930 0.3260 0.6547 0.157 Uiso 1 1 calc R . . C26 C 0.7466(17) 0.619(3) -0.226(2) 0.17(2) Uani 1 1 d . . . H26A H 0.7723 0.6026 -0.2302 0.209 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 Bi2 0.0242(4) 0.0346(4) 0.0333(4) -0.0046(3) 0.0014(3) -0.0044(3) Bi1 0.0348(4) 0.0368(4) 0.0245(4) -0.0006(3) 0.0042(3) -0.0052(3) O5 0.022(7) 0.030(7) 0.034(8) 0.011(6) 0.000(6) -0.002(5) C55 0.028(10) 0.039(11) 0.035(11) -0.003(9) 0.003(10) -0.011(9) O4 0.013(6) 0.049(8) 0.037(8) 0.000(6) 0.004(6) -0.001(6) O1 0.029(7) 0.035(7) 0.024(7) -0.008(6) -0.008(6) -0.003(6) O3 0.034(8) 0.044(8) 0.031(8) 0.002(6) 0.013(6) 0.002(6) O2 0.024(7) 0.037(7) 0.027(7) 0.002(6) 0.007(6) -0.003(6) C42 0.011(9) 0.024(10) 0.062(15) 0.000(9) 0.002(9) -0.002(8) C56 0.011(9) 0.045(12) 0.027(11) 0.007(9) 0.003(8) -0.003(8) C2 0.022(10) 0.030(10) 0.036(12) 0.007(9) 0.004(9) 0.002(8) C4 0.019(10) 0.051(12) 0.046(13) -0.018(11) -0.008(10) -0.013(9) C15 0.070(15) 0.040(12) 0.015(11) -0.003(9) -0.011(10) -0.016(11) C63 0.016(10) 0.055(14) 0.043(14) -0.001(11) 0.011(9) -0.002(9) C45 0.029(12) 0.061(15) 0.050(15) 0.005(12) 0.002(11) -0.003(11) C60 0.026(10) 0.042(12) 0.020(11) 0.003(8) 0.008(8) 0.002(9) C14 0.045(12) 0.027(10) 0.035(12) -0.020(9) -0.017(10) -0.006(9) C43 0.023(10) 0.032(10) 0.041(14) 0.005(9) 0.003(9) 0.007(8) C29 0.024(10) 0.016(9) 0.040(12) -0.001(8) -0.005(9) 0.000(7) C33 0.030(11) 0.041(12) 0.028(11) -0.003(9) -0.007(9) -0.011(9) C34 0.036(12) 0.059(14) 0.021(11) 0.015(10) -0.003(9) -0.001(11) C31 0.026(11) 0.044(13) 0.040(13) 0.002(10) 0.002(10) -0.007(10) C59 0.017(10) 0.039(12) 0.035(12) -0.013(9) 0.007(9) 0.001(8) C70 0.015(9) 0.043(12) 0.060(14) -0.002(11) 0.008(10) -0.008(9) C6 0.037(12) 0.015(9) 0.045(13) -0.003(9) 0.001(10) -0.010(8) C5 0.038(12) 0.044(12) 0.031(12) -0.014(10) -0.011(10) -0.007(10) C40 0.048(16) 0.09(2) 0.058(16) 0.028(15) -0.025(13) -0.023(14) C20 0.014(10) 0.038(11) 0.048(14) -0.019(10) -0.007(9) 0.003(8) C49 0.040(14) 0.10(2) 0.027(13) 0.000(13) -0.011(11) 0.005(13) C1 0.019(10) 0.032(11) 0.045(13) 0.001(9) -0.013(9) -0.008(8) C48 0.038(14) 0.081(18) 0.044(15) -0.001(13) -0.007(11) 0.007(12) C62 0.027(11) 0.042(12) 0.063(15) -0.004(11) 0.018(11) -0.014(10) C36 0.021(11) 0.028(10) 0.061(15) 0.008(10) -0.008(10) -0.005(8) C58 0.028(11) 0.031(11) 0.027(11) 0.001(8) -0.004(9) 0.003(8) C57 0.030(11) 0.040(11) 0.024(11) 0.010(9) 0.000(9) -0.004(9) C30 0.022(11) 0.069(15) 0.026(12) 0.001(10) 0.003(9) 0.005(10) C41 0.047(15) 0.052(14) 0.073(18) -0.001(13) 0.006(13) -0.007(11) C16 0.047(14) 0.048(13) 0.036(13) 0.000(10) -0.007(10) -0.006(11) C35 0.025(11) 0.074(15) 0.038(13) 0.021(11) 0.003(9) -0.005(11) C64 0.017(10) 0.047(14) 0.076(17) 0.009(12) -0.005(11) -0.004(9) C23 0.13(3) 0.08(2) 0.08(2) -0.034(19) 0.01(2) 0.00(2) C3 0.015(10) 0.048(13) 0.051(14) -0.012(11) 0.003(9) 0.002(9) C44 0.039(13) 0.041(12) 0.043(14) -0.004(10) -0.006(11) 0.012(10) O6 0.024(7) 0.025(6) 0.028(7) 0.009(5) 0.002(6) -0.012(5) C61 0.036(12) 0.019(10) 0.039(12) -0.008(9) -0.006(10) 0.002(8) C47 0.054(14) 0.016(9) 0.022(11) -0.006(8) 0.008(9) 0.005(8) C28 0.027(11) 0.051(13) 0.045(13) -0.010(10) -0.008(10) -0.010(10) C69 0.041(12) 0.030(11) 0.023(11) 0.003(9) -0.001(9) 0.006(9) C17 0.052(14) 0.032(11) 0.040(13) 0.007(10) 0.000(11) -0.007(10) C19 0.024(10) 0.032(10) 0.032(12) 0.000(9) -0.001(9) -0.001(8) C18 0.035(12) 0.054(13) 0.036(13) 0.010(11) 0.005(10) -0.006(10) C68 0.036(12) 0.063(15) 0.043(14) -0.010(12) -0.002(11) -0.016(11) C32 0.019(11) 0.058(14) 0.063(16) 0.011(13) -0.012(11) -0.021(10) C22 0.07(2) 0.09(2) 0.034(15) 0.007(14) 0.009(14) -0.004(16) C21 0.065(16) 0.068(15) 0.034(14) 0.009(12) -0.003(12) -0.025(13) C11 0.09(2) 0.08(2) 0.040(16) -0.011(14) -0.041(15) 0.014(15) C8 0.028(11) 0.043(13) 0.056(16) -0.007(12) -0.005(10) -0.005(10) C9 0.050(15) 0.055(15) 0.048(15) -0.002(12) -0.006(12) 0.006(11) C46 0.030(12) 0.065(16) 0.061(17) 0.010(12) 0.015(12) 0.012(11) C39 0.048(17) 0.046(15) 0.14(3) -0.006(18) -0.011(19) 0.001(12) C38 0.028(13) 0.075(18) 0.073(19) 0.005(15) 0.003(13) -0.013(12) C12 0.030(13) 0.075(18) 0.08(2) -0.021(16) -0.002(13) -0.015(12) C13 0.051(15) 0.060(16) 0.037(13) -0.011(12) 0.000(11) -0.015(12) C65 0.058(16) 0.036(13) 0.08(2) 0.009(13) 0.006(14) -0.015(11) C67 0.041(15) 0.09(2) 0.064(19) -0.025(16) -0.007(13) 0.000(14) C7 0.033(13) 0.068(16) 0.070(17) -0.004(13) -0.021(12) 0.000(12) C37 0.028(12) 0.040(12) 0.050(14) -0.008(10) 0.009(10) -0.005(9) C10 0.09(2) 0.079(19) 0.029(14) -0.007(13) -0.010(13) 0.001(15) C50 0.057(17) 0.060(16) 0.065(18) 0.017(14) -0.005(14) -0.001(13) C66 0.053(16) 0.059(16) 0.08(2) 0.004(16) -0.001(15) -0.024(13) C54 0.10(3) 0.15(3) 0.040(17) -0.014(19) 0.006(17) -0.02(2) C51 0.10(3) 0.16(4) 0.06(2) 0.00(2) -0.01(2) 0.02(3) C24 0.12(3) 0.12(3) 0.07(3) -0.02(2) 0.00(2) -0.01(2) C25 0.20(5) 0.11(3) 0.05(2) -0.01(2) 0.02(3) 0.02(3) C27 0.10(3) 0.16(3) 0.048(19) -0.03(2) 0.027(18) 0.02(2) C53 0.15(4) 0.14(3) 0.07(2) 0.04(2) 0.03(2) -0.04(3) C52 0.20(5) 0.08(2) 0.11(3) -0.01(2) -0.09(3) 0.07(3) C26 0.17(5) 0.27(6) 0.09(3) -0.02(4) 0.00(3) 0.11(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 Bi2 O6 2.127(11) . ? Bi2 O5 2.182(12) . ? Bi2 O3 2.206(13) . ? Bi2 O1 2.391(12) . ? Bi2 O2 2.476(12) . ? Bi2 Bi1 3.6820(12) . ? Bi2 Bi1 3.6868(11) 4_565 ? Bi1 O6 2.142(12) 4_565 ? Bi1 O6 2.166(11) . ? Bi1 O2 2.368(12) 4_565 ? Bi1 O4 2.382(12) . ? Bi1 O1 2.392(11) . ? Bi1 Bi1 3.5583(16) 4_565 ? Bi1 Bi2 3.6868(11) 4_565 ? O5 C20 1.38(2) . ? C55 C47 1.50(3) . ? C55 C56 1.57(3) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? O4 C34 1.40(2) . ? O1 C1 1.39(2) . ? O3 C42 1.34(2) . ? O2 C61 1.36(2) . ? O2 Bi1 2.368(12) 4_565 ? C42 C43 1.42(3) . ? C42 C47 1.45(3) . ? C56 C61 1.38(2) . ? C56 C57 1.42(2) . ? C2 C1 1.38(2) . ? C2 C3 1.41(3) . ? C2 C69 1.53(2) 4_565 ? C4 C3 1.37(3) . ? C4 C5 1.41(3) . ? C4 C7 1.54(3) . ? C15 C16 1.40(3) . ? C15 C20 1.43(3) . ? C15 C14 1.51(3) . ? C63 C68 1.38(3) . ? C63 C64 1.39(3) . ? C63 C62 1.51(3) . ? C45 C46 1.37(3) . ? C45 C44 1.39(3) . ? C45 C48 1.54(3) . ? C60 C59 1.41(2) . ? C60 C61 1.46(2) . ? C60 C69 1.49(2) . ? C14 C6 1.51(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C43 C44 1.42(3) . ? C43 C70 1.55(3) . ? C29 C30 1.37(3) . ? C29 C34 1.38(3) . ? C29 C28 1.56(2) . ? C33 C34 1.35(3) . ? C33 C32 1.37(3) . ? C33 C70 1.52(3) 4_565 ? C31 C32 1.36(3) . ? C31 C30 1.39(3) . ? C31 C35 1.49(3) . ? C59 C58 1.38(3) . ? C59 H59A 0.9400 . ? C70 C33 1.52(3) 4_565 ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C6 C5 1.38(3) . ? C6 C1 1.40(3) . ? C5 H5A 0.9400 . ? C40 C41 1.35(3) . ? C40 C39 1.38(4) . ? C40 H40A 0.9400 . ? C20 C19 1.39(2) . ? C49 C50 1.35(3) . ? C49 C54 1.42(3) . ? C49 C48 1.50(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C62 C58 1.49(2) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C36 C37 1.36(3) . ? C36 C41 1.41(3) . ? C36 C35 1.54(3) . ? C58 C57 1.42(3) . ? C57 H57A 0.9400 . ? C30 H30A 0.9400 . ? C41 H41A 0.9400 . ? C16 C17 1.36(3) . ? C16 H16A 0.9400 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C64 C65 1.41(3) . ? C64 H64A 0.9400 . ? C23 C24 1.31(4) . ? C23 C22 1.32(4) . ? C23 H23A 0.9400 . ? C3 H3A 0.9400 . ? C44 H44A 0.9400 . ? O6 Bi1 2.142(12) 4_565 ? C47 C46 1.36(3) . ? C28 C19 1.51(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C69 C2 1.53(2) 4_565 ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C17 C18 1.37(3) . ? C17 C21 1.52(3) . ? C19 C18 1.44(3) . ? C18 H18A 0.9400 . ? C68 C67 1.41(3) . ? C68 H68A 0.9400 . ? C32 H32A 0.9400 . ? C22 C27 1.31(4) . ? C22 C21 1.49(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C11 C12 1.41(3) . ? C11 C10 1.42(3) . ? C11 H11A 0.9400 . ? C8 C13 1.34(3) . ? C8 C9 1.40(3) . ? C8 C7 1.54(3) . ? C9 C10 1.31(3) . ? C9 H9A 0.9400 . ? C46 H46A 0.9400 . ? C39 C38 1.36(4) . ? C39 H39A 0.9400 . ? C38 C37 1.33(3) . ? C38 H38A 0.9400 . ? C12 C13 1.39(3) . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C65 C66 1.35(3) . ? C65 H65A 0.9400 . ? C67 C66 1.34(3) . ? C67 H67A 0.9400 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C37 H37A 0.9400 . ? C10 H10A 0.9400 . ? C50 C51 1.33(4) . ? C50 H50A 0.9400 . ? C66 H66A 0.9400 . ? C54 C53 1.44(5) . ? C54 H54A 0.9400 . ? C51 C52 1.31(6) . ? C51 H51A 0.9400 . ? C24 C25 1.36(5) . ? C24 H24A 0.9400 . ? C25 C26 1.32(6) . ? C25 H25A 0.9400 . ? C27 C26 1.47(5) . ? C27 H27A 0.9400 . ? C53 C52 1.45(5) . ? C53 H53A 0.9400 . ? C52 H52A 0.9400 . ? C26 H26A 0.9400 . ? 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 O6 Bi2 O5 85.4(4) . . ? O6 Bi2 O3 87.1(5) . . ? O5 Bi2 O3 79.3(4) . . ? O6 Bi2 O1 69.1(4) . . ? O5 Bi2 O1 86.4(4) . . ? O3 Bi2 O1 153.2(4) . . ? O6 Bi2 O2 66.6(4) . . ? O5 Bi2 O2 150.2(4) . . ? O3 Bi2 O2 89.0(4) . . ? O1 Bi2 O2 92.5(4) . . ? O6 Bi2 Bi1 31.3(3) . . ? O5 Bi2 Bi1 76.6(3) . . ? O3 Bi2 Bi1 114.2(3) . . ? O1 Bi2 Bi1 39.7(3) . . ? O2 Bi2 Bi1 83.6(3) . . ? O6 Bi2 Bi1 30.4(3) . 4_565 ? O5 Bi2 Bi1 110.8(3) . 4_565 ? O3 Bi2 Bi1 76.5(3) . 4_565 ? O1 Bi2 Bi1 87.8(3) . 4_565 ? O2 Bi2 Bi1 39.4(3) . 4_565 ? Bi1 Bi2 Bi1 57.75(2) . 4_565 ? O6 Bi1 O6 68.3(5) 4_565 . ? O6 Bi1 O2 68.4(4) 4_565 4_565 ? O6 Bi1 O2 112.7(4) . 4_565 ? O6 Bi1 O4 77.1(4) 4_565 . ? O6 Bi1 O4 75.0(4) . . ? O2 Bi1 O4 137.1(4) 4_565 . ? O6 Bi1 O1 118.0(4) 4_565 . ? O6 Bi1 O1 68.5(4) . . ? O2 Bi1 O1 90.5(4) 4_565 . ? O4 Bi1 O1 129.1(4) . . ? O6 Bi1 Bi1 34.5(3) 4_565 4_565 ? O6 Bi1 Bi1 34.1(3) . 4_565 ? O2 Bi1 Bi1 87.9(3) 4_565 4_565 ? O4 Bi1 Bi1 77.0(3) . 4_565 ? O1 Bi1 Bi1 90.8(3) . 4_565 ? O6 Bi1 Bi2 95.4(3) 4_565 . ? O6 Bi1 Bi2 30.6(3) . . ? O2 Bi1 Bi2 113.1(3) 4_565 . ? O4 Bi1 Bi2 94.4(3) . . ? O1 Bi1 Bi2 39.6(3) . . ? Bi1 Bi1 Bi2 61.19(2) 4_565 . ? O6 Bi1 Bi2 30.2(3) 4_565 4_565 ? O6 Bi1 Bi2 94.8(3) . 4_565 ? O2 Bi1 Bi2 41.5(3) 4_565 4_565 ? O4 Bi1 Bi2 97.4(3) . 4_565 ? O1 Bi1 Bi2 119.5(3) . 4_565 ? Bi1 Bi1 Bi2 61.06(3) 4_565 4_565 ? Bi2 Bi1 Bi2 116.05(3) . 4_565 ? C20 O5 Bi2 125.0(10) . . ? C47 C55 C56 108.3(15) . . ? C47 C55 H55A 110.0 . . ? C56 C55 H55A 110.0 . . ? C47 C55 H55B 110.0 . . ? C56 C55 H55B 110.0 . . ? H55A C55 H55B 108.4 . . ? C34 O4 Bi1 133.6(10) . . ? C1 O1 Bi2 122.3(10) . . ? C1 O1 Bi1 136.8(10) . . ? Bi2 O1 Bi1 100.7(4) . . ? C42 O3 Bi2 121.3(11) . . ? C61 O2 Bi1 133.7(11) . 4_565 ? C61 O2 Bi2 124.8(10) . . ? Bi1 O2 Bi2 99.1(4) 4_565 . ? O3 C42 C43 119.3(17) . . ? O3 C42 C47 122.2(16) . . ? C43 C42 C47 118.5(19) . . ? C61 C56 C57 123.1(17) . . ? C61 C56 C55 120.6(15) . . ? C57 C56 C55 116.2(16) . . ? C1 C2 C3 118.4(17) . . ? C1 C2 C69 120.3(17) . 4_565 ? C3 C2 C69 121.2(16) . 4_565 ? C3 C4 C5 117.1(17) . . ? C3 C4 C7 120.6(18) . . ? C5 C4 C7 122.2(18) . . ? C16 C15 C20 117(2) . . ? C16 C15 C14 121.3(18) . . ? C20 C15 C14 121.5(17) . . ? C68 C63 C64 116(2) . . ? C68 C63 C62 123(2) . . ? C64 C63 C62 121(2) . . ? C46 C45 C44 117(2) . . ? C46 C45 C48 123(2) . . ? C44 C45 C48 120(2) . . ? C59 C60 C61 116.1(17) . . ? C59 C60 C69 122.6(16) . . ? C61 C60 C69 121.3(16) . . ? C6 C14 C15 113.1(16) . . ? C6 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C6 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C44 C43 C42 119.7(18) . . ? C44 C43 C70 120.0(17) . . ? C42 C43 C70 120.3(17) . . ? C30 C29 C34 117.5(17) . . ? C30 C29 C28 122.2(18) . . ? C34 C29 C28 120.0(17) . . ? C34 C33 C32 117.1(19) . . ? C34 C33 C70 120.0(18) . 4_565 ? C32 C33 C70 122.6(18) . 4_565 ? C33 C34 C29 122.6(18) . . ? C33 C34 O4 119.7(18) . . ? C29 C34 O4 117.6(17) . . ? C32 C31 C30 116.1(18) . . ? C32 C31 C35 123.2(19) . . ? C30 C31 C35 120.5(19) . . ? C58 C59 C60 126.2(17) . . ? C58 C59 H59A 116.9 . . ? C60 C59 H59A 116.9 . . ? C33 C70 C43 111.0(16) 4_565 . ? C33 C70 H70A 109.4 4_565 . ? C43 C70 H70A 109.4 . . ? C33 C70 H70B 109.4 4_565 . ? C43 C70 H70B 109.4 . . ? H70A C70 H70B 108.0 . . ? C5 C6 C1 120.4(18) . . ? C5 C6 C14 118.5(16) . . ? C1 C6 C14 120.7(17) . . ? C6 C5 C4 121.1(18) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C41 C40 C39 120(3) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? O5 C20 C19 119.1(16) . . ? O5 C20 C15 120.7(16) . . ? C19 C20 C15 119.8(19) . . ? C50 C49 C54 120(3) . . ? C50 C49 C48 121(2) . . ? C54 C49 C48 120(3) . . ? C2 C1 O1 121.3(17) . . ? C2 C1 C6 119.7(17) . . ? O1 C1 C6 118.6(16) . . ? C49 C48 C45 113(2) . . ? C49 C48 H48A 109.1 . . ? C45 C48 H48A 109.1 . . ? C49 C48 H48B 109.1 . . ? C45 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? C58 C62 C63 115.1(17) . . ? C58 C62 H62A 108.5 . . ? C63 C62 H62A 108.5 . . ? C58 C62 H62B 108.5 . . ? C63 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? C37 C36 C41 114.8(19) . . ? C37 C36 C35 122.0(19) . . ? C41 C36 C35 123.1(18) . . ? C59 C58 C57 116.9(17) . . ? C59 C58 C62 122.7(17) . . ? C57 C58 C62 120.3(17) . . ? C58 C57 C56 119.1(17) . . ? C58 C57 H57A 120.4 . . ? C56 C57 H57A 120.4 . . ? C29 C30 C31 122.2(19) . . ? C29 C30 H30A 118.9 . . ? C31 C30 H30A 118.9 . . ? C40 C41 C36 122(2) . . ? C40 C41 H41A 119.0 . . ? C36 C41 H41A 119.0 . . ? C17 C16 C15 126(2) . . ? C17 C16 H16A 117.2 . . ? C15 C16 H16A 117.2 . . ? C31 C35 C36 118.4(17) . . ? C31 C35 H35A 107.7 . . ? C36 C35 H35A 107.7 . . ? C31 C35 H35B 107.7 . . ? C36 C35 H35B 107.7 . . ? H35A C35 H35B 107.1 . . ? C63 C64 C65 121(2) . . ? C63 C64 H64A 119.4 . . ? C65 C64 H64A 119.4 . . ? C24 C23 C22 130(4) . . ? C24 C23 H23A 115.0 . . ? C22 C23 H23A 115.0 . . ? C4 C3 C2 123.1(17) . . ? C4 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C45 C44 C43 121(2) . . ? C45 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? Bi2 O6 Bi1 119.4(5) . 4_565 ? Bi2 O6 Bi1 118.1(5) . . ? Bi1 O6 Bi1 111.4(5) 4_565 . ? O2 C61 C56 121.9(16) . . ? O2 C61 C60 119.4(15) . . ? C56 C61 C60 118.5(17) . . ? C46 C47 C42 117.4(19) . . ? C46 C47 C55 121.9(18) . . ? C42 C47 C55 120.2(17) . . ? C19 C28 C29 111.2(16) . . ? C19 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C19 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C60 C69 C2 113.9(15) . 4_565 ? C60 C69 H69A 108.8 . . ? C2 C69 H69A 108.8 4_565 . ? C60 C69 H69B 108.8 . . ? C2 C69 H69B 108.8 4_565 . ? H69A C69 H69B 107.7 . . ? C16 C17 C18 117.0(19) . . ? C16 C17 C21 121(2) . . ? C18 C17 C21 121.3(19) . . ? C20 C19 C18 118.8(17) . . ? C20 C19 C28 121.8(17) . . ? C18 C19 C28 119.4(17) . . ? C17 C18 C19 122.0(18) . . ? C17 C18 H18A 119.0 . . ? C19 C18 H18A 119.0 . . ? C63 C68 C67 121(2) . . ? C63 C68 H68A 119.3 . . ? C67 C68 H68A 119.3 . . ? C31 C32 C33 124(2) . . ? C31 C32 H32A 117.9 . . ? C33 C32 H32A 117.9 . . ? C27 C22 C23 115(3) . . ? C27 C22 C21 119(3) . . ? C23 C22 C21 126(3) . . ? C22 C21 C17 112(2) . . ? C22 C21 H21A 109.2 . . ? C17 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C17 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C12 C11 C10 115(2) . . ? C12 C11 H11A 122.3 . . ? C10 C11 H11A 122.3 . . ? C13 C8 C9 115(2) . . ? C13 C8 C7 123(2) . . ? C9 C8 C7 122(2) . . ? C10 C9 C8 123(2) . . ? C10 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? C47 C46 C45 126(2) . . ? C47 C46 H46A 117.0 . . ? C45 C46 H46A 117.0 . . ? C38 C39 C40 119(3) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C37 C38 C39 120(2) . . ? C37 C38 H38A 120.2 . . ? C39 C38 H38A 120.2 . . ? C13 C12 C11 119(2) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C8 C13 C12 125(2) . . ? C8 C13 H13A 117.6 . . ? C12 C13 H13A 117.6 . . ? C66 C65 C64 120(2) . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C66 C67 C68 120(2) . . ? C66 C67 H67A 119.8 . . ? C68 C67 H67A 119.8 . . ? C8 C7 C4 115.5(18) . . ? C8 C7 H7A 108.4 . . ? C4 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C4 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C38 C37 C36 124(2) . . ? C38 C37 H37A 117.8 . . ? C36 C37 H37A 117.8 . . ? C9 C10 C11 122(2) . . ? C9 C10 H10A 118.8 . . ? C11 C10 H10A 118.8 . . ? C51 C50 C49 124(3) . . ? C51 C50 H50A 118.0 . . ? C49 C50 H50A 118.0 . . ? C67 C66 C65 120(2) . . ? C67 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C49 C54 C53 117(3) . . ? C49 C54 H54A 121.4 . . ? C53 C54 H54A 121.4 . . ? C52 C51 C50 119(4) . . ? C52 C51 H51A 120.3 . . ? C50 C51 H51A 120.3 . . ? C23 C24 C25 115(4) . . ? C23 C24 H24A 122.6 . . ? C25 C24 H24A 122.6 . . ? C26 C25 C24 123(4) . . ? C26 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? C22 C27 C26 120(4) . . ? C22 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C54 C53 C52 116(3) . . ? C54 C53 H53A 121.9 . . ? C52 C53 H53A 121.9 . . ? C51 C52 C53 123(4) . . ? C51 C52 H52A 118.6 . . ? C53 C52 H52A 118.6 . . ? C25 C26 C27 117(4) . . ? C25 C26 H26A 121.4 . . ? C27 C26 H26A 121.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.179 _refine_diff_density_min -1.961 _refine_diff_density_rms 0.292 # Attachment '7.CIF' data_tcu157m _database_code_depnum_ccdc_archive 'CCDC 716839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H26 O6 Sb2, C6 H6' _chemical_formula_sum 'C41 H32 O6 Sb2' _chemical_formula_weight 864.17 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.538(2) _cell_length_b 18.489(2) _cell_length_c 25.417(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.258(3) _cell_angle_gamma 90.00 _cell_volume 6590.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 1.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 15662 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4735 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4735 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 Sb2 Sb 0.98309(3) 0.15701(2) 0.668215(14) 0.02538(15) Uani 1 1 d . . . Sb1 Sb 1.05013(3) 0.06597(2) 0.560315(14) 0.02528(15) Uani 1 1 d . . . O2 O 0.9453(3) 0.1314(2) 0.51932(14) 0.0268(9) Uani 1 1 d . . . O5 O 1.0735(3) -0.0629(2) 0.72088(16) 0.0364(11) Uani 1 1 d . . . H5A H 1.0900 -0.0374 0.7487 0.055 Uiso 1 1 calc R . . O4 O 1.0867(3) 0.1452(2) 0.73760(14) 0.0254(9) Uani 1 1 d . . . C13 C 0.8773(4) 0.1620(3) 0.5415(2) 0.0241(13) Uani 1 1 d . . . O1 O 0.9709(3) -0.02413(19) 0.54455(14) 0.0232(8) Uani 1 1 d . . . O6 O 1.0219(3) 0.0772(2) 0.63059(14) 0.0310(10) Uani 1 1 d . . . C34 C 1.1361(4) -0.0526(3) 0.6889(2) 0.0270(13) Uani 1 1 d . . . O3 O 1.0678(3) 0.2231(2) 0.64037(14) 0.0262(9) Uani 1 1 d . . . C12 C 0.8852(4) 0.2358(3) 0.5551(2) 0.0253(13) Uani 1 1 d . . . C11 C 0.8170(5) 0.2654(3) 0.5790(2) 0.0341(15) Uani 1 1 d . . . H11A H 0.8203 0.3148 0.5881 0.041 Uiso 1 1 calc R . . C3 C 0.8805(5) -0.1310(3) 0.6411(2) 0.0343(15) Uani 1 1 d . . . H3A H 0.8995 -0.1702 0.6651 0.041 Uiso 1 1 calc R . . C9 C 0.7371(4) 0.1525(3) 0.5742(2) 0.0339(15) Uani 1 1 d . . . H9A H 0.6870 0.1249 0.5808 0.041 Uiso 1 1 calc R . . C7 C 0.7858(4) 0.0433(3) 0.5284(2) 0.0279(13) Uani 1 1 d . . . H7A H 0.8166 0.0377 0.4987 0.033 Uiso 1 1 calc R . . H7B H 0.7172 0.0362 0.5129 0.033 Uiso 1 1 calc R . . C6 C 0.8217(4) -0.0164(3) 0.5696(2) 0.0273(13) Uani 1 1 d . . . C26 C 1.2514(4) 0.1136(3) 0.7591(2) 0.0289(14) Uani 1 1 d . . . C27 C 1.1809(4) 0.1667(3) 0.7466(2) 0.0269(14) Uani 1 1 d . . . C22 C 1.2044(4) 0.2404(3) 0.7485(2) 0.0274(13) Uani 1 1 d . . . C25 C 1.3462(5) 0.1359(4) 0.7708(2) 0.0377(16) Uani 1 1 d . . . H25A H 1.3951 0.1011 0.7799 0.045 Uiso 1 1 calc R . . C17 C 1.0285(5) 0.4444(3) 0.6405(3) 0.0403(17) Uani 1 1 d . . . H17A H 1.0215 0.4949 0.6398 0.048 Uiso 1 1 calc R . . C16 C 0.9956(5) 0.4046(3) 0.5928(3) 0.0347(15) Uani 1 1 d . . . H16A H 0.9654 0.4284 0.5602 0.042 Uiso 1 1 calc R . . C29 C 1.2118(4) -0.0056(3) 0.7084(2) 0.0281(14) Uani 1 1 d . . . C28 C 1.2246(5) 0.0350(3) 0.7615(2) 0.0309(14) Uani 1 1 d . . . H28A H 1.1651 0.0322 0.7726 0.037 Uiso 1 1 calc R . . H28B H 1.2743 0.0109 0.7896 0.037 Uiso 1 1 calc R . . C4 C 0.7915(5) -0.1007(3) 0.6359(2) 0.0386(16) Uani 1 1 d . . . H4A H 0.7509 -0.1186 0.6562 0.046 Uiso 1 1 calc R . . C15 C 1.0068(4) 0.3312(3) 0.5930(2) 0.0288(14) Uani 1 1 d . . . C20 C 1.0547(4) 0.2965(3) 0.6422(2) 0.0261(13) Uani 1 1 d . . . C32 C 1.1888(5) -0.0790(3) 0.6098(2) 0.0317(15) Uani 1 1 d . . . H32A H 1.1806 -0.1028 0.5762 0.038 Uiso 1 1 calc R . . C24 C 1.3696(5) 0.2080(4) 0.7693(2) 0.0381(16) Uani 1 1 d . . . H24A H 1.4338 0.2218 0.7755 0.046 Uiso 1 1 calc R . . C10 C 0.7461(5) 0.2242(3) 0.5895(3) 0.0372(16) Uani 1 1 d . . . H10A H 0.7032 0.2448 0.6071 0.045 Uiso 1 1 calc R . . C33 C 1.1235(4) -0.0899(3) 0.6394(2) 0.0256(13) Uani 1 1 d . . . C5 C 0.7636(5) -0.0439(3) 0.6006(2) 0.0327(15) Uani 1 1 d . . . H5B H 0.7034 -0.0228 0.5972 0.039 Uiso 1 1 calc R . . C2 C 0.9430(4) -0.1055(3) 0.6120(2) 0.0284(14) Uani 1 1 d . . . C8 C 0.8014(4) 0.1203(3) 0.5491(2) 0.0276(13) Uani 1 1 d . . . C14 C 0.9624(4) 0.2835(3) 0.5442(2) 0.0293(14) Uani 1 1 d . . . H14A H 0.9352 0.3141 0.5124 0.035 Uiso 1 1 calc R . . H14B H 1.0120 0.2533 0.5357 0.035 Uiso 1 1 calc R . . C1 C 0.9105(4) -0.0481(3) 0.5758(2) 0.0256(14) Uani 1 1 d . . . C18 C 1.0711(5) 0.4099(3) 0.6886(3) 0.0349(15) Uani 1 1 d . . . H18A H 1.0911 0.4371 0.7208 0.042 Uiso 1 1 calc R . . C19 C 1.0855(4) 0.3351(3) 0.6905(2) 0.0274(13) Uani 1 1 d . . . C23 C 1.2996(4) 0.2595(3) 0.7590(2) 0.0325(15) Uani 1 1 d . . . H23A H 1.3163 0.3086 0.7589 0.039 Uiso 1 1 calc R . . C30 C 1.2773(4) 0.0033(3) 0.6767(2) 0.0315(14) Uani 1 1 d . . . H30A H 1.3292 0.0349 0.6887 0.038 Uiso 1 1 calc R . . C35 C 1.0374(5) -0.1396(3) 0.6177(2) 0.0329(15) Uani 1 1 d . . . H35A H 1.0398 -0.1580 0.5819 0.040 Uiso 1 1 calc R . . H35B H 1.0431 -0.1812 0.6422 0.040 Uiso 1 1 calc R . . C31 C 1.2662(5) -0.0340(3) 0.6281(2) 0.0345(15) Uani 1 1 d . . . H31A H 1.3113 -0.0286 0.6078 0.041 Uiso 1 1 calc R . . C41 C 0.3946(9) 0.1562(5) 0.6232(4) 0.079(3) Uani 1 1 d . . . H41A H 0.4352 0.1545 0.6588 0.095 Uiso 1 1 calc R . . C21 C 1.1288(4) 0.2998(3) 0.7449(2) 0.0309(14) Uani 1 1 d . . . H21A H 1.0767 0.2790 0.7577 0.037 Uiso 1 1 calc R . . H21B H 1.1576 0.3381 0.7707 0.037 Uiso 1 1 calc R . . C38 C 0.2773(8) 0.1626(5) 0.5218(4) 0.073(3) Uani 1 1 d . . . H38A H 0.2348 0.1656 0.4869 0.087 Uiso 1 1 calc R . . C37 C 0.3654(9) 0.1353(5) 0.5275(4) 0.078(3) Uani 1 1 d . . . H37A H 0.3839 0.1179 0.4971 0.094 Uiso 1 1 calc R . . C40 C 0.3061(8) 0.1805(5) 0.6162(4) 0.068(2) Uani 1 1 d . . . H40A H 0.2841 0.1938 0.6465 0.082 Uiso 1 1 calc R . . C39 C 0.2492(7) 0.1860(5) 0.5663(4) 0.070(2) Uani 1 1 d . . . H39A H 0.1882 0.2063 0.5612 0.084 Uiso 1 1 calc R . . C36 C 0.4296(8) 0.1332(5) 0.5800(6) 0.098(4) Uani 1 1 d . . . H36A H 0.4928 0.1171 0.5855 0.118 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 Sb2 0.0302(3) 0.0256(3) 0.0212(2) -0.00196(15) 0.00838(17) 0.00041(16) Sb1 0.0308(3) 0.0198(2) 0.0270(2) -0.00118(15) 0.01087(17) 0.00014(16) O2 0.035(2) 0.026(2) 0.0219(19) -0.0001(16) 0.0127(17) 0.0040(18) O5 0.047(3) 0.043(3) 0.025(2) -0.0059(18) 0.018(2) -0.008(2) O4 0.026(2) 0.032(2) 0.0196(19) -0.0027(16) 0.0072(16) -0.0015(17) C13 0.026(3) 0.031(3) 0.015(3) 0.001(2) 0.005(2) 0.008(3) O1 0.029(2) 0.019(2) 0.0239(19) -0.0009(16) 0.0129(16) -0.0006(17) O6 0.054(3) 0.021(2) 0.0193(19) 0.0001(16) 0.0117(19) 0.0042(19) C34 0.035(4) 0.024(3) 0.025(3) 0.007(2) 0.013(3) 0.004(3) O3 0.037(2) 0.020(2) 0.0230(19) 0.0001(16) 0.0087(17) 0.0038(17) C12 0.033(3) 0.021(3) 0.021(3) 0.004(2) 0.006(2) 0.006(3) C11 0.036(4) 0.028(4) 0.038(3) -0.005(3) 0.009(3) 0.006(3) C3 0.050(4) 0.027(3) 0.030(3) 0.005(3) 0.018(3) -0.005(3) C9 0.027(4) 0.037(4) 0.037(3) 0.001(3) 0.006(3) 0.003(3) C7 0.028(3) 0.033(4) 0.022(3) -0.002(2) 0.006(2) -0.001(3) C6 0.035(4) 0.024(3) 0.025(3) -0.006(2) 0.012(3) -0.004(3) C26 0.038(4) 0.029(4) 0.022(3) -0.001(2) 0.011(3) 0.002(3) C27 0.035(4) 0.030(4) 0.017(3) -0.004(2) 0.010(2) 0.001(3) C22 0.034(4) 0.030(4) 0.018(3) 0.000(2) 0.006(2) 0.004(3) C25 0.033(4) 0.041(4) 0.038(3) -0.002(3) 0.007(3) 0.007(3) C17 0.045(4) 0.023(4) 0.054(4) -0.004(3) 0.015(3) -0.001(3) C16 0.033(4) 0.023(3) 0.047(4) 0.005(3) 0.009(3) 0.001(3) C29 0.039(4) 0.022(3) 0.024(3) 0.009(2) 0.012(3) 0.008(3) C28 0.040(4) 0.027(3) 0.024(3) 0.002(3) 0.007(3) 0.003(3) C4 0.053(5) 0.032(4) 0.039(4) -0.003(3) 0.027(3) -0.012(3) C15 0.028(3) 0.028(3) 0.032(3) 0.003(3) 0.010(3) 0.002(3) C20 0.031(3) 0.023(3) 0.030(3) 0.001(3) 0.018(3) 0.000(3) C32 0.043(4) 0.028(4) 0.027(3) -0.001(3) 0.014(3) 0.011(3) C24 0.029(4) 0.046(4) 0.039(3) -0.013(3) 0.009(3) -0.008(3) C10 0.038(4) 0.031(4) 0.046(4) -0.007(3) 0.017(3) 0.007(3) C33 0.031(3) 0.015(3) 0.030(3) 0.005(2) 0.007(3) 0.010(3) C5 0.028(4) 0.038(4) 0.035(3) -0.007(3) 0.015(3) -0.007(3) C2 0.042(4) 0.019(3) 0.024(3) -0.004(2) 0.008(3) -0.006(3) C8 0.031(3) 0.025(3) 0.026(3) -0.001(3) 0.007(2) 0.005(3) C14 0.036(4) 0.024(3) 0.027(3) 0.006(2) 0.006(3) 0.007(3) C1 0.043(4) 0.017(3) 0.020(3) -0.006(2) 0.015(3) -0.010(3) C18 0.039(4) 0.023(3) 0.044(4) -0.006(3) 0.013(3) -0.003(3) C19 0.025(3) 0.022(3) 0.037(3) -0.006(3) 0.010(3) -0.001(3) C23 0.038(4) 0.031(4) 0.028(3) -0.008(3) 0.007(3) -0.006(3) C30 0.029(4) 0.032(4) 0.035(3) 0.000(3) 0.011(3) 0.002(3) C35 0.054(4) 0.019(3) 0.028(3) 0.006(2) 0.016(3) 0.005(3) C31 0.038(4) 0.039(4) 0.032(3) -0.001(3) 0.018(3) 0.000(3) C41 0.099(9) 0.063(6) 0.060(6) 0.014(5) -0.006(6) -0.028(6) C21 0.040(4) 0.027(3) 0.028(3) -0.011(3) 0.012(3) 0.000(3) C38 0.095(8) 0.057(6) 0.059(5) 0.001(4) 0.009(5) -0.021(5) C37 0.109(9) 0.060(6) 0.083(7) -0.004(5) 0.056(7) -0.015(6) C40 0.096(8) 0.051(5) 0.060(6) -0.013(4) 0.024(5) -0.018(5) C39 0.075(7) 0.048(5) 0.092(7) 0.001(5) 0.029(6) -0.015(5) C36 0.068(7) 0.064(7) 0.169(12) 0.051(8) 0.043(8) 0.011(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 Sb2 O6 1.922(4) . ? Sb2 O3 1.992(4) . ? Sb2 O4 2.007(4) . ? Sb1 O6 1.946(4) . ? Sb1 O1 2.005(4) . ? Sb1 O2 2.009(4) . ? O2 C13 1.381(7) . ? O5 C34 1.384(7) . ? O5 H5A 0.8300 . ? O4 C27 1.387(7) . ? C13 C12 1.404(8) . ? C13 C8 1.402(8) . ? O1 C1 1.403(6) . ? C34 C29 1.387(9) . ? C34 C33 1.405(8) . ? O3 C20 1.373(7) . ? C12 C11 1.404(8) . ? C12 C14 1.510(8) . ? C11 C10 1.362(9) . ? C11 H11A 0.9400 . ? C3 C4 1.385(9) . ? C3 C2 1.397(8) . ? C3 H3A 0.9400 . ? C9 C10 1.378(9) . ? C9 C8 1.396(8) . ? C9 H9A 0.9400 . ? C7 C8 1.513(8) . ? C7 C6 1.517(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C6 C5 1.394(8) . ? C6 C1 1.388(8) . ? C26 C25 1.394(9) . ? C26 C27 1.393(8) . ? C26 C28 1.509(8) . ? C27 C22 1.403(8) . ? C22 C23 1.385(8) . ? C22 C21 1.539(8) . ? C25 C24 1.379(9) . ? C25 H25A 0.9400 . ? C17 C18 1.373(9) . ? C17 C16 1.390(9) . ? C17 H17A 0.9400 . ? C16 C15 1.366(8) . ? C16 H16A 0.9400 . ? C29 C30 1.407(8) . ? C29 C28 1.513(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C4 C5 1.371(9) . ? C4 H4A 0.9400 . ? C15 C20 1.416(8) . ? C15 C14 1.520(8) . ? C20 C19 1.389(8) . ? C32 C33 1.371(8) . ? C32 C31 1.378(9) . ? C32 H32A 0.9400 . ? C24 C23 1.368(9) . ? C24 H24A 0.9400 . ? C10 H10A 0.9400 . ? C33 C35 1.533(9) . ? C5 H5B 0.9400 . ? C2 C1 1.402(8) . ? C2 C35 1.482(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C18 C19 1.397(8) . ? C18 H18A 0.9400 . ? C19 C21 1.508(8) . ? C23 H23A 0.9400 . ? C30 C31 1.387(8) . ? C30 H30A 0.9400 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C31 H31A 0.9400 . ? C41 C40 1.330(14) . ? C41 C36 1.393(15) . ? C41 H41A 0.9400 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C38 C37 1.348(14) . ? C38 C39 1.369(12) . ? C38 H38A 0.9400 . ? C37 C36 1.412(15) . ? C37 H37A 0.9400 . ? C40 C39 1.324(12) . ? C40 H40A 0.9400 . ? C39 H39A 0.9400 . ? C36 H36A 0.9400 . ? 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 O6 Sb2 O3 90.23(16) . . ? O6 Sb2 O4 95.91(16) . . ? O3 Sb2 O4 89.31(15) . . ? O6 Sb1 O1 91.35(15) . . ? O6 Sb1 O2 95.60(15) . . ? O1 Sb1 O2 94.52(16) . . ? C13 O2 Sb1 124.2(3) . . ? C34 O5 H5A 109.5 . . ? C27 O4 Sb2 126.4(3) . . ? O2 C13 C12 118.6(5) . . ? O2 C13 C8 120.3(5) . . ? C12 C13 C8 121.1(5) . . ? C1 O1 Sb1 124.2(3) . . ? Sb2 O6 Sb1 134.3(2) . . ? C29 C34 O5 117.4(5) . . ? C29 C34 C33 122.1(5) . . ? O5 C34 C33 120.5(5) . . ? C20 O3 Sb2 119.3(3) . . ? C13 C12 C11 117.7(5) . . ? C13 C12 C14 122.6(5) . . ? C11 C12 C14 119.7(5) . . ? C10 C11 C12 121.6(6) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C4 C3 C2 122.3(6) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C10 C9 C8 120.9(6) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C8 C7 C6 116.9(5) . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C5 C6 C1 117.8(5) . . ? C5 C6 C7 120.3(5) . . ? C1 C6 C7 121.8(5) . . ? C25 C26 C27 117.9(6) . . ? C25 C26 C28 121.7(6) . . ? C27 C26 C28 120.3(6) . . ? O4 C27 C26 118.2(5) . . ? O4 C27 C22 120.3(5) . . ? C26 C27 C22 121.3(6) . . ? C23 C22 C27 118.4(6) . . ? C23 C22 C21 119.4(5) . . ? C27 C22 C21 121.9(5) . . ? C24 C25 C26 121.0(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C15 C16 C17 120.7(6) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C34 C29 C30 117.5(5) . . ? C34 C29 C28 122.0(5) . . ? C30 C29 C28 120.5(6) . . ? C26 C28 C29 114.6(5) . . ? C26 C28 H28A 108.6 . . ? C29 C28 H28A 108.6 . . ? C26 C28 H28B 108.6 . . ? C29 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C5 C4 C3 118.7(6) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C16 C15 C20 118.9(6) . . ? C16 C15 C14 123.3(5) . . ? C20 C15 C14 117.6(5) . . ? O3 C20 C19 121.5(5) . . ? O3 C20 C15 117.3(5) . . ? C19 C20 C15 121.2(5) . . ? C33 C32 C31 121.7(6) . . ? C33 C32 H32A 119.1 . . ? C31 C32 H32A 119.1 . . ? C23 C24 C25 120.2(6) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C11 C10 C9 120.2(6) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C32 C33 C34 118.2(6) . . ? C32 C33 C35 120.6(5) . . ? C34 C33 C35 121.2(5) . . ? C4 C5 C6 122.0(6) . . ? C4 C5 H5B 119.0 . . ? C6 C5 H5B 119.0 . . ? C1 C2 C3 116.7(6) . . ? C1 C2 C35 122.0(5) . . ? C3 C2 C35 121.3(5) . . ? C9 C8 C13 118.3(5) . . ? C9 C8 C7 120.2(5) . . ? C13 C8 C7 121.4(5) . . ? C12 C14 C15 111.5(5) . . ? C12 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C12 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? O1 C1 C6 120.3(5) . . ? O1 C1 C2 117.2(5) . . ? C6 C1 C2 122.5(5) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C20 C19 C18 117.8(5) . . ? C20 C19 C21 123.2(5) . . ? C18 C19 C21 118.9(5) . . ? C24 C23 C22 121.0(6) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C31 C30 C29 120.9(6) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C2 C35 C33 115.3(5) . . ? C2 C35 H35A 108.4 . . ? C33 C35 H35A 108.4 . . ? C2 C35 H35B 108.4 . . ? C33 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C32 C31 C30 119.6(6) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C40 C41 C36 122.5(9) . . ? C40 C41 H41A 118.7 . . ? C36 C41 H41A 118.7 . . ? C19 C21 C22 118.9(4) . . ? C19 C21 H21A 107.6 . . ? C22 C21 H21A 107.6 . . ? C19 C21 H21B 107.6 . . ? C22 C21 H21B 107.6 . . ? H21A C21 H21B 107.0 . . ? C37 C38 C39 120.7(9) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C37 C36 119.0(9) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C41 C40 C39 119.6(9) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C40 C39 C38 121.3(10) . . ? C40 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? C41 C36 C37 116.6(10) . . ? C41 C36 H36A 121.7 . . ? C37 C36 H36A 121.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.190 _refine_diff_density_min -1.736 _refine_diff_density_rms 0.146 # Attachment 'CCDC_716840.cif' data_tcu82m _database_code_depnum_ccdc_archive 'CCDC 716840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C114 H144 Bi4 O14 S2, 3.5(C2H6SO)' _chemical_formula_sum 'C121 H165 Bi4 O17.5 S5.5' _chemical_formula_weight 2911.87 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 18.6628(13) _cell_length_b 33.463(2) _cell_length_c 22.8640(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.8140(10) _cell_angle_gamma 90.00 _cell_volume 13433.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5208 _exptl_absorpt_coefficient_mu 5.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2583 _exptl_absorpt_correction_T_max 0.5456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% 'not recorded' _diffrn_reflns_number 91378 _diffrn_reflns_av_R_equivalents 0.1009 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 24057 _reflns_number_gt 17260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. Disorder for the tert-butyl groups was due to 2-fold axis, and was modeled using partial occupancies and isotropic displacement parameters. PLATON/SQUEEZE estimated the solvent-accessible region void to occupy 3858 \%A^3^ and contain 587 electrons. The electron density was modelled as 14 DMSO molecules (3.5 DMSO per assymetric unit) which accounts for 588 electrons. The 1.5 DMSO molecules where added in the formula weight on the structure of assymetric unit. The very large solvent accesible void shown in the checkCIF report can be asssosiated with the use of squeeze indicating where solvent could be located. There is a residual peak of 6.33 eA-3 that was associated with the bismuth atoms. The data adquisition for one more crystal of this compound shows the same problem and we were unable of getting a higher quality crystal. ; _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^)+(0.1168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24057 _refine_ls_number_parameters 1210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1915 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.001 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 0.77021(2) 0.696605(11) 1.402131(19) 0.02595(12) Uani 1 1 d . . . O1 O 0.8784(4) 0.7012(2) 1.4834(4) 0.0308(18) Uani 1 1 d . . . C1 C 0.9290(6) 0.6706(3) 1.5064(5) 0.032(3) Uani 1 1 d . . . S1 S 0.5363(6) 0.7500 1.6376(4) 0.115(3) Uani 1 2 d S . . Bi2 Bi 0.66380(3) 0.7500 1.48807(3) 0.02498(15) Uani 1 2 d S . . Bi2A Bi 0.78856(4) 0.7500 1.26513(3) 0.03338(17) Uani 1 2 d S . . C2 C 0.9256(7) 0.6505(3) 1.5584(5) 0.035(3) Uani 1 1 d . . . S2 S 0.9945(6) 0.7500 1.2700(5) 0.115(3) Uani 1 2 d S . . O2 O 0.8459(5) 0.6960(2) 1.3309(3) 0.0298(18) Uani 1 1 d . . . Bi3 Bi 0.74824(2) 0.696651(11) 1.901822(19) 0.02587(12) Uani 1 1 d . . . O3 O 0.6872(4) 0.7097(2) 1.2286(3) 0.0313(18) Uani 1 1 d . . . C3 C 0.9799(7) 0.6198(3) 1.5816(6) 0.040(3) Uani 1 1 d . . . H3A H 0.9788 0.6057 1.6168 0.048 Uiso 1 1 calc R . . S3 S 0.4743(3) 0.7500 0.9359(3) 0.0575(14) Uani 1 2 d S . . Bi4A Bi 0.72678(3) 0.7500 1.75388(3) 0.02560(15) Uani 1 2 d S . . Bi4 Bi 0.85726(4) 0.7500 2.04506(3) 0.02848(16) Uani 1 2 d S . . O4 O 0.6434(4) 0.69925(19) 1.4146(3) 0.0247(16) Uani 1 1 d . . . C4 C 1.0356(8) 0.6087(4) 1.5558(6) 0.045(3) Uani 1 1 d . A . S4 S 1.0370(3) 0.7500 0.5864(2) 0.0450(11) Uani 1 2 d S . . O5 O 0.7350(5) 0.7044(2) 1.5549(4) 0.035(2) Uani 1 1 d . . . C5 C 1.0393(7) 0.6314(4) 1.5069(6) 0.041(3) Uani 1 1 d . . . H5A H 1.0778 0.6263 1.4900 0.049 Uiso 1 1 calc R . . C6 C 0.9855(6) 0.6627(3) 1.4811(5) 0.031(3) Uani 1 1 d . . . O6 O 0.7570(6) 0.7500 1.3490(5) 0.030(3) Uani 1 2 d S . . O7 O 0.7617(5) 0.7500 1.4607(5) 0.025(2) Uiso 1 2 d S . . C7 C 1.0901(9) 0.5739(5) 1.5818(7) 0.067(5) Uani 1 1 d . . . O8 O 0.6408(5) 0.7014(2) 1.9225(4) 0.041(2) Uani 1 1 d . . . C8 C 1.144(2) 0.5626(13) 1.542(2) 0.084(14) Uiso 0.46(3) 1 d P A 1 H8A H 1.1926 0.5762 1.5590 0.125 Uiso 0.46(3) 1 calc PR A 1 H8B H 1.1195 0.5710 1.4988 0.125 Uiso 0.46(3) 1 calc PR A 1 H8C H 1.1522 0.5340 1.5430 0.125 Uiso 0.46(3) 1 calc PR A 1 C9 C 1.161(2) 0.5923(12) 1.636(2) 0.083(14) Uiso 0.46(3) 1 d P A 1 H9A H 1.1428 0.6090 1.6623 0.125 Uiso 0.46(3) 1 calc PR A 1 H9B H 1.1913 0.6083 1.6173 0.125 Uiso 0.46(3) 1 calc PR A 1 H9C H 1.1919 0.5709 1.6599 0.125 Uiso 0.46(3) 1 calc PR A 1 C8A C 1.067(2) 0.5421(11) 1.5174(18) 0.100(14) Uiso 0.54(3) 1 d P A 2 H8AA H 1.0154 0.5321 1.5085 0.150 Uiso 0.54(3) 1 calc PR A 2 H8AB H 1.1022 0.5199 1.5263 0.150 Uiso 0.54(3) 1 calc PR A 2 H8AC H 1.0698 0.5568 1.4817 0.150 Uiso 0.54(3) 1 calc PR A 2 C9A C 1.160(3) 0.5831(16) 1.581(3) 0.15(2) Uiso 0.54(3) 1 d P A 2 H9AA H 1.1842 0.6013 1.6146 0.224 Uiso 0.54(3) 1 calc PR A 2 H9AB H 1.1550 0.5956 1.5415 0.224 Uiso 0.54(3) 1 calc PR A 2 H9AC H 1.1896 0.5589 1.5858 0.224 Uiso 0.54(3) 1 calc PR A 2 O9 O 0.6727(4) 0.6946(2) 1.7875(3) 0.0233(16) Uani 1 1 d . . . O10A O 0.8748(4) 0.7003(2) 1.9794(4) 0.0304(18) Uani 1 1 d . . . O10 O 0.8284(4) 0.7098(2) 1.7713(3) 0.0280(17) Uani 1 1 d . . . C10 C 1.090(3) 0.5546(15) 1.636(2) 0.090(14) Uiso 0.46(3) 1 d P A 3 H10L H 1.1028 0.5736 1.6698 0.135 Uiso 0.46(3) 1 calc PR A 3 H10M H 1.1270 0.5332 1.6455 0.135 Uiso 0.46(3) 1 calc PR A 3 H10N H 1.0397 0.5437 1.6292 0.135 Uiso 0.46(3) 1 calc PR A 3 C10A C 1.056(2) 0.5408(10) 1.6091(18) 0.077(10) Uiso 0.54(3) 1 d P A 4 H10O H 1.0576 0.5483 1.6506 0.115 Uiso 0.54(3) 1 calc PR A 4 H10P H 1.0845 0.5163 1.6112 0.115 Uiso 0.54(3) 1 calc PR A 4 H10Q H 1.0033 0.5365 1.5830 0.115 Uiso 0.54(3) 1 calc PR A 4 C11 C 0.9944(7) 0.6865(3) 1.4275(5) 0.037(3) Uani 1 1 d . . . H11A H 1.0480 0.6939 1.4377 0.044 Uiso 1 1 calc R . . H11B H 0.9647 0.7112 1.4225 0.044 Uiso 1 1 calc R . . C12 C 0.9685(6) 0.6637(3) 1.3659(6) 0.033(3) Uani 1 1 d . . . O12 O 0.7880(5) 0.7026(2) 2.0711(3) 0.0333(19) Uani 1 1 d . . . C13 C 1.0176(8) 0.6347(4) 1.3555(6) 0.044(3) Uani 1 1 d . . . H13A H 1.0655 0.6309 1.3863 0.053 Uiso 1 1 calc R . . O13 O 0.7615(5) 0.7500 1.8550(4) 0.021(2) Uani 1 2 d S . . C14 C 0.9994(7) 0.6121(4) 1.3034(6) 0.043(3) Uani 1 1 d . . . O14 O 0.7584(5) 0.7500 1.9632(5) 0.026(2) Uiso 1 2 d S . . C15 C 0.9284(7) 0.6195(3) 1.2582(6) 0.039(3) Uani 1 1 d . . . H15A H 0.9153 0.6049 1.2210 0.047 Uiso 1 1 calc R . . O15 O 0.5987(11) 0.7500 1.6109(9) 0.092(5) Uiso 1 2 d S . . C16 C 0.8752(7) 0.6476(3) 1.2650(5) 0.038(3) Uani 1 1 d . . . O16 O 0.9217(10) 0.7500 1.2165(16) 0.165(13) Uani 1 2 d S . . C17 C 0.8973(7) 0.6691(3) 1.3218(6) 0.036(3) Uani 1 1 d . . . O17 O 0.5504(7) 0.7500 0.9890(6) 0.046(3) Uani 1 2 d S . . C18 C 1.0476(9) 0.5787(4) 1.2928(7) 0.053(4) Uani 1 1 d . . . O18 O 0.9649(6) 0.7500 0.6006(5) 0.040(3) Uani 1 2 d S . . C19 C 1.0667(10) 0.5850(5) 1.2332(8) 0.077(6) Uani 1 1 d . . . H19A H 1.0199 0.5879 1.1981 0.115 Uiso 1 1 calc R . . H19B H 1.0949 0.5621 1.2265 0.115 Uiso 1 1 calc R . . H19C H 1.0974 0.6089 1.2373 0.115 Uiso 1 1 calc R . . C20 C 1.1237(11) 0.5759(6) 1.3496(8) 0.103(8) Uani 1 1 d . . . H20A H 1.1121 0.5716 1.3874 0.155 Uiso 1 1 calc R . . H20B H 1.1520 0.6006 1.3531 0.155 Uiso 1 1 calc R . . H20C H 1.1540 0.5538 1.3434 0.155 Uiso 1 1 calc R . . C21 C 1.0099(13) 0.5385(5) 1.2890(13) 0.125(10) Uani 1 1 d . . . H21A H 0.9614 0.5387 1.2553 0.187 Uiso 1 1 calc R . . H21B H 1.0016 0.5330 1.3279 0.187 Uiso 1 1 calc R . . H21C H 1.0424 0.5180 1.2814 0.187 Uiso 1 1 calc R . . C22 C 0.7987(7) 0.6518(3) 1.2173(5) 0.034(3) Uani 1 1 d . . . H22A H 0.7918 0.6793 1.2016 0.041 Uiso 1 1 calc R . . H22B H 0.7945 0.6340 1.1823 0.041 Uiso 1 1 calc R . . C23 C 0.7387(7) 0.6421(3) 1.2434(4) 0.027(3) Uani 1 1 d . . . C24 C 0.7374(7) 0.6043(4) 1.2677(6) 0.039(3) Uani 1 1 d . . . H24A H 0.7726 0.5851 1.2640 0.047 Uiso 1 1 calc R . . C25 C 0.6853(8) 0.5932(4) 1.2978(6) 0.044(3) Uani 1 1 d . . . C26 C 0.6368(7) 0.6219(3) 1.3020(5) 0.033(3) Uani 1 1 d . . . H26A H 0.6017 0.6153 1.3217 0.039 Uiso 1 1 calc R . . C27 C 0.6347(6) 0.6600(3) 1.2796(5) 0.028(3) Uani 1 1 d . . . C28 C 0.6863(6) 0.6712(3) 1.2497(5) 0.028(3) Uani 1 1 d . . . C29 C 0.6926(12) 0.5520(4) 1.3262(9) 0.076(6) Uani 1 1 d . . . C30 C 0.6403(12) 0.5455(5) 1.3609(9) 0.090(6) Uani 1 1 d . . . H30A H 0.5881 0.5474 1.3328 0.134 Uiso 1 1 calc R . . H30B H 0.6493 0.5655 1.3932 0.134 Uiso 1 1 calc R . . H30C H 0.6489 0.5191 1.3796 0.134 Uiso 1 1 calc R . . C31 C 0.7746(16) 0.5482(6) 1.3784(12) 0.142(11) Uani 1 1 d . . . H31A H 0.7802 0.5218 1.3969 0.213 Uiso 1 1 calc R . . H31B H 0.7797 0.5682 1.4103 0.213 Uiso 1 1 calc R . . H31C H 0.8136 0.5523 1.3598 0.213 Uiso 1 1 calc R . . C32 C 0.6938(18) 0.5195(5) 1.2831(11) 0.145(12) Uani 1 1 d . . . H32A H 0.6452 0.5185 1.2495 0.217 Uiso 1 1 calc R . . H32B H 0.7027 0.4942 1.3052 0.217 Uiso 1 1 calc R . . H32C H 0.7342 0.5244 1.2662 0.217 Uiso 1 1 calc R . . C33 C 0.5722(7) 0.6898(4) 1.2826(6) 0.040(3) Uani 1 1 d . . . H33A H 0.5950 0.7163 1.2942 0.048 Uiso 1 1 calc R . . H33B H 0.5331 0.6919 1.2413 0.048 Uiso 1 1 calc R . . C34 C 0.5358(7) 0.6770(3) 1.3284(5) 0.031(3) Uani 1 1 d . . . C35 C 0.4683(7) 0.6561(4) 1.3082(5) 0.041(3) Uani 1 1 d . . . H35A H 0.4424 0.6542 1.2652 0.049 Uiso 1 1 calc R . . C36 C 0.4363(7) 0.6375(4) 1.3485(6) 0.045(3) Uani 1 1 d . B . C37 C 0.4745(7) 0.6431(3) 1.4111(6) 0.041(3) Uani 1 1 d . . . H37A H 0.4525 0.6326 1.4392 0.049 Uiso 1 1 calc R . . C38 C 0.5427(6) 0.6631(3) 1.4352(5) 0.028(2) Uani 1 1 d . . . C39 C 0.5738(6) 0.6802(3) 1.3928(5) 0.024(2) Uani 1 1 d . . . C40 C 0.3632(10) 0.6125(7) 1.3235(8) 0.090(7) Uani 1 1 d . . . C41 C 0.396(3) 0.5662(18) 1.323(3) 0.12(2) Uiso 0.40(2) 1 d P B 5 H41A H 0.4415 0.5625 1.3596 0.183 Uiso 0.40(2) 1 calc PR B 5 H41B H 0.4083 0.5619 1.2860 0.183 Uiso 0.40(2) 1 calc PR B 5 H41C H 0.3575 0.5471 1.3249 0.183 Uiso 0.40(2) 1 calc PR B 5 C42 C 0.292(2) 0.6448(12) 1.2855(19) 0.060(11) Uiso 0.40(2) 1 d P B 5 H42A H 0.2998 0.6699 1.3078 0.090 Uiso 0.40(2) 1 calc PR B 5 H42B H 0.2436 0.6335 1.2830 0.090 Uiso 0.40(2) 1 calc PR B 5 H42C H 0.2933 0.6493 1.2438 0.090 Uiso 0.40(2) 1 calc PR B 5 C43 C 0.321(2) 0.6139(14) 1.371(2) 0.071(13) Uiso 0.40(2) 1 d P B 5 H43A H 0.3456 0.5963 1.4053 0.106 Uiso 0.40(2) 1 calc PR B 5 H43B H 0.2684 0.6052 1.3505 0.106 Uiso 0.40(2) 1 calc PR B 5 H43C H 0.3210 0.6410 1.3857 0.106 Uiso 0.40(2) 1 calc PR B 5 C41A C 0.369(2) 0.5858(13) 1.274(2) 0.120(15) Uiso 0.60(2) 1 d P B 6 H41D H 0.4088 0.5661 1.2925 0.181 Uiso 0.60(2) 1 calc PR B 6 H41E H 0.3825 0.6013 1.2437 0.181 Uiso 0.60(2) 1 calc PR B 6 H41F H 0.3211 0.5724 1.2547 0.181 Uiso 0.60(2) 1 calc PR B 6 C42A C 0.311(3) 0.6242(15) 1.265(2) 0.142(18) Uiso 0.60(2) 1 d P B 6 H42D H 0.3183 0.6074 1.2327 0.213 Uiso 0.60(2) 1 calc PR B 6 H42E H 0.3205 0.6519 1.2569 0.213 Uiso 0.60(2) 1 calc PR B 6 H42F H 0.2596 0.6214 1.2648 0.213 Uiso 0.60(2) 1 calc PR B 6 C43A C 0.3413(19) 0.5911(10) 1.3686(15) 0.082(10) Uiso 0.60(2) 1 d P B 6 H43D H 0.3815 0.5727 1.3906 0.123 Uiso 0.60(2) 1 calc PR B 6 H43E H 0.2949 0.5763 1.3480 0.123 Uiso 0.60(2) 1 calc PR B 6 H43F H 0.3325 0.6098 1.3979 0.123 Uiso 0.60(2) 1 calc PR B 6 C44 C 0.5814(7) 0.6632(3) 1.5047(5) 0.034(3) Uani 1 1 d . . . H44A H 0.5476 0.6503 1.5236 0.041 Uiso 1 1 calc R . . H44B H 0.5879 0.6911 1.5189 0.041 Uiso 1 1 calc R . . C45 C 0.6584(6) 0.6428(3) 1.5287(4) 0.024(2) Uani 1 1 d . . . C46 C 0.6575(7) 0.6014(4) 1.5285(5) 0.035(3) Uani 1 1 d . . . H46A H 0.6105 0.5883 1.5118 0.042 Uiso 1 1 calc R . . C47 C 0.7232(8) 0.5785(3) 1.5520(5) 0.037(3) Uani 1 1 d . . . C48 C 0.7920(7) 0.5988(3) 1.5698(5) 0.035(3) Uani 1 1 d . . . H48A H 0.8375 0.5841 1.5841 0.042 Uiso 1 1 calc R . . C49 C 0.7962(6) 0.6406(3) 1.5674(5) 0.028(3) Uani 1 1 d . . . C50 C 0.7286(7) 0.6631(3) 1.5485(5) 0.031(3) Uani 1 1 d . . . C51 C 0.7219(9) 0.5327(4) 1.5620(6) 0.050(4) Uani 1 1 d . . . C52 C 0.7782(10) 0.5106(4) 1.5386(8) 0.069(5) Uani 1 1 d . . . H52A H 0.7652 0.5150 1.4943 0.104 Uiso 1 1 calc R . . H52B H 0.7760 0.4822 1.5465 0.104 Uiso 1 1 calc R . . H52C H 0.8293 0.5204 1.5602 0.104 Uiso 1 1 calc R . . C53 C 0.6437(10) 0.5152(4) 1.5314(7) 0.074(5) Uani 1 1 d . . . H53A H 0.6281 0.5190 1.4868 0.111 Uiso 1 1 calc R . . H53B H 0.6077 0.5283 1.5472 0.111 Uiso 1 1 calc R . . H53C H 0.6449 0.4868 1.5405 0.111 Uiso 1 1 calc R . . C54 C 0.7418(9) 0.5255(4) 1.6315(6) 0.059(4) Uani 1 1 d . . . H54A H 0.7415 0.4971 1.6393 0.089 Uiso 1 1 calc R . . H54B H 0.7046 0.5387 1.6459 0.089 Uiso 1 1 calc R . . H54C H 0.7920 0.5363 1.6535 0.089 Uiso 1 1 calc R . . C55 C 0.8720(6) 0.6606(3) 1.5909(5) 0.034(3) Uani 1 1 d . . . H55A H 0.8639 0.6895 1.5883 0.040 Uiso 1 1 calc R . . H55B H 0.8960 0.6538 1.6349 0.040 Uiso 1 1 calc R . . C56 C 0.5894(7) 0.6719(3) 1.9169(6) 0.037(3) Uani 1 1 d . . . C57 C 0.5871(7) 0.6508(4) 1.9677(6) 0.041(3) Uani 1 1 d . . . C58 C 0.5339(8) 0.6209(4) 1.9627(6) 0.045(3) Uani 1 1 d . . . H58A H 0.5356 0.6067 1.9986 0.054 Uiso 1 1 calc R . . C59 C 0.4780(7) 0.6112(4) 1.9061(6) 0.041(3) Uani 1 1 d . . . C60 C 0.4795(7) 0.6336(4) 1.8555(7) 0.046(3) Uani 1 1 d . . . H60A H 0.4433 0.6278 1.8164 0.055 Uiso 1 1 calc R . . C61 C 0.5309(7) 0.6639(3) 1.8590(5) 0.032(3) Uani 1 1 d . . . C62 C 0.4187(9) 0.5795(5) 1.9029(8) 0.060(4) Uani 1 1 d . . . C63 C 0.4538(12) 0.5425(5) 1.9389(11) 0.105(7) Uani 1 1 d . . . H63A H 0.4814 0.5496 1.9817 0.158 Uiso 1 1 calc R . . H63B H 0.4887 0.5306 1.9206 0.158 Uiso 1 1 calc R . . H63C H 0.4140 0.5235 1.9374 0.158 Uiso 1 1 calc R . . C64 C 0.3637(10) 0.5947(6) 1.9332(9) 0.087(6) Uani 1 1 d . . . H64A H 0.3917 0.6027 1.9756 0.130 Uiso 1 1 calc R . . H64B H 0.3278 0.5738 1.9333 0.130 Uiso 1 1 calc R . . H64C H 0.3363 0.6176 1.9102 0.130 Uiso 1 1 calc R . . C65 C 0.3769(15) 0.5653(7) 1.8364(10) 0.148(12) Uani 1 1 d . . . H65A H 0.3404 0.5447 1.8368 0.223 Uiso 1 1 calc R . . H65B H 0.4134 0.5544 1.8189 0.223 Uiso 1 1 calc R . . H65C H 0.3504 0.5876 1.8113 0.223 Uiso 1 1 calc R . . C66 C 0.5240(8) 0.6885(4) 1.8005(6) 0.039(3) Uani 1 1 d . . . H66A H 0.4710 0.6970 1.7809 0.047 Uiso 1 1 calc R . . H66B H 0.5555 0.7125 1.8127 0.047 Uiso 1 1 calc R . . C67 C 0.5488(6) 0.6650(3) 1.7531(5) 0.032(3) Uani 1 1 d . . . C68 C 0.4971(7) 0.6378(4) 1.7120(6) 0.042(3) Uani 1 1 d . . . H68A H 0.4477 0.6355 1.7139 0.050 Uiso 1 1 calc R . . C69 C 0.5156(7) 0.6153(4) 1.6709(6) 0.044(3) Uani 1 1 d . . . C70 C 0.5873(7) 0.6206(4) 1.6668(5) 0.040(3) Uani 1 1 d . . . H70A H 0.6005 0.6060 1.6369 0.048 Uiso 1 1 calc R . . C71 C 0.6409(7) 0.6470(3) 1.7054(5) 0.034(3) Uani 1 1 d . . . C72 C 0.6201(6) 0.6693(3) 1.7492(5) 0.025(2) Uani 1 1 d . . . C73 C 0.4617(9) 0.5831(5) 1.6303(7) 0.070(5) Uani 1 1 d . . . C74 C 0.3905(8) 0.5786(5) 1.6452(8) 0.069(5) Uani 1 1 d . . . H74A H 0.3611 0.6031 1.6346 0.104 Uiso 1 1 calc R . . H74B H 0.4033 0.5733 1.6892 0.104 Uiso 1 1 calc R . . H74C H 0.3608 0.5566 1.6215 0.104 Uiso 1 1 calc R . . C75 C 0.4531(11) 0.5875(6) 1.5642(8) 0.106(8) Uani 1 1 d . . . H75A H 0.4263 0.6122 1.5483 0.159 Uiso 1 1 calc R . . H75B H 0.4242 0.5651 1.5409 0.159 Uiso 1 1 calc R . . H75C H 0.5030 0.5881 1.5598 0.159 Uiso 1 1 calc R . . C76 C 0.5059(16) 0.5404(6) 1.6453(14) 0.156(12) Uani 1 1 d . . . H76A H 0.4733 0.5196 1.6207 0.235 Uiso 1 1 calc R . . H76B H 0.5186 0.5342 1.6892 0.235 Uiso 1 1 calc R . . H76C H 0.5522 0.5419 1.6352 0.235 Uiso 1 1 calc R . . C77 C 0.7183(5) 0.6506(3) 1.6993(5) 0.022(2) Uiso 1 1 d . . . H77A H 0.7203 0.6328 1.6659 0.027 Uiso 1 1 calc R . . H77B H 0.7242 0.6780 1.6865 0.027 Uiso 1 1 calc R . . C78 C 0.7839(6) 0.6413(3) 1.7562(5) 0.025(2) Uani 1 1 d . . . C79 C 0.8328(6) 0.6711(3) 1.7920(5) 0.024(2) Uani 1 1 d . . . C80 C 0.8879(6) 0.6603(3) 1.8480(5) 0.029(3) Uani 1 1 d . . . C81 C 0.8939(8) 0.6208(3) 1.8669(5) 0.039(3) Uani 1 1 d . . . H81A H 0.9320 0.6140 1.9046 0.047 Uiso 1 1 calc R . . C82 C 0.8474(7) 0.5908(3) 1.8337(5) 0.039(3) Uani 1 1 d . . . C83 C 0.7913(7) 0.6021(3) 1.7776(5) 0.034(3) Uani 1 1 d . . . H83A H 0.7576 0.5826 1.7538 0.041 Uiso 1 1 calc R . . C84 C 0.8607(11) 0.5477(4) 1.8547(7) 0.074(6) Uani 1 1 d . . . C85 C 0.8128(12) 0.5192(5) 1.8164(9) 0.113(9) Uani 1 1 d . . . H85A H 0.7607 0.5242 1.8142 0.169 Uiso 1 1 calc R . . H85B H 0.8281 0.4927 1.8333 0.169 Uiso 1 1 calc R . . H85C H 0.8161 0.5209 1.7750 0.169 Uiso 1 1 calc R . . C86 C 0.875(2) 0.5437(5) 1.9218(9) 0.175(16) Uani 1 1 d . . . H86A H 0.8293 0.5514 1.9306 0.262 Uiso 1 1 calc R . . H86B H 0.9167 0.5609 1.9447 0.262 Uiso 1 1 calc R . . H86C H 0.8874 0.5161 1.9344 0.262 Uiso 1 1 calc R . . C87 C 0.9430(16) 0.5332(6) 1.8496(18) 0.199(17) Uani 1 1 d . . . H87A H 0.9527 0.5056 1.8630 0.298 Uiso 1 1 calc R . . H87B H 0.9835 0.5500 1.8759 0.298 Uiso 1 1 calc R . . H87C H 0.9413 0.5354 1.8068 0.298 Uiso 1 1 calc R . . C88 C 0.9431(6) 0.6919(3) 1.8867(5) 0.029(3) Uani 1 1 d . . . H88A H 0.9818 0.6975 1.8677 0.035 Uiso 1 1 calc R . . H88B H 0.9152 0.7167 1.8867 0.035 Uiso 1 1 calc R . . C89 C 0.9808(6) 0.6784(3) 1.9515(5) 0.027(2) Uani 1 1 d . . . C90 C 1.0506(6) 0.6586(3) 1.9688(5) 0.030(3) Uani 1 1 d . . . H90A H 1.0763 0.6577 1.9398 0.036 Uiso 1 1 calc R . . C91 C 1.0854(7) 0.6399(3) 2.0274(5) 0.034(3) Uani 1 1 d . B . C92 C 1.0455(6) 0.6429(3) 2.0683(5) 0.029(3) Uani 1 1 d . . . H92A H 1.0664 0.6310 2.1077 0.035 Uiso 1 1 calc R . . C93 C 0.9755(6) 0.6629(3) 2.0543(5) 0.022(2) Uani 1 1 d . . . C94 C 0.9444(6) 0.6813(3) 1.9965(5) 0.026(2) Uani 1 1 d . . . C95 C 1.1596(8) 0.6170(4) 2.0430(6) 0.049(3) Uani 1 1 d . . . C96 C 1.218(3) 0.6387(14) 2.021(2) 0.082(15) Uiso 0.40(2) 1 d P B 7 H96A H 1.2075 0.6333 1.9773 0.122 Uiso 0.40(2) 1 calc PR B 7 H96B H 1.2687 0.6294 2.0448 0.122 Uiso 0.40(2) 1 calc PR B 7 H96C H 1.2145 0.6673 2.0273 0.122 Uiso 0.40(2) 1 calc PR B 7 C97 C 1.223(2) 0.6419(13) 2.0984(18) 0.059(11) Uiso 0.40(2) 1 d P B 7 H97D H 1.2116 0.6392 2.1367 0.089 Uiso 0.40(2) 1 calc PR B 7 H97E H 1.2209 0.6699 2.0870 0.089 Uiso 0.40(2) 1 calc PR B 7 H97F H 1.2732 0.6314 2.1044 0.089 Uiso 0.40(2) 1 calc PR B 7 C98 C 1.150(2) 0.5736(11) 2.061(2) 0.059(11) Uiso 0.40(2) 1 d P B 7 H98A H 1.1112 0.5605 2.0269 0.088 Uiso 0.40(2) 1 calc PR B 7 H98B H 1.1338 0.5735 2.0974 0.088 Uiso 0.40(2) 1 calc PR B 7 H98C H 1.1976 0.5595 2.0707 0.088 Uiso 0.40(2) 1 calc PR B 7 C96A C 1.1945(15) 0.6145(8) 1.9951(12) 0.058(8) Uiso 0.60(2) 1 d P B 8 H96D H 1.1613 0.5997 1.9598 0.087 Uiso 0.60(2) 1 calc PR B 8 H96E H 1.2431 0.6008 2.0115 0.087 Uiso 0.60(2) 1 calc PR B 8 H96F H 1.2025 0.6412 1.9820 0.087 Uiso 0.60(2) 1 calc PR B 8 C97A C 1.2064(18) 0.6179(11) 2.1084(15) 0.083(10) Uiso 0.60(2) 1 d P B 8 H97A H 1.1952 0.5947 2.1292 0.125 Uiso 0.60(2) 1 calc PR B 8 H97B H 1.1953 0.6420 2.1274 0.125 Uiso 0.60(2) 1 calc PR B 8 H97C H 1.2598 0.6177 2.1123 0.125 Uiso 0.60(2) 1 calc PR B 8 C98A C 1.143(3) 0.5757(16) 2.022(3) 0.18(2) Uiso 0.60(2) 1 d P B 8 H98D H 1.0982 0.5750 1.9851 0.264 Uiso 0.60(2) 1 calc PR B 8 H98E H 1.1338 0.5601 2.0547 0.264 Uiso 0.60(2) 1 calc PR B 8 H98F H 1.1860 0.5646 2.0130 0.264 Uiso 0.60(2) 1 calc PR B 8 C99 C 0.9349(7) 0.6626(3) 2.1025(5) 0.035(3) Uani 1 1 d . . . H99A H 0.9684 0.6498 2.1405 0.042 Uiso 1 1 calc R . . H99B H 0.9272 0.6904 2.1129 0.042 Uiso 1 1 calc R . . C100 C 0.8579(7) 0.6412(4) 2.0820(5) 0.034(3) Uani 1 1 d . . . C101 C 0.8597(7) 0.6000(3) 2.0808(5) 0.033(3) Uani 1 1 d . . . H10A H 0.9067 0.5867 2.0900 0.040 Uiso 1 1 calc R . . C102 C 0.7930(8) 0.5778(4) 2.0663(6) 0.040(3) Uani 1 1 d . . . C103 C 0.7259(7) 0.5985(4) 2.0498(6) 0.041(3) Uani 1 1 d . . . H10B H 0.6802 0.5842 2.0408 0.050 Uiso 1 1 calc R . . C104 C 0.7228(7) 0.6409(3) 2.0457(5) 0.033(3) Uani 1 1 d . . . C105 C 0.7898(8) 0.6626(3) 2.0654(5) 0.035(3) Uani 1 1 d . . . C106 C 0.7912(8) 0.5320(4) 2.0747(6) 0.045(3) Uani 1 1 d . . . C107 C 0.8670(10) 0.5133(4) 2.0845(8) 0.070(5) Uani 1 1 d . . . H10C H 0.9047 0.5251 2.1207 0.105 Uiso 1 1 calc R . . H10D H 0.8817 0.5178 2.0482 0.105 Uiso 1 1 calc R . . H10E H 0.8640 0.4848 2.0911 0.105 Uiso 1 1 calc R . . C108 C 0.7672(9) 0.5235(5) 2.1303(8) 0.067(5) Uani 1 1 d . . . H10I H 0.8033 0.5357 2.1671 0.101 Uiso 1 1 calc R . . H10J H 0.7660 0.4949 2.1364 0.101 Uiso 1 1 calc R . . H10K H 0.7169 0.5346 2.1232 0.101 Uiso 1 1 calc R . . C109 C 0.7325(8) 0.5120(4) 2.0169(8) 0.065(4) Uani 1 1 d . . . H10F H 0.7467 0.5172 1.9805 0.097 Uiso 1 1 calc R . . H10G H 0.6822 0.5230 2.0105 0.097 Uiso 1 1 calc R . . H10H H 0.7318 0.4834 2.0236 0.097 Uiso 1 1 calc R . . C110 C 0.6472(7) 0.6602(4) 2.0340(5) 0.037(3) Uani 1 1 d . . . H11C H 0.6544 0.6892 2.0384 0.045 Uiso 1 1 calc R . . H11D H 0.6265 0.6512 2.0659 0.045 Uiso 1 1 calc R . . C111 C 0.4749(13) 0.7099(6) 1.5972(11) 0.106(7) Uani 1 1 d . . . H11K H 0.4310 0.7084 1.6107 0.159 Uiso 1 1 calc R . . H11L H 0.5027 0.6848 1.6064 0.159 Uiso 1 1 calc R . . H11M H 0.4581 0.7148 1.5528 0.159 Uiso 1 1 calc R . . C112 C 1.0537(11) 0.7089(5) 1.2598(10) 0.090(6) Uani 1 1 d . . . H11N H 1.1016 0.7088 1.2941 0.134 Uiso 1 1 calc R . . H11O H 1.0634 0.7125 1.2210 0.134 Uiso 1 1 calc R . . H11P H 1.0275 0.6838 1.2588 0.134 Uiso 1 1 calc R . . C113 C 0.4200(10) 0.7100(5) 0.9518(10) 0.087(6) Uani 1 1 d . . . H11H H 0.3707 0.7087 0.9191 0.130 Uiso 1 1 calc R . . H11I H 0.4130 0.7147 0.9914 0.130 Uiso 1 1 calc R . . H11J H 0.4469 0.6850 0.9535 0.130 Uiso 1 1 calc R . . C114 C 1.0931(8) 0.7100(4) 0.6322(8) 0.069(5) Uani 1 1 d . . . H11E H 1.1417 0.7086 0.6256 0.104 Uiso 1 1 calc R . . H11F H 1.0662 0.6849 0.6198 0.104 Uiso 1 1 calc R . . H11G H 1.1016 0.7148 0.6759 0.104 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 0.0317(2) 0.0185(2) 0.0255(2) 0.00049(16) 0.00695(18) 0.00033(16) O1 0.029(4) 0.029(4) 0.031(5) -0.005(3) 0.006(4) 0.007(3) C1 0.029(6) 0.035(7) 0.022(6) -0.009(5) -0.006(5) 0.006(5) S1 0.151(8) 0.077(5) 0.086(6) 0.000 0.000(6) 0.000 Bi2 0.0281(3) 0.0230(3) 0.0215(3) 0.000 0.0053(2) 0.000 Bi2A 0.0519(4) 0.0238(3) 0.0302(4) 0.000 0.0214(3) 0.000 C2 0.038(7) 0.031(6) 0.028(7) -0.006(5) 0.000(5) -0.007(5) S2 0.121(7) 0.074(5) 0.178(10) 0.000 0.088(7) 0.000 O2 0.060(5) 0.026(4) 0.015(4) 0.001(3) 0.029(4) 0.009(4) Bi3 0.0330(2) 0.0191(2) 0.0233(2) 0.00139(16) 0.00654(18) 0.00016(17) O3 0.042(5) 0.026(4) 0.025(4) 0.009(3) 0.010(4) 0.007(3) C3 0.037(7) 0.033(7) 0.039(7) 0.008(6) -0.002(6) 0.012(6) S3 0.060(3) 0.048(3) 0.068(4) 0.000 0.027(3) 0.000 Bi4A 0.0320(3) 0.0228(3) 0.0154(3) 0.000 -0.0007(2) 0.000 Bi4 0.0391(4) 0.0258(3) 0.0187(3) 0.000 0.0074(3) 0.000 O4 0.026(4) 0.023(4) 0.026(4) -0.010(3) 0.011(3) -0.002(3) C4 0.053(8) 0.032(7) 0.049(8) 0.008(6) 0.015(7) 0.015(6) S4 0.040(3) 0.050(3) 0.034(3) 0.000 -0.002(2) 0.000 O5 0.067(6) 0.018(4) 0.028(4) 0.004(3) 0.027(4) -0.002(4) C5 0.041(7) 0.041(7) 0.035(7) 0.004(6) 0.007(6) 0.024(6) C6 0.021(6) 0.037(7) 0.026(6) 0.001(5) -0.003(5) 0.004(5) O6 0.047(7) 0.010(5) 0.045(7) 0.000 0.032(6) 0.000 C7 0.064(10) 0.085(12) 0.053(10) 0.026(9) 0.022(8) 0.046(9) O8 0.049(5) 0.025(4) 0.058(6) -0.017(4) 0.030(5) -0.014(4) O9 0.015(4) 0.031(4) 0.013(4) -0.004(3) -0.009(3) -0.007(3) O10A 0.017(4) 0.032(4) 0.034(5) -0.003(3) -0.002(3) 0.004(3) O10 0.044(5) 0.019(4) 0.020(4) 0.006(3) 0.010(3) 0.003(3) C11 0.041(7) 0.034(7) 0.031(7) -0.003(5) 0.007(6) 0.008(5) C12 0.027(6) 0.030(6) 0.037(7) 0.002(5) 0.005(5) -0.002(5) O12 0.063(6) 0.021(4) 0.025(4) -0.003(3) 0.026(4) -0.013(4) C13 0.062(9) 0.035(7) 0.039(8) 0.001(6) 0.021(7) 0.016(6) O13 0.030(6) 0.013(5) 0.008(5) 0.000 -0.008(4) 0.000 C14 0.047(8) 0.047(8) 0.041(8) 0.014(6) 0.021(7) 0.017(6) C15 0.063(9) 0.032(7) 0.026(7) -0.001(5) 0.020(6) 0.005(6) C16 0.059(8) 0.026(6) 0.026(7) -0.007(5) 0.012(6) -0.006(6) O16 0.031(10) 0.072(13) 0.36(4) 0.000 0.021(16) 0.000 C17 0.042(7) 0.032(6) 0.032(7) 0.003(5) 0.013(6) -0.006(5) O17 0.049(8) 0.039(7) 0.061(9) 0.000 0.033(7) 0.000 C18 0.065(10) 0.058(9) 0.046(9) 0.002(7) 0.030(8) 0.013(8) O18 0.040(7) 0.042(7) 0.035(7) 0.000 0.010(6) 0.000 C19 0.090(13) 0.085(12) 0.082(12) 0.033(10) 0.063(11) 0.047(10) C20 0.113(16) 0.127(17) 0.068(12) 0.030(12) 0.029(11) 0.093(14) C21 0.15(2) 0.049(11) 0.22(3) 0.031(14) 0.13(2) 0.038(13) C22 0.057(8) 0.031(6) 0.021(6) -0.002(5) 0.022(6) 0.022(6) C23 0.050(7) 0.026(6) 0.006(5) -0.001(4) 0.012(5) -0.009(5) C24 0.051(8) 0.033(7) 0.035(7) -0.005(5) 0.016(6) 0.004(6) C25 0.053(8) 0.035(7) 0.052(8) 0.002(6) 0.030(7) 0.002(6) C26 0.048(7) 0.028(6) 0.023(6) 0.002(5) 0.013(5) -0.002(5) C27 0.035(6) 0.030(6) 0.015(5) -0.014(5) 0.001(5) -0.011(5) C28 0.038(7) 0.024(6) 0.017(6) 0.007(5) 0.004(5) -0.001(5) C29 0.121(16) 0.034(8) 0.105(15) 0.022(9) 0.080(13) 0.025(9) C30 0.142(18) 0.052(10) 0.090(14) 0.014(9) 0.060(14) -0.026(11) C31 0.21(3) 0.085(16) 0.17(3) 0.083(17) 0.12(2) 0.045(18) C32 0.32(4) 0.040(10) 0.13(2) -0.008(12) 0.15(2) -0.024(16) C33 0.043(8) 0.042(7) 0.030(7) -0.006(5) 0.006(6) -0.025(6) C34 0.038(7) 0.035(7) 0.022(6) 0.004(5) 0.012(5) 0.002(5) C35 0.033(7) 0.057(8) 0.018(6) 0.003(6) -0.010(5) -0.018(6) C36 0.027(7) 0.061(9) 0.037(8) 0.005(6) 0.000(6) -0.016(6) C37 0.052(8) 0.033(7) 0.043(8) 0.003(6) 0.021(7) -0.004(6) C38 0.028(6) 0.030(6) 0.020(6) -0.006(5) 0.001(5) -0.005(5) C39 0.020(6) 0.023(5) 0.025(6) 0.003(4) 0.005(5) -0.003(4) C40 0.075(12) 0.148(19) 0.038(9) -0.020(10) 0.008(9) -0.073(13) C44 0.045(7) 0.031(6) 0.034(7) 0.002(5) 0.022(6) 0.002(5) C45 0.039(7) 0.028(6) 0.003(5) -0.003(4) 0.002(4) 0.001(5) C46 0.045(7) 0.047(7) 0.015(6) -0.001(5) 0.012(5) -0.013(6) C47 0.060(9) 0.021(6) 0.029(7) 0.005(5) 0.014(6) 0.011(6) C48 0.046(8) 0.035(7) 0.019(6) -0.002(5) 0.003(5) 0.008(6) C49 0.041(7) 0.025(6) 0.018(6) 0.000(4) 0.008(5) 0.009(5) C50 0.053(8) 0.027(6) 0.017(6) 0.005(5) 0.019(5) 0.008(5) C51 0.084(11) 0.027(7) 0.035(8) 0.000(6) 0.013(7) 0.003(7) C52 0.113(14) 0.031(8) 0.065(11) 0.001(7) 0.031(10) 0.028(8) C53 0.124(15) 0.027(8) 0.057(10) 0.001(7) 0.012(10) -0.013(9) C54 0.090(12) 0.045(8) 0.036(8) 0.006(7) 0.013(8) 0.004(8) C55 0.035(7) 0.035(7) 0.025(6) 0.000(5) 0.002(5) 0.010(5) C56 0.054(8) 0.028(6) 0.036(7) -0.002(5) 0.025(6) -0.007(6) C57 0.051(8) 0.033(7) 0.036(7) 0.006(6) 0.010(6) 0.009(6) C58 0.057(9) 0.040(7) 0.051(9) -0.011(6) 0.036(7) -0.014(6) C59 0.046(8) 0.036(7) 0.044(8) 0.001(6) 0.020(6) -0.009(6) C60 0.040(8) 0.048(8) 0.049(9) -0.010(7) 0.013(6) -0.010(6) C61 0.036(7) 0.038(7) 0.024(6) 0.000(5) 0.015(5) 0.006(5) C62 0.056(9) 0.062(10) 0.065(11) -0.008(8) 0.026(8) -0.020(8) C63 0.105(16) 0.060(12) 0.14(2) 0.026(12) 0.030(14) -0.028(11) C64 0.075(12) 0.088(13) 0.112(16) -0.011(12) 0.051(12) -0.027(11) C65 0.21(3) 0.15(2) 0.118(19) -0.077(16) 0.102(19) -0.16(2) C66 0.048(8) 0.037(7) 0.037(7) -0.008(6) 0.020(6) -0.004(6) C67 0.033(7) 0.032(6) 0.021(6) -0.012(5) -0.003(5) -0.005(5) C68 0.037(7) 0.051(8) 0.044(8) -0.006(6) 0.022(6) -0.015(6) C69 0.041(8) 0.060(9) 0.037(7) -0.021(6) 0.021(6) -0.032(7) C70 0.054(8) 0.040(7) 0.020(6) -0.017(5) 0.004(6) -0.011(6) C71 0.057(8) 0.019(6) 0.028(7) 0.006(5) 0.016(6) -0.002(5) C72 0.040(7) 0.018(5) 0.016(5) 0.006(4) 0.008(5) -0.005(5) C73 0.065(10) 0.099(13) 0.055(10) -0.039(9) 0.033(8) -0.043(10) C74 0.042(8) 0.082(12) 0.075(11) -0.036(9) 0.009(8) -0.041(8) C75 0.108(16) 0.139(18) 0.059(12) -0.014(12) 0.012(11) -0.082(14) C76 0.20(3) 0.089(17) 0.21(3) -0.081(19) 0.11(3) -0.058(19) C78 0.025(6) 0.028(6) 0.012(5) 0.004(4) -0.008(4) 0.012(5) C79 0.030(6) 0.023(6) 0.021(6) 0.001(4) 0.012(5) 0.006(5) C80 0.041(7) 0.028(6) 0.018(6) 0.005(5) 0.011(5) 0.000(5) C81 0.060(8) 0.035(7) 0.019(6) 0.004(5) 0.010(6) 0.011(6) C82 0.055(8) 0.025(6) 0.024(6) 0.001(5) -0.004(6) 0.004(6) C83 0.052(8) 0.025(6) 0.023(6) -0.009(5) 0.009(6) -0.003(5) C84 0.116(15) 0.024(7) 0.052(10) 0.001(7) -0.013(9) -0.015(8) C85 0.149(19) 0.043(10) 0.081(14) 0.028(9) -0.044(13) 0.001(11) C86 0.40(5) 0.042(11) 0.053(13) 0.019(9) 0.04(2) -0.044(18) C87 0.18(3) 0.071(16) 0.36(5) 0.04(2) 0.10(3) 0.073(18) C88 0.033(6) 0.035(6) 0.026(6) -0.002(5) 0.018(5) 0.005(5) C89 0.035(6) 0.028(6) 0.012(5) -0.004(4) 0.000(5) -0.002(5) C90 0.040(7) 0.032(6) 0.018(6) -0.004(5) 0.009(5) 0.003(5) C91 0.036(7) 0.037(7) 0.020(6) 0.005(5) -0.002(5) 0.001(5) C92 0.033(6) 0.031(6) 0.018(6) 0.004(5) 0.001(5) 0.001(5) C93 0.032(6) 0.020(5) 0.015(5) -0.004(4) 0.010(5) -0.005(4) C94 0.022(6) 0.034(6) 0.012(5) 0.012(4) -0.008(4) 0.002(5) C95 0.048(8) 0.053(8) 0.038(8) 0.003(6) 0.006(6) 0.018(7) C99 0.046(7) 0.034(7) 0.025(6) -0.001(5) 0.011(5) -0.002(6) C100 0.041(7) 0.038(7) 0.028(7) 0.001(5) 0.018(6) -0.008(6) C101 0.045(7) 0.036(7) 0.021(6) 0.004(5) 0.013(5) 0.008(6) C102 0.061(9) 0.034(7) 0.033(7) 0.005(5) 0.025(6) 0.006(6) C103 0.038(7) 0.052(8) 0.033(7) -0.003(6) 0.010(6) -0.008(6) C104 0.053(8) 0.029(6) 0.020(6) 0.003(5) 0.016(6) 0.002(6) C105 0.063(9) 0.019(6) 0.029(7) 0.003(5) 0.023(6) -0.005(6) C106 0.048(8) 0.036(7) 0.051(9) -0.008(6) 0.019(7) -0.011(6) C107 0.118(15) 0.029(8) 0.069(11) -0.002(7) 0.039(10) -0.008(8) C108 0.087(12) 0.053(9) 0.073(11) 0.017(8) 0.042(10) 0.000(9) C109 0.062(10) 0.040(8) 0.086(12) -0.015(8) 0.016(9) -0.006(7) C110 0.045(8) 0.041(7) 0.025(6) -0.001(5) 0.010(6) -0.012(6) C111 0.129(19) 0.084(14) 0.13(2) -0.025(13) 0.077(16) -0.021(13) C112 0.109(16) 0.066(11) 0.109(16) -0.008(11) 0.057(13) -0.025(11) C113 0.071(12) 0.062(11) 0.148(19) -0.022(11) 0.064(13) -0.014(9) C114 0.039(8) 0.052(9) 0.081(12) 0.010(8) -0.027(8) 0.006(7) _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 O6 2.127(6) . ? Bi1 O1 2.239(8) . ? Bi1 O7 2.270(6) . ? Bi1 O4 2.481(7) . ? Bi1 O2 2.491(7) . ? Bi1 Bi1 3.5735(8) 4_575 ? Bi1 Bi2 3.6936(7) . ? O1 C1 1.369(13) . ? C1 C2 1.387(16) . ? C1 C6 1.389(16) . ? S1 O15 1.49(2) . ? S1 C111 1.80(2) . ? S1 C111 1.80(2) 4_575 ? Bi2 O7 2.122(10) . ? Bi2 O5 2.246(8) 4_575 ? Bi2 O5 2.246(8) . ? Bi2 O4 2.327(7) . ? Bi2 O4 2.327(7) 4_575 ? Bi2 Bi1 3.6936(7) 4_575 ? Bi2A O6 2.190(10) . ? Bi2A O3 2.241(8) . ? Bi2A O3 2.241(8) 4_575 ? Bi2A O2 2.363(7) 4_575 ? Bi2A O2 2.363(7) . ? C2 C3 1.415(16) . ? C2 C55 1.473(16) . ? S2 O16 1.49(3) . ? S2 C112 1.826(19) 4_575 ? S2 C112 1.826(19) . ? O2 C17 1.382(14) . ? Bi3 O13 2.138(5) . ? Bi3 O8 2.217(8) . ? Bi3 O14 2.239(6) . ? Bi3 O10A 2.429(7) . ? Bi3 O9 2.515(6) . ? Bi3 Bi3 3.5704(8) 4_575 ? Bi3 Bi4 3.6790(7) . ? O3 C28 1.378(12) . ? C3 C4 1.406(18) . ? C3 H3A 0.9400 . ? S3 O17 1.524(14) . ? S3 C113 1.788(16) 4_575 ? S3 C113 1.788(16) . ? Bi4A O13 2.179(9) . ? Bi4A O10 2.249(7) 4_575 ? Bi4A O10 2.249(7) . ? Bi4A O9 2.360(7) 4_575 ? Bi4A O9 2.360(7) . ? Bi4 O14 2.137(10) . ? Bi4 O12 2.250(7) 4_575 ? Bi4 O12 2.250(7) . ? Bi4 O10A 2.335(7) 4_575 ? Bi4 O10A 2.335(7) . ? Bi4 Bi3 3.6790(7) 4_575 ? O4 C39 1.379(12) . ? C4 C5 1.373(18) . ? C4 C7 1.528(17) . ? S4 O18 1.488(12) . ? S4 C114 1.800(13) 4_575 ? S4 C114 1.800(13) . ? O5 C50 1.392(13) . ? C5 C6 1.431(15) . ? C5 H5A 0.9400 . ? C6 C11 1.517(16) . ? O6 Bi1 2.127(6) 4_575 ? O7 Bi1 2.270(6) 4_575 ? C7 C9A 1.34(5) . ? C7 C10 1.39(4) . ? C7 C10A 1.52(4) . ? C7 C9 1.59(4) . ? C7 C8 1.62(4) . ? C7 C8A 1.75(4) . ? O8 C56 1.353(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C8A H8AC 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? O9 C72 1.367(12) . ? O10A C94 1.380(12) . ? O10 C79 1.371(12) . ? C10 H10L 0.9700 . ? C10 H10M 0.9700 . ? C10 H10N 0.9700 . ? C10A H10O 0.9700 . ? C10A H10P 0.9700 . ? C10A H10Q 0.9700 . ? C11 C12 1.529(16) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C17 1.381(16) . ? C12 C13 1.409(16) . ? O12 C105 1.346(12) . ? C13 C14 1.354(18) . ? C13 H13A 0.9400 . ? O13 Bi3 2.138(5) 4_575 ? C14 C15 1.397(17) . ? C14 C18 1.505(17) . ? O14 Bi3 2.239(6) 4_575 ? C15 C16 1.413(17) . ? C15 H15A 0.9400 . ? C16 C17 1.417(16) . ? C16 C22 1.481(17) . ? C18 C21 1.51(2) . ? C18 C19 1.537(19) . ? C18 C20 1.57(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.472(15) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.386(16) . ? C23 C28 1.423(15) . ? C24 C25 1.420(17) . ? C24 H24A 0.9400 . ? C25 C26 1.345(16) . ? C25 C29 1.511(18) . ? C26 C27 1.370(15) . ? C26 H26A 0.9400 . ? C27 C28 1.406(16) . ? C27 C33 1.553(17) . ? C29 C30 1.47(2) . ? C29 C32 1.47(2) . ? C29 C31 1.59(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.491(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.377(16) . ? C34 C39 1.404(15) . ? C35 C36 1.402(17) . ? C35 H35A 0.9400 . ? C36 C37 1.378(17) . ? C36 C40 1.536(18) . ? C37 C38 1.376(16) . ? C37 H37A 0.9400 . ? C38 C39 1.411(15) . ? C38 C44 1.505(15) . ? C40 C42A 1.42(5) . ? C40 C43A 1.42(3) . ? C40 C41A 1.47(4) . ? C40 C43 1.54(4) . ? C40 C41 1.67(6) . ? C40 C42 1.70(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C41A H41D 0.9700 . ? C41A H41E 0.9700 . ? C41A H41F 0.9700 . ? C42A H42D 0.9700 . ? C42A H42E 0.9700 . ? C42A H42F 0.9700 . ? C43A H43D 0.9700 . ? C43A H43E 0.9700 . ? C43A H43F 0.9700 . ? C44 C45 1.515(15) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.385(15) . ? C45 C50 1.407(16) . ? C46 C47 1.391(17) . ? C46 H46A 0.9400 . ? C47 C48 1.387(17) . ? C47 C51 1.549(16) . ? C48 C49 1.402(15) . ? C48 H48A 0.9400 . ? C49 C50 1.406(15) . ? C49 C55 1.491(16) . ? C51 C53 1.51(2) . ? C51 C52 1.52(2) . ? C51 C54 1.524(18) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.372(17) . ? C56 C61 1.426(17) . ? C57 C58 1.386(17) . ? C57 C110 1.582(17) . ? C58 C59 1.397(18) . ? C58 H58A 0.9400 . ? C59 C60 1.388(18) . ? C59 C62 1.518(18) . ? C60 C61 1.377(16) . ? C60 H60A 0.9400 . ? C61 C66 1.539(16) . ? C62 C63 1.51(2) . ? C62 C64 1.51(2) . ? C62 C65 1.53(2) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C66 C67 1.532(16) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C67 C72 1.371(16) . ? C67 C68 1.424(15) . ? C68 C69 1.337(17) . ? C68 H68A 0.9400 . ? C69 C70 1.385(17) . ? C69 C73 1.550(17) . ? C70 C71 1.399(16) . ? C70 H70A 0.9400 . ? C71 C72 1.405(15) . ? C71 C77 1.501(15) . ? C73 C75 1.47(2) . ? C73 C74 1.49(2) . ? C73 C76 1.63(3) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C74 H74C 0.9700 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C75 H75C 0.9700 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C76 H76C 0.9700 . ? C77 C78 1.488(13) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C78 C83 1.388(15) . ? C78 C79 1.411(15) . ? C79 C80 1.390(15) . ? C80 C81 1.385(15) . ? C80 C88 1.530(15) . ? C81 C82 1.375(16) . ? C81 H81A 0.9400 . ? C82 C83 1.406(16) . ? C82 C84 1.514(17) . ? C83 H83A 0.9400 . ? C84 C85 1.39(2) . ? C84 C86 1.47(2) . ? C84 C87 1.65(3) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C85 H85C 0.9700 . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C86 H86C 0.9700 . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C87 H87C 0.9700 . ? C88 C89 1.479(15) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C89 C90 1.393(15) . ? C89 C94 1.414(15) . ? C90 C91 1.423(15) . ? C90 H90A 0.9400 . ? C91 C92 1.384(16) . ? C91 C95 1.515(17) . ? C92 C93 1.405(15) . ? C92 H92A 0.9400 . ? C93 C94 1.393(13) . ? C93 C99 1.534(15) . ? C95 C96A 1.45(3) . ? C95 C97A 1.45(3) . ? C95 C98A 1.46(5) . ? C95 C96 1.53(5) . ? C95 C98 1.54(4) . ? C95 C97 1.64(4) . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C96 H96C 0.9700 . ? C97 H97D 0.9700 . ? C97 H97E 0.9700 . ? C97 H97F 0.9700 . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C98 H98C 0.9700 . ? C96A H96D 0.9700 . ? C96A H96E 0.9700 . ? C96A H96F 0.9700 . ? C97A H97A 0.9700 . ? C97A H97B 0.9700 . ? C97A H97C 0.9700 . ? C98A H98D 0.9700 . ? C98A H98E 0.9700 . ? C98A H98F 0.9700 . ? C99 C100 1.529(16) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C100 C101 1.382(16) . ? C100 C105 1.395(17) . ? C101 C102 1.390(17) . ? C101 H10A 0.9400 . ? C102 C103 1.367(17) . ? C102 C106 1.546(17) . ? C103 C104 1.423(17) . ? C103 H10B 0.9400 . ? C104 C105 1.382(17) . ? C104 C110 1.489(17) . ? C106 C107 1.49(2) . ? C106 C108 1.512(19) . ? C106 C109 1.553(19) . ? C107 H10C 0.9700 . ? C107 H10D 0.9700 . ? C107 H10E 0.9700 . ? C108 H10I 0.9700 . ? C108 H10J 0.9700 . ? C108 H10K 0.9700 . ? C109 H10F 0.9700 . ? C109 H10G 0.9700 . ? C109 H10H 0.9700 . ? C110 H11C 0.9800 . ? C110 H11D 0.9800 . ? C111 H11K 0.9700 . ? C111 H11L 0.9700 . ? C111 H11M 0.9700 . ? C112 H11N 0.9700 . ? C112 H11O 0.9700 . ? C112 H11P 0.9700 . ? C113 H11H 0.9700 . ? C113 H11I 0.9700 . ? C113 H11J 0.9700 . ? C114 H11E 0.9700 . ? C114 H11F 0.9700 . ? C114 H11G 0.9700 . ? 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 O6 Bi1 O1 108.3(3) . . ? O6 Bi1 O7 70.0(3) . . ? O1 Bi1 O7 71.4(3) . . ? O6 Bi1 O4 96.0(3) . . ? O1 Bi1 O4 122.0(3) . . ? O7 Bi1 O4 69.1(3) . . ? O6 Bi1 O2 67.4(3) . . ? O1 Bi1 O2 89.5(3) . . ? O7 Bi1 O2 124.1(3) . . ? O4 Bi1 O2 148.2(3) . . ? O6 Bi1 Bi1 32.8(2) . 4_575 ? O1 Bi1 Bi1 86.10(18) . 4_575 ? O7 Bi1 Bi1 38.1(2) . 4_575 ? O4 Bi1 Bi1 87.96(15) . 4_575 ? O2 Bi1 Bi1 90.50(15) . 4_575 ? O6 Bi1 Bi2 85.3(2) . . ? O1 Bi1 Bi2 91.24(19) . . ? O7 Bi1 Bi2 31.5(2) . . ? O4 Bi1 Bi2 38.29(15) . . ? O2 Bi1 Bi2 151.42(15) . . ? Bi1 Bi1 Bi2 61.071(8) 4_575 . ? C1 O1 Bi1 125.3(6) . . ? O1 C1 C2 117.7(11) . . ? O1 C1 C6 120.4(11) . . ? C2 C1 C6 121.7(11) . . ? O15 S1 C111 103.9(9) . . ? O15 S1 C111 103.9(9) . 4_575 ? C111 S1 C111 96.3(15) . 4_575 ? O7 Bi2 O5 80.3(3) . 4_575 ? O7 Bi2 O5 80.3(3) . . ? O5 Bi2 O5 85.5(4) 4_575 . ? O7 Bi2 O4 74.6(2) . . ? O5 Bi2 O4 154.2(3) 4_575 . ? O5 Bi2 O4 84.8(3) . . ? O7 Bi2 O4 74.6(2) . 4_575 ? O5 Bi2 O4 84.8(3) 4_575 4_575 ? O5 Bi2 O4 154.2(3) . 4_575 ? O4 Bi2 O4 93.8(4) . 4_575 ? O7 Bi2 Bi1 34.03(14) . . ? O5 Bi2 Bi1 112.9(2) 4_575 . ? O5 Bi2 Bi1 74.49(19) . . ? O4 Bi2 Bi1 41.35(17) . . ? O4 Bi2 Bi1 87.45(17) 4_575 . ? O7 Bi2 Bi1 34.03(14) . 4_575 ? O5 Bi2 Bi1 74.49(19) 4_575 4_575 ? O5 Bi2 Bi1 112.9(2) . 4_575 ? O4 Bi2 Bi1 87.45(18) . 4_575 ? O4 Bi2 Bi1 41.35(17) 4_575 4_575 ? Bi1 Bi2 Bi1 57.859(15) . 4_575 ? O6 Bi2A O3 83.2(3) . . ? O6 Bi2A O3 83.2(3) . 4_575 ? O3 Bi2A O3 73.9(4) . 4_575 ? O6 Bi2A O2 69.0(2) . 4_575 ? O3 Bi2A O2 147.2(3) . 4_575 ? O3 Bi2A O2 85.4(3) 4_575 4_575 ? O6 Bi2A O2 69.0(2) . . ? O3 Bi2A O2 85.4(3) . . ? O3 Bi2A O2 147.2(3) 4_575 . ? O2 Bi2A O2 99.9(4) 4_575 . ? C1 C2 C3 116.0(11) . . ? C1 C2 C55 123.9(11) . . ? C3 C2 C55 120.0(11) . . ? O16 S2 C112 108.6(11) . 4_575 ? O16 S2 C112 108.6(11) . . ? C112 S2 C112 97.6(12) 4_575 . ? C17 O2 Bi2A 126.2(6) . . ? C17 O2 Bi1 132.9(6) . . ? Bi2A O2 Bi1 100.1(3) . . ? O13 Bi3 O8 108.2(3) . . ? O13 Bi3 O14 69.4(3) . . ? O8 Bi3 O14 72.5(3) . . ? O13 Bi3 O10A 94.3(3) . . ? O8 Bi3 O10A 124.5(3) . . ? O14 Bi3 O10A 69.3(3) . . ? O13 Bi3 O9 67.8(3) . . ? O8 Bi3 O9 89.7(3) . . ? O14 Bi3 O9 124.8(3) . . ? O10A Bi3 O9 145.5(3) . . ? O13 Bi3 Bi3 33.4(2) . 4_575 ? O8 Bi3 Bi3 85.88(19) . 4_575 ? O14 Bi3 Bi3 37.1(2) . 4_575 ? O10A Bi3 Bi3 87.08(17) . 4_575 ? O9 Bi3 Bi3 91.53(15) . 4_575 ? O13 Bi3 Bi4 85.3(2) . . ? O8 Bi3 Bi4 92.4(2) . . ? O14 Bi3 Bi4 31.9(2) . . ? O10A Bi3 Bi4 38.53(17) . . ? O9 Bi3 Bi4 152.15(15) . . ? Bi3 Bi3 Bi4 60.972(8) 4_575 . ? C28 O3 Bi2A 122.7(6) . . ? C4 C3 C2 124.9(12) . . ? C4 C3 H3A 117.6 . . ? C2 C3 H3A 117.6 . . ? O17 S3 C113 106.1(8) . 4_575 ? O17 S3 C113 106.1(8) . . ? C113 S3 C113 96.9(11) 4_575 . ? O13 Bi4A O10 83.2(3) . 4_575 ? O13 Bi4A O10 83.2(3) . . ? O10 Bi4A O10 73.5(4) 4_575 . ? O13 Bi4A O9 70.1(2) . 4_575 ? O10 Bi4A O9 84.3(2) 4_575 4_575 ? O10 Bi4A O9 147.2(2) . 4_575 ? O13 Bi4A O9 70.1(2) . . ? O10 Bi4A O9 147.2(2) 4_575 . ? O10 Bi4A O9 84.3(2) . . ? O9 Bi4A O9 103.4(4) 4_575 . ? O14 Bi4 O12 80.1(3) . 4_575 ? O14 Bi4 O12 80.1(3) . . ? O12 Bi4 O12 89.7(4) 4_575 . ? O14 Bi4 O10A 72.8(2) . 4_575 ? O12 Bi4 O10A 83.5(3) 4_575 4_575 ? O12 Bi4 O10A 152.9(3) . 4_575 ? O14 Bi4 O10A 72.8(2) . . ? O12 Bi4 O10A 152.9(3) 4_575 . ? O12 Bi4 O10A 83.5(3) . . ? O10A Bi4 O10A 90.7(4) 4_575 . ? O14 Bi4 Bi3 33.64(13) . . ? O12 Bi4 Bi3 112.6(2) 4_575 . ? O12 Bi4 Bi3 72.50(19) . . ? O10A Bi4 Bi3 85.92(18) 4_575 . ? O10A Bi4 Bi3 40.40(17) . . ? O14 Bi4 Bi3 33.64(13) . 4_575 ? O12 Bi4 Bi3 72.50(19) 4_575 4_575 ? O12 Bi4 Bi3 112.6(2) . 4_575 ? O10A Bi4 Bi3 40.40(17) 4_575 4_575 ? O10A Bi4 Bi3 85.92(18) . 4_575 ? Bi3 Bi4 Bi3 58.057(15) . 4_575 ? C39 O4 Bi2 120.2(6) . . ? C39 O4 Bi1 139.4(6) . . ? Bi2 O4 Bi1 100.4(3) . . ? C5 C4 C3 116.4(11) . . ? C5 C4 C7 121.9(12) . . ? C3 C4 C7 121.7(12) . . ? O18 S4 C114 105.3(7) . 4_575 ? O18 S4 C114 105.3(7) . . ? C114 S4 C114 96.2(9) 4_575 . ? C50 O5 Bi2 126.4(7) . . ? C4 C5 C6 121.2(12) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 119.6(11) . . ? C1 C6 C11 122.8(10) . . ? C5 C6 C11 117.6(11) . . ? Bi1 O6 Bi1 114.3(5) 4_575 . ? Bi1 O6 Bi2A 119.1(3) 4_575 . ? Bi1 O6 Bi2A 119.1(3) . . ? Bi2 O7 Bi1 114.4(3) . . ? Bi2 O7 Bi1 114.4(3) . 4_575 ? Bi1 O7 Bi1 103.8(4) . 4_575 ? C9A C7 C10 114(3) . . ? C9A C7 C10A 136(3) . . ? C10 C7 C10A 34(2) . . ? C9A C7 C4 110(3) . . ? C10 C7 C4 120(2) . . ? C10A C7 C4 113.5(18) . . ? C9A C7 C9 51(3) . . ? C10 C7 C9 75(3) . . ? C10A C7 C9 109(2) . . ? C4 C7 C9 106.0(19) . . ? C9A C7 C8 42(3) . . ? C10 C7 C8 126(3) . . ? C10A C7 C8 119(2) . . ? C4 C7 C8 114.7(19) . . ? C9 C7 C8 91(2) . . ? C9A C7 C8A 95(3) . . ? C10 C7 C8A 113(3) . . ? C10A C7 C8A 83(2) . . ? C4 C7 C8A 101.1(16) . . ? C9 C7 C8A 142(2) . . ? C8 C7 C8A 53.5(19) . . ? C56 O8 Bi3 126.2(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C8A H8AA 109.5 . . ? C7 C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7 C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7 C9A H9AA 109.5 . . ? C7 C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C7 C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C72 O9 Bi4A 124.9(6) . . ? C72 O9 Bi3 135.3(6) . . ? Bi4A O9 Bi3 99.6(2) . . ? C94 O10A Bi4 118.1(6) . . ? C94 O10A Bi3 140.5(6) . . ? Bi4 O10A Bi3 101.1(3) . . ? C79 O10 Bi4A 125.0(6) . . ? C7 C10 H10L 109.5 . . ? C7 C10 H10M 109.5 . . ? H10L C10 H10M 109.5 . . ? C7 C10 H10N 109.5 . . ? H10L C10 H10N 109.5 . . ? H10M C10 H10N 109.5 . . ? C7 C10A H10O 109.5 . . ? C7 C10A H10P 109.5 . . ? H10O C10A H10P 109.5 . . ? C7 C10A H10Q 109.5 . . ? H10O C10A H10Q 109.5 . . ? H10P C10A H10Q 109.5 . . ? C6 C11 C12 113.2(10) . . ? C6 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C6 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 119.1(11) . . ? C17 C12 C11 122.2(11) . . ? C13 C12 C11 118.6(11) . . ? C105 O12 Bi4 129.8(7) . . ? C14 C13 C12 123.3(13) . . ? C14 C13 H13A 118.4 . . ? C12 C13 H13A 118.4 . . ? Bi3 O13 Bi3 113.2(4) 4_575 . ? Bi3 O13 Bi4A 119.2(2) 4_575 . ? Bi3 O13 Bi4A 119.2(2) . . ? C13 C14 C15 116.3(12) . . ? C13 C14 C18 124.8(12) . . ? C15 C14 C18 118.8(12) . . ? Bi4 O14 Bi3 114.4(3) . . ? Bi4 O14 Bi3 114.4(3) . 4_575 ? Bi3 O14 Bi3 105.8(4) . 4_575 ? C14 C15 C16 124.2(11) . . ? C14 C15 H15A 117.9 . . ? C16 C15 H15A 117.9 . . ? C15 C16 C17 116.1(11) . . ? C15 C16 C22 121.4(10) . . ? C17 C16 C22 122.3(11) . . ? C12 C17 O2 121.4(11) . . ? C12 C17 C16 120.8(12) . . ? O2 C17 C16 117.8(11) . . ? C14 C18 C21 112.3(13) . . ? C14 C18 C19 111.9(12) . . ? C21 C18 C19 108.3(15) . . ? C14 C18 C20 109.5(12) . . ? C21 C18 C20 105.6(15) . . ? C19 C18 C20 108.9(13) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C16 110.9(10) . . ? C23 C22 H22A 109.5 . . ? C16 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 118.6(10) . . ? C24 C23 C22 118.9(11) . . ? C28 C23 C22 122.2(9) . . ? C23 C24 C25 122.7(11) . . ? C23 C24 H24A 118.6 . . ? C25 C24 H24A 118.6 . . ? C26 C25 C24 115.8(11) . . ? C26 C25 C29 126.0(12) . . ? C24 C25 C29 118.1(12) . . ? C25 C26 C27 125.1(12) . . ? C25 C26 H26A 117.4 . . ? C27 C26 H26A 117.4 . . ? C26 C27 C28 119.4(11) . . ? C26 C27 C33 120.6(10) . . ? C28 C27 C33 119.9(10) . . ? O3 C28 C27 120.7(10) . . ? O3 C28 C23 120.9(10) . . ? C27 C28 C23 118.4(9) . . ? C30 C29 C32 114.6(17) . . ? C30 C29 C25 112.8(13) . . ? C32 C29 C25 114.0(15) . . ? C30 C29 C31 103.2(16) . . ? C32 C29 C31 102.4(18) . . ? C25 C29 C31 108.5(15) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C27 112.0(10) . . ? C34 C33 H33A 109.2 . . ? C27 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C27 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C39 117.9(10) . . ? C35 C34 C33 119.6(10) . . ? C39 C34 C33 121.7(10) . . ? C34 C35 C36 123.5(11) . . ? C34 C35 H35A 118.3 . . ? C36 C35 H35A 118.3 . . ? C37 C36 C35 115.8(11) . . ? C37 C36 C40 122.8(12) . . ? C35 C36 C40 121.4(12) . . ? C38 C37 C36 124.5(12) . . ? C38 C37 H37A 117.8 . . ? C36 C37 H37A 117.8 . . ? C37 C38 C39 117.4(10) . . ? C37 C38 C44 118.2(10) . . ? C39 C38 C44 124.2(10) . . ? O4 C39 C34 119.6(9) . . ? O4 C39 C38 119.6(9) . . ? C34 C39 C38 120.8(10) . . ? C42A C40 C43A 124(3) . . ? C42A C40 C41A 70(3) . . ? C43A C40 C41A 111(3) . . ? C42A C40 C36 116(2) . . ? C43A C40 C36 116.2(18) . . ? C41A C40 C36 109(2) . . ? C42A C40 C43 108(3) . . ? C43A C40 C43 33.5(18) . . ? C41A C40 C43 138(3) . . ? C36 C40 C43 109(2) . . ? C42A C40 C41 113(4) . . ? C43A C40 C41 74(3) . . ? C41A C40 C41 46(2) . . ? C36 C40 C41 103(3) . . ? C43 C40 C41 108(3) . . ? C42A C40 C42 35(2) . . ? C43A C40 C42 109(2) . . ? C41A C40 C42 104(3) . . ? C36 C40 C42 106.4(19) . . ? C43 C40 C42 81(3) . . ? C41 C40 C42 144(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.3 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.6 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C41A H41D 109.5 . . ? C40 C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40 C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40 C42A H42D 109.5 . . ? C40 C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40 C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C40 C43A H43D 109.4 . . ? C40 C43A H43E 109.4 . . ? H43D C43A H43E 109.5 . . ? C40 C43A H43F 109.6 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C38 C44 C45 115.9(9) . . ? C38 C44 H44A 108.3 . . ? C45 C44 H44A 108.3 . . ? C38 C44 H44B 108.3 . . ? C45 C44 H44B 108.3 . . ? H44A C44 H44B 107.4 . . ? C46 C45 C50 119.5(10) . . ? C46 C45 C44 116.2(10) . . ? C50 C45 C44 124.3(10) . . ? C45 C46 C47 122.9(11) . . ? C45 C46 H46A 118.6 . . ? C47 C46 H46A 118.6 . . ? C48 C47 C46 116.8(10) . . ? C48 C47 C51 120.0(11) . . ? C46 C47 C51 123.1(12) . . ? C47 C48 C49 122.4(11) . . ? C47 C48 H48A 118.8 . . ? C49 C48 H48A 118.8 . . ? C48 C49 C50 119.3(11) . . ? C48 C49 C55 119.4(10) . . ? C50 C49 C55 121.0(10) . . ? O5 C50 C49 117.6(10) . . ? O5 C50 C45 123.4(10) . . ? C49 C50 C45 118.8(10) . . ? C53 C51 C52 108.8(12) . . ? C53 C51 C54 106.1(13) . . ? C52 C51 C54 109.6(12) . . ? C53 C51 C47 112.2(12) . . ? C52 C51 C47 112.5(12) . . ? C54 C51 C47 107.5(10) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C2 C55 C49 116.1(10) . . ? C2 C55 H55A 108.3 . . ? C49 C55 H55A 108.3 . . ? C2 C55 H55B 108.3 . . ? C49 C55 H55B 108.3 . . ? H55A C55 H55B 107.4 . . ? O8 C56 C57 121.3(12) . . ? O8 C56 C61 121.4(11) . . ? C57 C56 C61 117.0(11) . . ? C56 C57 C58 121.9(12) . . ? C56 C57 C110 119.7(11) . . ? C58 C57 C110 118.5(11) . . ? C57 C58 C59 122.2(12) . . ? C57 C58 H58A 118.9 . . ? C59 C58 H58A 118.9 . . ? C60 C59 C58 115.3(12) . . ? C60 C59 C62 124.0(13) . . ? C58 C59 C62 120.7(12) . . ? C61 C60 C59 123.9(12) . . ? C61 C60 H60A 118.0 . . ? C59 C60 H60A 118.0 . . ? C60 C61 C56 119.5(11) . . ? C60 C61 C66 119.3(11) . . ? C56 C61 C66 121.2(11) . . ? C63 C62 C64 105.4(16) . . ? C63 C62 C59 111.9(13) . . ? C64 C62 C59 109.8(13) . . ? C63 C62 C65 105.6(16) . . ? C64 C62 C65 111.4(16) . . ? C59 C62 C65 112.5(13) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C61 112.6(10) . . ? C67 C66 H66A 109.1 . . ? C61 C66 H66A 109.1 . . ? C67 C66 H66B 109.1 . . ? C61 C66 H66B 109.1 . . ? H66A C66 H66B 107.8 . . ? C72 C67 C68 118.7(10) . . ? C72 C67 C66 121.7(10) . . ? C68 C67 C66 119.6(11) . . ? C69 C68 C67 123.0(11) . . ? C69 C68 H68A 118.5 . . ? C67 C68 H68A 118.5 . . ? C68 C69 C70 117.4(11) . . ? C68 C69 C73 122.9(11) . . ? C70 C69 C73 119.7(11) . . ? C69 C70 C71 122.7(11) . . ? C69 C70 H70A 118.6 . . ? C71 C70 H70A 118.6 . . ? C70 C71 C72 118.2(11) . . ? C70 C71 C77 119.9(10) . . ? C72 C71 C77 121.9(10) . . ? O9 C72 C67 121.6(9) . . ? O9 C72 C71 118.4(10) . . ? C67 C72 C71 120.0(10) . . ? C75 C73 C74 116.8(15) . . ? C75 C73 C69 111.7(13) . . ? C74 C73 C69 112.4(12) . . ? C75 C73 C76 100.2(17) . . ? C74 C73 C76 107.0(16) . . ? C69 C73 C76 107.7(15) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C71 115.7(9) . . ? C78 C77 H77A 108.4 . . ? C71 C77 H77A 108.4 . . ? C78 C77 H77B 108.4 . . ? C71 C77 H77B 108.4 . . ? H77A C77 H77B 107.4 . . ? C83 C78 C79 119.7(9) . . ? C83 C78 C77 117.4(10) . . ? C79 C78 C77 122.5(9) . . ? O10 C79 C80 120.1(10) . . ? O10 C79 C78 121.1(9) . . ? C80 C79 C78 118.7(9) . . ? C81 C80 C79 119.5(11) . . ? C81 C80 C88 120.7(10) . . ? C79 C80 C88 119.8(9) . . ? C82 C81 C80 123.8(11) . . ? C82 C81 H81A 118.1 . . ? C80 C81 H81A 118.1 . . ? C81 C82 C83 116.2(10) . . ? C81 C82 C84 121.1(11) . . ? C83 C82 C84 122.6(11) . . ? C78 C83 C82 122.1(10) . . ? C78 C83 H83A 119.0 . . ? C82 C83 H83A 119.0 . . ? C85 C84 C86 116.2(17) . . ? C85 C84 C82 116.8(13) . . ? C86 C84 C82 111.6(13) . . ? C85 C84 C87 99.8(18) . . ? C86 C84 C87 102(2) . . ? C82 C84 C87 108.3(16) . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C89 C88 C80 111.6(9) . . ? C89 C88 H88A 109.3 . . ? C80 C88 H88A 109.3 . . ? C89 C88 H88B 109.3 . . ? C80 C88 H88B 109.3 . . ? H88A C88 H88B 108.0 . . ? C90 C89 C94 117.4(9) . . ? C90 C89 C88 120.7(10) . . ? C94 C89 C88 121.6(10) . . ? C89 C90 C91 124.1(11) . . ? C89 C90 H90A 118.0 . . ? C91 C90 H90A 118.0 . . ? C92 C91 C90 115.2(10) . . ? C92 C91 C95 122.5(10) . . ? C90 C91 C95 122.2(11) . . ? C91 C92 C93 123.6(10) . . ? C91 C92 H92A 118.2 . . ? C93 C92 H92A 118.2 . . ? C94 C93 C92 118.8(9) . . ? C94 C93 C99 122.5(10) . . ? C92 C93 C99 118.7(9) . . ? O10A C94 C93 121.4(10) . . ? O10A C94 C89 117.7(9) . . ? C93 C94 C89 120.8(10) . . ? C96A C95 C97A 121(2) . . ? C96A C95 C98A 78(3) . . ? C97A C95 C98A 110(3) . . ? C96A C95 C91 117.4(14) . . ? C97A C95 C91 114.4(16) . . ? C98A C95 C91 109(3) . . ? C96A C95 C96 39.7(19) . . ? C97A C95 C96 95(3) . . ? C98A C95 C96 116(3) . . ? C91 C95 C96 112(2) . . ? C96A C95 C98 106(2) . . ? C97A C95 C98 80(2) . . ? C98A C95 C98 33(3) . . ? C91 C95 C98 110.8(19) . . ? C96 C95 C98 135(3) . . ? C96A C95 C97 103(2) . . ? C97A C95 C97 33.8(16) . . ? C98A C95 C97 139(3) . . ? C91 C95 C97 106.5(16) . . ? C96 C95 C97 67(3) . . ? C98 C95 C97 113(2) . . ? C95 C96 H96A 109.4 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C95 C97 H97D 109.5 . . ? C95 C97 H97E 109.5 . . ? H97D C97 H97E 109.5 . . ? C95 C97 H97F 109.5 . . ? H97D C97 H97F 109.5 . . ? H97E C97 H97F 109.5 . . ? C95 C98 H98A 109.5 . . ? C95 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C95 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C95 C96A H96D 109.5 . . ? C95 C96A H96E 109.5 . . ? H96D C96A H96E 109.5 . . ? C95 C96A H96F 109.5 . . ? H96D C96A H96F 109.5 . . ? H96E C96A H96F 109.5 . . ? C95 C97A H97A 109.5 . . ? C95 C97A H97B 109.5 . . ? H97A C97A H97B 109.5 . . ? C95 C97A H97C 109.5 . . ? H97A C97A H97C 109.5 . . ? H97B C97A H97C 109.5 . . ? C95 C98A H98D 109.5 . . ? C95 C98A H98E 109.5 . . ? H98D C98A H98E 109.5 . . ? C95 C98A H98F 109.5 . . ? H98D C98A H98F 109.5 . . ? H98E C98A H98F 109.5 . . ? C100 C99 C93 115.1(9) . . ? C100 C99 H99A 108.5 . . ? C93 C99 H99A 108.5 . . ? C100 C99 H99B 108.5 . . ? C93 C99 H99B 108.5 . . ? H99A C99 H99B 107.5 . . ? C101 C100 C105 122.1(11) . . ? C101 C100 C99 116.6(11) . . ? C105 C100 C99 121.2(11) . . ? C100 C101 C102 120.9(11) . . ? C100 C101 H10A 119.5 . . ? C102 C101 H10A 119.5 . . ? C103 C102 C101 117.1(11) . . ? C103 C102 C106 118.7(12) . . ? C101 C102 C106 123.8(12) . . ? C102 C103 C104 122.6(12) . . ? C102 C103 H10B 118.7 . . ? C104 C103 H10B 118.7 . . ? C105 C104 C103 119.2(11) . . ? C105 C104 C110 122.0(10) . . ? C103 C104 C110 117.3(11) . . ? O12 C105 C104 120.2(11) . . ? O12 C105 C100 122.2(11) . . ? C104 C105 C100 117.5(10) . . ? C107 C106 C108 109.3(13) . . ? C107 C106 C102 112.0(11) . . ? C108 C106 C102 108.4(11) . . ? C107 C106 C109 107.9(11) . . ? C108 C106 C109 108.1(12) . . ? C102 C106 C109 111.1(12) . . ? C106 C107 H10C 109.5 . . ? C106 C107 H10D 109.5 . . ? H10C C107 H10D 109.5 . . ? C106 C107 H10E 109.5 . . ? H10C C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C106 C108 H10I 109.5 . . ? C106 C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C106 C108 H10K 109.5 . . ? H10I C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C106 C109 H10F 109.5 . . ? C106 C109 H10G 109.5 . . ? H10F C109 H10G 109.5 . . ? C106 C109 H10H 109.5 . . ? H10F C109 H10H 109.5 . . ? H10G C109 H10H 109.5 . . ? C104 C110 C57 114.1(10) . . ? C104 C110 H11C 108.7 . . ? C57 C110 H11C 108.7 . . ? C104 C110 H11D 108.7 . . ? C57 C110 H11D 108.7 . . ? H11C C110 H11D 107.6 . . ? S1 C111 H11K 109.5 . . ? S1 C111 H11L 109.5 . . ? H11K C111 H11L 109.5 . . ? S1 C111 H11M 109.5 . . ? H11K C111 H11M 109.5 . . ? H11L C111 H11M 109.5 . . ? S2 C112 H11N 109.5 . . ? S2 C112 H11O 109.5 . . ? H11N C112 H11O 109.5 . . ? S2 C112 H11P 109.5 . . ? H11N C112 H11P 109.5 . . ? H11O C112 H11P 109.5 . . ? S3 C113 H11H 109.5 . . ? S3 C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? S3 C113 H11J 109.5 . . ? H11H C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? S4 C114 H11E 109.5 . . ? S4 C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? S4 C114 H11G 109.5 . . ? H11E C114 H11G 109.5 . . ? H11F C114 H11G 109.5 . . ? 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 O6 Bi1 O1 C1 -140.2(9) . . . . ? O7 Bi1 O1 C1 159.3(9) . . . . ? O4 Bi1 O1 C1 110.1(8) . . . . ? O2 Bi1 O1 C1 -74.2(9) . . . . ? Bi1 Bi1 O1 C1 -164.7(9) 4_575 . . . ? Bi2 Bi1 O1 C1 134.4(9) . . . . ? Bi1 O1 C1 C2 -99.5(10) . . . . ? Bi1 O1 C1 C6 85.7(12) . . . . ? O6 Bi1 Bi2 O7 -58.5(5) . . . . ? O1 Bi1 Bi2 O7 49.8(5) . . . . ? O4 Bi1 Bi2 O7 -164.4(5) . . . . ? O2 Bi1 Bi2 O7 -41.5(6) . . . . ? Bi1 Bi1 Bi2 O7 -35.1(4) 4_575 . . . ? O6 Bi1 Bi2 O5 -76.0(4) . . . 4_575 ? O1 Bi1 Bi2 O5 32.3(3) . . . 4_575 ? O7 Bi1 Bi2 O5 -17.5(5) . . . 4_575 ? O4 Bi1 Bi2 O5 178.1(3) . . . 4_575 ? O2 Bi1 Bi2 O5 -59.0(4) . . . 4_575 ? Bi1 Bi1 Bi2 O5 -52.5(2) 4_575 . . 4_575 ? O6 Bi1 Bi2 O5 -154.1(4) . . . . ? O1 Bi1 Bi2 O5 -45.8(3) . . . . ? O7 Bi1 Bi2 O5 -95.6(5) . . . . ? O4 Bi1 Bi2 O5 100.0(3) . . . . ? O2 Bi1 Bi2 O5 -137.1(5) . . . . ? Bi1 Bi1 Bi2 O5 -130.7(2) 4_575 . . . ? O6 Bi1 Bi2 O4 105.9(4) . . . . ? O1 Bi1 Bi2 O4 -145.8(3) . . . . ? O7 Bi1 Bi2 O4 164.4(5) . . . . ? O2 Bi1 Bi2 O4 122.9(5) . . . . ? Bi1 Bi1 Bi2 O4 129.4(3) 4_575 . . . ? O6 Bi1 Bi2 O4 7.3(3) . . . 4_575 ? O1 Bi1 Bi2 O4 115.6(3) . . . 4_575 ? O7 Bi1 Bi2 O4 65.8(4) . . . 4_575 ? O4 Bi1 Bi2 O4 -98.6(4) . . . 4_575 ? O2 Bi1 Bi2 O4 24.3(4) . . . 4_575 ? Bi1 Bi1 Bi2 O4 30.75(18) 4_575 . . 4_575 ? O6 Bi1 Bi2 Bi1 -23.4(3) . . . 4_575 ? O1 Bi1 Bi2 Bi1 84.85(19) . . . 4_575 ? O7 Bi1 Bi2 Bi1 35.1(4) . . . 4_575 ? O4 Bi1 Bi2 Bi1 -129.4(3) . . . 4_575 ? O2 Bi1 Bi2 Bi1 -6.4(4) . . . 4_575 ? O1 C1 C2 C3 -178.6(9) . . . . ? C6 C1 C2 C3 -3.8(16) . . . . ? O1 C1 C2 C55 -1.4(17) . . . . ? C6 C1 C2 C55 173.4(11) . . . . ? O6 Bi2A O2 C17 -175.4(9) . . . . ? O3 Bi2A O2 C17 100.1(8) . . . . ? O3 Bi2A O2 C17 150.6(8) 4_575 . . . ? O2 Bi2A O2 C17 -112.6(8) 4_575 . . . ? O6 Bi2A O2 Bi1 14.2(3) . . . . ? O3 Bi2A O2 Bi1 -70.3(3) . . . . ? O3 Bi2A O2 Bi1 -19.8(6) 4_575 . . . ? O2 Bi2A O2 Bi1 77.0(4) 4_575 . . . ? O6 Bi1 O2 C17 175.8(10) . . . . ? O1 Bi1 O2 C17 65.6(9) . . . . ? O7 Bi1 O2 C17 132.6(9) . . . . ? O4 Bi1 O2 C17 -121.3(9) . . . . ? Bi1 Bi1 O2 C17 151.7(9) 4_575 . . . ? Bi2 Bi1 O2 C17 157.4(7) . . . . ? O6 Bi1 O2 Bi2A -14.8(3) . . . . ? O1 Bi1 O2 Bi2A -124.9(3) . . . . ? O7 Bi1 O2 Bi2A -58.0(4) . . . . ? O4 Bi1 O2 Bi2A 48.1(5) . . . . ? Bi1 Bi1 O2 Bi2A -38.9(2) 4_575 . . . ? Bi2 Bi1 O2 Bi2A -33.2(6) . . . . ? O6 Bi2A O3 C28 -70.2(8) . . . . ? O3 Bi2A O3 C28 -155.1(7) 4_575 . . . ? O2 Bi2A O3 C28 -102.0(8) 4_575 . . . ? O2 Bi2A O3 C28 -0.9(8) . . . . ? C1 C2 C3 C4 -0.1(18) . . . . ? C55 C2 C3 C4 -177.4(12) . . . . ? O13 Bi3 Bi4 O14 57.7(5) . . . . ? O8 Bi3 Bi4 O14 -50.4(5) . . . . ? O10A Bi3 Bi4 O14 160.6(5) . . . . ? O9 Bi3 Bi4 O14 43.5(6) . . . . ? Bi3 Bi3 Bi4 O14 33.5(4) 4_575 . . . ? O13 Bi3 Bi4 O12 74.2(3) . . . 4_575 ? O8 Bi3 Bi4 O12 -33.9(3) . . . 4_575 ? O14 Bi3 Bi4 O12 16.5(5) . . . 4_575 ? O10A Bi3 Bi4 O12 177.1(4) . . . 4_575 ? O9 Bi3 Bi4 O12 60.0(4) . . . 4_575 ? Bi3 Bi3 Bi4 O12 50.0(2) 4_575 . . 4_575 ? O13 Bi3 Bi4 O12 156.3(3) . . . . ? O8 Bi3 Bi4 O12 48.2(3) . . . . ? O14 Bi3 Bi4 O12 98.6(5) . . . . ? O10A Bi3 Bi4 O12 -100.8(4) . . . . ? O9 Bi3 Bi4 O12 142.1(4) . . . . ? Bi3 Bi3 Bi4 O12 132.1(2) 4_575 . . . ? O13 Bi3 Bi4 O10A -7.0(3) . . . 4_575 ? O8 Bi3 Bi4 O10A -115.1(3) . . . 4_575 ? O14 Bi3 Bi4 O10A -64.7(5) . . . 4_575 ? O10A Bi3 Bi4 O10A 95.9(4) . . . 4_575 ? O9 Bi3 Bi4 O10A -21.2(4) . . . 4_575 ? Bi3 Bi3 Bi4 O10A -31.20(18) 4_575 . . 4_575 ? O13 Bi3 Bi4 O10A -102.9(4) . . . . ? O8 Bi3 Bi4 O10A 149.0(4) . . . . ? O14 Bi3 Bi4 O10A -160.6(5) . . . . ? O9 Bi3 Bi4 O10A -117.1(5) . . . . ? Bi3 Bi3 Bi4 O10A -127.1(3) 4_575 . . . ? O13 Bi3 Bi4 Bi3 24.2(3) . . . 4_575 ? O8 Bi3 Bi4 Bi3 -83.9(2) . . . 4_575 ? O14 Bi3 Bi4 Bi3 -33.5(4) . . . 4_575 ? O10A Bi3 Bi4 Bi3 127.1(3) . . . 4_575 ? O9 Bi3 Bi4 Bi3 10.0(3) . . . 4_575 ? O7 Bi2 O4 C39 -172.1(7) . . . . ? O5 Bi2 O4 C39 174.9(7) 4_575 . . . ? O5 Bi2 O4 C39 106.5(7) . . . . ? O4 Bi2 O4 C39 -99.3(7) 4_575 . . . ? Bi1 Bi2 O4 C39 178.9(8) . . . . ? Bi1 Bi2 O4 C39 -140.2(7) 4_575 . . . ? O7 Bi2 O4 Bi1 9.0(3) . . . . ? O5 Bi2 O4 Bi1 -4.0(7) 4_575 . . . ? O5 Bi2 O4 Bi1 -72.4(3) . . . . ? O4 Bi2 O4 Bi1 81.8(3) 4_575 . . . ? Bi1 Bi2 O4 Bi1 40.9(2) 4_575 . . . ? O6 Bi1 O4 C39 107.0(10) . . . . ? O1 Bi1 O4 C39 -137.0(9) . . . . ? O7 Bi1 O4 C39 172.8(10) . . . . ? O2 Bi1 O4 C39 51.2(11) . . . . ? Bi1 Bi1 O4 C39 138.9(9) 4_575 . . . ? Bi2 Bi1 O4 C39 -178.5(11) . . . . ? O6 Bi1 O4 Bi2 -74.5(3) . . . . ? O1 Bi1 O4 Bi2 41.5(4) . . . . ? O7 Bi1 O4 Bi2 -8.6(3) . . . . ? O2 Bi1 O4 Bi2 -130.3(4) . . . . ? Bi1 Bi1 O4 Bi2 -42.6(2) 4_575 . . . ? C2 C3 C4 C5 4(2) . . . . ? C2 C3 C4 C7 -177.2(13) . . . . ? O7 Bi2 O5 C50 -98.8(8) . . . . ? O5 Bi2 O5 C50 -179.7(7) 4_575 . . . ? O4 Bi2 O5 C50 -23.6(8) . . . . ? O4 Bi2 O5 C50 -111.5(9) 4_575 . . . ? Bi1 Bi2 O5 C50 -64.4(8) . . . . ? Bi1 Bi2 O5 C50 -108.6(8) 4_575 . . . ? C3 C4 C5 C6 -4.4(19) . . . . ? C7 C4 C5 C6 176.9(13) . . . . ? O1 C1 C6 C5 178.1(10) . . . . ? C2 C1 C6 C5 3.5(17) . . . . ? O1 C1 C6 C11 -0.4(16) . . . . ? C2 C1 C6 C11 -175.0(11) . . . . ? C4 C5 C6 C1 0.8(18) . . . . ? C4 C5 C6 C11 179.4(12) . . . . ? O1 Bi1 O6 Bi1 -49.8(5) . . . 4_575 ? O7 Bi1 O6 Bi1 11.6(4) . . . 4_575 ? O4 Bi1 O6 Bi1 76.7(5) . . . 4_575 ? O2 Bi1 O6 Bi1 -131.4(6) . . . 4_575 ? Bi2 Bi1 O6 Bi1 39.9(4) . . . 4_575 ? O1 Bi1 O6 Bi2A 99.7(5) . . . . ? O7 Bi1 O6 Bi2A 161.1(7) . . . . ? O4 Bi1 O6 Bi2A -133.8(5) . . . . ? O2 Bi1 O6 Bi2A 18.1(4) . . . . ? Bi1 Bi1 O6 Bi2A 149.5(9) 4_575 . . . ? Bi2 Bi1 O6 Bi2A -170.6(5) . . . . ? O3 Bi2A O6 Bi1 -143.2(5) . . . 4_575 ? O3 Bi2A O6 Bi1 -68.7(5) 4_575 . . 4_575 ? O2 Bi2A O6 Bi1 18.9(5) 4_575 . . 4_575 ? O2 Bi2A O6 Bi1 129.1(6) . . . 4_575 ? O3 Bi2A O6 Bi1 68.7(5) . . . . ? O3 Bi2A O6 Bi1 143.2(5) 4_575 . . . ? O2 Bi2A O6 Bi1 -129.1(6) 4_575 . . . ? O2 Bi2A O6 Bi1 -18.9(5) . . . . ? O5 Bi2 O7 Bi1 163.7(4) 4_575 . . . ? O5 Bi2 O7 Bi1 76.7(4) . . . . ? O4 Bi2 O7 Bi1 -10.6(3) . . . . ? O4 Bi2 O7 Bi1 -109.0(4) 4_575 . . . ? Bi1 Bi2 O7 Bi1 -119.6(7) 4_575 . . . ? O5 Bi2 O7 Bi1 -76.7(4) 4_575 . . 4_575 ? O5 Bi2 O7 Bi1 -163.7(4) . . . 4_575 ? O4 Bi2 O7 Bi1 109.0(4) . . . 4_575 ? O4 Bi2 O7 Bi1 10.6(3) 4_575 . . 4_575 ? Bi1 Bi2 O7 Bi1 119.6(7) . . . 4_575 ? O6 Bi1 O7 Bi2 115.2(5) . . . . ? O1 Bi1 O7 Bi2 -126.3(4) . . . . ? O4 Bi1 O7 Bi2 10.3(3) . . . . ? O2 Bi1 O7 Bi2 157.5(3) . . . . ? Bi1 Bi1 O7 Bi2 125.4(6) 4_575 . . . ? O6 Bi1 O7 Bi1 -10.2(4) . . . 4_575 ? O1 Bi1 O7 Bi1 108.3(4) . . . 4_575 ? O4 Bi1 O7 Bi1 -115.2(4) . . . 4_575 ? O2 Bi1 O7 Bi1 32.1(5) . . . 4_575 ? Bi2 Bi1 O7 Bi1 -125.4(6) . . . 4_575 ? C5 C4 C7 C9A 37(4) . . . . ? C3 C4 C7 C9A -141(3) . . . . ? C5 C4 C7 C10 173(3) . . . . ? C3 C4 C7 C10 -6(4) . . . . ? C5 C4 C7 C10A -150(2) . . . . ? C3 C4 C7 C10A 31(3) . . . . ? C5 C4 C7 C9 91(2) . . . . ? C3 C4 C7 C9 -88(2) . . . . ? C5 C4 C7 C8 -8(3) . . . . ? C3 C4 C7 C8 174(2) . . . . ? C5 C4 C7 C8A -63(2) . . . . ? C3 C4 C7 C8A 118.9(19) . . . . ? O13 Bi3 O8 C56 138.8(9) . . . . ? O14 Bi3 O8 C56 -160.7(10) . . . . ? O10A Bi3 O8 C56 -112.5(9) . . . . ? O9 Bi3 O8 C56 72.4(10) . . . . ? Bi3 Bi3 O8 C56 163.9(10) 4_575 . . . ? Bi4 Bi3 O8 C56 -135.4(9) . . . . ? O13 Bi4A O9 C72 172.5(8) . . . . ? O10 Bi4A O9 C72 -149.7(7) 4_575 . . . ? O10 Bi4A O9 C72 -102.6(8) . . . . ? O9 Bi4A O9 C72 109.8(7) 4_575 . . . ? O13 Bi4A O9 Bi3 -12.3(3) . . . . ? O10 Bi4A O9 Bi3 25.5(6) 4_575 . . . ? O10 Bi4A O9 Bi3 72.6(3) . . . . ? O9 Bi4A O9 Bi3 -75.0(3) 4_575 . . . ? O13 Bi3 O9 C72 -172.9(10) . . . . ? O8 Bi3 O9 C72 -63.0(9) . . . . ? O14 Bi3 O9 C72 -131.3(9) . . . . ? O10A Bi3 O9 C72 124.0(9) . . . . ? Bi3 Bi3 O9 C72 -148.9(9) 4_575 . . . ? Bi4 Bi3 O9 C72 -157.6(7) . . . . ? O13 Bi3 O9 Bi4A 12.7(3) . . . . ? O8 Bi3 O9 Bi4A 122.6(3) . . . . ? O14 Bi3 O9 Bi4A 54.3(4) . . . . ? O10A Bi3 O9 Bi4A -50.3(5) . . . . ? Bi3 Bi3 O9 Bi4A 36.8(2) 4_575 . . . ? Bi4 Bi3 O9 Bi4A 28.0(5) . . . . ? O14 Bi4 O10A C94 173.6(8) . . . . ? O12 Bi4 O10A C94 178.9(7) 4_575 . . . ? O12 Bi4 O10A C94 -104.7(7) . . . . ? O10A Bi4 O10A C94 101.9(7) 4_575 . . . ? Bi3 Bi4 O10A C94 -175.3(9) . . . . ? Bi3 Bi4 O10A C94 142.0(7) 4_575 . . . ? O14 Bi4 O10A Bi3 -11.1(3) . . . . ? O12 Bi4 O10A Bi3 -5.8(7) 4_575 . . . ? O12 Bi4 O10A Bi3 70.6(3) . . . . ? O10A Bi4 O10A Bi3 -82.9(3) 4_575 . . . ? Bi3 Bi4 O10A Bi3 -42.7(2) 4_575 . . . ? O13 Bi3 O10A C94 -109.6(10) . . . . ? O8 Bi3 O10A C94 134.8(10) . . . . ? O14 Bi3 O10A C94 -175.7(11) . . . . ? O9 Bi3 O10A C94 -53.8(12) . . . . ? Bi3 Bi3 O10A C94 -142.3(10) 4_575 . . . ? Bi4 Bi3 O10A C94 173.4(12) . . . . ? O13 Bi3 O10A Bi4 76.9(3) . . . . ? O8 Bi3 O10A Bi4 -38.7(4) . . . . ? O14 Bi3 O10A Bi4 10.8(3) . . . . ? O9 Bi3 O10A Bi4 132.7(3) . . . . ? Bi3 Bi3 O10A Bi4 44.3(2) 4_575 . . . ? O13 Bi4A O10 C79 71.4(7) . . . . ? O10 Bi4A O10 C79 156.3(6) 4_575 . . . ? O9 Bi4A O10 C79 106.8(8) 4_575 . . . ? O9 Bi4A O10 C79 0.7(7) . . . . ? C1 C6 C11 C12 -106.4(13) . . . . ? C5 C6 C11 C12 75.1(13) . . . . ? C6 C11 C12 C17 97.9(13) . . . . ? C6 C11 C12 C13 -78.7(14) . . . . ? O14 Bi4 O12 C105 95.1(10) . . . . ? O12 Bi4 O12 C105 175.2(8) 4_575 . . . ? O10A Bi4 O12 C105 100.3(11) 4_575 . . . ? O10A Bi4 O12 C105 21.5(10) . . . . ? Bi3 Bi4 O12 C105 61.4(9) . . . . ? Bi3 Bi4 O12 C105 104.3(10) 4_575 . . . ? C17 C12 C13 C14 1.5(19) . . . . ? C11 C12 C13 C14 178.1(12) . . . . ? O8 Bi3 O13 Bi3 50.4(5) . . . 4_575 ? O14 Bi3 O13 Bi3 -12.1(4) . . . 4_575 ? O10A Bi3 O13 Bi3 -78.1(4) . . . 4_575 ? O9 Bi3 O13 Bi3 132.3(5) . . . 4_575 ? Bi4 Bi3 O13 Bi3 -40.6(4) . . . 4_575 ? O8 Bi3 O13 Bi4A -97.5(5) . . . . ? O14 Bi3 O13 Bi4A -160.0(6) . . . . ? O10A Bi3 O13 Bi4A 133.9(5) . . . . ? O9 Bi3 O13 Bi4A -15.6(4) . . . . ? Bi3 Bi3 O13 Bi4A -147.9(8) 4_575 . . . ? Bi4 Bi3 O13 Bi4A 171.5(4) . . . . ? O10 Bi4A O13 Bi3 69.9(4) 4_575 . . 4_575 ? O10 Bi4A O13 Bi3 144.1(5) . . . 4_575 ? O9 Bi4A O13 Bi3 -16.4(4) 4_575 . . 4_575 ? O9 Bi4A O13 Bi3 -129.6(5) . . . 4_575 ? O10 Bi4A O13 Bi3 -144.1(5) 4_575 . . . ? O10 Bi4A O13 Bi3 -69.9(4) . . . . ? O9 Bi4A O13 Bi3 129.6(5) 4_575 . . . ? O9 Bi4A O13 Bi3 16.4(4) . . . . ? C12 C13 C14 C15 1.6(19) . . . . ? C12 C13 C14 C18 -174.8(12) . . . . ? O12 Bi4 O14 Bi3 -164.5(4) 4_575 . . . ? O12 Bi4 O14 Bi3 -73.1(4) . . . . ? O10A Bi4 O14 Bi3 109.3(5) 4_575 . . . ? O10A Bi4 O14 Bi3 13.0(4) . . . . ? Bi3 Bi4 O14 Bi3 122.3(7) 4_575 . . . ? O12 Bi4 O14 Bi3 73.1(4) 4_575 . . 4_575 ? O12 Bi4 O14 Bi3 164.5(4) . . . 4_575 ? O10A Bi4 O14 Bi3 -13.0(4) 4_575 . . 4_575 ? O10A Bi4 O14 Bi3 -109.3(5) . . . 4_575 ? Bi3 Bi4 O14 Bi3 -122.3(7) . . . 4_575 ? O13 Bi3 O14 Bi4 -115.9(5) . . . . ? O8 Bi3 O14 Bi4 126.2(5) . . . . ? O10A Bi3 O14 Bi4 -12.8(3) . . . . ? O9 Bi3 O14 Bi4 -156.9(3) . . . . ? Bi3 Bi3 O14 Bi4 -126.9(6) 4_575 . . . ? O13 Bi3 O14 Bi3 11.0(4) . . . 4_575 ? O8 Bi3 O14 Bi3 -106.9(4) . . . 4_575 ? O10A Bi3 O14 Bi3 114.1(4) . . . 4_575 ? O9 Bi3 O14 Bi3 -30.0(5) . . . 4_575 ? Bi4 Bi3 O14 Bi3 126.9(6) . . . 4_575 ? C13 C14 C15 C16 -2.4(19) . . . . ? C18 C14 C15 C16 174.3(12) . . . . ? C14 C15 C16 C17 0.1(18) . . . . ? C14 C15 C16 C22 -175.3(12) . . . . ? C13 C12 C17 O2 177.4(10) . . . . ? C11 C12 C17 O2 0.9(17) . . . . ? C13 C12 C17 C16 -3.9(18) . . . . ? C11 C12 C17 C16 179.6(11) . . . . ? Bi2A O2 C17 C12 122.8(10) . . . . ? Bi1 O2 C17 C12 -70.2(14) . . . . ? Bi2A O2 C17 C16 -56.0(13) . . . . ? Bi1 O2 C17 C16 111.1(11) . . . . ? C15 C16 C17 C12 3.1(17) . . . . ? C22 C16 C17 C12 178.5(11) . . . . ? C15 C16 C17 O2 -178.2(10) . . . . ? C22 C16 C17 O2 -2.8(17) . . . . ? C13 C14 C18 C21 113.8(18) . . . . ? C15 C14 C18 C21 -62.5(19) . . . . ? C13 C14 C18 C19 -124.1(16) . . . . ? C15 C14 C18 C19 59.6(18) . . . . ? C13 C14 C18 C20 -3(2) . . . . ? C15 C14 C18 C20 -179.6(13) . . . . ? C15 C16 C22 C23 117.7(12) . . . . ? C17 C16 C22 C23 -57.4(15) . . . . ? C16 C22 C23 C24 -59.9(13) . . . . ? C16 C22 C23 C28 114.3(11) . . . . ? C28 C23 C24 C25 0.8(18) . . . . ? C22 C23 C24 C25 175.2(12) . . . . ? C23 C24 C25 C26 -0.4(19) . . . . ? C23 C24 C25 C29 -176.0(14) . . . . ? C24 C25 C26 C27 0.0(19) . . . . ? C29 C25 C26 C27 175.2(15) . . . . ? C25 C26 C27 C28 -0.1(18) . . . . ? C25 C26 C27 C33 175.4(11) . . . . ? Bi2A O3 C28 C27 117.4(9) . . . . ? Bi2A O3 C28 C23 -60.9(12) . . . . ? C26 C27 C28 O3 -177.8(10) . . . . ? C33 C27 C28 O3 6.7(15) . . . . ? C26 C27 C28 C23 0.5(15) . . . . ? C33 C27 C28 C23 -175.0(9) . . . . ? C24 C23 C28 O3 177.4(10) . . . . ? C22 C23 C28 O3 3.2(16) . . . . ? C24 C23 C28 C27 -0.9(15) . . . . ? C22 C23 C28 C27 -175.1(10) . . . . ? C26 C25 C29 C30 -1(3) . . . . ? C24 C25 C29 C30 174.7(15) . . . . ? C26 C25 C29 C32 132.4(19) . . . . ? C24 C25 C29 C32 -52(2) . . . . ? C26 C25 C29 C31 -114.2(18) . . . . ? C24 C25 C29 C31 61.0(19) . . . . ? C26 C27 C33 C34 18.5(14) . . . . ? C28 C27 C33 C34 -166.0(10) . . . . ? C27 C33 C34 C35 -96.3(13) . . . . ? C27 C33 C34 C39 73.5(13) . . . . ? C39 C34 C35 C36 -0.7(19) . . . . ? C33 C34 C35 C36 169.5(13) . . . . ? C34 C35 C36 C37 3(2) . . . . ? C34 C35 C36 C40 -176.6(15) . . . . ? C35 C36 C37 C38 -4(2) . . . . ? C40 C36 C37 C38 175.6(15) . . . . ? C36 C37 C38 C39 2.5(18) . . . . ? C36 C37 C38 C44 -173.9(12) . . . . ? Bi2 O4 C39 C34 128.0(9) . . . . ? Bi1 O4 C39 C34 -53.7(14) . . . . ? Bi2 O4 C39 C38 -53.7(11) . . . . ? Bi1 O4 C39 C38 124.6(10) . . . . ? C35 C34 C39 O4 176.9(10) . . . . ? C33 C34 C39 O4 6.8(16) . . . . ? C35 C34 C39 C38 -1.4(17) . . . . ? C33 C34 C39 C38 -171.4(11) . . . . ? C37 C38 C39 O4 -177.7(10) . . . . ? C44 C38 C39 O4 -1.5(16) . . . . ? C37 C38 C39 C34 0.6(16) . . . . ? C44 C38 C39 C34 176.8(10) . . . . ? C37 C36 C40 C42A 150(3) . . . . ? C35 C36 C40 C42A -30(4) . . . . ? C37 C36 C40 C43A -7(3) . . . . ? C35 C36 C40 C43A 173(2) . . . . ? C37 C36 C40 C41A -134(2) . . . . ? C35 C36 C40 C41A 46(3) . . . . ? C37 C36 C40 C43 28(3) . . . . ? C35 C36 C40 C43 -152(2) . . . . ? C37 C36 C40 C41 -86(3) . . . . ? C35 C36 C40 C41 94(3) . . . . ? C37 C36 C40 C42 114(2) . . . . ? C35 C36 C40 C42 -66(2) . . . . ? C37 C38 C44 C45 116.5(12) . . . . ? C39 C38 C44 C45 -59.7(15) . . . . ? C38 C44 C45 C46 -75.6(13) . . . . ? C38 C44 C45 C50 102.1(12) . . . . ? C50 C45 C46 C47 5.5(16) . . . . ? C44 C45 C46 C47 -176.7(10) . . . . ? C45 C46 C47 C48 -7.0(17) . . . . ? C45 C46 C47 C51 169.6(11) . . . . ? C46 C47 C48 C49 2.9(17) . . . . ? C51 C47 C48 C49 -173.8(11) . . . . ? C47 C48 C49 C50 2.5(17) . . . . ? C47 C48 C49 C55 176.4(10) . . . . ? Bi2 O5 C50 C49 141.7(8) . . . . ? Bi2 O5 C50 C45 -43.2(13) . . . . ? C48 C49 C50 O5 171.2(9) . . . . ? C55 C49 C50 O5 -2.5(15) . . . . ? C48 C49 C50 C45 -4.1(15) . . . . ? C55 C49 C50 C45 -177.8(10) . . . . ? C46 C45 C50 O5 -174.8(9) . . . . ? C44 C45 C50 O5 7.6(16) . . . . ? C46 C45 C50 C49 0.3(15) . . . . ? C44 C45 C50 C49 -177.4(10) . . . . ? C48 C47 C51 C53 -171.6(12) . . . . ? C46 C47 C51 C53 12.0(18) . . . . ? C48 C47 C51 C52 -48.6(16) . . . . ? C46 C47 C51 C52 135.0(13) . . . . ? C48 C47 C51 C54 72.1(16) . . . . ? C46 C47 C51 C54 -104.3(14) . . . . ? C1 C2 C55 C49 88.3(14) . . . . ? C3 C2 C55 C49 -94.6(13) . . . . ? C48 C49 C55 C2 62.0(14) . . . . ? C50 C49 C55 C2 -124.3(11) . . . . ? Bi3 O8 C56 C57 100.8(12) . . . . ? Bi3 O8 C56 C61 -85.5(13) . . . . ? O8 C56 C57 C58 178.9(11) . . . . ? C61 C56 C57 C58 4.9(18) . . . . ? O8 C56 C57 C110 -2.2(18) . . . . ? C61 C56 C57 C110 -176.2(10) . . . . ? C56 C57 C58 C59 -2(2) . . . . ? C110 C57 C58 C59 178.9(12) . . . . ? C57 C58 C59 C60 0.0(19) . . . . ? C57 C58 C59 C62 -177.5(12) . . . . ? C58 C59 C60 C61 -0.9(19) . . . . ? C62 C59 C60 C61 176.5(12) . . . . ? C59 C60 C61 C56 3.8(19) . . . . ? C59 C60 C61 C66 -176.1(12) . . . . ? O8 C56 C61 C60 -179.6(11) . . . . ? C57 C56 C61 C60 -5.6(17) . . . . ? O8 C56 C61 C66 0.3(17) . . . . ? C57 C56 C61 C66 174.3(11) . . . . ? C60 C59 C62 C63 136.9(16) . . . . ? C58 C59 C62 C63 -46(2) . . . . ? C60 C59 C62 C64 -106.4(17) . . . . ? C58 C59 C62 C64 70.8(18) . . . . ? C60 C59 C62 C65 18(2) . . . . ? C58 C59 C62 C65 -164.5(17) . . . . ? C60 C61 C66 C67 -73.0(14) . . . . ? C56 C61 C66 C67 107.1(12) . . . . ? C61 C66 C67 C72 -98.4(13) . . . . ? C61 C66 C67 C68 81.4(14) . . . . ? C72 C67 C68 C69 2(2) . . . . ? C66 C67 C68 C69 -177.7(13) . . . . ? C67 C68 C69 C70 -3(2) . . . . ? C67 C68 C69 C73 174.6(14) . . . . ? C68 C69 C70 C71 3(2) . . . . ? C73 C69 C70 C71 -175.1(13) . . . . ? C69 C70 C71 C72 -1.1(18) . . . . ? C69 C70 C71 C77 178.7(12) . . . . ? Bi4A O9 C72 C67 -118.7(9) . . . . ? Bi3 O9 C72 C67 68.0(13) . . . . ? Bi4A O9 C72 C71 62.0(11) . . . . ? Bi3 O9 C72 C71 -111.2(10) . . . . ? C68 C67 C72 O9 -179.5(10) . . . . ? C66 C67 C72 O9 0.3(16) . . . . ? C68 C67 C72 C71 -0.2(17) . . . . ? C66 C67 C72 C71 179.6(10) . . . . ? C70 C71 C72 O9 179.1(9) . . . . ? C77 C71 C72 O9 -0.7(15) . . . . ? C70 C71 C72 C67 -0.2(16) . . . . ? C77 C71 C72 C67 180.0(10) . . . . ? C68 C69 C73 C75 129.9(18) . . . . ? C70 C69 C73 C75 -52(2) . . . . ? C68 C69 C73 C74 -4(2) . . . . ? C70 C69 C73 C74 174.2(14) . . . . ? C68 C69 C73 C76 -121.1(18) . . . . ? C70 C69 C73 C76 56.7(19) . . . . ? C70 C71 C77 C78 -121.1(11) . . . . ? C72 C71 C77 C78 58.7(14) . . . . ? C71 C77 C78 C83 65.9(13) . . . . ? C71 C77 C78 C79 -107.2(12) . . . . ? Bi4A O10 C79 C80 -119.3(9) . . . . ? Bi4A O10 C79 C78 63.1(12) . . . . ? C83 C78 C79 O10 178.1(10) . . . . ? C77 C78 C79 O10 -9.0(16) . . . . ? C83 C78 C79 C80 0.4(16) . . . . ? C77 C78 C79 C80 173.4(10) . . . . ? O10 C79 C80 C81 -177.0(10) . . . . ? C78 C79 C80 C81 0.6(16) . . . . ? O10 C79 C80 C88 0.6(15) . . . . ? C78 C79 C80 C88 178.3(10) . . . . ? C79 C80 C81 C82 -0.8(19) . . . . ? C88 C80 C81 C82 -178.4(11) . . . . ? C80 C81 C82 C83 0(2) . . . . ? C80 C81 C82 C84 175.5(14) . . . . ? C79 C78 C83 C82 -1.4(18) . . . . ? C77 C78 C83 C82 -174.7(11) . . . . ? C81 C82 C83 C78 1.2(19) . . . . ? C84 C82 C83 C78 -174.4(14) . . . . ? C81 C82 C84 C85 -177.1(18) . . . . ? C83 C82 C84 C85 -2(3) . . . . ? C81 C82 C84 C86 46(3) . . . . ? C83 C82 C84 C86 -139(2) . . . . ? C81 C82 C84 C87 -66(2) . . . . ? C83 C82 C84 C87 109.7(19) . . . . ? C81 C80 C88 C89 -19.6(15) . . . . ? C79 C80 C88 C89 162.8(10) . . . . ? C80 C88 C89 C90 92.2(12) . . . . ? C80 C88 C89 C94 -81.3(13) . . . . ? C94 C89 C90 C91 2.9(17) . . . . ? C88 C89 C90 C91 -170.8(11) . . . . ? C89 C90 C91 C92 -1.2(17) . . . . ? C89 C90 C91 C95 176.9(11) . . . . ? C90 C91 C92 C93 0.1(17) . . . . ? C95 C91 C92 C93 -178.0(11) . . . . ? C91 C92 C93 C94 -0.9(16) . . . . ? C91 C92 C93 C99 177.2(10) . . . . ? Bi4 O10A C94 C93 54.3(12) . . . . ? Bi3 O10A C94 C93 -118.4(11) . . . . ? Bi4 O10A C94 C89 -130.1(9) . . . . ? Bi3 O10A C94 C89 57.2(15) . . . . ? C92 C93 C94 O10A 178.1(9) . . . . ? C99 C93 C94 O10A 0.1(16) . . . . ? C92 C93 C94 C89 2.7(16) . . . . ? C99 C93 C94 C89 -175.3(10) . . . . ? C90 C89 C94 O10A -179.2(9) . . . . ? C88 C89 C94 O10A -5.6(16) . . . . ? C90 C89 C94 C93 -3.7(16) . . . . ? C88 C89 C94 C93 170.0(10) . . . . ? C92 C91 C95 C96A 177.4(16) . . . . ? C90 C91 C95 C96A -1(2) . . . . ? C92 C91 C95 C97A -33(2) . . . . ? C90 C91 C95 C97A 149(2) . . . . ? C92 C91 C95 C98A 91(3) . . . . ? C90 C91 C95 C98A -87(3) . . . . ? C92 C91 C95 C96 -139(2) . . . . ? C90 C91 C95 C96 43(3) . . . . ? C92 C91 C95 C98 56(2) . . . . ? C90 C91 C95 C98 -122(2) . . . . ? C92 C91 C95 C97 -68(2) . . . . ? C90 C91 C95 C97 114(2) . . . . ? C94 C93 C99 C100 62.1(14) . . . . ? C92 C93 C99 C100 -115.9(11) . . . . ? C93 C99 C100 C101 74.4(13) . . . . ? C93 C99 C100 C105 -105.6(12) . . . . ? C105 C100 C101 C102 -3.7(18) . . . . ? C99 C100 C101 C102 176.3(10) . . . . ? C100 C101 C102 C103 3.7(17) . . . . ? C100 C101 C102 C106 -169.3(11) . . . . ? C101 C102 C103 C104 1.7(18) . . . . ? C106 C102 C103 C104 175.0(11) . . . . ? C102 C103 C104 C105 -7.2(18) . . . . ? C102 C103 C104 C110 -173.6(11) . . . . ? Bi4 O12 C105 C104 -138.7(9) . . . . ? Bi4 O12 C105 C100 44.8(15) . . . . ? C103 C104 C105 O12 -169.7(10) . . . . ? C110 C104 C105 O12 -4.0(16) . . . . ? C103 C104 C105 C100 7.0(16) . . . . ? C110 C104 C105 C100 172.7(10) . . . . ? C101 C100 C105 O12 174.8(10) . . . . ? C99 C100 C105 O12 -5.2(17) . . . . ? C101 C100 C105 C104 -1.8(17) . . . . ? C99 C100 C105 C104 178.2(10) . . . . ? C103 C102 C106 C107 172.6(12) . . . . ? C101 C102 C106 C107 -14.5(18) . . . . ? C103 C102 C106 C108 -66.7(16) . . . . ? C101 C102 C106 C108 106.2(14) . . . . ? C103 C102 C106 C109 51.9(16) . . . . ? C101 C102 C106 C109 -135.2(13) . . . . ? C105 C104 C110 C57 127.3(12) . . . . ? C103 C104 C110 C57 -66.7(14) . . . . ? C56 C57 C110 C104 -80.6(14) . . . . ? C58 C57 C110 C104 98.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 6.330 _refine_diff_density_min -7.823 _refine_diff_density_rms 0.252 # Attachment '9a.CIF' data_tcu160m _database_code_depnum_ccdc_archive 'CCDC 716841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H66 O6 Sb2, 3(C6H6)' _chemical_formula_sum 'C73 H84 O6 Sb2' _chemical_formula_weight 1300.90 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' Sb Sb -0.5866 1.5461 '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 14.965(3) _cell_length_b 15.239(3) _cell_length_c 16.261(4) _cell_angle_alpha 72.976(5) _cell_angle_beta 68.079(4) _cell_angle_gamma 70.384(4) _cell_volume 3180.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 12994 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.29 _reflns_number_total 8992 _reflns_number_gt 6550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. Disorder for the tert-butyl groups was due to 2-fold axis, and was modeled using partial occupancies and isotropic displacement parameters. ; _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^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8992 _refine_ls_number_parameters 696 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.948 _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 Sb1 Sb 0.25839(2) 0.11906(2) 0.24472(2) 0.03011(12) Uani 1 1 d . . . O1 O 0.4003(2) 0.0506(2) 0.2023(2) 0.0332(9) Uani 1 1 d . . . C1 C 0.4356(3) -0.0399(4) 0.1839(3) 0.0298(13) Uani 1 1 d . . . O2 O 0.2122(2) 0.0214(2) 0.2247(2) 0.0281(8) Uani 1 1 d . . . C2 C 0.4983(4) -0.1076(4) 0.2305(4) 0.0322(13) Uani 1 1 d . . . Sb2 Sb 0.14840(2) -0.02071(2) 0.45477(2) 0.02686(12) Uani 1 1 d . . . O3 O 0.0236(2) 0.0640(2) 0.4242(2) 0.0251(8) Uani 1 1 d . . . C3 C 0.5423(4) -0.1966(4) 0.2055(4) 0.0344(13) Uani 1 1 d . . . H3A H 0.5863 -0.2419 0.2354 0.041 Uiso 1 1 calc R . . O4 O 0.1270(2) 0.0389(2) 0.5559(2) 0.0252(8) Uani 1 1 d . . . C4 C 0.5238(4) -0.2211(4) 0.1385(4) 0.0362(13) Uani 1 1 d . A . O5 O 0.4380(3) 0.0410(2) 0.4254(2) 0.0354(9) Uani 1 1 d . . . H5A H 0.4739 0.0419 0.4535 0.053 Uiso 1 1 calc R . . C5 C 0.4610(4) -0.1507(4) 0.0929(4) 0.0389(14) Uani 1 1 d . . . H5B H 0.4472 -0.1651 0.0472 0.047 Uiso 1 1 calc R . . C6 C 0.4184(4) -0.0597(4) 0.1133(3) 0.0319(13) Uani 1 1 d . . . C7 C 0.5779(4) -0.3187(4) 0.1109(4) 0.0529(17) Uani 1 1 d D . . C8 C 0.5465(13) -0.3350(13) 0.0428(10) 0.115(7) Uiso 0.559(13) 1 d PD A 1 H8A H 0.5564 -0.2851 -0.0102 0.173 Uiso 0.559(13) 1 calc PR A 1 H8B H 0.4766 -0.3347 0.0672 0.173 Uiso 0.559(13) 1 calc PR A 1 H8C H 0.5858 -0.3959 0.0264 0.173 Uiso 0.559(13) 1 calc PR A 1 C9 C 0.6893(8) -0.3281(10) 0.0792(10) 0.079(5) Uiso 0.559(13) 1 d PD A 1 H9A H 0.7062 -0.2815 0.0246 0.119 Uiso 0.559(13) 1 calc PR A 1 H9B H 0.7249 -0.3913 0.0669 0.119 Uiso 0.559(13) 1 calc PR A 1 H9C H 0.7080 -0.3175 0.1259 0.119 Uiso 0.559(13) 1 calc PR A 1 C10 C 0.5602(10) -0.3957(9) 0.1964(7) 0.072(4) Uiso 0.559(13) 1 d PD A 1 H10A H 0.6216 -0.4250 0.2121 0.108 Uiso 0.559(13) 1 calc PR A 1 H10B H 0.5388 -0.4435 0.1854 0.108 Uiso 0.559(13) 1 calc PR A 1 H10C H 0.5091 -0.3672 0.2458 0.108 Uiso 0.559(13) 1 calc PR A 1 C8A C 0.5059(11) -0.3576(12) 0.0952(12) 0.069(5) Uiso 0.441(13) 1 d PD A 2 H8AA H 0.4936 -0.3237 0.0382 0.104 Uiso 0.441(13) 1 calc PR A 2 H8AB H 0.4436 -0.3493 0.1439 0.104 Uiso 0.441(13) 1 calc PR A 2 H8AC H 0.5344 -0.4245 0.0933 0.104 Uiso 0.441(13) 1 calc PR A 2 C9A C 0.6536(12) -0.2991(13) 0.0168(10) 0.092(7) Uiso 0.441(13) 1 d PD A 2 H9AA H 0.6249 -0.2398 -0.0179 0.138 Uiso 0.441(13) 1 calc PR A 2 H9AB H 0.6699 -0.3504 -0.0145 0.138 Uiso 0.441(13) 1 calc PR A 2 H9AC H 0.7137 -0.2948 0.0235 0.138 Uiso 0.441(13) 1 calc PR A 2 C10A C 0.6310(15) -0.3870(14) 0.1719(13) 0.122(9) Uiso 0.441(13) 1 d PD A 2 H10D H 0.5851 -0.4185 0.2220 0.182 Uiso 0.441(13) 1 calc PR A 2 H10E H 0.6594 -0.3541 0.1948 0.182 Uiso 0.441(13) 1 calc PR A 2 H10F H 0.6839 -0.4337 0.1396 0.182 Uiso 0.441(13) 1 calc PR A 2 O6 O 0.2338(2) 0.0599(2) 0.3710(2) 0.0331(9) Uani 1 1 d . . . C11 C 0.3689(4) 0.0184(4) 0.0495(4) 0.0379(14) Uani 1 1 d . . . H11A H 0.3823 0.0772 0.0493 0.045 Uiso 1 1 calc R . . H11B H 0.4043 0.0041 -0.0112 0.045 Uiso 1 1 calc R . . C12 C 0.2595(4) 0.0407(4) 0.0617(3) 0.0306(12) Uani 1 1 d . . . C13 C 0.2285(4) 0.0686(4) -0.0143(4) 0.0337(13) Uani 1 1 d . . . H13A H 0.2771 0.0656 -0.0710 0.040 Uiso 1 1 calc R . . C14 C 0.1287(4) 0.1007(4) -0.0105(4) 0.0334(13) Uani 1 1 d . B . C15 C 0.0578(4) 0.1011(3) 0.0752(3) 0.0305(12) Uani 1 1 d . . . H15A H -0.0102 0.1210 0.0798 0.037 Uiso 1 1 calc R . . C16 C 0.0852(4) 0.0727(3) 0.1538(3) 0.0260(12) Uani 1 1 d . . . C17 C 0.1857(4) 0.0436(3) 0.1466(3) 0.0277(12) Uani 1 1 d . . . C18 C 0.0972(4) 0.1396(4) -0.0966(4) 0.0406(14) Uani 1 1 d D . . C19 C 0.1455(11) 0.0704(10) -0.1616(11) 0.071(6) Uiso 0.416(9) 1 d PD B 1 H19A H 0.2172 0.0531 -0.1741 0.106 Uiso 0.416(9) 1 calc PR B 1 H19B H 0.1292 0.1002 -0.2175 0.106 Uiso 0.416(9) 1 calc PR B 1 H19C H 0.1209 0.0139 -0.1346 0.106 Uiso 0.416(9) 1 calc PR B 1 C20 C -0.0163(8) 0.1573(12) -0.0756(12) 0.075(6) Uiso 0.416(9) 1 d PD B 1 H20A H -0.0321 0.0978 -0.0664 0.112 Uiso 0.416(9) 1 calc PR B 1 H20B H -0.0371 0.2013 -0.1257 0.112 Uiso 0.416(9) 1 calc PR B 1 H20C H -0.0510 0.1841 -0.0213 0.112 Uiso 0.416(9) 1 calc PR B 1 C21 C 0.1254(13) 0.2313(10) -0.1410(13) 0.084(7) Uiso 0.416(9) 1 d PD B 1 H21A H 0.1951 0.2221 -0.1486 0.126 Uiso 0.416(9) 1 calc PR B 1 H21B H 0.0849 0.2784 -0.1036 0.126 Uiso 0.416(9) 1 calc PR B 1 H21C H 0.1144 0.2529 -0.1996 0.126 Uiso 0.416(9) 1 calc PR B 1 C19A C 0.1873(7) 0.1359(8) -0.1835(7) 0.057(4) Uiso 0.584(9) 1 d PD B 2 H19D H 0.2449 0.1377 -0.1707 0.086 Uiso 0.584(9) 1 calc PR B 2 H19E H 0.1719 0.1901 -0.2299 0.086 Uiso 0.584(9) 1 calc PR B 2 H19F H 0.2016 0.0778 -0.2043 0.086 Uiso 0.584(9) 1 calc PR B 2 C20A C 0.0313(8) 0.0866(7) -0.0992(8) 0.064(4) Uiso 0.584(9) 1 d PD B 2 H20D H 0.0715 0.0273 -0.1189 0.096 Uiso 0.584(9) 1 calc PR B 2 H20E H -0.0057 0.1245 -0.1411 0.096 Uiso 0.584(9) 1 calc PR B 2 H20F H -0.0148 0.0735 -0.0394 0.096 Uiso 0.584(9) 1 calc PR B 2 C21A C 0.0433(8) 0.2450(6) -0.0981(8) 0.057(3) Uiso 0.584(9) 1 d PD B 2 H21D H 0.0910 0.2806 -0.1099 0.086 Uiso 0.584(9) 1 calc PR B 2 H21E H -0.0067 0.2525 -0.0401 0.086 Uiso 0.584(9) 1 calc PR B 2 H21F H 0.0114 0.2685 -0.1452 0.086 Uiso 0.584(9) 1 calc PR B 2 C22 C 0.0105(3) 0.0816(3) 0.2461(3) 0.0278(12) Uani 1 1 d . . . H22A H 0.0246 0.0221 0.2888 0.033 Uiso 1 1 calc R . . H22B H -0.0566 0.0924 0.2430 0.033 Uiso 1 1 calc R . . C23 C 0.0139(3) 0.1625(3) 0.2801(3) 0.0250(12) Uani 1 1 d . . . C24 C 0.0113(3) 0.2518(4) 0.2237(3) 0.0291(12) Uani 1 1 d . . . H24A H 0.0077 0.2596 0.1654 0.035 Uiso 1 1 calc R . . C25 C 0.0139(4) 0.3297(4) 0.2505(3) 0.0294(12) Uani 1 1 d . . . C26 C 0.0162(3) 0.3170(3) 0.3375(3) 0.0295(12) Uani 1 1 d . . . H26A H 0.0157 0.3692 0.3574 0.035 Uiso 1 1 calc R . . C27 C 0.0191(3) 0.2283(3) 0.3979(3) 0.0230(11) Uani 1 1 d . . . C28 C 0.0205(3) 0.1510(3) 0.3670(3) 0.0235(11) Uani 1 1 d . . . C29 C 0.0094(4) 0.4256(4) 0.1861(4) 0.0383(14) Uani 1 1 d . . . C30 C 0.0871(7) 0.4140(5) 0.0955(5) 0.104(4) Uani 1 1 d . . . H30A H 0.1527 0.3885 0.1034 0.156 Uiso 1 1 calc R . . H30B H 0.0839 0.4753 0.0550 0.156 Uiso 1 1 calc R . . H30C H 0.0745 0.3709 0.0700 0.156 Uiso 1 1 calc R . . C31 C -0.0936(6) 0.4669(5) 0.1756(6) 0.094(3) Uani 1 1 d . . . H31A H -0.1089 0.4237 0.1524 0.142 Uiso 1 1 calc R . . H31B H -0.0959 0.5274 0.1339 0.142 Uiso 1 1 calc R . . H31C H -0.1420 0.4763 0.2339 0.142 Uiso 1 1 calc R . . C32 C 0.0299(6) 0.4974(5) 0.2204(5) 0.079(2) Uani 1 1 d . . . H32A H 0.0960 0.4737 0.2272 0.118 Uiso 1 1 calc R . . H32B H -0.0191 0.5073 0.2783 0.118 Uiso 1 1 calc R . . H32C H 0.0259 0.5571 0.1775 0.118 Uiso 1 1 calc R . . C33 C 0.0097(3) 0.2214(3) 0.4949(3) 0.0256(11) Uani 1 1 d . . . H33A H -0.0193 0.1682 0.5313 0.031 Uiso 1 1 calc R . . H33B H -0.0379 0.2793 0.5145 0.031 Uiso 1 1 calc R . . C34 C 0.1043(3) 0.2081(3) 0.5170(3) 0.0241(11) Uani 1 1 d . . . C35 C 0.1356(4) 0.2845(3) 0.5138(3) 0.0291(12) Uani 1 1 d . . . H35A H 0.0990 0.3456 0.4942 0.035 Uiso 1 1 calc R . . C36 C 0.2185(4) 0.2767(4) 0.5379(3) 0.0300(12) Uani 1 1 d . . . C37 C 0.2717(4) 0.1840(4) 0.5647(3) 0.0305(12) Uani 1 1 d . . . H37A H 0.3290 0.1755 0.5801 0.037 Uiso 1 1 calc R . . C38 C 0.2438(4) 0.1047(3) 0.5693(3) 0.0257(12) Uani 1 1 d . . . C39 C 0.1591(3) 0.1167(3) 0.5457(3) 0.0253(12) Uani 1 1 d . . . C40 C 0.2516(4) 0.3616(4) 0.5372(4) 0.0375(14) Uani 1 1 d . . . C41 C 0.1765(5) 0.4547(4) 0.5181(5) 0.065(2) Uani 1 1 d . . . H41A H 0.1684 0.4616 0.4599 0.097 Uiso 1 1 calc R . . H41B H 0.2003 0.5070 0.5173 0.097 Uiso 1 1 calc R . . H41C H 0.1130 0.4551 0.5648 0.097 Uiso 1 1 calc R . . C42 C 0.2624(5) 0.3540(4) 0.6286(5) 0.0601(19) Uani 1 1 d . . . H42A H 0.2841 0.4078 0.6271 0.090 Uiso 1 1 calc R . . H42B H 0.3112 0.2957 0.6420 0.090 Uiso 1 1 calc R . . H42C H 0.1987 0.3537 0.6749 0.090 Uiso 1 1 calc R . . C43 C 0.3514(5) 0.3653(5) 0.4636(5) 0.066(2) Uani 1 1 d . . . H43A H 0.3444 0.3704 0.4053 0.098 Uiso 1 1 calc R . . H43B H 0.4017 0.3079 0.4759 0.098 Uiso 1 1 calc R . . H43C H 0.3712 0.4200 0.4629 0.098 Uiso 1 1 calc R . . C44 C 0.2997(4) 0.0054(3) 0.6049(3) 0.0295(12) Uani 1 1 d . . . H44A H 0.3531 0.0115 0.6222 0.035 Uiso 1 1 calc R . . H44B H 0.2536 -0.0216 0.6599 0.035 Uiso 1 1 calc R . . C45 C 0.3449(4) -0.0642(3) 0.5422(3) 0.0270(12) Uani 1 1 d . . . C46 C 0.3233(4) -0.1520(3) 0.5697(4) 0.0278(12) Uani 1 1 d . . . H46A H 0.2788 -0.1661 0.6275 0.033 Uiso 1 1 calc R . . C47 C 0.3653(4) -0.2205(3) 0.5148(4) 0.0313(13) Uani 1 1 d . . . C48 C 0.4278(4) -0.1950(4) 0.4285(4) 0.0316(13) Uani 1 1 d . . . H48A H 0.4550 -0.2385 0.3893 0.038 Uiso 1 1 calc R . . C49 C 0.4515(3) -0.1083(4) 0.3981(3) 0.0284(12) Uani 1 1 d . . . C50 C 0.4112(3) -0.0439(3) 0.4559(3) 0.0264(12) Uani 1 1 d . . . C51 C 0.3408(4) -0.3167(4) 0.5499(4) 0.0367(14) Uani 1 1 d . . . C52 C 0.2311(4) -0.3043(4) 0.5628(5) 0.064(2) Uani 1 1 d . . . H52A H 0.2174 -0.2746 0.5057 0.096 Uiso 1 1 calc R . . H52B H 0.1898 -0.2645 0.6071 0.096 Uiso 1 1 calc R . . H52C H 0.2164 -0.3659 0.5837 0.096 Uiso 1 1 calc R . . C53 C 0.3645(6) -0.3642(4) 0.6395(5) 0.065(2) Uani 1 1 d . . . H53A H 0.4340 -0.3703 0.6305 0.098 Uiso 1 1 calc R . . H53B H 0.3519 -0.4267 0.6596 0.098 Uiso 1 1 calc R . . H53C H 0.3226 -0.3257 0.6847 0.098 Uiso 1 1 calc R . . C54 C 0.4025(5) -0.3847(4) 0.4840(5) 0.0587(19) Uani 1 1 d . . . H54A H 0.3900 -0.3571 0.4263 0.088 Uiso 1 1 calc R . . H54B H 0.3840 -0.4445 0.5082 0.088 Uiso 1 1 calc R . . H54C H 0.4727 -0.3957 0.4759 0.088 Uiso 1 1 calc R . . C55 C 0.5214(4) -0.0841(4) 0.3029(4) 0.0337(13) Uani 1 1 d . . . H55A H 0.5176 -0.0161 0.2888 0.040 Uiso 1 1 calc R . . H55B H 0.5899 -0.1188 0.3019 0.040 Uiso 1 1 calc R . . C56 C 0.2929(6) 0.3324(6) 0.2698(6) 0.081(2) Uani 1 1 d . . . H56A H 0.2243 0.3381 0.2975 0.097 Uiso 1 1 calc R . . C57 C 0.3577(8) 0.2514(7) 0.2936(6) 0.096(3) Uani 1 1 d . . . H57A H 0.3341 0.2027 0.3391 0.115 Uiso 1 1 calc R . . C58 C 0.4549(9) 0.2402(8) 0.2527(8) 0.122(4) Uani 1 1 d . . . H58A H 0.4991 0.1813 0.2660 0.146 Uiso 1 1 calc R . . C59 C 0.4932(9) 0.3152(12) 0.1897(10) 0.158(5) Uani 1 1 d . . . H59A H 0.5622 0.3088 0.1660 0.190 Uiso 1 1 calc R . . C60 C 0.4255(10) 0.4006(10) 0.1625(8) 0.135(4) Uani 1 1 d . . . H60A H 0.4489 0.4496 0.1173 0.162 Uiso 1 1 calc R . . C61 C 0.3250(8) 0.4095(7) 0.2040(7) 0.105(3) Uani 1 1 d . . . H61A H 0.2784 0.4657 0.1891 0.126 Uiso 1 1 calc R . . C62 C 0.1583(7) 0.6324(6) 0.3030(5) 0.076(2) Uani 1 1 d . . . H62A H 0.1435 0.5737 0.3154 0.092 Uiso 1 1 calc R . . C63 C 0.2517(6) 0.6337(5) 0.2979(6) 0.075(2) Uani 1 1 d . . . H63A H 0.3009 0.5769 0.3053 0.090 Uiso 1 1 calc R . . C64 C 0.2708(6) 0.7197(6) 0.2817(5) 0.074(2) Uani 1 1 d . . . H64A H 0.3339 0.7228 0.2780 0.089 Uiso 1 1 calc R . . C65 C 0.1983(8) 0.8009(6) 0.2708(5) 0.079(3) Uani 1 1 d . . . H65A H 0.2110 0.8603 0.2603 0.094 Uiso 1 1 calc R . . C66 C 0.1100(8) 0.7962(7) 0.2752(6) 0.090(3) Uani 1 1 d . . . H66A H 0.0607 0.8528 0.2671 0.108 Uiso 1 1 calc R . . C67 C 0.0885(6) 0.7119(8) 0.2909(5) 0.079(2) Uani 1 1 d . . . H67A H 0.0256 0.7098 0.2931 0.095 Uiso 1 1 calc R . . C68 C -0.2458(8) 0.3621(8) 0.0177(8) 0.121(4) Uiso 1 1 d . . . H68A H -0.2453 0.4265 0.0010 0.146 Uiso 1 1 calc R . . C69 C -0.2592(8) 0.3212(9) -0.0351(8) 0.127(4) Uiso 1 1 d . . . H69A H -0.2668 0.3577 -0.0909 0.153 Uiso 1 1 calc R . . C70 C -0.2626(8) 0.2367(8) -0.0167(8) 0.120(4) Uiso 1 1 d . . . H70A H -0.2693 0.2121 -0.0601 0.144 Uiso 1 1 calc R . . C71 C -0.2571(8) 0.1798(8) 0.0620(8) 0.122(4) Uiso 1 1 d . . . H71A H -0.2653 0.1181 0.0758 0.146 Uiso 1 1 calc R . . C72 C -0.2392(8) 0.2136(8) 0.1226(8) 0.123(4) Uiso 1 1 d . . . H72A H -0.2319 0.1741 0.1774 0.148 Uiso 1 1 calc R . . C73 C -0.2319(8) 0.3060(8) 0.1022(8) 0.128(4) Uiso 1 1 d . . . H73A H -0.2186 0.3310 0.1416 0.154 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 Sb1 0.0267(2) 0.0298(2) 0.0318(2) -0.00720(17) -0.00977(17) -0.00261(16) O1 0.0198(18) 0.033(2) 0.042(2) -0.0098(18) -0.0045(17) -0.0035(15) C1 0.017(3) 0.035(3) 0.031(3) -0.009(3) 0.000(2) -0.004(2) O2 0.0283(19) 0.032(2) 0.0234(19) -0.0034(16) -0.0108(16) -0.0048(15) C2 0.025(3) 0.039(3) 0.028(3) -0.007(3) -0.003(2) -0.007(2) Sb2 0.0255(2) 0.0264(2) 0.0309(2) -0.00939(16) -0.01357(16) -0.00041(15) O3 0.0254(18) 0.0263(19) 0.0244(19) -0.0053(16) -0.0102(15) -0.0042(14) C3 0.026(3) 0.040(3) 0.032(3) -0.008(3) -0.008(3) -0.002(2) O4 0.0244(18) 0.0298(19) 0.0244(19) -0.0078(15) -0.0091(15) -0.0065(15) C4 0.028(3) 0.040(3) 0.038(3) -0.014(3) -0.006(3) -0.004(3) O5 0.038(2) 0.037(2) 0.039(2) -0.0020(18) -0.0182(18) -0.0169(17) C5 0.028(3) 0.056(4) 0.034(3) -0.020(3) -0.007(3) -0.004(3) C6 0.021(3) 0.044(3) 0.024(3) -0.007(3) -0.001(2) -0.006(2) C7 0.043(4) 0.046(4) 0.068(5) -0.029(3) -0.016(3) 0.006(3) O6 0.0256(19) 0.050(2) 0.027(2) -0.0135(18) -0.0075(16) -0.0096(17) C11 0.033(3) 0.050(4) 0.026(3) -0.006(3) -0.007(3) -0.009(3) C12 0.026(3) 0.033(3) 0.027(3) -0.004(2) -0.008(2) -0.003(2) C13 0.037(3) 0.034(3) 0.025(3) -0.007(2) -0.011(3) -0.001(3) C14 0.043(3) 0.030(3) 0.028(3) -0.004(2) -0.014(3) -0.008(3) C15 0.030(3) 0.033(3) 0.030(3) -0.011(2) -0.013(3) -0.002(2) C16 0.025(3) 0.029(3) 0.023(3) -0.007(2) -0.006(2) -0.006(2) C17 0.037(3) 0.024(3) 0.025(3) -0.007(2) -0.012(3) -0.006(2) C18 0.043(3) 0.051(4) 0.026(3) -0.006(3) -0.015(3) -0.007(3) C22 0.019(3) 0.033(3) 0.031(3) -0.006(2) -0.009(2) -0.004(2) C23 0.020(3) 0.027(3) 0.028(3) -0.012(2) -0.009(2) 0.002(2) C24 0.022(3) 0.041(3) 0.020(3) -0.004(2) -0.009(2) -0.001(2) C25 0.024(3) 0.031(3) 0.028(3) -0.004(2) -0.007(2) -0.002(2) C26 0.025(3) 0.027(3) 0.035(3) -0.009(3) -0.008(2) -0.001(2) C27 0.013(2) 0.031(3) 0.024(3) -0.006(2) -0.007(2) -0.002(2) C28 0.012(2) 0.027(3) 0.026(3) -0.004(2) -0.006(2) 0.001(2) C29 0.042(3) 0.031(3) 0.032(3) 0.002(3) -0.010(3) -0.006(3) C30 0.154(9) 0.050(5) 0.049(5) 0.006(4) 0.020(5) -0.024(5) C31 0.086(6) 0.047(5) 0.136(8) 0.029(5) -0.067(6) -0.003(4) C32 0.118(7) 0.046(4) 0.082(6) 0.018(4) -0.053(5) -0.034(4) C33 0.025(3) 0.028(3) 0.025(3) -0.011(2) -0.008(2) -0.001(2) C34 0.023(3) 0.033(3) 0.018(3) -0.009(2) -0.005(2) -0.006(2) C35 0.031(3) 0.027(3) 0.025(3) -0.005(2) -0.008(2) -0.003(2) C36 0.035(3) 0.033(3) 0.026(3) -0.008(2) -0.010(2) -0.008(2) C37 0.027(3) 0.038(3) 0.029(3) -0.010(3) -0.011(2) -0.006(2) C38 0.025(3) 0.027(3) 0.021(3) -0.007(2) -0.005(2) -0.003(2) C39 0.024(3) 0.032(3) 0.019(3) -0.011(2) -0.004(2) -0.003(2) C40 0.046(3) 0.032(3) 0.043(4) -0.009(3) -0.019(3) -0.012(3) C41 0.082(5) 0.035(4) 0.097(6) -0.008(4) -0.052(5) -0.016(3) C42 0.087(5) 0.041(4) 0.071(5) -0.015(3) -0.044(4) -0.013(4) C43 0.063(5) 0.067(5) 0.080(5) -0.024(4) -0.013(4) -0.034(4) C44 0.035(3) 0.028(3) 0.031(3) -0.009(2) -0.017(3) -0.003(2) C45 0.025(3) 0.028(3) 0.033(3) -0.005(2) -0.018(2) -0.003(2) C46 0.025(3) 0.027(3) 0.029(3) -0.007(2) -0.012(2) 0.001(2) C47 0.025(3) 0.029(3) 0.041(4) -0.007(3) -0.017(3) 0.000(2) C48 0.025(3) 0.029(3) 0.038(3) -0.011(3) -0.010(3) 0.001(2) C49 0.018(3) 0.035(3) 0.030(3) -0.004(3) -0.012(2) -0.002(2) C50 0.021(3) 0.026(3) 0.033(3) -0.002(2) -0.016(2) -0.001(2) C51 0.030(3) 0.028(3) 0.051(4) -0.005(3) -0.016(3) -0.004(2) C52 0.033(4) 0.041(4) 0.110(6) -0.018(4) -0.011(4) -0.010(3) C53 0.084(5) 0.042(4) 0.065(5) 0.007(4) -0.024(4) -0.024(4) C54 0.049(4) 0.037(4) 0.085(5) -0.020(4) -0.007(4) -0.012(3) C55 0.026(3) 0.036(3) 0.038(3) -0.007(3) -0.011(3) -0.005(2) C56 0.079(6) 0.089(6) 0.073(6) -0.005(5) -0.023(5) -0.026(5) C57 0.095(7) 0.105(7) 0.077(6) 0.007(5) -0.047(6) -0.009(6) C58 0.096(9) 0.101(8) 0.132(10) -0.008(7) -0.029(7) 0.003(7) C59 0.078(8) 0.184(14) 0.173(14) -0.041(12) -0.018(9) -0.002(9) C60 0.112(10) 0.159(12) 0.130(11) -0.042(9) 0.004(8) -0.062(9) C61 0.095(8) 0.102(8) 0.121(9) -0.023(7) -0.043(7) -0.015(6) C62 0.120(8) 0.065(5) 0.062(5) 0.004(4) -0.038(5) -0.048(5) C63 0.081(6) 0.047(4) 0.093(6) 0.000(4) -0.039(5) -0.005(4) C64 0.067(5) 0.090(6) 0.069(5) -0.002(5) -0.020(4) -0.035(5) C65 0.139(9) 0.056(5) 0.052(5) -0.004(4) -0.043(6) -0.029(6) C66 0.125(9) 0.078(7) 0.057(5) -0.026(5) -0.053(6) 0.026(6) C67 0.069(5) 0.130(8) 0.037(4) -0.017(5) -0.020(4) -0.019(6) _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 Sb1 O6 1.934(3) . ? Sb1 O1 1.978(3) . ? Sb1 O2 1.986(3) . ? O1 C1 1.381(6) . ? C1 C2 1.394(7) . ? C1 C6 1.397(7) . ? O2 C17 1.386(6) . ? C2 C3 1.400(7) . ? C2 C55 1.505(7) . ? Sb2 O6 1.942(3) . ? Sb2 O4 1.979(3) . ? Sb2 O3 2.024(3) . ? O3 C28 1.377(5) . ? C3 C4 1.391(7) . ? C3 H3A 0.9400 . ? O4 C39 1.368(6) . ? C4 C5 1.400(7) . ? C4 C7 1.543(8) . ? O5 C50 1.379(6) . ? O5 H5A 0.8300 . ? C5 C6 1.400(7) . ? C5 H5B 0.9400 . ? C6 C11 1.517(7) . ? C7 C10A 1.460(12) . ? C7 C8 1.460(11) . ? C7 C8A 1.517(11) . ? C7 C9 1.519(10) . ? C7 C10 1.536(10) . ? C7 C9A 1.543(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C8A H8AC 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C10A H10D 0.9700 . ? C10A H10E 0.9700 . ? C10A H10F 0.9700 . ? C11 C12 1.503(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.382(7) . ? C12 C17 1.411(7) . ? C13 C14 1.391(7) . ? C13 H13A 0.9400 . ? C14 C15 1.402(7) . ? C14 C18 1.535(7) . ? C15 C16 1.391(7) . ? C15 H15A 0.9400 . ? C16 C17 1.386(7) . ? C16 C22 1.512(7) . ? C18 C20A 1.487(9) . ? C18 C21 1.493(11) . ? C18 C19 1.523(11) . ? C18 C21A 1.534(9) . ? C18 C20 1.545(11) . ? C18 C19A 1.546(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C19A H19D 0.9700 . ? C19A H19E 0.9700 . ? C19A H19F 0.9700 . ? C20A H20D 0.9700 . ? C20A H20E 0.9700 . ? C20A H20F 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22 C23 1.514(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.397(7) . ? C23 C28 1.408(7) . ? C24 C25 1.396(7) . ? C24 H24A 0.9400 . ? C25 C26 1.383(7) . ? C25 C29 1.525(7) . ? C26 C27 1.416(7) . ? C26 H26A 0.9400 . ? C27 C28 1.401(7) . ? C27 C33 1.506(7) . ? C29 C31 1.510(9) . ? C29 C30 1.513(9) . ? C29 C32 1.522(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.522(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.375(7) . ? C34 C39 1.403(7) . ? C35 C36 1.393(7) . ? C35 H35A 0.9400 . ? C36 C37 1.400(7) . ? C36 C40 1.529(7) . ? C37 C38 1.379(7) . ? C37 H37A 0.9400 . ? C38 C39 1.398(7) . ? C38 C44 1.524(7) . ? C40 C41 1.519(8) . ? C40 C42 1.521(8) . ? C40 C43 1.533(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 C45 1.503(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.387(7) . ? C45 C50 1.401(7) . ? C46 C47 1.403(7) . ? C46 H46A 0.9400 . ? C47 C48 1.393(7) . ? C47 C51 1.524(7) . ? C48 C49 1.386(7) . ? C48 H48A 0.9400 . ? C49 C50 1.389(7) . ? C49 C55 1.530(7) . ? C51 C52 1.527(7) . ? C51 C54 1.531(8) . ? C51 C53 1.539(8) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.345(11) . ? C56 C61 1.419(12) . ? C56 H56A 0.9400 . ? C57 C58 1.329(13) . ? C57 H57A 0.9400 . ? C58 C59 1.415(15) . ? C58 H58A 0.9400 . ? C59 C60 1.423(15) . ? C59 H59A 0.9400 . ? C60 C61 1.376(13) . ? C60 H60A 0.9400 . ? C61 H61A 0.9400 . ? C62 C67 1.326(11) . ? C62 C63 1.376(11) . ? C62 H62A 0.9400 . ? C63 C64 1.364(10) . ? C63 H63A 0.9400 . ? C64 C65 1.362(11) . ? C64 H64A 0.9400 . ? C65 C66 1.322(12) . ? C65 H65A 0.9400 . ? C66 C67 1.358(11) . ? C66 H66A 0.9400 . ? C67 H67A 0.9400 . ? C68 C69 1.300(13) . ? C68 C73 1.439(14) . ? C68 H68A 0.9400 . ? C69 C70 1.247(12) . ? C69 H69A 0.9400 . ? C70 C71 1.333(13) . ? C70 H70A 0.9400 . ? C71 C72 1.376(13) . ? C71 H71A 0.9400 . ? C72 C73 1.381(12) . ? C72 H72A 0.9400 . ? C73 H73A 0.9400 . ? 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 O6 Sb1 O1 97.41(14) . . ? O6 Sb1 O2 89.61(14) . . ? O1 Sb1 O2 92.78(13) . . ? C1 O1 Sb1 125.7(3) . . ? O1 C1 C2 118.0(5) . . ? O1 C1 C6 120.7(5) . . ? C2 C1 C6 121.0(5) . . ? C17 O2 Sb1 115.9(3) . . ? C1 C2 C3 118.1(5) . . ? C1 C2 C55 120.8(5) . . ? C3 C2 C55 121.1(5) . . ? O6 Sb2 O4 91.49(13) . . ? O6 Sb2 O3 94.68(13) . . ? O4 Sb2 O3 95.06(13) . . ? C28 O3 Sb2 123.1(3) . . ? C4 C3 C2 123.0(5) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C39 O4 Sb2 123.9(3) . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C7 120.8(5) . . ? C5 C4 C7 122.0(5) . . ? C50 O5 H5A 109.5 . . ? C6 C5 C4 121.9(5) . . ? C6 C5 H5B 119.0 . . ? C4 C5 H5B 119.0 . . ? C1 C6 C5 118.9(5) . . ? C1 C6 C11 121.4(5) . . ? C5 C6 C11 119.0(5) . . ? C10A C7 C8 129.4(12) . . ? C10A C7 C8A 112.5(9) . . ? C8 C7 C8A 34.8(8) . . ? C10A C7 C9 65.4(8) . . ? C8 C7 C9 111.4(8) . . ? C8A C7 C9 138.0(9) . . ? C10A C7 C10 39.9(8) . . ? C8 C7 C10 110.1(8) . . ? C8A C7 C10 79.8(8) . . ? C9 C7 C10 104.9(7) . . ? C10A C7 C9A 108.8(9) . . ? C8 C7 C9A 70.3(8) . . ? C8A C7 C9A 104.6(8) . . ? C9 C7 C9A 47.1(7) . . ? C10 C7 C9A 141.9(10) . . ? C10A C7 C4 114.6(10) . . ? C8 C7 C4 113.9(9) . . ? C8A C7 C4 109.8(8) . . ? C9 C7 C4 108.2(7) . . ? C10 C7 C4 108.0(7) . . ? C9A C7 C4 105.9(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8A H8AA 109.5 . . ? C7 C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7 C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7 C9A H9AA 109.5 . . ? C7 C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C7 C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C7 C10A H10D 109.5 . . ? C7 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C7 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? Sb1 O6 Sb2 134.85(18) . . ? C12 C11 C6 122.2(4) . . ? C12 C11 H11A 106.8 . . ? C6 C11 H11A 106.8 . . ? C12 C11 H11B 106.8 . . ? C6 C11 H11B 106.8 . . ? H11A C11 H11B 106.6 . . ? C13 C12 C17 117.9(5) . . ? C13 C12 C11 118.6(5) . . ? C17 C12 C11 123.3(5) . . ? C12 C13 C14 122.9(5) . . ? C12 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? C13 C14 C15 117.3(5) . . ? C13 C14 C18 121.5(5) . . ? C15 C14 C18 121.2(5) . . ? C16 C15 C14 121.9(5) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C17 C16 C15 118.7(5) . . ? C17 C16 C22 118.2(4) . . ? C15 C16 C22 122.8(4) . . ? O2 C17 C16 118.3(4) . . ? O2 C17 C12 120.4(4) . . ? C16 C17 C12 121.2(5) . . ? C20A C18 C21 139.1(10) . . ? C20A C18 C19 64.5(7) . . ? C21 C18 C19 110.2(8) . . ? C20A C18 C21A 110.7(6) . . ? C21 C18 C21A 44.5(7) . . ? C19 C18 C21A 138.6(9) . . ? C20A C18 C14 111.2(6) . . ? C21 C18 C14 108.1(9) . . ? C19 C18 C14 112.2(8) . . ? C21A C18 C14 107.6(6) . . ? C20A C18 C20 44.8(6) . . ? C21 C18 C20 109.0(8) . . ? C19 C18 C20 105.7(8) . . ? C21A C18 C20 68.2(7) . . ? C14 C18 C20 111.7(8) . . ? C20A C18 C19A 108.7(6) . . ? C21 C18 C19A 64.8(7) . . ? C19 C18 C19A 48.0(6) . . ? C21A C18 C19A 106.0(6) . . ? C14 C18 C19A 112.5(6) . . ? C20 C18 C19A 134.9(9) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21A H21D 109.5 . . ? C18 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C18 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C16 C22 C23 111.6(4) . . ? C16 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C16 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C28 118.4(4) . . ? C24 C23 C22 119.4(5) . . ? C28 C23 C22 122.2(4) . . ? C25 C24 C23 122.6(5) . . ? C25 C24 H24A 118.7 . . ? C23 C24 H24A 118.7 . . ? C26 C25 C24 117.5(5) . . ? C26 C25 C29 122.4(5) . . ? C24 C25 C29 120.0(5) . . ? C25 C26 C27 122.5(5) . . ? C25 C26 H26A 118.7 . . ? C27 C26 H26A 118.7 . . ? C28 C27 C26 118.0(5) . . ? C28 C27 C33 121.7(4) . . ? C26 C27 C33 120.0(4) . . ? O3 C28 C27 119.2(4) . . ? O3 C28 C23 119.9(4) . . ? C27 C28 C23 120.8(4) . . ? C31 C29 C30 110.6(7) . . ? C31 C29 C32 107.0(5) . . ? C30 C29 C32 107.0(6) . . ? C31 C29 C25 109.7(5) . . ? C30 C29 C25 110.0(5) . . ? C32 C29 C25 112.5(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 C34 117.5(4) . . ? C27 C33 H33A 107.9 . . ? C34 C33 H33A 107.9 . . ? C27 C33 H33B 107.9 . . ? C34 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? C35 C34 C39 118.3(5) . . ? C35 C34 C33 121.4(4) . . ? C39 C34 C33 120.3(4) . . ? C34 C35 C36 123.9(5) . . ? C34 C35 H35A 118.0 . . ? C36 C35 H35A 118.0 . . ? C35 C36 C37 115.7(5) . . ? C35 C36 C40 124.0(5) . . ? C37 C36 C40 120.3(5) . . ? C38 C37 C36 123.0(5) . . ? C38 C37 H37A 118.5 . . ? C36 C37 H37A 118.5 . . ? C37 C38 C39 118.9(4) . . ? C37 C38 C44 121.3(5) . . ? C39 C38 C44 119.7(4) . . ? O4 C39 C38 119.3(4) . . ? O4 C39 C34 120.3(4) . . ? C38 C39 C34 120.2(5) . . ? C41 C40 C42 107.7(5) . . ? C41 C40 C36 111.6(5) . . ? C42 C40 C36 110.2(5) . . ? C41 C40 C43 107.7(5) . . ? C42 C40 C43 109.5(5) . . ? C36 C40 C43 110.1(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C38 117.0(4) . . ? C45 C44 H44A 108.0 . . ? C38 C44 H44A 108.0 . . ? C45 C44 H44B 108.0 . . ? C38 C44 H44B 108.0 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C50 118.2(5) . . ? C46 C45 C44 120.3(5) . . ? C50 C45 C44 121.5(4) . . ? C45 C46 C47 122.7(5) . . ? C45 C46 H46A 118.7 . . ? C47 C46 H46A 118.7 . . ? C48 C47 C46 116.6(5) . . ? C48 C47 C51 123.1(5) . . ? C46 C47 C51 120.2(5) . . ? C49 C48 C47 122.7(5) . . ? C49 C48 H48A 118.7 . . ? C47 C48 H48A 118.7 . . ? C48 C49 C50 118.8(5) . . ? C48 C49 C55 120.6(5) . . ? C50 C49 C55 120.6(5) . . ? O5 C50 C49 117.9(4) . . ? O5 C50 C45 121.1(4) . . ? C49 C50 C45 121.0(5) . . ? C47 C51 C52 109.9(4) . . ? C47 C51 C54 112.0(5) . . ? C52 C51 C54 107.5(5) . . ? C47 C51 C53 110.1(5) . . ? C52 C51 C53 110.4(5) . . ? C54 C51 C53 106.8(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C2 C55 C49 114.0(4) . . ? C2 C55 H55A 108.8 . . ? C49 C55 H55A 108.8 . . ? C2 C55 H55B 108.8 . . ? C49 C55 H55B 108.8 . . ? H55A C55 H55B 107.6 . . ? C57 C56 C61 122.0(9) . . ? C57 C56 H56A 119.0 . . ? C61 C56 H56A 119.0 . . ? C58 C57 C56 120.1(10) . . ? C58 C57 H57A 119.9 . . ? C56 C57 H57A 119.9 . . ? C57 C58 C59 121.2(10) . . ? C57 C58 H58A 119.4 . . ? C59 C58 H58A 119.4 . . ? C58 C59 C60 119.0(11) . . ? C58 C59 H59A 120.5 . . ? C60 C59 H59A 120.5 . . ? C61 C60 C59 118.4(12) . . ? C61 C60 H60A 120.8 . . ? C59 C60 H60A 120.8 . . ? C60 C61 C56 118.9(10) . . ? C60 C61 H61A 120.5 . . ? C56 C61 H61A 120.5 . . ? C67 C62 C63 121.7(8) . . ? C67 C62 H62A 119.2 . . ? C63 C62 H62A 119.2 . . ? C64 C63 C62 118.1(7) . . ? C64 C63 H63A 120.9 . . ? C62 C63 H63A 120.9 . . ? C65 C64 C63 119.9(8) . . ? C65 C64 H64A 120.1 . . ? C63 C64 H64A 120.1 . . ? C66 C65 C64 119.9(8) . . ? C66 C65 H65A 120.1 . . ? C64 C65 H65A 120.1 . . ? C65 C66 C67 121.8(8) . . ? C65 C66 H66A 119.1 . . ? C67 C66 H66A 119.1 . . ? C62 C67 C66 118.6(8) . . ? C62 C67 H67A 120.7 . . ? C66 C67 H67A 120.7 . . ? C69 C68 C73 118.1(12) . . ? C69 C68 H68A 120.9 . . ? C73 C68 H68A 120.9 . . ? C70 C69 C68 124.3(14) . . ? C70 C69 H69A 117.8 . . ? C68 C69 H69A 117.8 . . ? C69 C70 C71 122.9(13) . . ? C69 C70 H70A 118.6 . . ? C71 C70 H70A 118.6 . . ? C70 C71 C72 118.4(12) . . ? C70 C71 H71A 120.8 . . ? C72 C71 H71A 120.8 . . ? C71 C72 C73 119.6(12) . . ? C71 C72 H72A 120.2 . . ? C73 C72 H72A 120.2 . . ? C72 C73 C68 116.5(12) . . ? C72 C73 H73A 121.7 . . ? C68 C73 H73A 121.7 . . ? 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 O6 Sb1 O1 C1 80.9(4) . . . . ? O2 Sb1 O1 C1 -9.1(4) . . . . ? Sb1 O1 C1 C2 -122.5(4) . . . . ? Sb1 O1 C1 C6 64.8(6) . . . . ? O6 Sb1 O2 C17 161.6(3) . . . . ? O1 Sb1 O2 C17 -101.0(3) . . . . ? O1 C1 C2 C3 -173.6(4) . . . . ? C6 C1 C2 C3 -1.0(8) . . . . ? O1 C1 C2 C55 3.8(7) . . . . ? C6 C1 C2 C55 176.4(5) . . . . ? O6 Sb2 O3 C28 -5.4(3) . . . . ? O4 Sb2 O3 C28 86.5(3) . . . . ? C1 C2 C3 C4 -2.0(8) . . . . ? C55 C2 C3 C4 -179.4(5) . . . . ? O6 Sb2 O4 C39 7.5(3) . . . . ? O3 Sb2 O4 C39 -87.3(3) . . . . ? C2 C3 C4 C5 2.5(8) . . . . ? C2 C3 C4 C7 177.3(5) . . . . ? C3 C4 C5 C6 -0.1(8) . . . . ? C7 C4 C5 C6 -174.8(5) . . . . ? O1 C1 C6 C5 175.7(4) . . . . ? C2 C1 C6 C5 3.3(7) . . . . ? O1 C1 C6 C11 5.6(7) . . . . ? C2 C1 C6 C11 -166.8(5) . . . . ? C4 C5 C6 C1 -2.8(8) . . . . ? C4 C5 C6 C11 167.6(5) . . . . ? C3 C4 C7 C10A 12.1(12) . . . . ? C5 C4 C7 C10A -173.3(10) . . . . ? C3 C4 C7 C8 177.1(9) . . . . ? C5 C4 C7 C8 -8.3(11) . . . . ? C3 C4 C7 C8A 139.8(9) . . . . ? C5 C4 C7 C8A -45.7(10) . . . . ? C3 C4 C7 C9 -58.5(9) . . . . ? C5 C4 C7 C9 116.0(8) . . . . ? C3 C4 C7 C10 54.5(8) . . . . ? C5 C4 C7 C10 -131.0(7) . . . . ? C3 C4 C7 C9A -107.8(9) . . . . ? C5 C4 C7 C9A 66.7(10) . . . . ? O1 Sb1 O6 Sb2 -116.6(3) . . . . ? O2 Sb1 O6 Sb2 -23.8(3) . . . . ? O4 Sb2 O6 Sb1 -145.4(3) . . . . ? O3 Sb2 O6 Sb1 -50.2(3) . . . . ? C1 C6 C11 C12 -97.4(6) . . . . ? C5 C6 C11 C12 92.5(6) . . . . ? C6 C11 C12 C13 -144.4(5) . . . . ? C6 C11 C12 C17 41.9(8) . . . . ? C17 C12 C13 C14 1.3(8) . . . . ? C11 C12 C13 C14 -172.7(5) . . . . ? C12 C13 C14 C15 -2.3(8) . . . . ? C12 C13 C14 C18 174.4(5) . . . . ? C13 C14 C15 C16 1.5(8) . . . . ? C18 C14 C15 C16 -175.2(5) . . . . ? C14 C15 C16 C17 0.2(8) . . . . ? C14 C15 C16 C22 173.7(5) . . . . ? Sb1 O2 C17 C16 -102.7(4) . . . . ? Sb1 O2 C17 C12 74.4(5) . . . . ? C15 C16 C17 O2 175.9(4) . . . . ? C22 C16 C17 O2 2.1(7) . . . . ? C15 C16 C17 C12 -1.3(7) . . . . ? C22 C16 C17 C12 -175.1(4) . . . . ? C13 C12 C17 O2 -176.6(4) . . . . ? C11 C12 C17 O2 -2.9(8) . . . . ? C13 C12 C17 C16 0.5(7) . . . . ? C11 C12 C17 C16 174.2(5) . . . . ? C13 C14 C18 C20A 123.5(7) . . . . ? C15 C14 C18 C20A -60.0(8) . . . . ? C13 C14 C18 C21 -68.3(9) . . . . ? C15 C14 C18 C21 108.2(9) . . . . ? C13 C14 C18 C19 53.4(9) . . . . ? C15 C14 C18 C19 -130.0(8) . . . . ? C13 C14 C18 C21A -115.1(6) . . . . ? C15 C14 C18 C21A 61.4(7) . . . . ? C13 C14 C18 C20 171.9(8) . . . . ? C15 C14 C18 C20 -11.6(9) . . . . ? C13 C14 C18 C19A 1.2(8) . . . . ? C15 C14 C18 C19A 177.8(6) . . . . ? C17 C16 C22 C23 68.1(6) . . . . ? C15 C16 C22 C23 -105.4(5) . . . . ? C16 C22 C23 C24 49.2(6) . . . . ? C16 C22 C23 C28 -130.3(5) . . . . ? C28 C23 C24 C25 -0.7(7) . . . . ? C22 C23 C24 C25 179.8(4) . . . . ? C23 C24 C25 C26 -2.0(7) . . . . ? C23 C24 C25 C29 -179.1(5) . . . . ? C24 C25 C26 C27 2.0(7) . . . . ? C29 C25 C26 C27 179.2(4) . . . . ? C25 C26 C27 C28 0.5(7) . . . . ? C25 C26 C27 C33 -173.1(4) . . . . ? Sb2 O3 C28 C27 -75.5(5) . . . . ? Sb2 O3 C28 C23 107.7(4) . . . . ? C26 C27 C28 O3 179.8(4) . . . . ? C33 C27 C28 O3 -6.7(6) . . . . ? C26 C27 C28 C23 -3.3(6) . . . . ? C33 C27 C28 C23 170.2(4) . . . . ? C24 C23 C28 O3 -179.8(4) . . . . ? C22 C23 C28 O3 -0.3(7) . . . . ? C24 C23 C28 C27 3.4(7) . . . . ? C22 C23 C28 C27 -177.1(4) . . . . ? C26 C25 C29 C31 -106.7(7) . . . . ? C24 C25 C29 C31 70.4(7) . . . . ? C26 C25 C29 C30 131.5(7) . . . . ? C24 C25 C29 C30 -51.5(8) . . . . ? C26 C25 C29 C32 12.3(7) . . . . ? C24 C25 C29 C32 -170.7(5) . . . . ? C28 C27 C33 C34 101.1(5) . . . . ? C26 C27 C33 C34 -85.5(5) . . . . ? C27 C33 C34 C35 89.2(6) . . . . ? C27 C33 C34 C39 -94.0(6) . . . . ? C39 C34 C35 C36 -0.4(7) . . . . ? C33 C34 C35 C36 176.5(5) . . . . ? C34 C35 C36 C37 1.4(8) . . . . ? C34 C35 C36 C40 -178.0(5) . . . . ? C35 C36 C37 C38 -1.5(7) . . . . ? C40 C36 C37 C38 178.0(5) . . . . ? C36 C37 C38 C39 0.5(8) . . . . ? C36 C37 C38 C44 -175.8(5) . . . . ? Sb2 O4 C39 C38 -103.2(4) . . . . ? Sb2 O4 C39 C34 80.6(5) . . . . ? C37 C38 C39 O4 -175.6(4) . . . . ? C44 C38 C39 O4 0.7(7) . . . . ? C37 C38 C39 C34 0.6(7) . . . . ? C44 C38 C39 C34 176.9(4) . . . . ? C35 C34 C39 O4 175.5(4) . . . . ? C33 C34 C39 O4 -1.4(7) . . . . ? C35 C34 C39 C38 -0.7(7) . . . . ? C33 C34 C39 C38 -177.5(4) . . . . ? C35 C36 C40 C41 6.8(8) . . . . ? C37 C36 C40 C41 -172.5(5) . . . . ? C35 C36 C40 C42 126.4(6) . . . . ? C37 C36 C40 C42 -53.0(7) . . . . ? C35 C36 C40 C43 -112.7(6) . . . . ? C37 C36 C40 C43 67.9(7) . . . . ? C37 C38 C44 C45 -121.4(5) . . . . ? C39 C38 C44 C45 62.3(6) . . . . ? C38 C44 C45 C46 -126.2(5) . . . . ? C38 C44 C45 C50 55.2(6) . . . . ? C50 C45 C46 C47 0.2(7) . . . . ? C44 C45 C46 C47 -178.5(4) . . . . ? C45 C46 C47 C48 -2.5(7) . . . . ? C45 C46 C47 C51 178.4(5) . . . . ? C46 C47 C48 C49 2.5(7) . . . . ? C51 C47 C48 C49 -178.4(5) . . . . ? C47 C48 C49 C50 -0.2(7) . . . . ? C47 C48 C49 C55 179.4(5) . . . . ? C48 C49 C50 O5 178.1(4) . . . . ? C55 C49 C50 O5 -1.5(7) . . . . ? C48 C49 C50 C45 -2.2(7) . . . . ? C55 C49 C50 C45 178.2(4) . . . . ? C46 C45 C50 O5 -178.1(4) . . . . ? C44 C45 C50 O5 0.5(7) . . . . ? C46 C45 C50 C49 2.2(7) . . . . ? C44 C45 C50 C49 -179.1(4) . . . . ? C48 C47 C51 C52 -112.3(6) . . . . ? C46 C47 C51 C52 66.8(7) . . . . ? C48 C47 C51 C54 7.1(7) . . . . ? C46 C47 C51 C54 -173.8(5) . . . . ? C48 C47 C51 C53 125.8(6) . . . . ? C46 C47 C51 C53 -55.0(6) . . . . ? C1 C2 C55 C49 92.4(6) . . . . ? C3 C2 C55 C49 -90.2(6) . . . . ? C48 C49 C55 C2 46.0(6) . . . . ? C50 C49 C55 C2 -134.4(5) . . . . ? C61 C56 C57 C58 -2.7(15) . . . . ? C56 C57 C58 C59 5.7(18) . . . . ? C57 C58 C59 C60 -7(2) . . . . ? C58 C59 C60 C61 5(2) . . . . ? C59 C60 C61 C56 -2.1(17) . . . . ? C57 C56 C61 C60 0.9(15) . . . . ? C67 C62 C63 C64 1.3(13) . . . . ? C62 C63 C64 C65 -0.2(12) . . . . ? C63 C64 C65 C66 -0.7(12) . . . . ? C64 C65 C66 C67 0.5(13) . . . . ? C63 C62 C67 C66 -1.5(12) . . . . ? C65 C66 C67 C62 0.6(12) . . . . ? C73 C68 C69 C70 1.4(19) . . . . ? C68 C69 C70 C71 3(2) . . . . ? C69 C70 C71 C72 -5.2(18) . . . . ? C70 C71 C72 C73 2.9(17) . . . . ? C71 C72 C73 C68 1.1(16) . . . . ? C69 C68 C73 C72 -3.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.157 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.086 # Attachment 'CCDC-716842.CIF' data_tcu100m _database_code_depnum_ccdc_archive 'CCDC 716842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H78 O8 S2 Sb2, 1.5(C2H6SO)' _chemical_formula_sum 'C62 H87 O9.5 S3.5 Sb2' _chemical_formula_weight 1340.1 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' S S 0.1246 0.1234 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 29.948(4) _cell_length_b 29.948(4) _cell_length_c 31.765(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28489(9) _cell_formula_units_Z 16 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10080 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8402 _exptl_absorpt_correction_T_max 0.8965 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'not recorded' _diffrn_standards_number 'not recorded' _diffrn_standards_interval_count 'not recorded' _diffrn_standards_interval_time 'not recorded' _diffrn_standards_decay_% ? _diffrn_reflns_number 100086 _diffrn_reflns_av_R_equivalents 0.1260 _diffrn_reflns_av_sigmaI/netI 0.1538 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.28 _reflns_number_total 17255 _reflns_number_gt 6905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHEXLTL' _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. Most of the tert-butyl groups were positionally disordered. Disorder for the tert-butyl groups was due to 2-fold axis, and was modeled using partial occupancies and isotropic displacement parameters. PLATON/SQUEEZE estimated the solvent-accessible region void to occupy 7210 \%A^3^ and contain 1021 electrons. The electron density was modelled as 24 DMSO molecules (1.5 DMSO per assymetric unit) which accounts for 1008 electrons. The 1.5 DMSO molecules where added in the formula weight on the structure of assymetric unit. The big solvent accesible void of 1656 A-3 shown in the checkCIF report can be asssosiated with the use of squeeze indicating where solvent could be located. There is a residual peak of 5.73 eA-3 that was associated with the antimony atom. The adquisition of two more crystals of this compound shows the same problem and we were unable of getting a higher quality crystal. ; _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^)+(0.1872P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17255 _refine_ls_number_parameters 636 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1921 _refine_ls_R_factor_gt 0.1081 _refine_ls_wR_factor_ref 0.3185 _refine_ls_wR_factor_gt 0.2801 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 C1 C 0.5482(3) 0.8987(3) 0.1370(3) 0.045(2) Uani 1 1 d . . . O1 O 0.5553(2) 0.9175(2) 0.09710(19) 0.0489(17) Uani 1 1 d . . . Sb1 Sb 0.59969(2) 0.96587(2) 0.090089(19) 0.0426(2) Uani 1 1 d . . . S1 S 0.57452(17) 1.01243(17) -0.00790(15) 0.1134(15) Uani 1 1 d . . . Sb2 Sb 0.64391(2) 0.99925(2) 0.189792(19) 0.0445(2) Uani 1 1 d . . . C2 C 0.5689(3) 0.8568(3) 0.1459(3) 0.047(2) Uani 1 1 d . . . O2 O 0.5556(2) 1.0145(2) 0.10269(19) 0.0461(16) Uani 1 1 d . . . S2 S 0.65332(13) 0.92086(12) 0.27777(10) 0.0769(10) Uani 1 1 d . . . C3 C 0.5611(3) 0.8387(4) 0.1846(3) 0.052(3) Uani 1 1 d . . . H3A H 0.5745 0.8112 0.1909 0.062 Uiso 1 1 calc R . . O3 O 0.6583(2) 1.0433(2) 0.14325(19) 0.0456(16) Uani 1 1 d . . . C4 C 0.5352(3) 0.8578(3) 0.2145(3) 0.050(2) Uani 1 1 d . . . O4 O 0.7067(2) 0.9773(3) 0.1879(2) 0.0536(18) Uani 1 1 d . . . C5 C 0.5157(4) 0.8986(4) 0.2055(3) 0.053(3) Uani 1 1 d . . . H5B H 0.4982 0.9125 0.2262 0.064 Uiso 1 1 calc R . . O5 O 0.6651(2) 0.8645(2) 0.1673(2) 0.0532(18) Uani 1 1 d . . . H5A H 0.6583 0.8880 0.1795 0.080 Uiso 1 1 calc R . . C6 C 0.5214(3) 0.9200(3) 0.1663(3) 0.043(2) Uani 1 1 d . . . O6 O 0.6203(2) 0.9596(2) 0.1492(2) 0.0448(15) Uani 1 1 d . . . C7 C 0.5279(4) 0.8371(4) 0.2585(3) 0.061(3) Uani 1 1 d . . . O7 O 0.5544(3) 0.9739(3) 0.0226(2) 0.080(3) Uani 1 1 d . . . C8 C 0.5634(4) 0.8041(6) 0.2693(4) 0.096(5) Uani 1 1 d . . . H8A H 0.5657 0.7821 0.2470 0.145 Uiso 1 1 calc R . . H8B H 0.5560 0.7893 0.2955 0.145 Uiso 1 1 calc R . . H8C H 0.5918 0.8194 0.2723 0.145 Uiso 1 1 calc R . . O8 O 0.6415(3) 0.9291(2) 0.2326(2) 0.071(2) Uani 1 1 d . . . C9 C 0.4812(4) 0.8144(5) 0.2554(4) 0.082(4) Uani 1 1 d . . . H9A H 0.4817 0.7922 0.2331 0.123 Uiso 1 1 calc R . . H9B H 0.4588 0.8368 0.2490 0.123 Uiso 1 1 calc R . . H9C H 0.4741 0.8002 0.2819 0.123 Uiso 1 1 calc R . . C10 C 0.5255(7) 0.8720(6) 0.2940(4) 0.115(6) Uani 1 1 d . . . H10A H 0.5542 0.8867 0.2968 0.173 Uiso 1 1 calc R . . H10B H 0.5179 0.8573 0.3203 0.173 Uiso 1 1 calc R . . H10C H 0.5028 0.8940 0.2873 0.173 Uiso 1 1 calc R . . C11 C 0.4980(3) 0.9636(3) 0.1560(3) 0.049(2) Uani 1 1 d . . . H11A H 0.4941 0.9651 0.1254 0.059 Uiso 1 1 calc R . . H11B H 0.4682 0.9627 0.1687 0.059 Uiso 1 1 calc R . . C12 C 0.5204(3) 1.0057(3) 0.1700(3) 0.052(3) Uani 1 1 d . . . C13 C 0.5141(4) 1.0216(4) 0.2116(3) 0.059(3) Uani 1 1 d . . . H13A H 0.4981 1.0040 0.2309 0.071 Uiso 1 1 calc R . . C14 C 0.5306(4) 1.0618(4) 0.2245(3) 0.055(3) Uani 1 1 d . A . C15 C 0.5552(3) 1.0874(4) 0.1953(3) 0.057(3) Uani 1 1 d . . . H15A H 0.5663 1.1155 0.2034 0.068 Uiso 1 1 calc R . . C16 C 0.5631(3) 1.0722(3) 0.1549(3) 0.046(2) Uani 1 1 d . . . C17 C 0.5470(4) 1.0299(4) 0.1425(3) 0.054(3) Uani 1 1 d . . . C18 C 0.5236(4) 1.0807(4) 0.2687(4) 0.078(4) Uani 1 1 d D . . C19 C 0.5387(16) 1.0442(13) 0.2978(15) 0.18(3) Uiso 0.409(17) 1 d PD A 1 H19A H 0.5597 1.0250 0.2833 0.269 Uiso 0.409(17) 1 calc PR A 1 H19B H 0.5131 1.0267 0.3067 0.269 Uiso 0.409(17) 1 calc PR A 1 H19C H 0.5530 1.0572 0.3223 0.269 Uiso 0.409(17) 1 calc PR A 1 C20 C 0.4736(7) 1.0846(17) 0.2751(18) 0.17(2) Uiso 0.409(17) 1 d PD A 1 H20A H 0.4671 1.1113 0.2913 0.261 Uiso 0.409(17) 1 calc PR A 1 H20B H 0.4628 1.0586 0.2902 0.261 Uiso 0.409(17) 1 calc PR A 1 H20C H 0.4589 1.0864 0.2480 0.261 Uiso 0.409(17) 1 calc PR A 1 C21 C 0.5438(16) 1.1236(11) 0.2838(18) 0.20(3) Uiso 0.409(17) 1 d PD A 1 H21A H 0.5734 1.1177 0.2951 0.296 Uiso 0.409(17) 1 calc PR A 1 H21B H 0.5252 1.1364 0.3056 0.296 Uiso 0.409(17) 1 calc PR A 1 H21C H 0.5461 1.1443 0.2604 0.296 Uiso 0.409(17) 1 calc PR A 1 C19A C 0.4936(7) 1.0539(7) 0.2963(8) 0.094(8) Uiso 0.591(17) 1 d PD A 2 H19D H 0.5049 1.0236 0.2983 0.141 Uiso 0.591(17) 1 calc PR A 2 H19E H 0.4638 1.0535 0.2845 0.141 Uiso 0.591(17) 1 calc PR A 2 H19F H 0.4928 1.0671 0.3242 0.141 Uiso 0.591(17) 1 calc PR A 2 C20A C 0.5045(7) 1.1281(6) 0.2681(8) 0.096(8) Uiso 0.591(17) 1 d PD A 2 H20D H 0.4753 1.1278 0.2549 0.143 Uiso 0.591(17) 1 calc PR A 2 H20E H 0.5243 1.1474 0.2522 0.143 Uiso 0.591(17) 1 calc PR A 2 H20F H 0.5018 1.1391 0.2967 0.143 Uiso 0.591(17) 1 calc PR A 2 C21A C 0.5680(6) 1.0850(8) 0.2913(7) 0.093(8) Uiso 0.591(17) 1 d PD A 2 H21D H 0.5824 1.0560 0.2926 0.139 Uiso 0.591(17) 1 calc PR A 2 H21E H 0.5630 1.0960 0.3197 0.139 Uiso 0.591(17) 1 calc PR A 2 H21F H 0.5870 1.1057 0.2762 0.139 Uiso 0.591(17) 1 calc PR A 2 C22 C 0.5886(3) 1.1017(3) 0.1234(3) 0.052(3) Uani 1 1 d . . . H22A H 0.5701 1.1274 0.1156 0.062 Uiso 1 1 calc R . . H22B H 0.5948 1.0846 0.0978 0.062 Uiso 1 1 calc R . . C23 C 0.6330(3) 1.1185(3) 0.1424(3) 0.046(2) Uani 1 1 d . . . C24 C 0.6405(4) 1.1637(4) 0.1497(3) 0.058(3) Uani 1 1 d . . . H24A H 0.6177 1.1844 0.1436 0.070 Uiso 1 1 calc R . . C25 C 0.6802(5) 1.1789(4) 0.1656(3) 0.069(3) Uani 1 1 d . A . C26 C 0.7116(4) 1.1464(4) 0.1775(3) 0.062(3) Uani 1 1 d . . . H26A H 0.7382 1.1558 0.1904 0.074 Uiso 1 1 calc R . . C27 C 0.7051(4) 1.1009(3) 0.1709(3) 0.050(2) Uani 1 1 d . . . C28 C 0.6654(3) 1.0879(3) 0.1516(3) 0.047(2) Uani 1 1 d . . . C29 C 0.6906(5) 1.2280(4) 0.1734(4) 0.085(4) Uani 1 1 d D . . C30 C 0.7410(8) 1.2356(12) 0.1865(10) 0.091(12) Uiso 0.409(17) 1 d PD A 1 H30A H 0.7441 1.2316 0.2166 0.137 Uiso 0.409(17) 1 calc PR A 1 H30B H 0.7500 1.2656 0.1789 0.137 Uiso 0.409(17) 1 calc PR A 1 H30C H 0.7597 1.2142 0.1719 0.137 Uiso 0.409(17) 1 calc PR A 1 C31 C 0.6826(10) 1.2573(10) 0.1349(8) 0.086(11) Uiso 0.409(17) 1 d PD A 1 H31A H 0.6534 1.2507 0.1231 0.129 Uiso 0.409(17) 1 calc PR A 1 H31B H 0.7054 1.2514 0.1139 0.129 Uiso 0.409(17) 1 calc PR A 1 H31C H 0.6837 1.2885 0.1430 0.129 Uiso 0.409(17) 1 calc PR A 1 C32 C 0.6618(12) 1.2433(16) 0.2107(9) 0.17(2) Uiso 0.409(17) 1 d PD A 1 H32A H 0.6305 1.2403 0.2035 0.254 Uiso 0.409(17) 1 calc PR A 1 H32B H 0.6683 1.2743 0.2171 0.254 Uiso 0.409(17) 1 calc PR A 1 H32C H 0.6684 1.2251 0.2352 0.254 Uiso 0.409(17) 1 calc PR A 1 C30A C 0.7108(10) 1.2376(11) 0.2163(7) 0.129(12) Uiso 0.591(17) 1 d PD A 2 H30D H 0.6873 1.2386 0.2373 0.194 Uiso 0.591(17) 1 calc PR A 2 H30E H 0.7262 1.2660 0.2156 0.194 Uiso 0.591(17) 1 calc PR A 2 H30F H 0.7318 1.2141 0.2235 0.194 Uiso 0.591(17) 1 calc PR A 2 C31A C 0.7213(10) 1.2425(14) 0.1376(9) 0.192(19) Uiso 0.591(17) 1 d PD A 2 H31D H 0.7035 1.2507 0.1133 0.288 Uiso 0.591(17) 1 calc PR A 2 H31E H 0.7411 1.2181 0.1302 0.288 Uiso 0.591(17) 1 calc PR A 2 H31F H 0.7389 1.2681 0.1465 0.288 Uiso 0.591(17) 1 calc PR A 2 C32A C 0.6455(8) 1.2532(11) 0.1694(10) 0.151(14) Uiso 0.591(17) 1 d PD A 2 H32D H 0.6220 1.2322 0.1625 0.227 Uiso 0.591(17) 1 calc PR A 2 H32E H 0.6478 1.2755 0.1473 0.227 Uiso 0.591(17) 1 calc PR A 2 H32F H 0.6386 1.2678 0.1959 0.227 Uiso 0.591(17) 1 calc PR A 2 C33 C 0.7396(4) 1.0676(4) 0.1881(3) 0.056(3) Uani 1 1 d . . . H33A H 0.7656 1.0845 0.1982 0.067 Uiso 1 1 calc R . . H33B H 0.7266 1.0523 0.2124 0.067 Uiso 1 1 calc R . . C34 C 0.7552(3) 1.0336(4) 0.1580(3) 0.047(2) Uani 1 1 d . . . C35 C 0.7900(3) 1.0433(4) 0.1316(3) 0.056(3) Uani 1 1 d . . . H35A H 0.8003 1.0730 0.1303 0.068 Uiso 1 1 calc R . . C36 C 0.8114(4) 1.0112(4) 0.1062(3) 0.057(3) Uani 1 1 d . . . C37 C 0.7956(3) 0.9675(4) 0.1098(3) 0.058(3) Uani 1 1 d . . . H37A H 0.8097 0.9451 0.0940 0.069 Uiso 1 1 calc R . . C38 C 0.7602(3) 0.9556(4) 0.1354(3) 0.052(3) Uani 1 1 d . . . C39 C 0.7394(3) 0.9895(4) 0.1599(3) 0.052(3) Uani 1 1 d . . . C40 C 0.8516(4) 1.0238(5) 0.0788(4) 0.071(3) Uani 1 1 d . . . C41 C 0.8677(5) 0.9842(5) 0.0504(5) 0.096(5) Uani 1 1 d . . . H41A H 0.8438 0.9756 0.0314 0.144 Uiso 1 1 calc R . . H41B H 0.8756 0.9589 0.0680 0.144 Uiso 1 1 calc R . . H41C H 0.8935 0.9934 0.0342 0.144 Uiso 1 1 calc R . . C42 C 0.8405(5) 1.0636(5) 0.0515(5) 0.099(5) Uani 1 1 d . . . H42A H 0.8162 1.0559 0.0326 0.148 Uiso 1 1 calc R . . H42B H 0.8665 1.0720 0.0352 0.148 Uiso 1 1 calc R . . H42C H 0.8315 1.0884 0.0691 0.148 Uiso 1 1 calc R . . C43 C 0.8910(4) 1.0375(7) 0.1086(6) 0.117(6) Uani 1 1 d . . . H43A H 0.8985 1.0126 0.1268 0.175 Uiso 1 1 calc R . . H43B H 0.8820 1.0629 0.1256 0.175 Uiso 1 1 calc R . . H43C H 0.9168 1.0456 0.0918 0.175 Uiso 1 1 calc R . . C44 C 0.7460(4) 0.9094(4) 0.1390(4) 0.057(3) Uani 1 1 d . . . H44A H 0.7354 0.9045 0.1679 0.068 Uiso 1 1 calc R . . H44B H 0.7722 0.8903 0.1348 0.068 Uiso 1 1 calc R . . C45 C 0.7102(3) 0.8941(3) 0.1095(3) 0.047(2) Uani 1 1 d . . . C46 C 0.7150(3) 0.8990(3) 0.0677(3) 0.051(3) Uani 1 1 d . . . H46A H 0.7408 0.9135 0.0579 0.062 Uiso 1 1 calc R . . C47 C 0.6840(3) 0.8840(3) 0.0377(3) 0.045(2) Uani 1 1 d . . . C48 C 0.6441(4) 0.8637(3) 0.0542(3) 0.049(2) Uani 1 1 d . . . H48A H 0.6219 0.8542 0.0353 0.058 Uiso 1 1 calc R . . C49 C 0.6373(4) 0.8577(3) 0.0967(3) 0.048(2) Uani 1 1 d . . . C50 C 0.6705(4) 0.8728(3) 0.1239(3) 0.048(2) Uani 1 1 d . . . C51 C 0.6898(4) 0.8894(3) -0.0098(3) 0.050(2) Uani 1 1 d . . . C52 C 0.6927(6) 0.8438(4) -0.0297(4) 0.090(5) Uani 1 1 d . . . H52A H 0.7183 0.8279 -0.0185 0.136 Uiso 1 1 calc R . . H52B H 0.6960 0.8470 -0.0600 0.136 Uiso 1 1 calc R . . H52C H 0.6657 0.8271 -0.0236 0.136 Uiso 1 1 calc R . . C53 C 0.7329(6) 0.9138(6) -0.0216(4) 0.110(6) Uani 1 1 d . . . H53A H 0.7326 0.9436 -0.0095 0.165 Uiso 1 1 calc R . . H53B H 0.7351 0.9160 -0.0520 0.165 Uiso 1 1 calc R . . H53C H 0.7584 0.8974 -0.0107 0.165 Uiso 1 1 calc R . . C54 C 0.6499(5) 0.9143(5) -0.0279(4) 0.097(5) Uani 1 1 d . . . H54A H 0.6480 0.9436 -0.0152 0.146 Uiso 1 1 calc R . . H54B H 0.6228 0.8977 -0.0220 0.146 Uiso 1 1 calc R . . H54C H 0.6535 0.9173 -0.0581 0.146 Uiso 1 1 calc R . . C55 C 0.5959(4) 0.8328(3) 0.1108(3) 0.054(3) Uani 1 1 d . . . H55A H 0.6048 0.8033 0.1211 0.065 Uiso 1 1 calc R . . H55B H 0.5764 0.8284 0.0864 0.065 Uiso 1 1 calc R . . C56 C 0.5380(6) 1.0643(5) -0.0103(7) 0.151(9) Uani 1 1 d . . . H56A H 0.5429 1.0822 0.0148 0.227 Uiso 1 1 calc R . . H56B H 0.5069 1.0556 -0.0118 0.227 Uiso 1 1 calc R . . H56C H 0.5457 1.0817 -0.0350 0.227 Uiso 1 1 calc R . . C57 C 0.5516(10) 0.9919(11) -0.0579(5) 0.233(16) Uani 1 1 d . . . H57A H 0.5655 0.9636 -0.0650 0.350 Uiso 1 1 calc R . . H57B H 0.5577 1.0135 -0.0800 0.350 Uiso 1 1 calc R . . H57C H 0.5196 0.9879 -0.0552 0.350 Uiso 1 1 calc R . . C58 C 0.6215(7) 0.9628(5) 0.3058(5) 0.115(6) Uani 1 1 d . . . H58A H 0.5899 0.9556 0.3041 0.172 Uiso 1 1 calc R . . H58B H 0.6267 0.9918 0.2932 0.172 Uiso 1 1 calc R . . H58C H 0.6307 0.9633 0.3351 0.172 Uiso 1 1 calc R . . C59 C 0.7074(6) 0.9483(7) 0.2890(6) 0.131(7) Uani 1 1 d . . . H59A H 0.7314 0.9311 0.2765 0.197 Uiso 1 1 calc R . . H59B H 0.7118 0.9501 0.3192 0.197 Uiso 1 1 calc R . . H59C H 0.7074 0.9782 0.2771 0.197 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 C1 0.042(5) 0.053(6) 0.039(5) -0.001(4) 0.005(4) -0.011(5) O1 0.056(4) 0.053(4) 0.038(4) 0.012(3) 0.002(3) -0.014(3) Sb1 0.0425(4) 0.0484(4) 0.0368(3) 0.0061(3) 0.0016(3) 0.0003(3) S1 0.125(4) 0.125(4) 0.090(3) 0.009(3) -0.002(3) -0.003(3) Sb2 0.0484(4) 0.0513(4) 0.0338(3) 0.0057(3) 0.0006(3) 0.0047(3) C2 0.052(6) 0.047(6) 0.042(5) 0.004(4) 0.003(4) -0.007(5) O2 0.038(4) 0.065(4) 0.036(3) 0.012(3) -0.003(3) 0.005(3) S2 0.097(3) 0.086(2) 0.0478(17) 0.0252(16) 0.0028(16) 0.0144(19) C3 0.046(6) 0.053(6) 0.057(6) 0.003(5) 0.007(5) -0.001(5) O3 0.049(4) 0.054(4) 0.034(3) -0.002(3) -0.004(3) 0.007(3) C4 0.056(6) 0.045(6) 0.050(6) 0.006(5) 0.003(5) -0.015(5) O4 0.041(4) 0.084(5) 0.036(4) 0.009(3) 0.002(3) 0.009(4) C5 0.054(6) 0.063(7) 0.042(6) 0.006(5) 0.006(5) 0.007(5) O5 0.072(5) 0.054(4) 0.033(4) 0.008(3) 0.000(3) 0.014(4) C6 0.033(5) 0.048(6) 0.048(6) 0.004(4) 0.005(4) -0.002(4) O6 0.049(4) 0.045(4) 0.041(4) 0.010(3) -0.005(3) 0.000(3) C7 0.064(7) 0.073(8) 0.048(6) 0.020(6) -0.001(5) -0.009(6) O7 0.062(5) 0.129(8) 0.048(5) 0.019(5) 0.001(4) -0.015(5) C8 0.075(9) 0.153(14) 0.061(8) 0.057(9) 0.027(7) 0.027(9) O8 0.114(7) 0.057(5) 0.043(4) 0.009(3) 0.006(4) 0.019(5) C9 0.063(8) 0.098(10) 0.084(9) 0.045(8) -0.005(7) -0.010(7) C10 0.186(18) 0.118(13) 0.042(7) -0.006(8) -0.008(9) 0.011(12) C11 0.038(5) 0.059(6) 0.049(6) 0.002(5) 0.002(4) 0.003(5) C12 0.053(6) 0.046(6) 0.057(6) 0.004(5) 0.011(5) 0.008(5) C13 0.057(7) 0.077(8) 0.044(6) 0.009(5) 0.017(5) -0.007(6) C14 0.061(7) 0.056(7) 0.048(6) 0.006(5) 0.017(5) 0.006(5) C15 0.052(6) 0.051(6) 0.067(7) -0.004(5) 0.026(5) 0.005(5) C16 0.052(6) 0.049(6) 0.038(5) 0.012(4) 0.003(4) 0.005(5) C17 0.054(6) 0.065(7) 0.044(6) 0.011(5) 0.001(5) 0.019(5) C18 0.066(8) 0.098(10) 0.068(8) -0.015(7) 0.013(6) 0.014(7) C22 0.057(6) 0.039(5) 0.060(7) 0.012(5) 0.001(5) 0.020(5) C23 0.050(6) 0.047(6) 0.042(5) -0.001(4) 0.003(4) -0.002(5) C24 0.079(8) 0.055(7) 0.041(6) 0.009(5) 0.013(5) 0.016(6) C25 0.112(11) 0.056(7) 0.041(6) -0.006(5) 0.000(7) -0.012(7) C26 0.070(8) 0.071(8) 0.044(6) -0.011(5) -0.002(5) -0.021(6) C27 0.060(7) 0.050(6) 0.038(5) -0.006(4) 0.003(5) 0.000(5) C28 0.052(6) 0.054(6) 0.035(5) 0.000(4) 0.007(4) 0.007(5) C29 0.127(13) 0.063(8) 0.067(8) -0.001(7) -0.007(8) -0.007(8) C33 0.062(7) 0.074(7) 0.031(5) -0.004(5) -0.008(5) 0.001(6) C34 0.047(6) 0.058(6) 0.035(5) 0.003(4) -0.012(4) 0.007(5) C35 0.047(6) 0.072(7) 0.051(6) 0.005(5) -0.008(5) -0.005(5) C36 0.046(6) 0.080(8) 0.044(6) 0.012(6) -0.002(5) 0.002(6) C37 0.043(6) 0.089(9) 0.040(6) -0.004(5) -0.001(5) 0.003(6) C38 0.034(5) 0.072(7) 0.050(6) 0.002(5) -0.011(5) 0.001(5) C39 0.038(5) 0.080(8) 0.039(5) 0.001(5) -0.013(4) 0.019(5) C40 0.055(7) 0.087(9) 0.071(8) 0.012(7) 0.008(6) -0.001(7) C41 0.096(11) 0.113(12) 0.078(10) 0.011(9) 0.024(8) 0.028(9) C42 0.108(12) 0.100(11) 0.088(11) 0.021(9) 0.019(9) 0.001(9) C43 0.046(8) 0.186(19) 0.119(14) 0.010(13) 0.004(8) 0.012(10) C44 0.053(6) 0.057(7) 0.059(7) 0.004(5) -0.006(5) 0.016(5) C45 0.047(6) 0.050(6) 0.045(6) 0.004(5) 0.004(5) 0.004(5) C46 0.048(6) 0.045(6) 0.062(7) 0.010(5) -0.003(5) -0.009(5) C47 0.054(6) 0.036(5) 0.044(5) 0.003(4) 0.005(5) -0.003(4) C48 0.061(6) 0.044(6) 0.041(6) -0.001(4) 0.004(5) -0.001(5) C49 0.061(7) 0.036(5) 0.048(6) 0.004(4) 0.013(5) 0.013(5) C50 0.064(7) 0.039(5) 0.041(5) 0.006(4) -0.005(5) 0.008(5) C51 0.060(6) 0.049(6) 0.040(5) 0.010(4) -0.002(5) 0.006(5) C52 0.157(14) 0.068(8) 0.046(7) -0.005(6) 0.036(8) 0.012(9) C53 0.138(14) 0.152(15) 0.042(7) 0.012(8) -0.002(8) -0.056(12) C54 0.114(12) 0.113(12) 0.065(9) 0.032(8) -0.025(8) 0.006(10) C55 0.067(7) 0.047(6) 0.049(6) 0.001(5) 0.008(5) 0.000(5) C56 0.153(17) 0.080(11) 0.22(2) -0.025(13) 0.125(17) -0.025(11) C57 0.28(3) 0.38(4) 0.042(10) 0.034(16) 0.001(14) 0.13(3) C58 0.191(18) 0.091(11) 0.063(9) 0.011(8) 0.033(10) 0.015(11) C59 0.109(13) 0.19(2) 0.093(12) 0.027(13) -0.022(10) -0.012(13) _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 C1 C6 1.384(13) . ? C1 O1 1.402(11) . ? C1 C2 1.428(14) . ? O1 Sb1 1.980(6) . ? Sb1 O6 1.986(6) . ? Sb1 O2 2.006(6) . ? Sb1 O7 2.548(8) . ? S1 O7 1.622(9) . ? S1 C57 1.84(2) . ? S1 C56 1.901(18) . ? Sb2 O6 1.890(6) . ? Sb2 O4 1.992(6) . ? Sb2 O3 2.027(6) . ? Sb2 O8 2.503(7) . ? C2 C3 1.365(13) . ? C2 C55 1.553(14) . ? O2 C17 1.371(12) . ? S2 O8 1.499(8) . ? S2 C58 1.811(16) . ? S2 C59 1.852(18) . ? C3 C4 1.352(14) . ? C3 H3A 0.9400 . ? O3 C28 1.380(12) . ? C4 C5 1.383(14) . ? C4 C7 1.546(14) . ? O4 C39 1.372(12) . ? C5 C6 1.411(13) . ? C5 H5B 0.9400 . ? O5 C50 1.411(11) . ? O5 H5A 0.8300 . ? C6 C11 1.515(13) . ? C7 C8 1.492(17) . ? C7 C10 1.538(18) . ? C7 C9 1.557(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.494(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C17 1.388(14) . ? C12 C13 1.418(14) . ? C13 C14 1.364(15) . ? C13 H13A 0.9400 . ? C14 C15 1.410(14) . ? C14 C18 1.530(16) . ? C15 C16 1.383(14) . ? C15 H15A 0.9400 . ? C16 C17 1.411(15) . ? C16 C22 1.539(13) . ? C18 C19A 1.489(16) . ? C18 C21 1.499(19) . ? C18 C19 1.502(19) . ? C18 C20 1.514(19) . ? C18 C21A 1.518(17) . ? C18 C20A 1.529(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C19A H19D 0.9700 . ? C19A H19E 0.9700 . ? C19A H19F 0.9700 . ? C20A H20D 0.9700 . ? C20A H20E 0.9700 . ? C20A H20F 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22 C23 1.545(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C28 1.364(14) . ? C23 C24 1.394(14) . ? C24 C25 1.369(17) . ? C24 H24A 0.9400 . ? C25 C26 1.406(17) . ? C25 C29 1.524(17) . ? C26 C27 1.390(15) . ? C26 H26A 0.9400 . ? C27 C28 1.394(14) . ? C27 C33 1.536(14) . ? C29 C30A 1.516(18) . ? C29 C31 1.527(18) . ? C29 C31A 1.527(19) . ? C29 C32 1.537(19) . ? C29 C32A 1.554(18) . ? C29 C30 1.580(18) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C30A H30D 0.9700 . ? C30A H30E 0.9700 . ? C30A H30F 0.9700 . ? C31A H31D 0.9700 . ? C31A H31E 0.9700 . ? C31A H31F 0.9700 . ? C32A H32D 0.9700 . ? C32A H32E 0.9700 . ? C32A H32F 0.9700 . ? C33 C34 1.473(14) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.370(14) . ? C34 C39 1.407(15) . ? C35 C36 1.409(15) . ? C35 H35A 0.9400 . ? C36 C37 1.394(16) . ? C36 C40 1.534(16) . ? C37 C38 1.383(14) . ? C37 H37A 0.9400 . ? C38 C39 1.422(14) . ? C38 C44 1.452(15) . ? C40 C42 1.512(19) . ? C40 C43 1.56(2) . ? C40 C41 1.568(19) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 C45 1.495(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.345(14) . ? C45 C50 1.424(14) . ? C46 C47 1.403(13) . ? C46 H46A 0.9400 . ? C47 C48 1.440(13) . ? C47 C51 1.526(13) . ? C48 C49 1.378(13) . ? C48 H48A 0.9400 . ? C49 C50 1.393(14) . ? C49 C55 1.512(14) . ? C51 C52 1.507(15) . ? C51 C54 1.523(16) . ? C51 C53 1.531(17) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C57 H57C 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C59 H59C 0.9700 . ? 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 C6 C1 O1 120.7(9) . . ? C6 C1 C2 121.6(9) . . ? O1 C1 C2 117.7(8) . . ? C1 O1 Sb1 119.8(5) . . ? O1 Sb1 O6 91.9(3) . . ? O1 Sb1 O2 93.8(3) . . ? O6 Sb1 O2 94.8(3) . . ? O1 Sb1 O7 78.8(3) . . ? O6 Sb1 O7 165.9(3) . . ? O2 Sb1 O7 75.5(3) . . ? O7 S1 C57 98.1(11) . . ? O7 S1 C56 113.0(6) . . ? C57 S1 C56 91.4(12) . . ? O6 Sb2 O4 97.2(3) . . ? O6 Sb2 O3 89.5(3) . . ? O4 Sb2 O3 89.6(3) . . ? O6 Sb2 O8 80.3(3) . . ? O4 Sb2 O8 76.6(3) . . ? O3 Sb2 O8 161.5(3) . . ? C3 C2 C1 116.9(9) . . ? C3 C2 C55 123.5(9) . . ? C1 C2 C55 119.4(8) . . ? C17 O2 Sb1 123.4(5) . . ? O8 S2 C58 103.4(6) . . ? O8 S2 C59 108.5(7) . . ? C58 S2 C59 93.4(10) . . ? C4 C3 C2 124.3(10) . . ? C4 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C28 O3 Sb2 121.5(5) . . ? C3 C4 C5 118.0(9) . . ? C3 C4 C7 123.1(10) . . ? C5 C4 C7 118.8(10) . . ? C39 O4 Sb2 127.3(6) . . ? C4 C5 C6 122.3(9) . . ? C4 C5 H5B 118.9 . . ? C6 C5 H5B 118.9 . . ? C50 O5 H5A 109.5 . . ? C1 C6 C5 117.0(9) . . ? C1 C6 C11 121.3(9) . . ? C5 C6 C11 121.7(9) . . ? Sb2 O6 Sb1 134.5(3) . . ? C8 C7 C10 108.4(11) . . ? C8 C7 C4 111.8(10) . . ? C10 C7 C4 113.4(10) . . ? C8 C7 C9 111.5(11) . . ? C10 C7 C9 107.5(12) . . ? C4 C7 C9 104.1(9) . . ? S1 O7 Sb1 111.9(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S2 O8 Sb2 130.7(5) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C6 117.1(8) . . ? C12 C11 H11A 108.0 . . ? C6 C11 H11A 108.0 . . ? C12 C11 H11B 108.0 . . ? C6 C11 H11B 108.0 . . ? H11A C11 H11B 107.3 . . ? C17 C12 C13 119.1(10) . . ? C17 C12 C11 120.7(10) . . ? C13 C12 C11 120.2(9) . . ? C14 C13 C12 122.0(10) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 118.2(10) . . ? C13 C14 C18 123.4(10) . . ? C15 C14 C18 118.4(10) . . ? C16 C15 C14 121.3(10) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C17 119.8(9) . . ? C15 C16 C22 119.9(9) . . ? C17 C16 C22 120.3(9) . . ? O2 C17 C12 120.9(10) . . ? O2 C17 C16 119.6(9) . . ? C12 C17 C16 119.4(10) . . ? C19A C18 C21 121(3) . . ? C19A C18 C19 55.0(18) . . ? C21 C18 C19 107.8(15) . . ? C19A C18 C20 50.8(18) . . ? C21 C18 C20 106.9(15) . . ? C19 C18 C20 105.7(15) . . ? C19A C18 C21A 107.1(11) . . ? C21 C18 C21A 54.6(18) . . ? C19 C18 C21A 60.4(18) . . ? C20 C18 C21A 143(3) . . ? C19A C18 C14 115.1(14) . . ? C21 C18 C14 124(3) . . ? C19 C18 C14 105(2) . . ? C20 C18 C14 107(2) . . ? C21A C18 C14 110.2(13) . . ? C19A C18 C20A 106.5(11) . . ? C21 C18 C20A 50.3(18) . . ? C19 C18 C20A 143(3) . . ? C20 C18 C20A 64.0(18) . . ? C21A C18 C20A 104.8(11) . . ? C14 C18 C20A 112.4(13) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.4 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.4 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21A H21D 109.5 . . ? C18 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C18 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C16 C22 C23 111.1(8) . . ? C16 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C16 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 120.2(10) . . ? C28 C23 C22 118.5(9) . . ? C24 C23 C22 121.3(9) . . ? C25 C24 C23 121.5(11) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C24 C25 C26 116.7(11) . . ? C24 C25 C29 124.0(13) . . ? C26 C25 C29 119.2(12) . . ? C27 C26 C25 123.0(11) . . ? C27 C26 H26A 118.5 . . ? C25 C26 H26A 118.5 . . ? C26 C27 C28 117.3(10) . . ? C26 C27 C33 119.3(10) . . ? C28 C27 C33 123.3(9) . . ? C23 C28 O3 119.9(9) . . ? C23 C28 C27 120.9(10) . . ? O3 C28 C27 119.2(9) . . ? C30A C29 C25 114.2(15) . . ? C30A C29 C31 132(2) . . ? C25 C29 C31 113.0(16) . . ? C30A C29 C31A 112.1(13) . . ? C25 C29 C31A 106.1(19) . . ? C31 C29 C31A 48.2(14) . . ? C30A C29 C32 58.3(15) . . ? C25 C29 C32 107(2) . . ? C31 C29 C32 111.0(14) . . ? C31A C29 C32 146(3) . . ? C30A C29 C32A 109.2(12) . . ? C25 C29 C32A 106.1(17) . . ? C31 C29 C32A 61.1(14) . . ? C31A C29 C32A 108.9(12) . . ? C32 C29 C32A 55.2(15) . . ? C30A C29 C30 50.0(13) . . ? C25 C29 C30 112.2(17) . . ? C31 C29 C30 106.2(12) . . ? C31A C29 C30 65.2(14) . . ? C32 C29 C30 106.9(13) . . ? C32A C29 C30 141(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C30A H30D 109.5 . . ? C29 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C29 C31A H31D 109.5 . . ? C29 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C29 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C29 C32A H32D 109.5 . . ? C29 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C29 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C34 C33 C27 115.6(8) . . ? C34 C33 H33A 108.4 . . ? C27 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? C27 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? C35 C34 C39 118.8(10) . . ? C35 C34 C33 119.6(10) . . ? C39 C34 C33 121.0(10) . . ? C34 C35 C36 123.5(11) . . ? C34 C35 H35A 118.3 . . ? C36 C35 H35A 118.3 . . ? C37 C36 C35 116.0(10) . . ? C37 C36 C40 123.1(11) . . ? C35 C36 C40 120.7(11) . . ? C38 C37 C36 123.5(11) . . ? C38 C37 H37A 118.3 . . ? C36 C37 H37A 118.3 . . ? C37 C38 C39 118.2(11) . . ? C37 C38 C44 121.2(11) . . ? C39 C38 C44 120.6(10) . . ? O4 C39 C34 121.2(9) . . ? O4 C39 C38 118.5(10) . . ? C34 C39 C38 120.0(10) . . ? C42 C40 C36 110.2(11) . . ? C42 C40 C43 107.9(13) . . ? C36 C40 C43 108.4(11) . . ? C42 C40 C41 109.5(12) . . ? C36 C40 C41 112.3(11) . . ? C43 C40 C41 108.4(12) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C38 C44 C45 116.9(9) . . ? C38 C44 H44A 108.1 . . ? C45 C44 H44A 108.1 . . ? C38 C44 H44B 108.1 . . ? C45 C44 H44B 108.1 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C50 117.1(9) . . ? C46 C45 C44 120.6(10) . . ? C50 C45 C44 122.3(9) . . ? C45 C46 C47 124.3(10) . . ? C45 C46 H46A 117.8 . . ? C47 C46 H46A 117.8 . . ? C46 C47 C48 116.0(9) . . ? C46 C47 C51 124.1(9) . . ? C48 C47 C51 119.9(9) . . ? C49 C48 C47 122.3(10) . . ? C49 C48 H48A 118.8 . . ? C47 C48 H48A 118.8 . . ? C48 C49 C50 117.4(10) . . ? C48 C49 C55 118.4(10) . . ? C50 C49 C55 124.2(9) . . ? C49 C50 O5 117.8(9) . . ? C49 C50 C45 122.8(9) . . ? O5 C50 C45 119.3(9) . . ? C52 C51 C54 109.2(11) . . ? C52 C51 C47 109.1(8) . . ? C54 C51 C47 109.6(9) . . ? C52 C51 C53 106.3(11) . . ? C54 C51 C53 109.5(11) . . ? C47 C51 C53 112.9(9) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 C2 114.3(8) . . ? C49 C55 H55A 108.7 . . ? C2 C55 H55A 108.7 . . ? C49 C55 H55B 108.7 . . ? C2 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? S1 C56 H56A 109.5 . . ? S1 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? S1 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? S1 C57 H57A 109.5 . . ? S1 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? S1 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? S2 C58 H58A 109.5 . . ? S2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? S2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? S2 C59 H59A 109.5 . . ? S2 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? S2 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 5.732 _refine_diff_density_min -1.665 _refine_diff_density_rms 0.221