# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1998 data_s92-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H37 O6 Sb' _chemical_formula_weight 807.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.082(2) _cell_length_b 20.406(4) _cell_length_c 18.756(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.87(3) _cell_angle_gamma 90.00 _cell_volume 3746.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51055 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.37 _exptl_crystal_description 'chunky needle' _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.956 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51055 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7657 _reflns_number_gt 6257 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7657 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.796 _refine_ls_restrained_S_all 0.796 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.149259(14) 0.355445(8) 0.100394(8) 0.01422(8) Uani 1 d . . . O1 O 0.05547(17) 0.26874(8) 0.04608(9) 0.0190(4) Uani 1 d . . . O2 O -0.06899(18) 0.33721(9) -0.03593(10) 0.0217(4) Uani 1 d . . . O3 O -0.17296(18) 0.24185(10) -0.12846(10) 0.0248(4) Uani 1 d . . . H3 H -0.2261 0.2722 -0.1281 0.037 Uiso 1 calc R . . O4 O 0.23601(17) 0.43469(8) 0.16708(9) 0.0200(4) Uani 1 d . . . O5 O 0.12187(18) 0.50225(9) 0.08049(10) 0.0226(4) Uani 1 d . . . O6 O 0.26448(17) 0.60533(8) 0.15212(10) 0.0201(4) Uani 1 d . . . H6 H 0.1925 0.6148 0.1230 0.030 Uiso 1 calc R . . C1 C 0.2393(3) 0.37390(13) 0.01235(14) 0.0195(5) Uani 1 d . . . C2 C 0.1793(3) 0.41332(13) -0.04695(15) 0.0243(6) Uani 1 d . . . H2 H 0.1015 0.4376 -0.0465 0.029 Uiso 1 calc R . . C3 C 0.2373(3) 0.41592(15) -0.10673(16) 0.0333(7) Uani 1 d . . . H3A H 0.1976 0.4417 -0.1471 0.040 Uiso 1 calc R . . C4 C 0.3541(4) 0.38030(19) -0.10681(18) 0.0453(9) Uani 1 d . . . H4 H 0.3924 0.3822 -0.1472 0.054 Uiso 1 calc R . . C5 C 0.4136(4) 0.34211(19) -0.0472(2) 0.0499(10) Uani 1 d . . . H5 H 0.4931 0.3189 -0.0470 0.060 Uiso 1 calc R . . C6 C 0.3559(3) 0.33824(17) 0.01211(18) 0.0356(7) Uani 1 d . . . H6A H 0.3952 0.3117 0.0519 0.043 Uiso 1 calc R . . C7 C -0.0379(2) 0.37242(12) 0.12890(14) 0.0178(5) Uani 1 d . . . C8 C -0.1440(3) 0.40851(14) 0.08610(15) 0.0240(6) Uani 1 d . . . H8 H -0.1318 0.4319 0.0456 0.029 Uiso 1 calc R . . C9 C -0.2684(3) 0.40905(14) 0.10488(17) 0.0311(7) Uani 1 d . . . H9 H -0.3409 0.4326 0.0762 0.037 Uiso 1 calc R . . C10 C -0.2867(3) 0.37513(16) 0.16569(19) 0.0351(7) Uani 1 d . . . H10 H -0.3717 0.3751 0.1769 0.042 Uiso 1 calc R . . C11 C -0.1792(3) 0.34136(16) 0.20966(17) 0.0330(7) Uani 1 d . . . H11 H -0.1907 0.3198 0.2514 0.040 Uiso 1 calc R . . C12 C -0.0546(3) 0.33974(14) 0.19151(16) 0.0249(6) Uani 1 d . . . H12 H 0.0182 0.3169 0.2209 0.030 Uiso 1 calc R . . C13 C 0.2857(2) 0.29361(13) 0.17322(14) 0.0174(5) Uani 1 d . . . C14 C 0.2919(3) 0.22717(13) 0.15674(15) 0.0229(6) Uani 1 d . . . H14 H 0.2288 0.2092 0.1171 0.028 Uiso 1 calc R . . C15 C 0.3921(3) 0.18796(14) 0.19961(16) 0.0267(6) Uani 1 d . . . H15 H 0.3959 0.1437 0.1884 0.032 Uiso 1 calc R . . C16 C 0.4858(3) 0.21353(14) 0.25833(16) 0.0277(6) Uani 1 d . . . H16 H 0.5529 0.1869 0.2868 0.033 Uiso 1 calc R . . C17 C 0.4798(3) 0.27913(16) 0.27484(17) 0.0365(7) Uani 1 d . . . H17 H 0.5433 0.2966 0.3146 0.044 Uiso 1 calc R . . C18 C 0.3804(3) 0.31931(14) 0.23295(16) 0.0281(6) Uani 1 d . . . H18 H 0.3771 0.3634 0.2448 0.034 Uiso 1 calc R . . C19 C -0.0378(2) 0.28152(13) -0.01323(13) 0.0171(5) Uani 1 d . . . C20 C -0.1125(2) 0.22184(13) -0.05449(14) 0.0188(5) Uani 1 d . . . C21 C -0.0059(2) 0.16937(13) -0.05835(14) 0.0212(6) Uani 1 d . . . C22 C 0.0095(3) 0.11370(14) -0.01488(16) 0.0280(6) Uani 1 d . . . H22 H -0.0484 0.1063 0.0162 0.034 Uiso 1 calc R . . C23 C 0.1128(3) 0.06870(16) -0.01799(18) 0.0365(7) Uani 1 d . . . H23 H 0.1229 0.0312 0.0109 0.044 Uiso 1 calc R . . C24 C 0.1987(3) 0.07932(18) -0.06300(19) 0.0427(9) Uani 1 d . . . H24 H 0.2665 0.0490 -0.0651 0.051 Uiso 1 calc R . . C25 C 0.1848(3) 0.13519(18) -0.1053(2) 0.0433(9) Uani 1 d . . . H25 H 0.2441 0.1430 -0.1355 0.052 Uiso 1 calc R . . C26 C 0.0825(3) 0.17971(17) -0.10302(16) 0.0340(7) Uani 1 d . . . H26 H 0.0732 0.2172 -0.1320 0.041 Uiso 1 calc R . . C27 C -0.2250(2) 0.19941(13) -0.01833(14) 0.0204(5) Uani 1 d . . . C28 C -0.3159(3) 0.15178(13) -0.05457(17) 0.0263(6) Uani 1 d . . . H28 H -0.3010 0.1319 -0.0966 0.032 Uiso 1 calc R . . C29 C -0.4281(3) 0.13382(14) -0.02853(18) 0.0326(7) Uani 1 d . . . H29 H -0.4882 0.1021 -0.0531 0.039 Uiso 1 calc R . . C30 C -0.4506(3) 0.16309(16) 0.03399(18) 0.0331(7) Uani 1 d . . . H30 H -0.5274 0.1519 0.0507 0.040 Uiso 1 calc R . . C31 C -0.3601(3) 0.20842(16) 0.07130(17) 0.0332(7) Uani 1 d . . . H31 H -0.3735 0.2268 0.1144 0.040 Uiso 1 calc R . . C32 C -0.2488(3) 0.22684(14) 0.04497(15) 0.0274(6) Uani 1 d . . . H32 H -0.1887 0.2583 0.0703 0.033 Uiso 1 calc R . . C33 C 0.1954(2) 0.49286(12) 0.14135(14) 0.0166(5) Uani 1 d . . . C34 C 0.2433(2) 0.55042(12) 0.19508(13) 0.0170(5) Uani 1 d . . . C35 C 0.3795(2) 0.53500(12) 0.24784(14) 0.0169(5) Uani 1 d . . . C36 C 0.4894(3) 0.51687(14) 0.21866(15) 0.0239(6) Uani 1 d . . . H36 H 0.4783 0.5155 0.1680 0.029 Uiso 1 calc R . . C37 C 0.6142(3) 0.50092(14) 0.26437(16) 0.0280(6) Uani 1 d . . . H37 H 0.6867 0.4890 0.2444 0.034 Uiso 1 calc R . . C38 C 0.6316(3) 0.50263(14) 0.33982(16) 0.0283(6) Uani 1 d . . . H38 H 0.7154 0.4913 0.3705 0.034 Uiso 1 calc R . . C39 C 0.5248(3) 0.52116(14) 0.36939(16) 0.0267(6) Uani 1 d . . . H39 H 0.5367 0.5227 0.4201 0.032 Uiso 1 calc R . . C40 C 0.3992(3) 0.53766(13) 0.32346(14) 0.0226(6) Uani 1 d . . . H40 H 0.3277 0.5506 0.3437 0.027 Uiso 1 calc R . . C41 C 0.1306(2) 0.56349(12) 0.23537(13) 0.0179(5) Uani 1 d . . . C42 C 0.0708(2) 0.51232(13) 0.26490(14) 0.0221(6) Uani 1 d . . . H42 H 0.0952 0.4694 0.2575 0.027 Uiso 1 calc R . . C43 C -0.0248(3) 0.52442(15) 0.30532(15) 0.0261(6) Uani 1 d . . . H43 H -0.0633 0.4897 0.3253 0.031 Uiso 1 calc R . . C44 C -0.0630(3) 0.58766(16) 0.31599(16) 0.0302(7) Uani 1 d . . . H44 H -0.1280 0.5957 0.3427 0.036 Uiso 1 calc R . . C45 C -0.0047(4) 0.63894(15) 0.2869(2) 0.0377(8) Uani 1 d . . . H45 H -0.0302 0.6818 0.2942 0.045 Uiso 1 calc R . . C46 C 0.0920(3) 0.62714(15) 0.24675(18) 0.0308(7) Uani 1 d . . . H46 H 0.1311 0.6621 0.2274 0.037 Uiso 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 0.01615(12) 0.01097(12) 0.01360(12) 0.00018(6) -0.00026(8) -0.00049(5) O1 0.0218(9) 0.0151(9) 0.0172(9) -0.0022(7) -0.0009(7) -0.0019(7) O2 0.0237(9) 0.0182(10) 0.0209(10) 0.0022(8) 0.0010(8) 0.0005(8) O3 0.0281(9) 0.0285(11) 0.0124(9) 0.0033(8) -0.0056(7) -0.0001(8) O4 0.0228(9) 0.0128(9) 0.0219(10) -0.0015(8) 0.0003(7) -0.0021(7) O5 0.0262(9) 0.0178(10) 0.0205(10) -0.0035(8) -0.0006(8) 0.0015(8) O6 0.0235(9) 0.0146(9) 0.0204(10) 0.0043(8) 0.0018(7) -0.0030(7) C1 0.0232(13) 0.0164(13) 0.0191(14) -0.0006(11) 0.0055(10) -0.0009(10) C2 0.0305(14) 0.0187(14) 0.0222(14) 0.0021(11) 0.0033(11) -0.0016(11) C3 0.0511(18) 0.0281(17) 0.0225(15) 0.0051(13) 0.0126(13) -0.0023(14) C4 0.070(3) 0.038(2) 0.040(2) 0.0077(16) 0.037(2) 0.0049(17) C5 0.056(2) 0.048(2) 0.057(2) 0.0174(19) 0.036(2) 0.0244(18) C6 0.0374(17) 0.0376(18) 0.0360(19) 0.0150(15) 0.0170(14) 0.0156(15) C7 0.0207(12) 0.0120(12) 0.0208(14) -0.0038(10) 0.0053(10) -0.0033(10) C8 0.0246(13) 0.0209(14) 0.0255(15) 0.0005(12) 0.0039(11) 0.0012(11) C9 0.0261(14) 0.0229(15) 0.0431(18) -0.0039(14) 0.0056(13) 0.0039(12) C10 0.0298(15) 0.0328(17) 0.048(2) -0.0084(15) 0.0197(14) -0.0041(13) C11 0.0447(18) 0.0308(16) 0.0279(17) -0.0051(13) 0.0176(14) -0.0078(14) C12 0.0314(15) 0.0221(14) 0.0208(15) -0.0017(12) 0.0051(12) -0.0022(12) C13 0.0182(12) 0.0167(13) 0.0166(13) 0.0027(10) 0.0025(10) 0.0014(10) C14 0.0256(13) 0.0167(14) 0.0218(14) 0.0014(11) -0.0035(11) 0.0000(11) C15 0.0300(14) 0.0163(14) 0.0331(16) 0.0035(12) 0.0060(12) 0.0036(11) C16 0.0237(13) 0.0257(15) 0.0302(16) 0.0071(13) -0.0007(12) 0.0067(12) C17 0.0375(16) 0.0323(18) 0.0274(16) -0.0017(14) -0.0166(13) 0.0048(13) C18 0.0317(15) 0.0209(15) 0.0256(15) -0.0053(12) -0.0051(12) 0.0022(12) C19 0.0160(11) 0.0195(14) 0.0154(13) -0.0016(11) 0.0028(10) -0.0015(10) C20 0.0208(12) 0.0195(14) 0.0121(12) 0.0002(10) -0.0038(10) -0.0024(10) C21 0.0213(12) 0.0201(14) 0.0190(14) -0.0077(11) -0.0014(10) -0.0036(11) C22 0.0259(14) 0.0257(16) 0.0304(16) -0.0013(13) 0.0031(12) -0.0007(12) C23 0.0319(15) 0.0286(17) 0.0449(19) -0.0030(15) 0.0008(14) 0.0049(13) C24 0.0266(15) 0.045(2) 0.052(2) -0.0230(18) -0.0009(14) 0.0096(14) C25 0.0320(17) 0.059(3) 0.042(2) -0.0090(17) 0.0156(15) 0.0053(15) C26 0.0329(15) 0.041(2) 0.0288(16) -0.0019(14) 0.0083(13) -0.0017(14) C27 0.0185(12) 0.0162(13) 0.0236(14) 0.0018(11) -0.0010(10) 0.0008(10) C28 0.0278(15) 0.0235(15) 0.0260(16) -0.0038(12) 0.0035(12) -0.0043(11) C29 0.0278(15) 0.0265(16) 0.0410(19) -0.0022(14) 0.0031(14) -0.0115(12) C30 0.0276(15) 0.0291(16) 0.045(2) 0.0062(15) 0.0135(14) -0.0054(13) C31 0.0362(16) 0.0319(18) 0.0343(17) -0.0032(14) 0.0135(13) -0.0047(13) C32 0.0303(14) 0.0249(16) 0.0272(15) -0.0068(12) 0.0073(12) -0.0098(12) C33 0.0138(11) 0.0140(13) 0.0221(14) -0.0016(11) 0.0046(10) -0.0014(9) C34 0.0192(12) 0.0140(13) 0.0167(13) 0.0007(10) 0.0021(10) -0.0034(9) C35 0.0195(12) 0.0095(12) 0.0197(13) -0.0009(10) 0.0008(10) -0.0026(9) C36 0.0237(13) 0.0264(16) 0.0206(14) -0.0070(12) 0.0034(11) -0.0028(11) C37 0.0201(13) 0.0283(16) 0.0347(17) -0.0060(13) 0.0047(12) 0.0004(11) C38 0.0235(13) 0.0241(15) 0.0311(16) 0.0036(13) -0.0058(12) -0.0002(11) C39 0.0290(14) 0.0270(16) 0.0208(14) 0.0045(12) -0.0002(11) -0.0020(12) C40 0.0228(12) 0.0210(14) 0.0231(14) -0.0003(11) 0.0038(11) -0.0028(11) C41 0.0184(11) 0.0164(13) 0.0163(13) -0.0006(10) -0.0007(10) 0.0002(10) C42 0.0208(13) 0.0202(14) 0.0244(14) -0.0017(11) 0.0036(11) 0.0004(10) C43 0.0223(13) 0.0330(17) 0.0229(14) 0.0030(12) 0.0053(11) -0.0039(11) C44 0.0249(14) 0.0393(18) 0.0281(16) 0.0002(13) 0.0098(12) 0.0064(12) C45 0.0444(19) 0.0243(17) 0.049(2) -0.0052(14) 0.0199(17) 0.0076(13) C46 0.0394(17) 0.0173(14) 0.0399(18) -0.0010(13) 0.0175(14) 0.0020(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C1 2.100(3) . ? Sb1 O4 2.1024(17) . ? Sb1 C13 2.109(2) . ? Sb1 C7 2.109(2) . ? Sb1 O1 2.1449(17) . ? O1 C19 1.299(3) . ? O2 C19 1.228(3) . ? O3 C20 1.434(3) . ? O4 C33 1.310(3) . ? O5 C33 1.218(3) . ? O6 C34 1.426(3) . ? C1 C6 1.384(4) . ? C1 C2 1.388(4) . ? C2 C3 1.384(4) . ? C3 C4 1.384(5) . ? C4 C5 1.377(5) . ? C5 C6 1.376(5) . ? C7 C8 1.386(4) . ? C7 C12 1.395(4) . ? C8 C9 1.382(4) . ? C9 C10 1.384(4) . ? C10 C11 1.379(5) . ? C11 C12 1.379(4) . ? C13 C18 1.389(4) . ? C13 C14 1.395(4) . ? C14 C15 1.385(4) . ? C15 C16 1.371(4) . ? C16 C17 1.379(4) . ? C17 C18 1.384(4) . ? C19 C20 1.540(4) . ? C20 C27 1.525(4) . ? C20 C21 1.531(4) . ? C21 C26 1.378(4) . ? C21 C22 1.385(4) . ? C22 C23 1.400(4) . ? C23 C24 1.364(5) . ? C24 C25 1.377(5) . ? C25 C26 1.383(5) . ? C27 C32 1.385(4) . ? C27 C28 1.396(4) . ? C28 C29 1.384(4) . ? C29 C30 1.382(4) . ? C30 C31 1.368(4) . ? C31 C32 1.382(4) . ? C33 C34 1.548(3) . ? C34 C35 1.521(3) . ? C34 C41 1.532(3) . ? C35 C40 1.385(4) . ? C35 C36 1.398(4) . ? C36 C37 1.381(4) . ? C37 C38 1.384(4) . ? C38 C39 1.377(4) . ? C39 C40 1.392(4) . ? C41 C42 1.386(4) . ? C41 C46 1.387(4) . ? C42 C43 1.384(4) . ? C43 C44 1.375(4) . ? C44 C45 1.376(4) . ? C45 C46 1.388(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sb1 O4 97.66(9) . . ? C1 Sb1 C13 106.19(10) . . ? O4 Sb1 C13 87.77(9) . . ? C1 Sb1 C7 138.70(10) . . ? O4 Sb1 C7 89.58(8) . . ? C13 Sb1 C7 114.71(10) . . ? C1 Sb1 O1 89.93(9) . . ? O4 Sb1 O1 171.98(7) . . ? C13 Sb1 O1 87.64(8) . . ? C7 Sb1 O1 86.37(8) . . ? C19 O1 Sb1 112.77(15) . . ? C33 O4 Sb1 115.41(15) . . ? C6 C1 C2 120.6(3) . . ? C6 C1 Sb1 115.9(2) . . ? C2 C1 Sb1 123.15(19) . . ? C3 C2 C1 119.0(3) . . ? C4 C3 C2 120.3(3) . . ? C5 C4 C3 120.1(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C1 119.8(3) . . ? C8 C7 C12 120.6(2) . . ? C8 C7 Sb1 123.63(19) . . ? C12 C7 Sb1 115.51(19) . . ? C9 C8 C7 118.6(3) . . ? C8 C9 C10 121.0(3) . . ? C11 C10 C9 120.1(3) . . ? C10 C11 C12 119.8(3) . . ? C11 C12 C7 119.8(3) . . ? C18 C13 C14 119.1(2) . . ? C18 C13 Sb1 120.80(19) . . ? C14 C13 Sb1 119.65(18) . . ? C15 C14 C13 119.9(2) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 119.4(2) . . ? C16 C17 C18 120.8(3) . . ? C17 C18 C13 119.9(3) . . ? O2 C19 O1 123.7(2) . . ? O2 C19 C20 120.3(2) . . ? O1 C19 C20 116.0(2) . . ? O3 C20 C27 109.1(2) . . ? O3 C20 C21 107.1(2) . . ? C27 C20 C21 114.6(2) . . ? O3 C20 C19 107.7(2) . . ? C27 C20 C19 109.9(2) . . ? C21 C20 C19 108.2(2) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C20 119.0(3) . . ? C22 C21 C20 121.8(2) . . ? C21 C22 C23 119.5(3) . . ? C24 C23 C22 120.7(3) . . ? C23 C24 C25 119.7(3) . . ? C24 C25 C26 120.0(3) . . ? C21 C26 C25 121.0(3) . . ? C32 C27 C28 118.1(2) . . ? C32 C27 C20 124.1(2) . . ? C28 C27 C20 117.7(2) . . ? C29 C28 C27 120.6(3) . . ? C30 C29 C28 120.0(3) . . ? C31 C30 C29 120.1(3) . . ? C30 C31 C32 120.0(3) . . ? C31 C32 C27 121.2(3) . . ? O5 C33 O4 123.7(2) . . ? O5 C33 C34 121.1(2) . . ? O4 C33 C34 115.3(2) . . ? O6 C34 C35 107.22(18) . . ? O6 C34 C41 111.8(2) . . ? C35 C34 C41 112.1(2) . . ? O6 C34 C33 107.12(19) . . ? C35 C34 C33 111.0(2) . . ? C41 C34 C33 107.49(19) . . ? C40 C35 C36 118.6(2) . . ? C40 C35 C34 122.9(2) . . ? C36 C35 C34 118.5(2) . . ? C37 C36 C35 120.6(3) . . ? C36 C37 C38 120.2(3) . . ? C39 C38 C37 119.9(2) . . ? C38 C39 C40 120.1(3) . . ? C35 C40 C39 120.6(2) . . ? C42 C41 C46 118.6(2) . . ? C42 C41 C34 120.8(2) . . ? C46 C41 C34 120.5(2) . . ? C43 C42 C41 120.8(3) . . ? C44 C43 C42 120.2(3) . . ? C43 C44 C45 119.7(3) . . ? C44 C45 C46 120.4(3) . . ? C41 C46 C45 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.840 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.092 data_s92-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H26 Cl3 O6 Sb' _chemical_formula_weight 746.64 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7855(1) _cell_length_b 17.7361(2) _cell_length_c 18.7408(2) _cell_angle_alpha 113.4792(7) _cell_angle_beta 104.5722(8) _cell_angle_gamma 93.1164(8) _cell_volume 3133.74(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39328 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.680 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39328 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12197 _reflns_number_gt 10310 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+6.8354P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12197 _refine_ls_number_parameters 849 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.17804(2) 0.220370(15) 0.369117(14) 0.01757(10) Uani 1 d . . . O11 O 0.3585(3) 0.23407(19) 0.34819(17) 0.0258(6) Uani 1 d . . . O12 O 0.3475(3) 0.09903(18) 0.27220(17) 0.0288(6) Uani 1 d . . . O13 O 0.5290(3) 0.05217(19) 0.20144(19) 0.0365(7) Uani 1 d . . . H13 H 0.4635 0.0453 0.2162 0.063(19) Uiso 1 calc R . . O21 O 0.0036(3) 0.23411(17) 0.40283(17) 0.0228(6) Uani 1 d . . . O22 O -0.0609(3) 0.09637(18) 0.34302(18) 0.0283(6) Uani 1 d . . . O23 O -0.2717(4) 0.0353(3) 0.3581(3) 0.0388(14) Uani 0.751(9) d PD A 1 H23 H -0.2078 0.0353 0.3401 0.05(2) Uiso 0.751(9) calc PR A 1 O23' O -0.1154(11) 0.3230(6) 0.4982(9) 0.038(4) Uani 0.249(9) d PD A 2 H23' H -0.0587 0.3110 0.4738 0.08(9) Uiso 0.249(9) calc PR A 2 C11 C 0.4001(4) 0.1724(3) 0.2994(2) 0.0236(8) Uani 1 d . . . C12 C 0.5746(4) 0.1344(3) 0.2314(2) 0.0275(9) Uani 1 d . . . C13 C 0.5146(4) 0.1965(3) 0.2783(2) 0.0238(9) Uani 1 d . . . C14 C 0.5656(4) 0.2797(3) 0.3044(3) 0.0326(10) Uani 1 d . . . H14 H 0.5261 0.3218 0.3362 0.030(12) Uiso 1 calc R . . C15 C 0.6721(5) 0.3027(3) 0.2852(3) 0.0426(12) Uani 1 d . . . H15 H 0.7053 0.3600 0.3030 0.043(14) Uiso 1 calc R . . C16 C 0.7302(5) 0.2413(4) 0.2395(3) 0.0436(13) Uani 1 d . . . H16 H 0.8037 0.2571 0.2260 0.044(14) Uiso 1 calc R . . C17 C 0.6847(4) 0.1585(3) 0.2132(3) 0.0365(11) Uani 1 d . . . H17 H 0.7272 0.1174 0.1827 0.039(14) Uiso 1 calc R . . C21 C -0.0774(4) 0.1669(3) 0.3849(2) 0.0222(8) Uani 1 d . . . C22 C -0.2790(4) 0.1105(3) 0.4027(3) 0.0299(10) Uani 1 d D . . H22 H -0.2715 0.0560 0.3676 0.036 Uiso 0.249(9) calc PR A 2 C23 C -0.1872(4) 0.1803(3) 0.4196(2) 0.0222(8) Uani 1 d . . . C24 C -0.2018(4) 0.2593(3) 0.4716(3) 0.0308(10) Uani 1 d D . . H22 H -0.1416 0.3068 0.4833 0.037 Uiso 0.751(9) calc PR A 1 C25 C -0.3015(5) 0.2695(4) 0.5061(3) 0.0425(12) Uani 1 d . . . H25 H -0.3095 0.3238 0.5414 0.064(19) Uiso 1 calc R . . C26 C -0.3903(5) 0.2011(4) 0.4898(3) 0.0434(13) Uani 1 d . . . H26 H -0.4585 0.2083 0.5143 0.034(13) Uiso 1 calc R . . C27 C -0.3794(4) 0.1218(4) 0.4373(3) 0.0424(13) Uani 1 d . . . H27 H -0.4416 0.0750 0.4251 0.048(15) Uiso 1 calc R . . C101 C 0.2396(4) 0.1602(2) 0.4448(2) 0.0205(8) Uani 1 d . . . C102 C 0.2352(5) 0.2016(3) 0.5243(3) 0.0363(11) Uani 1 d . . . H102 H 0.2046 0.2533 0.5413 0.049(16) Uiso 1 calc R . . C103 C 0.2763(5) 0.1665(4) 0.5789(3) 0.0462(13) Uani 1 d . . . H103 H 0.2730 0.1940 0.6333 0.066(18) Uiso 1 calc R . . C104 C 0.3216(4) 0.0919(3) 0.5543(3) 0.0367(11) Uani 1 d . . . H104 H 0.3511 0.0687 0.5920 0.035(13) Uiso 1 calc R . . C105 C 0.3243(4) 0.0512(3) 0.4757(3) 0.0339(10) Uani 1 d . . . H105 H 0.3542 -0.0007 0.4589 0.038(13) Uiso 1 calc R . . C106 C 0.2837(4) 0.0851(3) 0.4203(3) 0.0276(9) Uani 1 d . . . H106 H 0.2863 0.0568 0.3658 0.037(13) Uiso 1 calc R . . C201 C 0.0785(4) 0.1686(3) 0.2442(2) 0.0204(8) Uani 1 d . . . C202 C 0.0552(4) 0.2228(3) 0.2076(3) 0.0277(9) Uani 1 d . . . H202 H 0.0843 0.2812 0.2383 0.026(11) Uiso 1 calc R . . C203 C -0.0116(5) 0.1897(3) 0.1249(3) 0.0352(11) Uani 1 d . . . H203 H -0.0307 0.2259 0.0990 0.051(16) Uiso 1 calc R . . C204 C -0.0506(4) 0.1039(3) 0.0798(3) 0.0312(10) Uani 1 d . . . H204 H -0.0959 0.0818 0.0233 0.024(11) Uiso 1 calc R . . C205 C -0.0240(4) 0.0508(3) 0.1166(3) 0.0276(9) Uani 1 d . . . H205 H -0.0494 -0.0078 0.0853 0.021(11) Uiso 1 calc R . . C206 C 0.0402(4) 0.0828(3) 0.1997(2) 0.0233(8) Uani 1 d . . . H206 H 0.0575 0.0465 0.2256 0.020(11) Uiso 1 calc R . . C301 C 0.2151(4) 0.3513(2) 0.4304(2) 0.0239(8) Uani 1 d . . . C302 C 0.1164(4) 0.3964(3) 0.4202(3) 0.0279(9) Uani 1 d . . . H302 H 0.0315 0.3682 0.3856 0.044(15) Uiso 1 calc R . . C303 C 0.1421(5) 0.4827(3) 0.4606(3) 0.0389(11) Uani 1 d . . . H303 H 0.0755 0.5139 0.4523 0.049(15) Uiso 1 calc R . . C304 C 0.2640(5) 0.5233(3) 0.5128(3) 0.0435(13) Uani 1 d . . . H304 H 0.2810 0.5825 0.5411 0.044(14) Uiso 1 calc R . . C305 C 0.3619(5) 0.4781(3) 0.5240(3) 0.0432(12) Uani 1 d . . . H305 H 0.4456 0.5065 0.5606 0.052(16) Uiso 1 calc R . . C306 C 0.3392(4) 0.3922(3) 0.4826(3) 0.0320(10) Uani 1 d . . . H306 H 0.4070 0.3615 0.4896 0.053(17) Uiso 1 calc R . . Sb2 Sb 0.18309(2) 0.234919(15) -0.123398(15) 0.01856(10) Uani 1 d . . . O31 O 0.3578(3) 0.22083(18) -0.15444(18) 0.0249(6) Uani 1 d . . . O32 O 0.3554(3) 0.32071(19) -0.1987(2) 0.0360(7) Uani 1 d . . . O33 O 0.5441(4) 0.3472(2) -0.2542(2) 0.0468(9) Uani 1 d . . . H33 H 0.4833 0.3596 -0.2334 0.14(4) Uiso 1 calc R . . O41 O 0.0136(3) 0.25085(17) -0.08692(18) 0.0241(6) Uani 1 d . . . O42 O -0.0597(3) 0.11384(18) -0.14762(17) 0.0260(6) Uani 1 d . . . O43 O -0.2594(3) 0.05578(19) -0.11840(19) 0.0328(7) Uani 1 d . . . H43 H -0.2002 0.0534 -0.1406 0.039(15) Uiso 1 calc R . . C31 C 0.4005(4) 0.2600(3) -0.1915(2) 0.0252(9) Uani 1 d . . . C32 C 0.5725(4) 0.2724(3) -0.2559(3) 0.0335(10) Uani 1 d . . . C33 C 0.5053(4) 0.2268(3) -0.2268(2) 0.0267(9) Uani 1 d . . . C34 C 0.5366(4) 0.1495(3) -0.2330(3) 0.0307(10) Uani 1 d . . . H34 H 0.4915 0.1183 -0.2133 0.025(11) Uiso 1 calc R . . C35 C 0.6314(5) 0.1183(3) -0.2671(3) 0.0382(11) Uani 1 d . . . H35 H 0.6506 0.0650 -0.2724 0.056(17) Uiso 1 calc R . . C36 C 0.6996(5) 0.1650(4) -0.2939(3) 0.0427(13) Uani 1 d . . . H36 H 0.7669 0.1438 -0.3163 0.044(14) Uiso 1 calc R . . C37 C 0.6715(5) 0.2412(4) -0.2886(3) 0.0425(12) Uani 1 d . . . H37 H 0.7192 0.2725 -0.3070 0.041(14) Uiso 1 calc R . . C41 C -0.0693(4) 0.1854(2) -0.1033(2) 0.0209(8) Uani 1 d . . . C42 C -0.2615(4) 0.1363(3) -0.0719(3) 0.0272(9) Uani 1 d . . . C43 C -0.1732(4) 0.2022(3) -0.0637(2) 0.0225(8) Uani 1 d . . . C44 C -0.1829(5) 0.2837(3) -0.0136(3) 0.0333(10) Uani 1 d . . . H44 H -0.1235 0.3291 -0.0072 0.024(11) Uiso 1 calc R . . C45 C -0.2755(5) 0.2997(3) 0.0264(3) 0.0456(13) Uani 1 d . . . H46 H -0.2809 0.3555 0.0596 0.069(19) Uiso 1 calc R . . C46 C -0.3617(5) 0.2326(4) 0.0175(3) 0.0458(13) Uani 1 d . . . H46 H -0.4263 0.2428 0.0450 0.049(15) Uiso 1 calc R . . C47 C -0.3538(4) 0.1522(3) -0.0304(3) 0.0384(11) Uani 1 d . . . H47 H -0.4121 0.1071 -0.0353 0.034(13) Uiso 1 calc R . . C401 C 0.0801(4) 0.1853(3) -0.2477(2) 0.0233(8) Uani 1 d . . . C402 C 0.0584(4) 0.1003(3) -0.2939(3) 0.0277(9) Uani 1 d . . . H402 H 0.0862 0.0642 -0.2691 0.034(13) Uiso 1 calc R . . C403 C -0.0048(5) 0.0678(3) -0.3772(3) 0.0362(11) Uani 1 d . . . H403 H -0.0192 0.0093 -0.4095 0.035(13) Uiso 1 calc R . . C404 C -0.0466(5) 0.1197(3) -0.4130(3) 0.0379(11) Uani 1 d . . . H404 H -0.0898 0.0971 -0.4698 0.045(15) Uiso 1 calc R . . C405 C -0.0255(5) 0.2050(4) -0.3661(3) 0.0414(12) Uani 1 d . . . H405 H -0.0551 0.2408 -0.3908 0.044(14) Uiso 1 calc R . . C406 C 0.0389(4) 0.2388(3) -0.2827(3) 0.0326(10) Uani 1 d . . . H406 H 0.0542 0.2974 -0.2505 0.017(10) Uiso 1 calc R . . C501 C 0.2349(4) 0.3644(2) -0.0539(2) 0.0248(9) Uani 1 d . . . C502 C 0.3607(5) 0.3983(3) -0.0031(3) 0.0334(10) Uani 1 d . . . H502 H 0.4243 0.3634 -0.0019 0.032(13) Uiso 1 calc R . . C503 C 0.3937(5) 0.4835(3) 0.0462(3) 0.0433(12) Uani 1 d . . . H503 H 0.4796 0.5069 0.0818 0.065(18) Uiso 1 calc R . . C505 C 0.1775(6) 0.5007(3) -0.0079(3) 0.0459(13) Uani 1 d . . . H505 H 0.1151 0.5361 -0.0107 0.055(16) Uiso 1 calc R . . C504 C 0.3015(6) 0.5344(3) 0.0437(3) 0.0468(14) Uani 1 d . . . H504 H 0.3241 0.5927 0.0777 0.057(16) Uiso 1 calc R . . C506 C 0.1424(5) 0.4154(3) -0.0562(3) 0.0342(10) Uani 1 d . . . H506 H 0.0557 0.3921 -0.0904 0.066(19) Uiso 1 calc R . . C601 C 0.2453(4) 0.1648(2) -0.0578(2) 0.0194(8) Uani 1 d . . . C602 C 0.2290(4) 0.1913(3) 0.0192(3) 0.0307(10) Uani 1 d . . . H602 H 0.1882 0.2382 0.0395 0.044(15) Uiso 1 calc R . . C603 C 0.2728(5) 0.1489(3) 0.0664(3) 0.0380(11) Uani 1 d . . . H603 H 0.2622 0.1669 0.1192 0.036(13) Uiso 1 calc R . . C604 C 0.3322(4) 0.0802(3) 0.0364(3) 0.0301(10) Uani 1 d . . . H604 H 0.3628 0.0514 0.0688 0.029(12) Uiso 1 calc R . . C605 C 0.3467(4) 0.0539(3) -0.0400(3) 0.0278(9) Uani 1 d . . . H605 H 0.3861 0.0063 -0.0605 0.022(11) Uiso 1 calc R . . C606 C 0.3044(4) 0.0960(2) -0.0879(2) 0.0246(9) Uani 1 d . . . H606 H 0.3159 0.0780 -0.1405 0.036(13) Uiso 1 calc R . . C1 C 0.2912(7) 0.4656(5) 0.2198(4) 0.0656(18) Uani 1 d . . . H1 H 0.3356 0.5120 0.2127 0.058(17) Uiso 1 calc R . . Cl1 Cl 0.1415(2) 0.41890(13) 0.14150(11) 0.0790(5) Uani 1 d . . . Cl2 Cl 0.2748(3) 0.50153(17) 0.31589(12) 0.1076(8) Uani 1 d . . . Cl3 Cl 0.3859(3) 0.38426(17) 0.20717(18) 0.1236(9) Uani 1 d . . . C2 C 0.1966(4) 0.4375(4) 0.7295(3) 0.085(2) Uani 1 d D . . H2 H 0.2123 0.3873 0.7399 0.12(3) Uiso 1 calc R B 1 Cl4 Cl 0.1371(3) 0.40790(17) 0.62535(14) 0.0868(10) Uani 0.756(4) d PD C 1 Cl5 Cl 0.0788(3) 0.4828(2) 0.77264(19) 0.1017(11) Uani 0.756(4) d PD C 1 Cl6 Cl 0.3415(3) 0.5089(2) 0.7700(3) 0.1301(18) Uani 0.756(4) d PD C 1 Cl4' Cl 0.2692(14) 0.4364(11) 0.6567(8) 0.203(6) Uiso 0.244(4) d PD C 2 Cl5' Cl 0.0277(7) 0.4199(11) 0.6870(9) 0.203(6) Uiso 0.244(4) d PD C 2 Cl6' Cl 0.2453(15) 0.5307(8) 0.8144(7) 0.203(6) Uiso 0.244(4) d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.01601(15) 0.01812(15) 0.01874(15) 0.00679(11) 0.00681(11) 0.00494(10) O11 0.0177(14) 0.0339(16) 0.0254(14) 0.0083(13) 0.0121(12) 0.0079(12) O12 0.0275(16) 0.0285(16) 0.0292(15) 0.0095(13) 0.0113(13) 0.0039(13) O13 0.0349(18) 0.0338(18) 0.0376(17) 0.0071(14) 0.0177(15) 0.0126(14) O21 0.0175(14) 0.0242(15) 0.0289(15) 0.0113(12) 0.0102(12) 0.0041(11) O22 0.0292(16) 0.0235(15) 0.0348(16) 0.0120(13) 0.0142(13) 0.0065(12) O23 0.030(2) 0.031(3) 0.059(3) 0.021(2) 0.017(2) 0.0026(18) O23' 0.031(7) 0.018(6) 0.061(9) 0.007(6) 0.025(7) 0.003(5) C11 0.020(2) 0.030(2) 0.0207(19) 0.0116(17) 0.0050(16) 0.0066(17) C12 0.023(2) 0.034(2) 0.022(2) 0.0084(18) 0.0050(17) 0.0061(18) C13 0.021(2) 0.033(2) 0.0162(18) 0.0093(17) 0.0054(16) 0.0058(17) C14 0.029(2) 0.033(2) 0.034(2) 0.011(2) 0.013(2) 0.0057(19) C15 0.039(3) 0.040(3) 0.045(3) 0.015(2) 0.016(2) -0.003(2) C16 0.029(3) 0.061(3) 0.042(3) 0.017(3) 0.021(2) 0.001(2) C17 0.024(2) 0.050(3) 0.032(2) 0.010(2) 0.014(2) 0.009(2) C21 0.0181(19) 0.027(2) 0.0227(19) 0.0136(17) 0.0036(16) 0.0039(16) C22 0.021(2) 0.042(3) 0.038(2) 0.027(2) 0.0097(19) 0.0087(19) C23 0.0170(19) 0.032(2) 0.0226(19) 0.0164(17) 0.0060(16) 0.0049(16) C24 0.023(2) 0.040(3) 0.029(2) 0.013(2) 0.0084(18) 0.0096(19) C25 0.029(3) 0.066(4) 0.033(2) 0.017(2) 0.012(2) 0.018(2) C26 0.025(2) 0.085(4) 0.039(3) 0.039(3) 0.019(2) 0.020(3) C27 0.020(2) 0.071(4) 0.058(3) 0.048(3) 0.012(2) 0.007(2) C101 0.0195(19) 0.027(2) 0.0165(18) 0.0107(16) 0.0059(15) 0.0050(16) C102 0.044(3) 0.045(3) 0.021(2) 0.012(2) 0.011(2) 0.023(2) C103 0.052(3) 0.070(4) 0.023(2) 0.022(2) 0.013(2) 0.029(3) C104 0.024(2) 0.056(3) 0.040(3) 0.034(2) 0.004(2) 0.004(2) C105 0.032(2) 0.032(2) 0.041(3) 0.022(2) 0.007(2) 0.0058(19) C106 0.032(2) 0.025(2) 0.025(2) 0.0095(17) 0.0072(18) 0.0075(18) C201 0.0155(18) 0.028(2) 0.0202(18) 0.0107(16) 0.0074(15) 0.0068(16) C202 0.032(2) 0.028(2) 0.028(2) 0.0144(18) 0.0118(18) 0.0111(18) C203 0.043(3) 0.043(3) 0.030(2) 0.024(2) 0.014(2) 0.018(2) C204 0.028(2) 0.047(3) 0.019(2) 0.0143(19) 0.0051(17) 0.014(2) C205 0.023(2) 0.027(2) 0.027(2) 0.0070(18) 0.0079(18) 0.0050(17) C206 0.022(2) 0.026(2) 0.0222(19) 0.0103(17) 0.0061(16) 0.0061(16) C301 0.025(2) 0.021(2) 0.027(2) 0.0078(17) 0.0144(17) 0.0062(16) C302 0.030(2) 0.026(2) 0.034(2) 0.0131(18) 0.0175(19) 0.0096(18) C303 0.050(3) 0.026(2) 0.051(3) 0.017(2) 0.029(3) 0.018(2) C304 0.060(3) 0.020(2) 0.046(3) 0.004(2) 0.026(3) 0.003(2) C305 0.042(3) 0.028(2) 0.046(3) 0.002(2) 0.014(2) -0.006(2) C306 0.027(2) 0.028(2) 0.035(2) 0.0063(19) 0.0117(19) 0.0038(19) Sb2 0.01917(16) 0.01804(15) 0.02214(15) 0.00995(11) 0.00953(11) 0.00521(10) O31 0.0249(15) 0.0302(16) 0.0300(15) 0.0169(13) 0.0169(13) 0.0120(12) O32 0.0423(19) 0.0323(17) 0.0447(18) 0.0204(15) 0.0236(15) 0.0129(14) O33 0.054(2) 0.041(2) 0.057(2) 0.0254(18) 0.0288(19) 0.0042(17) O41 0.0207(14) 0.0224(14) 0.0347(16) 0.0129(12) 0.0154(12) 0.0067(11) O42 0.0284(16) 0.0243(15) 0.0285(15) 0.0110(13) 0.0138(13) 0.0071(12) O43 0.0314(17) 0.0285(16) 0.0374(17) 0.0133(14) 0.0113(14) -0.0020(13) C31 0.023(2) 0.026(2) 0.026(2) 0.0100(17) 0.0087(17) 0.0022(17) C32 0.032(2) 0.039(3) 0.028(2) 0.011(2) 0.0111(19) 0.001(2) C33 0.023(2) 0.037(2) 0.0196(19) 0.0107(18) 0.0081(17) 0.0042(18) C34 0.029(2) 0.040(3) 0.025(2) 0.016(2) 0.0091(18) 0.010(2) C35 0.037(3) 0.049(3) 0.030(2) 0.015(2) 0.014(2) 0.016(2) C36 0.028(3) 0.067(4) 0.032(2) 0.014(2) 0.017(2) 0.013(2) C37 0.036(3) 0.058(3) 0.039(3) 0.021(2) 0.022(2) 0.004(2) C41 0.0162(19) 0.024(2) 0.0249(19) 0.0148(17) 0.0036(16) 0.0030(16) C42 0.021(2) 0.035(2) 0.029(2) 0.0202(19) 0.0048(18) 0.0021(18) C43 0.022(2) 0.027(2) 0.026(2) 0.0167(17) 0.0092(17) 0.0086(16) C44 0.035(3) 0.031(2) 0.043(3) 0.020(2) 0.019(2) 0.012(2) C45 0.051(3) 0.046(3) 0.058(3) 0.027(3) 0.036(3) 0.028(3) C46 0.039(3) 0.066(4) 0.059(3) 0.038(3) 0.035(3) 0.027(3) C47 0.025(2) 0.050(3) 0.056(3) 0.035(3) 0.017(2) 0.009(2) C401 0.021(2) 0.032(2) 0.0217(19) 0.0153(17) 0.0070(16) 0.0063(17) C402 0.030(2) 0.028(2) 0.026(2) 0.0131(18) 0.0078(18) 0.0073(18) C403 0.040(3) 0.040(3) 0.027(2) 0.013(2) 0.010(2) 0.010(2) C404 0.030(2) 0.063(3) 0.025(2) 0.023(2) 0.0063(19) 0.011(2) C405 0.038(3) 0.063(4) 0.045(3) 0.043(3) 0.014(2) 0.019(2) C406 0.035(3) 0.035(2) 0.039(2) 0.024(2) 0.013(2) 0.013(2) C501 0.032(2) 0.0171(19) 0.027(2) 0.0074(16) 0.0159(18) 0.0016(17) C502 0.034(3) 0.028(2) 0.035(2) 0.010(2) 0.011(2) 0.002(2) C503 0.045(3) 0.036(3) 0.037(3) 0.008(2) 0.010(2) -0.010(2) C505 0.061(4) 0.022(2) 0.056(3) 0.014(2) 0.022(3) 0.013(2) C504 0.074(4) 0.017(2) 0.043(3) 0.004(2) 0.023(3) 0.002(2) C506 0.040(3) 0.023(2) 0.043(3) 0.015(2) 0.015(2) 0.009(2) C601 0.0174(19) 0.0207(19) 0.0230(19) 0.0112(16) 0.0077(15) 0.0027(15) C602 0.034(2) 0.037(2) 0.027(2) 0.0153(19) 0.0145(19) 0.017(2) C603 0.041(3) 0.054(3) 0.030(2) 0.025(2) 0.013(2) 0.018(2) C604 0.024(2) 0.039(3) 0.035(2) 0.025(2) 0.0059(19) 0.0056(19) C605 0.021(2) 0.025(2) 0.040(2) 0.0164(19) 0.0083(18) 0.0049(17) C606 0.026(2) 0.023(2) 0.025(2) 0.0084(17) 0.0101(17) 0.0040(17) C1 0.077(5) 0.072(4) 0.058(4) 0.033(3) 0.030(3) 0.006(4) Cl1 0.0874(13) 0.0873(13) 0.0566(10) 0.0241(9) 0.0225(9) 0.0181(10) Cl2 0.1179(18) 0.130(2) 0.0529(10) 0.0165(12) 0.0316(11) -0.0039(15) Cl3 0.134(2) 0.1032(19) 0.126(2) 0.0511(16) 0.0172(17) 0.0462(17) C2 0.069(5) 0.068(5) 0.149(8) 0.067(5) 0.048(5) 0.028(4) Cl4 0.131(3) 0.0808(17) 0.0519(13) 0.0247(12) 0.0310(14) 0.0521(17) Cl5 0.126(3) 0.105(2) 0.106(2) 0.0496(19) 0.073(2) 0.0513(19) Cl6 0.080(2) 0.101(2) 0.216(4) 0.107(3) -0.006(2) 0.0001(17) _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 C201 2.095(4) . ? Sb1 C101 2.097(4) . ? Sb1 O11 2.100(3) . ? Sb1 C301 2.100(4) . ? Sb1 O21 2.127(3) . ? O11 C11 1.302(5) . ? O12 C11 1.233(5) . ? O13 C12 1.348(5) . ? O21 C21 1.310(5) . ? O22 C21 1.234(5) . ? O23 C22 1.280(6) . ? O23' C24 1.264(8) . ? C11 C13 1.480(6) . ? C12 C17 1.405(6) . ? C12 C13 1.412(6) . ? C13 C14 1.386(6) . ? C14 C15 1.374(6) . ? C15 C16 1.384(7) . ? C16 C17 1.365(8) . ? C21 C23 1.476(6) . ? C22 C27 1.381(6) . ? C22 C23 1.417(6) . ? C23 C24 1.397(6) . ? C24 C25 1.374(6) . ? C25 C26 1.383(8) . ? C26 C27 1.390(8) . ? C101 C106 1.380(6) . ? C101 C102 1.389(6) . ? C102 C103 1.394(7) . ? C103 C104 1.379(7) . ? C104 C105 1.366(7) . ? C105 C106 1.390(6) . ? C201 C202 1.388(6) . ? C201 C206 1.388(6) . ? C202 C203 1.391(6) . ? C203 C204 1.391(7) . ? C204 C205 1.375(6) . ? C205 C206 1.392(6) . ? C301 C302 1.386(6) . ? C301 C306 1.395(6) . ? C302 C303 1.385(6) . ? C303 C304 1.375(8) . ? C304 C305 1.385(8) . ? C305 C306 1.379(7) . ? Sb2 C401 2.096(4) . ? Sb2 C501 2.097(4) . ? Sb2 C601 2.099(4) . ? Sb2 O41 2.102(3) . ? Sb2 O31 2.107(3) . ? O31 C31 1.298(5) . ? O32 C31 1.246(5) . ? O33 C32 1.367(6) . ? O41 C41 1.307(5) . ? O42 C41 1.236(5) . ? O43 C42 1.350(5) . ? C31 C33 1.485(6) . ? C32 C37 1.394(7) . ? C32 C33 1.402(6) . ? C33 C34 1.397(6) . ? C34 C35 1.367(6) . ? C35 C36 1.390(7) . ? C36 C37 1.371(8) . ? C41 C43 1.475(6) . ? C42 C47 1.386(6) . ? C42 C43 1.398(6) . ? C43 C44 1.402(6) . ? C44 C45 1.370(7) . ? C45 C46 1.398(8) . ? C46 C47 1.370(8) . ? C401 C402 1.378(6) . ? C401 C406 1.387(6) . ? C402 C403 1.392(6) . ? C403 C404 1.373(7) . ? C404 C405 1.384(8) . ? C405 C406 1.394(7) . ? C501 C502 1.384(6) . ? C501 C506 1.386(6) . ? C502 C503 1.390(7) . ? C503 C504 1.383(8) . ? C505 C504 1.373(8) . ? C505 C506 1.388(6) . ? C601 C602 1.389(6) . ? C601 C606 1.390(6) . ? C602 C603 1.389(6) . ? C603 C604 1.390(7) . ? C604 C605 1.372(6) . ? C605 C606 1.391(6) . ? C1 Cl2 1.715(7) . ? C1 Cl1 1.772(7) . ? C1 Cl3 1.786(8) . ? C2 Cl6' 1.711(6) . ? C2 Cl4' 1.730(6) . ? C2 Cl4 1.735(5) . ? C2 Cl5 1.738(5) . ? C2 Cl6 1.744(5) . ? C2 Cl5' 1.749(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C201 Sb1 C101 129.28(15) . . ? C201 Sb1 O11 92.09(13) . . ? C101 Sb1 O11 94.59(13) . . ? C201 Sb1 C301 116.51(16) . . ? C101 Sb1 C301 114.14(16) . . ? O11 Sb1 C301 85.19(14) . . ? C201 Sb1 O21 93.10(13) . . ? C101 Sb1 O21 90.43(13) . . ? O11 Sb1 O21 168.05(11) . . ? C301 Sb1 O21 82.86(13) . . ? C11 O11 Sb1 122.9(3) . . ? C21 O21 Sb1 118.8(2) . . ? O12 C11 O11 122.6(4) . . ? O12 C11 C13 122.1(4) . . ? O11 C11 C13 115.3(4) . . ? O13 C12 C17 117.9(4) . . ? O13 C12 C13 122.7(4) . . ? C17 C12 C13 119.4(4) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 C11 121.1(4) . . ? C12 C13 C11 120.2(4) . . ? C15 C14 C13 121.5(4) . . ? C14 C15 C16 119.1(5) . . ? C17 C16 C15 121.7(4) . . ? C16 C17 C12 119.5(4) . . ? O22 C21 O21 121.9(4) . . ? O22 C21 C23 122.0(4) . . ? O21 C21 C23 116.1(4) . . ? O23 C22 C27 117.0(5) . . ? O23 C22 C23 123.0(4) . . ? C27 C22 C23 120.0(4) . . ? C24 C23 C22 118.1(4) . . ? C24 C23 C21 122.4(4) . . ? C22 C23 C21 119.4(4) . . ? O23' C24 C25 116.0(7) . . ? O23' C24 C23 122.0(7) . . ? C25 C24 C23 121.3(4) . . ? C24 C25 C26 120.3(5) . . ? C25 C26 C27 119.8(4) . . ? C22 C27 C26 120.5(5) . . ? C106 C101 C102 120.3(4) . . ? C106 C101 Sb1 124.2(3) . . ? C102 C101 Sb1 115.5(3) . . ? C101 C102 C103 119.2(4) . . ? C104 C103 C102 120.2(4) . . ? C105 C104 C103 120.2(4) . . ? C104 C105 C106 120.5(4) . . ? C101 C106 C105 119.6(4) . . ? C202 C201 C206 121.5(4) . . ? C202 C201 Sb1 117.6(3) . . ? C206 C201 Sb1 120.9(3) . . ? C201 C202 C203 118.5(4) . . ? C202 C203 C204 120.4(4) . . ? C205 C204 C203 120.3(4) . . ? C204 C205 C206 120.2(4) . . ? C201 C206 C205 119.1(4) . . ? C302 C301 C306 120.3(4) . . ? C302 C301 Sb1 120.3(3) . . ? C306 C301 Sb1 119.4(3) . . ? C303 C302 C301 119.8(4) . . ? C304 C303 C302 120.1(5) . . ? C303 C304 C305 120.1(4) . . ? C306 C305 C304 120.7(5) . . ? C305 C306 C301 119.0(4) . . ? C401 Sb2 C501 120.47(16) . . ? C401 Sb2 C601 125.37(15) . . ? C501 Sb2 C601 114.15(16) . . ? C401 Sb2 O41 93.36(13) . . ? C501 Sb2 O41 83.90(14) . . ? C601 Sb2 O41 92.85(13) . . ? C401 Sb2 O31 89.20(13) . . ? C501 Sb2 O31 94.93(14) . . ? C601 Sb2 O31 85.53(13) . . ? O41 Sb2 O31 177.44(11) . . ? C31 O31 Sb2 123.8(3) . . ? C41 O41 Sb2 119.7(2) . . ? O32 C31 O31 122.8(4) . . ? O32 C31 C33 121.5(4) . . ? O31 C31 C33 115.7(4) . . ? O33 C32 C37 118.0(4) . . ? O33 C32 C33 122.3(4) . . ? C37 C32 C33 119.8(5) . . ? C34 C33 C32 119.2(4) . . ? C34 C33 C31 120.8(4) . . ? C32 C33 C31 120.0(4) . . ? C35 C34 C33 120.6(4) . . ? C34 C35 C36 119.6(5) . . ? C37 C36 C35 121.2(4) . . ? C36 C37 C32 119.5(5) . . ? O42 C41 O41 122.2(4) . . ? O42 C41 C43 122.2(4) . . ? O41 C41 C43 115.6(3) . . ? O43 C42 C47 117.4(4) . . ? O43 C42 C43 122.3(4) . . ? C47 C42 C43 120.3(4) . . ? C42 C43 C44 118.0(4) . . ? C42 C43 C41 120.5(4) . . ? C44 C43 C41 121.5(4) . . ? C45 C44 C43 121.9(4) . . ? C44 C45 C46 118.8(5) . . ? C47 C46 C45 120.6(5) . . ? C46 C47 C42 120.5(4) . . ? C402 C401 C406 121.1(4) . . ? C402 C401 Sb2 119.4(3) . . ? C406 C401 Sb2 119.5(3) . . ? C401 C402 C403 119.3(4) . . ? C404 C403 C402 120.5(5) . . ? C403 C404 C405 119.8(4) . . ? C404 C405 C406 120.5(4) . . ? C401 C406 C405 118.7(4) . . ? C502 C501 C506 120.2(4) . . ? C502 C501 Sb2 119.5(3) . . ? C506 C501 Sb2 120.3(3) . . ? C501 C502 C503 119.6(5) . . ? C504 C503 C502 120.1(5) . . ? C504 C505 C506 120.5(5) . . ? C505 C504 C503 120.0(4) . . ? C501 C506 C505 119.5(5) . . ? C602 C601 C606 120.4(4) . . ? C602 C601 Sb2 117.4(3) . . ? C606 C601 Sb2 122.2(3) . . ? C601 C602 C603 119.7(4) . . ? C602 C603 C604 120.0(4) . . ? C605 C604 C603 120.0(4) . . ? C604 C605 C606 120.9(4) . . ? C601 C606 C605 119.1(4) . . ? Cl2 C1 Cl1 113.3(4) . . ? Cl2 C1 Cl3 108.1(4) . . ? Cl1 C1 Cl3 105.2(4) . . ? Cl6' C2 Cl4' 111.5(5) . . ? Cl6' C2 Cl4 135.2(8) . . ? Cl4' C2 Cl4 46.8(5) . . ? Cl6' C2 Cl5 62.0(5) . . ? Cl4' C2 Cl5 140.0(8) . . ? Cl4 C2 Cl5 107.2(3) . . ? Cl6' C2 Cl6 50.1(5) . . ? Cl4' C2 Cl6 66.8(5) . . ? Cl4 C2 Cl6 109.9(3) . . ? Cl5 C2 Cl6 110.5(3) . . ? Cl6' C2 Cl5' 109.8(5) . . ? Cl4' C2 Cl5' 108.6(5) . . ? Cl4 C2 Cl5' 62.7(5) . . ? Cl5 C2 Cl5' 50.2(5) . . ? Cl6 C2 Cl5' 146.3(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O12 0.84 1.89 2.625(4) 145.4 . O23 H23 O22 0.84 1.85 2.593(5) 147.2 . O23' H23' O21 0.84 1.78 2.541(13) 148.8 . O33 H33 O32 0.84 1.87 2.607(5) 145.2 . O43 H43 O42 0.84 1.87 2.608(4) 145.7 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.762 _refine_diff_density_min -1.441 _refine_diff_density_rms 0.121 data_s92-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H37 Bi O6' _chemical_formula_weight 894.74 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.102(2) _cell_length_b 20.609(4) _cell_length_c 18.706(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.59(3) _cell_angle_gamma 90.00 _cell_volume 3785.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 114607 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 4.707 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_correction_T_min 0.482 _exptl_absorpt_correction_T_max 0.634 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114607 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8684 _reflns_number_gt 7696 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8684 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 0.751 _refine_ls_restrained_S_all 0.751 _refine_ls_shift/su_max 0.037 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.358412(8) 0.358125(4) 0.402453(4) 0.01671(6) Uani 1 d . . . O1 O 0.45730(19) 0.26484(9) 0.45699(9) 0.0228(4) Uani 1 d . . . O2 O 0.5726(2) 0.33505(9) 0.53858(11) 0.0257(4) Uani 1 d . . . O3 O 0.6814(2) 0.24221(10) 0.63313(9) 0.0270(4) Uani 1 d . . . H3 H 0.6983 0.2811 0.6333 0.041 Uiso 1 calc R . . O4 O 0.26565(19) 0.43878(9) 0.32597(10) 0.0243(4) Uani 1 d . . . O5 O 0.37152(19) 0.50402(10) 0.41565(10) 0.0248(4) Uani 1 d . . . O6 O 0.23493(18) 0.60763(8) 0.34433(10) 0.0230(4) Uani 1 d . . . H6 H 0.2949 0.6085 0.3824 0.034 Uiso 1 calc R . . C1 C 0.5462(2) 0.27936(12) 0.51662(13) 0.0204(5) Uani 1 d . . . C2 C 0.6212(3) 0.22167(13) 0.55964(13) 0.0197(5) Uani 1 d . . . C3 C 0.5174(3) 0.16892(13) 0.56387(14) 0.0238(5) Uani 1 d . . . C4 C 0.4996(3) 0.11469(14) 0.51942(16) 0.0318(6) Uani 1 d . . . H4 H 0.5573 0.1076 0.4881 0.038 Uiso 1 calc R . . C5 C 0.3960(3) 0.07042(15) 0.52104(19) 0.0402(7) Uani 1 d . . . H5 H 0.3852 0.0341 0.4907 0.048 Uiso 1 calc R . . C6 C 0.3101(3) 0.07989(17) 0.56680(19) 0.0421(8) Uani 1 d . . . H6 H 0.2415 0.0501 0.5680 0.050 Uiso 1 calc R . . C7 C 0.3266(4) 0.13437(19) 0.6113(2) 0.0472(10) Uani 1 d . . . H7 H 0.2684 0.1413 0.6424 0.057 Uiso 1 calc R . . C8 C 0.4292(3) 0.17857(16) 0.60979(17) 0.0363(7) Uani 1 d . . . H8 H 0.4392 0.2151 0.6398 0.044 Uiso 1 calc R . . C9 C 0.7364(3) 0.19937(12) 0.52397(14) 0.0221(5) Uani 1 d . . . C10 C 0.7624(3) 0.22800(14) 0.46184(15) 0.0299(6) Uani 1 d . . . H10 H 0.7033 0.2595 0.4370 0.036 Uiso 1 calc R . . C11 C 0.8755(3) 0.21036(15) 0.43599(17) 0.0357(7) Uani 1 d . . . H11 H 0.8912 0.2298 0.3939 0.043 Uiso 1 calc R . . C12 C 0.9645(3) 0.16410(16) 0.47285(18) 0.0368(7) Uani 1 d . . . H12 H 1.0415 0.1530 0.4564 0.044 Uiso 1 calc R . . C13 C 0.9389(3) 0.13450(14) 0.5341(2) 0.0340(7) Uani 1 d . . . H13 H 0.9981 0.1028 0.5586 0.041 Uiso 1 calc R . . C14 C 0.8253(3) 0.15162(14) 0.55960(17) 0.0278(6) Uani 1 d . . . H14 H 0.8084 0.1310 0.6008 0.033 Uiso 1 calc R . . C15 C 0.3028(3) 0.49542(12) 0.35360(15) 0.0210(5) Uani 1 d . . . C16 C 0.2560(3) 0.55345(12) 0.30082(13) 0.0195(5) Uani 1 d . . . C17 C 0.1210(3) 0.53855(11) 0.24793(13) 0.0203(5) Uani 1 d . . . C18 C 0.1017(3) 0.54109(13) 0.17194(14) 0.0248(5) Uani 1 d . . . H18 H 0.1730 0.5542 0.1516 0.030 Uiso 1 calc R . . C19 C -0.0232(3) 0.52429(14) 0.12576(15) 0.0299(6) Uani 1 d . . . H19 H -0.0347 0.5260 0.0750 0.036 Uiso 1 calc R . . C20 C -0.1293(3) 0.50517(13) 0.15528(16) 0.0306(6) Uani 1 d . . . H20 H -0.2123 0.4935 0.1246 0.037 Uiso 1 calc R . . C21 C -0.1123(3) 0.50337(14) 0.23111(16) 0.0317(6) Uani 1 d . . . H21 H -0.1845 0.4911 0.2512 0.038 Uiso 1 calc R . . C22 C 0.0112(3) 0.51967(14) 0.27673(15) 0.0270(6) Uani 1 d . . . H22 H 0.0217 0.5181 0.3274 0.032 Uiso 1 calc R . . C23 C 0.3691(3) 0.56714(12) 0.26071(13) 0.0210(5) Uani 1 d . . . C24 C 0.4306(3) 0.51613(13) 0.23137(14) 0.0245(5) Uani 1 d . . . H24 H 0.4066 0.4735 0.2387 0.029 Uiso 1 calc R . . C25 C 0.5269(3) 0.52888(14) 0.19145(15) 0.0306(6) Uani 1 d . . . H25 H 0.5675 0.4946 0.1723 0.037 Uiso 1 calc R . . C26 C 0.5634(3) 0.59152(16) 0.17974(16) 0.0339(6) Uani 1 d . . . H26 H 0.6284 0.5997 0.1530 0.041 Uiso 1 calc R . . C27 C 0.5026(4) 0.64221(13) 0.2081(2) 0.0428(9) Uani 1 d . . . H27 H 0.5268 0.6847 0.2004 0.051 Uiso 1 calc R . . C28 C 0.4052(3) 0.63018(15) 0.24812(19) 0.0331(7) Uani 1 d . . . H28 H 0.3640 0.6647 0.2665 0.040 Uiso 1 calc R . . C29 C 0.2152(3) 0.29307(13) 0.32795(14) 0.0205(5) Uani 1 d . . . C30 C 0.2097(3) 0.22819(13) 0.34666(15) 0.0269(6) Uani 1 d . . . H30 H 0.2730 0.2112 0.3866 0.032 Uiso 1 calc R . . C31 C 0.1091(3) 0.18882(13) 0.30542(15) 0.0286(6) Uani 1 d . . . H31 H 0.1049 0.1453 0.3177 0.034 Uiso 1 calc R . . C32 C 0.0149(3) 0.21405(14) 0.24589(16) 0.0314(6) Uani 1 d . . . H32 H -0.0523 0.1874 0.2181 0.038 Uiso 1 calc R . . C33 C 0.0208(3) 0.27833(16) 0.22799(17) 0.0376(7) Uani 1 d . . . H33 H -0.0430 0.2951 0.1881 0.045 Uiso 1 calc R . . C34 C 0.1211(3) 0.31895(15) 0.26866(16) 0.0302(6) Uani 1 d . . . H34 H 0.1248 0.3625 0.2563 0.036 Uiso 1 calc R . . C35 C 0.5537(3) 0.37524(13) 0.37357(15) 0.0227(5) Uani 1 d . . . C36 C 0.5707(3) 0.34320(17) 0.31119(17) 0.0296(6) Uani 1 d . . . H36 H 0.4988 0.3207 0.2813 0.036 Uiso 1 calc R . . C37 C 0.6971(4) 0.34536(16) 0.29415(19) 0.0372(7) Uani 1 d . . . H37 H 0.7109 0.3244 0.2525 0.045 Uiso 1 calc R . . C38 C 0.8024(3) 0.37900(17) 0.33978(19) 0.0382(7) Uani 1 d . . . H38 H 0.8881 0.3794 0.3295 0.046 Uiso 1 calc R . . C39 C 0.7817(3) 0.41207(15) 0.40060(19) 0.0371(7) Uani 1 d . . . H39 H 0.8529 0.4355 0.4299 0.044 Uiso 1 calc R . . C40 C 0.6564(3) 0.41075(14) 0.41833(16) 0.0287(6) Uani 1 d . . . H40 H 0.6418 0.4330 0.4590 0.034 Uiso 1 calc R . . C41 C 0.2643(3) 0.37577(14) 0.49511(14) 0.0228(5) Uani 1 d . . . C42 C 0.3257(3) 0.41452(13) 0.55356(15) 0.0280(6) Uani 1 d . . . H42 H 0.4028 0.4388 0.5526 0.034 Uiso 1 calc R . . C43 C 0.2681(3) 0.41599(15) 0.61395(16) 0.0376(7) Uani 1 d . . . H43 H 0.3076 0.4413 0.6545 0.045 Uiso 1 calc R . . C44 C 0.1529(4) 0.3803(2) 0.6145(2) 0.0497(9) Uani 1 d . . . H44 H 0.1154 0.3817 0.6554 0.060 Uiso 1 calc R . . C45 C 0.0929(5) 0.3426(2) 0.5548(2) 0.0560(11) Uani 1 d . . . H45 H 0.0145 0.3191 0.5554 0.067 Uiso 1 calc R . . C46 C 0.1489(4) 0.3394(2) 0.4939(2) 0.0396(8) Uani 1 d . . . H46 H 0.1101 0.3136 0.4536 0.047 Uiso 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 0.01686(8) 0.01493(8) 0.01666(8) 0.00037(3) 0.00056(5) 0.00055(3) O1 0.0247(9) 0.0206(9) 0.0195(9) 0.0006(7) -0.0017(7) 0.0009(7) O2 0.0260(10) 0.0201(9) 0.0282(10) -0.0025(8) 0.0008(8) -0.0020(8) O3 0.0326(11) 0.0285(10) 0.0149(9) -0.0026(8) -0.0045(8) 0.0036(9) O4 0.0269(10) 0.0177(9) 0.0247(9) 0.0006(7) -0.0011(7) 0.0012(7) O5 0.0265(10) 0.0241(10) 0.0210(9) 0.0045(8) 0.0000(8) 0.0011(7) O6 0.0244(9) 0.0197(9) 0.0230(9) -0.0031(7) 0.0022(7) 0.0023(7) C1 0.0201(12) 0.0226(13) 0.0181(12) -0.0003(9) 0.0036(9) 0.0029(10) C2 0.0201(12) 0.0233(13) 0.0133(12) -0.0012(9) -0.0005(9) 0.0016(10) C3 0.0222(13) 0.0277(14) 0.0193(12) 0.0067(10) 0.0002(10) 0.0020(10) C4 0.0289(15) 0.0299(15) 0.0351(16) 0.0030(12) 0.0044(12) 0.0000(12) C5 0.0335(17) 0.0343(16) 0.0468(18) 0.0040(14) -0.0028(14) -0.0079(13) C6 0.0283(16) 0.0444(19) 0.0501(19) 0.0187(15) 0.0024(14) -0.0058(14) C7 0.0313(19) 0.070(3) 0.043(2) 0.0100(17) 0.0152(17) -0.0041(15) C8 0.0342(16) 0.0435(18) 0.0319(16) -0.0008(13) 0.0097(13) -0.0025(13) C9 0.0190(12) 0.0215(12) 0.0246(13) -0.0030(10) 0.0026(10) -0.0001(9) C10 0.0315(15) 0.0308(15) 0.0277(14) 0.0037(11) 0.0074(11) 0.0065(11) C11 0.0397(17) 0.0335(15) 0.0365(17) 0.0025(13) 0.0143(13) 0.0043(13) C12 0.0278(15) 0.0349(16) 0.0490(19) -0.0063(14) 0.0114(13) 0.0051(13) C13 0.0260(16) 0.0286(15) 0.046(2) 0.0006(12) 0.0057(14) 0.0111(11) C14 0.0259(15) 0.0294(14) 0.0262(15) 0.0042(11) 0.0026(12) 0.0041(11) C15 0.0166(12) 0.0214(12) 0.0255(13) 0.0045(10) 0.0056(10) 0.0024(10) C16 0.0217(12) 0.0163(11) 0.0195(12) 0.0009(9) 0.0030(9) 0.0034(9) C17 0.0222(12) 0.0147(11) 0.0223(12) -0.0002(9) 0.0019(10) 0.0039(9) C18 0.0235(13) 0.0272(14) 0.0233(13) 0.0007(10) 0.0044(10) 0.0023(10) C19 0.0329(15) 0.0309(14) 0.0217(13) -0.0039(11) -0.0021(11) 0.0031(12) C20 0.0239(14) 0.0263(13) 0.0362(15) -0.0026(11) -0.0041(11) -0.0008(11) C21 0.0207(14) 0.0343(15) 0.0391(16) 0.0087(12) 0.0052(12) -0.0020(11) C22 0.0237(14) 0.0331(15) 0.0245(13) 0.0049(11) 0.0060(11) 0.0046(11) C23 0.0201(12) 0.0206(12) 0.0201(12) 0.0012(9) 0.0003(9) 0.0006(9) C24 0.0217(13) 0.0234(12) 0.0284(13) -0.0006(10) 0.0059(10) -0.0010(10) C25 0.0261(14) 0.0357(15) 0.0307(14) -0.0057(12) 0.0078(11) 0.0021(12) C26 0.0315(16) 0.0426(17) 0.0315(15) -0.0016(13) 0.0154(12) -0.0074(13) C27 0.052(2) 0.0272(18) 0.057(2) 0.0065(12) 0.029(2) -0.0080(12) C28 0.0382(18) 0.0231(13) 0.0425(18) 0.0007(12) 0.0185(14) -0.0002(12) C29 0.0180(12) 0.0225(12) 0.0191(12) -0.0052(10) 0.0007(9) -0.0039(10) C30 0.0270(14) 0.0229(13) 0.0277(13) 0.0000(10) 0.0005(11) 0.0013(10) C31 0.0283(14) 0.0211(13) 0.0344(15) -0.0029(11) 0.0038(11) -0.0040(11) C32 0.0267(15) 0.0322(15) 0.0320(15) -0.0086(12) 0.0004(12) -0.0063(12) C33 0.0325(16) 0.0396(17) 0.0308(15) 0.0015(13) -0.0124(12) -0.0047(13) C34 0.0313(15) 0.0263(14) 0.0280(14) 0.0042(11) -0.0031(12) 0.0022(12) C35 0.0222(13) 0.0213(11) 0.0247(13) 0.0046(11) 0.0055(10) 0.0030(10) C36 0.0328(17) 0.0319(14) 0.0251(15) -0.0013(13) 0.0086(13) 0.0015(13) C37 0.0432(19) 0.0385(16) 0.0355(17) 0.0020(14) 0.0204(15) 0.0068(15) C38 0.0280(16) 0.0412(17) 0.051(2) 0.0114(15) 0.0198(14) 0.0045(14) C39 0.0285(16) 0.0348(16) 0.0477(18) 0.0045(13) 0.0086(13) -0.0064(12) C40 0.0284(14) 0.0249(14) 0.0321(15) -0.0013(11) 0.0056(11) -0.0025(11) C41 0.0239(13) 0.0235(12) 0.0219(13) -0.0003(10) 0.0074(10) 0.0030(11) C42 0.0278(14) 0.0300(14) 0.0254(13) -0.0047(11) 0.0049(11) 0.0013(11) C43 0.0503(19) 0.0376(17) 0.0250(15) -0.0059(12) 0.0087(13) 0.0020(14) C44 0.073(3) 0.046(2) 0.0411(18) -0.0054(18) 0.0351(18) -0.0071(18) C45 0.065(3) 0.059(2) 0.057(3) -0.018(2) 0.040(2) -0.028(2) C46 0.0373(19) 0.0471(18) 0.0406(19) -0.0146(17) 0.0218(15) -0.0173(17) _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 C35 2.193(3) . ? Bi1 C41 2.194(3) . ? Bi1 C29 2.210(2) . ? Bi1 O4 2.2490(18) . ? Bi1 O1 2.2925(18) . ? O1 C1 1.292(3) . ? O2 C1 1.227(3) . ? O3 C2 1.430(3) . ? O4 C15 1.296(3) . ? O5 C15 1.217(3) . ? O6 C16 1.427(3) . ? C1 C2 1.533(3) . ? C2 C3 1.526(4) . ? C2 C9 1.541(4) . ? C3 C4 1.379(4) . ? C3 C8 1.389(4) . ? C4 C5 1.394(4) . ? C5 C6 1.369(5) . ? C6 C7 1.384(5) . ? C7 C8 1.386(5) . ? C9 C10 1.382(4) . ? C9 C14 1.392(4) . ? C10 C11 1.390(4) . ? C11 C12 1.379(4) . ? C12 C13 1.375(5) . ? C13 C14 1.389(4) . ? C15 C16 1.552(3) . ? C16 C17 1.516(3) . ? C16 C23 1.534(4) . ? C17 C18 1.390(4) . ? C17 C22 1.397(4) . ? C18 C19 1.395(4) . ? C19 C20 1.373(4) . ? C20 C21 1.389(4) . ? C21 C22 1.378(4) . ? C23 C28 1.384(4) . ? C23 C24 1.397(4) . ? C24 C25 1.384(4) . ? C25 C26 1.374(4) . ? C26 C27 1.380(5) . ? C27 C28 1.391(5) . ? C29 C30 1.387(4) . ? C29 C34 1.387(4) . ? C30 C31 1.384(4) . ? C31 C32 1.385(4) . ? C32 C33 1.371(4) . ? C33 C34 1.394(4) . ? C35 C40 1.380(4) . ? C35 C36 1.386(4) . ? C36 C37 1.388(5) . ? C37 C38 1.384(5) . ? C38 C39 1.384(5) . ? C39 C40 1.382(4) . ? C41 C46 1.382(4) . ? C41 C42 1.378(4) . ? C42 C43 1.387(4) . ? C43 C44 1.378(5) . ? C44 C45 1.379(6) . ? C45 C46 1.388(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C35 Bi1 C41 138.58(10) . . ? C35 Bi1 C29 115.82(10) . . ? C41 Bi1 C29 104.94(10) . . ? C35 Bi1 O4 89.36(9) . . ? C41 Bi1 O4 100.77(9) . . ? C29 Bi1 O4 86.22(9) . . ? C35 Bi1 O1 85.49(8) . . ? C41 Bi1 O1 90.68(9) . . ? C29 Bi1 O1 85.64(8) . . ? O4 Bi1 O1 167.36(7) . . ? C1 O1 Bi1 109.37(15) . . ? C15 O4 Bi1 111.95(15) . . ? O2 C1 O1 123.9(2) . . ? O2 C1 C2 120.5(2) . . ? O1 C1 C2 115.5(2) . . ? O3 C2 C3 107.6(2) . . ? O3 C2 C1 108.7(2) . . ? C3 C2 C1 108.6(2) . . ? O3 C2 C9 108.1(2) . . ? C3 C2 C9 114.1(2) . . ? C1 C2 C9 109.6(2) . . ? C4 C3 C8 118.5(3) . . ? C4 C3 C2 122.6(2) . . ? C8 C3 C2 118.6(3) . . ? C3 C4 C5 120.6(3) . . ? C6 C5 C4 120.7(3) . . ? C5 C6 C7 119.2(3) . . ? C6 C7 C8 120.4(3) . . ? C7 C8 C3 120.7(3) . . ? C10 C9 C14 118.4(3) . . ? C10 C9 C2 123.3(2) . . ? C14 C9 C2 118.1(2) . . ? C9 C10 C11 121.0(3) . . ? C12 C11 C10 120.0(3) . . ? C11 C12 C13 119.7(3) . . ? C12 C13 C14 120.4(3) . . ? C13 C14 C9 120.5(3) . . ? O5 C15 O4 123.9(2) . . ? O5 C15 C16 121.0(2) . . ? O4 C15 C16 115.1(2) . . ? O6 C16 C17 107.39(19) . . ? O6 C16 C23 111.3(2) . . ? C17 C16 C23 112.2(2) . . ? O6 C16 C15 107.70(19) . . ? C17 C16 C15 110.6(2) . . ? C23 C16 C15 107.59(19) . . ? C18 C17 C22 118.2(2) . . ? C18 C17 C16 123.2(2) . . ? C22 C17 C16 118.6(2) . . ? C17 C18 C19 120.9(3) . . ? C20 C19 C18 120.0(3) . . ? C19 C20 C21 119.8(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C17 121.0(3) . . ? C28 C23 C24 118.7(3) . . ? C28 C23 C16 120.8(2) . . ? C24 C23 C16 120.3(2) . . ? C25 C24 C23 120.2(3) . . ? C26 C25 C24 120.9(3) . . ? C25 C26 C27 119.3(3) . . ? C26 C27 C28 120.5(3) . . ? C23 C28 C27 120.4(3) . . ? C30 C29 C34 120.8(2) . . ? C30 C29 Bi1 119.02(18) . . ? C34 C29 Bi1 119.7(2) . . ? C31 C30 C29 119.5(2) . . ? C32 C31 C30 120.2(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C34 121.0(3) . . ? C29 C34 C33 118.6(3) . . ? C40 C35 C36 122.6(3) . . ? C40 C35 Bi1 121.8(2) . . ? C36 C35 Bi1 115.3(2) . . ? C37 C36 C35 118.7(3) . . ? C36 C37 C38 119.4(3) . . ? C37 C38 C39 120.7(3) . . ? C40 C39 C38 120.8(3) . . ? C35 C40 C39 117.7(3) . . ? C46 C41 C42 123.3(3) . . ? C46 C41 Bi1 114.7(2) . . ? C42 C41 Bi1 121.7(2) . . ? C41 C42 C43 117.5(3) . . ? C44 C43 C42 120.7(3) . . ? C43 C44 C45 120.4(3) . . ? C44 C45 C46 120.3(4) . . ? C41 C46 C45 117.7(3) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.001 _refine_diff_density_min -1.986 _refine_diff_density_rms 0.111