# 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 of Bismuth and Antimony Complexes of the "Larger" Calix[n]arenes (n = 6-8); From Mononuclear to Tetranuclear Complexes ; loop_ _publ_author_name 'Tracy Hanna' 'Daniel Mendoza-Espinosa' 'Arnold Rheingold' data_tcu107m _database_code_depnum_ccdc_archive 'CCDC 721515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C132 H162 Bi2 O12, 2(C4 H10 O)' _chemical_formula_sum 'C140 H182 Bi2 O14' _chemical_formula_weight 2506.90 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' 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 14.536(3) _cell_length_b 16.592(3) _cell_length_c 17.299(3) _cell_angle_alpha 117.870(3) _cell_angle_beta 107.174(3) _cell_angle_gamma 94.819(3) _cell_volume 3399.9(11) _cell_formula_units_Z 1 _cell_measurement_temperature 223(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 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 2.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6484 _exptl_absorpt_correction_T_max 0.8168 _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 23002 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.1403 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11845 _reflns_number_gt 7937 _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. 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 781.2 \%A^3^ and contain 80 electrons. The electron density was modelled as 2 diethyl ether molecules which accounts for 84 electrons. The 2 diethyl molecules where added in the formula weight on the structure of asymmetric unit. ; _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^)+(0.0678P)^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 11845 _refine_ls_number_parameters 657 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.946 _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 0.50016(2) 0.53455(2) 0.40688(2) 0.03030(12) Uani 1 1 d . . . O1 O 0.6275(4) 0.5960(4) 0.3910(4) 0.0385(14) Uani 1 1 d . . . C1 C 0.6791(6) 0.5480(6) 0.3379(6) 0.033(2) Uani 1 1 d . . . O2 O 0.5402(4) 0.4092(4) 0.3508(4) 0.0343(14) Uani 1 1 d . . . C2 C 0.7836(6) 0.5834(6) 0.3747(6) 0.035(2) Uani 1 1 d . . . O3 O 0.4132(4) 0.4386(4) 0.4557(4) 0.0290(13) Uani 1 1 d . . . C3 C 0.8366(6) 0.5336(7) 0.3199(7) 0.043(2) Uani 1 1 d . . . H3A H 0.9065 0.5563 0.3453 0.051 Uiso 1 1 calc R . . C4 C 0.7925(6) 0.4540(7) 0.2318(7) 0.041(2) Uani 1 1 d . . . O4 O 0.3023(4) 0.6837(4) 0.5307(5) 0.0511(17) Uani 1 1 d . . . H4A H 0.3216 0.7411 0.5517 0.077 Uiso 1 1 calc R . . O5 O 0.5467(5) 0.8525(5) 0.5370(5) 0.061(2) Uani 1 1 d . . . H5A H 0.5969 0.8321 0.5360 0.092 Uiso 1 1 calc R . . C5 C 0.6890(6) 0.4236(6) 0.1959(6) 0.034(2) Uani 1 1 d . . . H5B H 0.6560 0.3699 0.1352 0.041 Uiso 1 1 calc R . . O6 O 0.7010(5) 0.7860(4) 0.5079(5) 0.0603(19) Uani 1 1 d . . . H6A H 0.6566 0.8145 0.5088 0.090 Uiso 1 1 calc R . . C6 C 0.6325(6) 0.4702(6) 0.2470(6) 0.032(2) Uani 1 1 d . . . C7 C 0.8501(7) 0.3992(9) 0.1707(7) 0.059(3) Uani 1 1 d . . . C8 C 0.9630(7) 0.4314(9) 0.2294(8) 0.083(4) Uani 1 1 d . . . H8A H 0.9973 0.3963 0.1895 0.124 Uiso 1 1 calc R . . H8B H 0.9752 0.4199 0.2811 0.124 Uiso 1 1 calc R . . H8C H 0.9875 0.4984 0.2545 0.124 Uiso 1 1 calc R . . C9 C 0.8317(8) 0.4219(10) 0.0910(8) 0.089(4) Uani 1 1 d . . . H9\A H 0.8660 0.3879 0.0504 0.133 Uiso 1 1 calc R . . H9\B H 0.8570 0.4893 0.1186 0.133 Uiso 1 1 calc R . . H9\C H 0.7607 0.4027 0.0539 0.133 Uiso 1 1 calc R . . C10 C 0.8140(9) 0.2916(8) 0.1272(8) 0.077(4) Uani 1 1 d . . . H10A H 0.8506 0.2595 0.0884 0.116 Uiso 1 1 calc R . . H10B H 0.7433 0.2699 0.0884 0.116 Uiso 1 1 calc R . . H10C H 0.8254 0.2778 0.1773 0.116 Uiso 1 1 calc R . . C11 C 0.5197(5) 0.4330(6) 0.1959(6) 0.031(2) Uani 1 1 d . . . H11A H 0.5014 0.4263 0.1335 0.037 Uiso 1 1 calc R . . H11B H 0.4886 0.4796 0.2315 0.037 Uiso 1 1 calc R . . C12 C 0.4776(6) 0.3377(6) 0.1830(6) 0.033(2) Uani 1 1 d . . . C13 C 0.4289(6) 0.2573(6) 0.0944(6) 0.037(2) Uani 1 1 d . . . H13A H 0.4227 0.2612 0.0407 0.045 Uiso 1 1 calc R . . C14 C 0.3883(6) 0.1703(6) 0.0820(6) 0.040(2) Uani 1 1 d . A . C15 C 0.3966(6) 0.1699(6) 0.1634(6) 0.038(2) Uani 1 1 d . . . H15A H 0.3695 0.1128 0.1573 0.046 Uiso 1 1 calc R . . C16 C 0.4423(5) 0.2482(6) 0.2531(6) 0.0270(18) Uani 1 1 d . . . C17 C 0.4872(6) 0.3338(6) 0.2630(6) 0.0293(19) Uani 1 1 d . . . C18 C 0.3326(9) 0.0852(8) -0.0171(7) 0.073(4) Uani 1 1 d . . . C19 C 0.424(3) 0.055(2) -0.057(2) 0.072(13) Uiso 0.37(3) 1 d P A 5 H19A H 0.3954 0.0013 -0.1206 0.108 Uiso 0.37(3) 1 calc PR A 5 H19B H 0.4702 0.0395 -0.0160 0.108 Uiso 0.37(3) 1 calc PR A 5 H19C H 0.4589 0.1082 -0.0562 0.108 Uiso 0.37(3) 1 calc PR A 5 C19A C 0.3660(17) 0.0847(15) -0.0875(15) 0.082(8) Uiso 0.63(3) 1 d P A 6 H19D H 0.3224 0.1085 -0.1214 0.124 Uiso 0.63(3) 1 calc PR A 6 H19E H 0.3646 0.0206 -0.1316 0.124 Uiso 0.63(3) 1 calc PR A 6 H19F H 0.4336 0.1245 -0.0572 0.124 Uiso 0.63(3) 1 calc PR A 6 C20 C 0.3016(11) -0.0053(8) -0.0186(9) 0.107(5) Uani 1 1 d . A . H20A H 0.2673 -0.0569 -0.0835 0.160 Uiso 1 1 calc R . . H20B H 0.2573 0.0025 0.0153 0.160 Uiso 1 1 calc R . . H20C H 0.3604 -0.0194 0.0116 0.160 Uiso 1 1 calc R . . C21 C 0.2350(14) 0.1028(12) -0.0615(12) 0.184(10) Uani 1 1 d . A . H21A H 0.2493 0.1596 -0.0639 0.276 Uiso 1 1 calc R . . H21B H 0.1949 0.1106 -0.0237 0.276 Uiso 1 1 calc R . . H21C H 0.1988 0.0494 -0.1251 0.276 Uiso 1 1 calc R . . C22 C 0.4344(6) 0.2488(6) 0.3383(6) 0.032(2) Uani 1 1 d . . . H22A H 0.4906 0.2968 0.3957 0.038 Uiso 1 1 calc R . . H22B H 0.4355 0.1870 0.3319 0.038 Uiso 1 1 calc R . . C23 C 0.3361(6) 0.2710(6) 0.3438(6) 0.0282(19) Uani 1 1 d . . . C24 C 0.2490(6) 0.1998(6) 0.2881(6) 0.032(2) Uani 1 1 d . . . H24A H 0.2532 0.1372 0.2554 0.038 Uiso 1 1 calc R . . C25 C 0.1564(6) 0.2158(6) 0.2782(6) 0.038(2) Uani 1 1 d . . . C26 C 0.1520(6) 0.3088(6) 0.3257(6) 0.034(2) Uani 1 1 d . . . H26A H 0.0891 0.3215 0.3161 0.041 Uiso 1 1 calc R . . C27 C 0.2355(6) 0.3829(6) 0.3859(6) 0.0275(19) Uani 1 1 d . . . C28 C 0.3286(5) 0.3638(6) 0.3954(6) 0.030(2) Uani 1 1 d . . . C29 C 0.0597(7) 0.1336(7) 0.2128(7) 0.052(3) Uani 1 1 d . . . C30 C -0.0140(8) 0.1485(8) 0.2630(9) 0.081(4) Uani 1 1 d . . . H30A H -0.0261 0.2102 0.2809 0.121 Uiso 1 1 calc R . . H30B H 0.0139 0.1447 0.3191 0.121 Uiso 1 1 calc R . . H30C H -0.0764 0.1000 0.2207 0.121 Uiso 1 1 calc R . . C31 C 0.0790(8) 0.0373(7) 0.1867(10) 0.095(5) Uani 1 1 d . . . H31A H 0.1253 0.0270 0.1547 0.142 Uiso 1 1 calc R . . H31B H 0.0167 -0.0115 0.1452 0.142 Uiso 1 1 calc R . . H31C H 0.1073 0.0349 0.2437 0.142 Uiso 1 1 calc R . . C32 C 0.0140(8) 0.1352(9) 0.1215(8) 0.093(5) Uani 1 1 d . . . H32A H -0.0002 0.1957 0.1367 0.140 Uiso 1 1 calc R . . H32B H -0.0474 0.0851 0.0801 0.140 Uiso 1 1 calc R . . H32C H 0.0607 0.1256 0.0899 0.140 Uiso 1 1 calc R . . C33 C 0.2312(6) 0.4838(6) 0.4349(6) 0.034(2) Uani 1 1 d . . . H33A H 0.2799 0.5169 0.5002 0.041 Uiso 1 1 calc R . . H33B H 0.1648 0.4856 0.4371 0.041 Uiso 1 1 calc R . . C34 C 0.2529(6) 0.5361(6) 0.3860(6) 0.031(2) Uani 1 1 d . . . C35 C 0.2356(6) 0.4858(6) 0.2902(6) 0.034(2) Uani 1 1 d . . . H35A H 0.2125 0.4195 0.2565 0.041 Uiso 1 1 calc R . . C36 C 0.2517(7) 0.5315(7) 0.2421(7) 0.041(2) Uani 1 1 d . . . C37 C 0.2900(7) 0.6287(7) 0.2961(7) 0.050(3) Uani 1 1 d . . . H37A H 0.3058 0.6602 0.2667 0.060 Uiso 1 1 calc R . . C38 C 0.3067(6) 0.6828(6) 0.3927(7) 0.042(2) Uani 1 1 d . . . C39 C 0.2864(6) 0.6344(6) 0.4372(6) 0.036(2) Uani 1 1 d . . . C40 C 0.2187(7) 0.4795(7) 0.1361(7) 0.050(3) Uani 1 1 d . . . C41 C 0.2046(11) 0.3726(8) 0.0924(8) 0.096(5) Uani 1 1 d . . . H41A H 0.1570 0.3481 0.1104 0.144 Uiso 1 1 calc R . . H41B H 0.2681 0.3602 0.1151 0.144 Uiso 1 1 calc R . . H41C H 0.1799 0.3419 0.0241 0.144 Uiso 1 1 calc R . . C42 C 0.1186(7) 0.4963(9) 0.0943(8) 0.079(4) Uani 1 1 d . . . H42A H 0.0693 0.4732 0.1116 0.119 Uiso 1 1 calc R . . H42B H 0.0967 0.4629 0.0259 0.119 Uiso 1 1 calc R . . H42C H 0.1266 0.5634 0.1187 0.119 Uiso 1 1 calc R . . C43 C 0.2947(8) 0.5146(9) 0.1047(7) 0.074(4) Uani 1 1 d . . . H43A H 0.3589 0.5053 0.1310 0.111 Uiso 1 1 calc R . . H43B H 0.3015 0.5812 0.1270 0.111 Uiso 1 1 calc R . . H43C H 0.2712 0.4791 0.0362 0.111 Uiso 1 1 calc R . . C44 C 0.3400(7) 0.7902(6) 0.4471(7) 0.052(3) Uani 1 1 d . . . H44A H 0.2805 0.8142 0.4438 0.062 Uiso 1 1 calc R . . H44B H 0.3779 0.8125 0.5137 0.062 Uiso 1 1 calc R . . C45 C 0.4036(8) 0.8327(6) 0.4128(7) 0.050(3) Uani 1 1 d . . . C46 C 0.3631(9) 0.8423(7) 0.3370(8) 0.062(3) Uani 1 1 d . . . H46A H 0.2932 0.8228 0.3061 0.074 Uiso 1 1 calc R . . C47 C 0.4180(11) 0.8790(8) 0.3027(9) 0.074(4) Uani 1 1 d . B . C48 C 0.5238(11) 0.9087(7) 0.3528(9) 0.070(4) Uani 1 1 d . . . H48A H 0.5636 0.9330 0.3304 0.084 Uiso 1 1 calc R . . C49 C 0.5717(9) 0.9040(7) 0.4331(8) 0.056(3) Uani 1 1 d . . . C50 C 0.5084(8) 0.8607(6) 0.4596(7) 0.049(3) Uani 1 1 d . . . C51 C 0.3712(13) 0.8839(9) 0.2121(10) 0.100(5) Uani 1 1 d D . . C52 C 0.3899(14) 0.8091(11) 0.1333(10) 0.137(7) Uani 1 1 d . B . H52A H 0.3578 0.8104 0.0763 0.206 Uiso 1 1 calc R . . H52B H 0.3629 0.7481 0.1236 0.206 Uiso 1 1 calc R . . H52C H 0.4611 0.8195 0.1482 0.206 Uiso 1 1 calc R . . C53 C 0.299(2) 0.942(2) 0.228(2) 0.083(10) Uiso 0.463(19) 1 d P B 1 H53A H 0.3353 1.0079 0.2707 0.125 Uiso 0.463(19) 1 calc PR B 1 H53B H 0.2599 0.9229 0.2565 0.125 Uiso 0.463(19) 1 calc PR B 1 H53C H 0.2557 0.9323 0.1686 0.125 Uiso 0.463(19) 1 calc PR B 1 C53A C 0.2503(16) 0.8338(17) 0.1610(16) 0.078(8) Uiso 0.537(19) 1 d P B 2 H53D H 0.2355 0.7848 0.1746 0.117 Uiso 0.537(19) 1 calc PR B 2 H53E H 0.2293 0.8062 0.0933 0.117 Uiso 0.537(19) 1 calc PR B 2 H53F H 0.2150 0.8810 0.1853 0.117 Uiso 0.537(19) 1 calc PR B 2 C54 C 0.452(2) 0.9644(17) 0.222(2) 0.086(10) Uiso 0.463(19) 1 d PD B 3 H54A H 0.5185 0.9685 0.2603 0.129 Uiso 0.463(19) 1 calc PR B 3 H54B H 0.4371 1.0248 0.2516 0.129 Uiso 0.463(19) 1 calc PR B 3 H54C H 0.4501 0.9483 0.1596 0.129 Uiso 0.463(19) 1 calc PR B 3 C54A C 0.385(2) 0.973(2) 0.226(2) 0.123(12) Uiso 0.537(19) 1 d P B 4 H54D H 0.4557 1.0040 0.2564 0.185 Uiso 0.537(19) 1 calc PR B 4 H54E H 0.3512 1.0081 0.2666 0.185 Uiso 0.537(19) 1 calc PR B 4 H54F H 0.3576 0.9689 0.1660 0.185 Uiso 0.537(19) 1 calc PR B 4 C55 C 0.6818(8) 0.9460(7) 0.4892(8) 0.066(3) Uani 1 1 d . . . H55A H 0.6950 0.9617 0.5542 0.079 Uiso 1 1 calc R . . H55B H 0.7009 1.0053 0.4913 0.079 Uiso 1 1 calc R . . C56 C 0.7483(8) 0.8840(7) 0.4524(7) 0.053(3) Uani 1 1 d . . . C57 C 0.8039(8) 0.9028(8) 0.4069(7) 0.065(3) Uani 1 1 d . . . H57A H 0.7969 0.9526 0.3956 0.078 Uiso 1 1 calc R . . C58 C 0.8698(8) 0.8502(8) 0.3772(7) 0.057(3) Uani 1 1 d . . . C59 C 0.8793(7) 0.7778(7) 0.3970(7) 0.051(3) Uani 1 1 d . . . H59A H 0.9239 0.7419 0.3790 0.061 Uiso 1 1 calc R . . C60 C 0.8252(7) 0.7576(6) 0.4421(6) 0.042(2) Uani 1 1 d . . . C61 C 0.7593(7) 0.8084(6) 0.4673(6) 0.046(3) Uani 1 1 d . . . C62 C 0.9263(9) 0.8655(9) 0.3215(9) 0.071(3) Uani 1 1 d . . . C63 C 0.9291(13) 0.9626(10) 0.3294(12) 0.129(6) Uani 1 1 d . . . H63A H 0.8615 0.9669 0.3057 0.193 Uiso 1 1 calc R . . H63B H 0.9647 0.9691 0.2923 0.193 Uiso 1 1 calc R . . H63C H 0.9630 1.0126 0.3950 0.193 Uiso 1 1 calc R . . C64 C 1.0353(10) 0.8678(11) 0.3628(10) 0.114(5) Uani 1 1 d . . . H64A H 1.0394 0.8081 0.3590 0.170 Uiso 1 1 calc R . . H64B H 1.0652 0.9187 0.4284 0.170 Uiso 1 1 calc R . . H64C H 1.0707 0.8779 0.3272 0.170 Uiso 1 1 calc R . . C65 C 0.8760(10) 0.7910(11) 0.2202(9) 0.110(5) Uani 1 1 d . . . H65A H 0.8074 0.7932 0.1971 0.166 Uiso 1 1 calc R . . H65B H 0.8773 0.7296 0.2129 0.166 Uiso 1 1 calc R . . H65C H 0.9106 0.8016 0.1842 0.166 Uiso 1 1 calc R . . C66 C 0.8353(7) 0.6778(6) 0.4617(6) 0.044(2) Uani 1 1 d . . . H66A H 0.9062 0.6814 0.4880 0.053 Uiso 1 1 calc R . . H66B H 0.8071 0.6855 0.5089 0.053 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 0.02980(17) 0.0305(2) 0.0337(2) 0.01929(16) 0.01183(14) 0.00595(13) O1 0.041(3) 0.038(4) 0.043(4) 0.022(3) 0.023(3) 0.013(3) C1 0.038(5) 0.040(6) 0.041(6) 0.031(5) 0.022(4) 0.012(4) O2 0.040(3) 0.027(3) 0.028(3) 0.011(3) 0.011(3) -0.003(3) C2 0.031(5) 0.038(6) 0.037(6) 0.029(5) 0.002(4) -0.005(4) O3 0.031(3) 0.021(3) 0.037(4) 0.016(3) 0.016(3) 0.000(3) C3 0.034(5) 0.059(7) 0.041(6) 0.033(6) 0.013(5) 0.004(5) C4 0.036(5) 0.054(7) 0.042(6) 0.032(6) 0.015(5) 0.010(5) O4 0.063(4) 0.027(4) 0.051(5) 0.027(4) -0.003(3) 0.002(3) O5 0.083(5) 0.075(5) 0.064(5) 0.056(5) 0.039(4) 0.032(4) C5 0.035(5) 0.039(5) 0.030(5) 0.020(5) 0.013(4) 0.006(4) O6 0.081(5) 0.052(5) 0.078(5) 0.043(4) 0.051(4) 0.024(4) C6 0.031(4) 0.043(6) 0.033(5) 0.028(5) 0.014(4) 0.010(4) C7 0.042(6) 0.093(9) 0.060(7) 0.047(7) 0.026(5) 0.028(6) C8 0.051(7) 0.114(11) 0.088(10) 0.050(9) 0.033(7) 0.034(7) C9 0.070(8) 0.164(14) 0.084(9) 0.086(10) 0.053(7) 0.057(9) C10 0.094(9) 0.070(9) 0.081(9) 0.035(8) 0.052(8) 0.041(7) C11 0.028(4) 0.040(5) 0.028(5) 0.022(5) 0.010(4) 0.002(4) C12 0.026(4) 0.037(6) 0.039(6) 0.020(5) 0.016(4) 0.006(4) C13 0.035(5) 0.045(6) 0.024(5) 0.014(5) 0.008(4) 0.003(4) C14 0.040(5) 0.031(5) 0.038(6) 0.012(5) 0.015(4) -0.003(4) C15 0.037(5) 0.032(5) 0.041(6) 0.019(5) 0.012(4) 0.001(4) C16 0.025(4) 0.020(5) 0.028(5) 0.010(4) 0.005(4) 0.004(4) C17 0.025(4) 0.032(5) 0.033(5) 0.017(5) 0.014(4) 0.005(4) C18 0.099(9) 0.042(7) 0.028(6) -0.001(6) 0.006(6) -0.035(6) C20 0.158(14) 0.047(8) 0.054(9) -0.004(7) 0.027(9) -0.026(9) C21 0.173(18) 0.121(16) 0.113(15) 0.051(13) -0.093(13) -0.046(13) C22 0.036(5) 0.019(5) 0.034(5) 0.014(4) 0.007(4) 0.000(4) C23 0.035(5) 0.023(5) 0.030(5) 0.016(4) 0.014(4) 0.005(4) C24 0.033(5) 0.027(5) 0.028(5) 0.013(4) 0.007(4) -0.003(4) C25 0.034(5) 0.037(6) 0.042(6) 0.026(5) 0.009(4) -0.003(4) C26 0.023(4) 0.047(6) 0.032(5) 0.026(5) 0.005(4) 0.002(4) C27 0.031(4) 0.028(5) 0.038(5) 0.025(5) 0.017(4) 0.007(4) C28 0.024(4) 0.038(5) 0.028(5) 0.021(5) 0.006(4) -0.004(4) C29 0.035(5) 0.044(6) 0.061(7) 0.021(6) 0.010(5) -0.001(5) C30 0.054(7) 0.061(8) 0.093(10) 0.020(7) 0.028(7) -0.018(6) C31 0.047(7) 0.037(7) 0.151(13) 0.026(8) 0.022(8) -0.016(5) C32 0.067(8) 0.110(11) 0.056(8) 0.035(8) -0.009(7) -0.029(8) C33 0.023(4) 0.039(6) 0.040(6) 0.019(5) 0.015(4) 0.006(4) C34 0.030(4) 0.027(5) 0.041(6) 0.019(5) 0.013(4) 0.012(4) C35 0.032(5) 0.030(5) 0.032(5) 0.011(5) 0.008(4) 0.010(4) C36 0.046(5) 0.050(7) 0.040(6) 0.030(6) 0.020(5) 0.023(5) C37 0.067(7) 0.046(7) 0.060(7) 0.039(6) 0.031(6) 0.025(6) C38 0.043(5) 0.035(6) 0.050(7) 0.025(5) 0.015(5) 0.016(4) C39 0.042(5) 0.034(6) 0.032(6) 0.016(5) 0.014(4) 0.014(4) C40 0.048(6) 0.065(7) 0.034(6) 0.026(6) 0.012(5) 0.022(5) C41 0.176(14) 0.059(9) 0.048(8) 0.023(7) 0.041(9) 0.037(9) C42 0.060(7) 0.127(11) 0.059(8) 0.052(8) 0.022(6) 0.042(8) C43 0.076(8) 0.118(11) 0.059(8) 0.059(8) 0.041(7) 0.037(8) C44 0.063(6) 0.040(6) 0.062(7) 0.028(6) 0.030(6) 0.023(5) C45 0.083(8) 0.023(5) 0.059(7) 0.029(5) 0.033(6) 0.020(5) C46 0.091(8) 0.045(7) 0.063(8) 0.038(7) 0.026(7) 0.032(6) C47 0.128(12) 0.047(8) 0.061(8) 0.031(7) 0.041(8) 0.049(8) C48 0.138(12) 0.035(7) 0.074(9) 0.041(7) 0.065(9) 0.034(7) C49 0.097(9) 0.032(6) 0.063(8) 0.030(6) 0.049(7) 0.027(6) C50 0.086(8) 0.024(5) 0.042(6) 0.019(5) 0.027(6) 0.013(5) C51 0.199(17) 0.062(9) 0.068(10) 0.048(9) 0.056(11) 0.054(11) C52 0.218(19) 0.088(12) 0.067(11) 0.037(10) 0.012(12) 0.036(13) C55 0.090(9) 0.044(7) 0.073(8) 0.038(7) 0.035(7) 0.000(6) C56 0.072(7) 0.033(6) 0.057(7) 0.022(6) 0.033(6) 0.001(5) C57 0.087(8) 0.053(7) 0.066(8) 0.040(7) 0.033(7) -0.003(6) C58 0.063(7) 0.062(8) 0.054(7) 0.037(6) 0.024(6) -0.001(6) C59 0.053(6) 0.050(6) 0.053(7) 0.035(6) 0.017(5) -0.005(5) C60 0.045(5) 0.035(6) 0.041(6) 0.022(5) 0.011(5) -0.007(5) C61 0.065(6) 0.034(6) 0.036(6) 0.018(5) 0.019(5) -0.010(5) C62 0.071(8) 0.082(9) 0.075(9) 0.052(8) 0.032(7) 0.002(7) C63 0.205(17) 0.105(12) 0.182(16) 0.111(13) 0.142(15) 0.047(12) C64 0.095(10) 0.153(15) 0.123(13) 0.098(12) 0.045(10) -0.007(10) C65 0.111(11) 0.149(15) 0.063(10) 0.054(10) 0.034(9) -0.003(10) C66 0.048(6) 0.039(6) 0.040(6) 0.022(5) 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 O2 2.063(6) . ? Bi1 O3 2.141(5) 2_666 ? Bi1 O1 2.188(5) . ? Bi1 O3 2.529(5) . ? O1 C1 1.366(9) . ? C1 C6 1.388(11) . ? C1 C2 1.409(11) . ? O2 C17 1.356(9) . ? C2 C3 1.408(12) . ? C2 C66 1.488(11) . ? O3 C28 1.384(9) . ? O3 Bi1 2.141(5) 2_666 ? C3 C4 1.370(12) . ? C3 H3A 0.9400 . ? C4 C5 1.389(11) . ? C4 C7 1.549(13) . ? O4 C39 1.360(10) . ? O4 H4A 0.8300 . ? O5 C50 1.367(11) . ? O5 H5A 0.8300 . ? C5 C6 1.397(11) . ? C5 H5B 0.9400 . ? O6 C61 1.375(10) . ? O6 H6A 0.8300 . ? C6 C11 1.521(10) . ? C7 C8 1.539(13) . ? C7 C10 1.543(15) . ? C7 C9 1.549(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9\A 0.9700 . ? C9 H9\B 0.9700 . ? C9 H9\C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.534(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C17 1.381(11) . ? C12 C13 1.385(11) . ? C13 C14 1.404(12) . ? C13 H13A 0.9400 . ? C14 C15 1.380(12) . ? C14 C18 1.521(12) . ? C15 C16 1.377(11) . ? C15 H15A 0.9400 . ? C16 C17 1.422(11) . ? C16 C22 1.507(11) . ? C18 C19A 1.43(2) . ? C18 C20 1.518(16) . ? C18 C21 1.52(2) . ? C18 C19 1.67(3) . ? 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 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.524(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.376(10) . ? C23 C28 1.407(11) . ? C24 C25 1.371(11) . ? C24 H24A 0.9400 . ? C25 C26 1.386(12) . ? C25 C29 1.553(12) . ? C26 C27 1.369(10) . ? C26 H26A 0.9400 . ? C27 C28 1.395(10) . ? C27 C33 1.500(11) . ? C29 C31 1.522(14) . ? C29 C30 1.534(13) . ? C29 C32 1.536(14) . ? 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 1.537(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.389(11) . ? C34 C39 1.394(11) . ? C35 C36 1.415(12) . ? C35 H35A 0.9400 . ? C36 C37 1.384(13) . ? C36 C40 1.506(12) . ? C37 C38 1.406(13) . ? C37 H37A 0.9400 . ? C38 C39 1.413(12) . ? C38 C44 1.522(12) . ? C40 C41 1.534(15) . ? C40 C42 1.535(13) . ? C40 C43 1.548(13) . ? 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 1.519(13) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.360(13) . ? C45 C50 1.412(14) . ? C46 C47 1.377(16) . ? C46 H46A 0.9400 . ? C47 C48 1.429(17) . ? C47 C51 1.558(16) . ? C48 C49 1.400(15) . ? C48 H48A 0.9400 . ? C49 C50 1.420(13) . ? C49 C55 1.501(15) . ? C51 C54A 1.36(3) . ? C51 C52 1.470(18) . ? C51 C53 1.48(3) . ? C51 C54 1.616(17) . ? C51 C53A 1.65(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C53A H53D 0.9700 . ? C53A H53E 0.9700 . ? C53A H53F 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C54A H54D 0.9700 . ? C54A H54E 0.9700 . ? C54A H54F 0.9700 . ? C55 C56 1.521(14) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.390(13) . ? C56 C61 1.406(13) . ? C57 C58 1.398(14) . ? C57 H57A 0.9400 . ? C58 C59 1.402(13) . ? C58 C62 1.524(13) . ? C59 C60 1.381(12) . ? C59 H59A 0.9400 . ? C60 C61 1.363(13) . ? C60 C66 1.520(12) . ? C62 C65 1.484(16) . ? C62 C64 1.523(17) . ? C62 C63 1.548(16) . ? 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 H66A 0.9800 . ? C66 H66B 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 O2 Bi1 O3 87.9(2) . 2_666 ? O2 Bi1 O1 86.6(2) . . ? O3 Bi1 O1 93.9(2) 2_666 . ? O2 Bi1 O3 76.64(18) . . ? O3 Bi1 O3 67.3(2) 2_666 . ? O1 Bi1 O3 154.91(19) . . ? C1 O1 Bi1 126.8(5) . . ? O1 C1 C6 122.7(7) . . ? O1 C1 C2 118.3(8) . . ? C6 C1 C2 118.8(8) . . ? C17 O2 Bi1 123.7(5) . . ? C3 C2 C1 118.1(8) . . ? C3 C2 C66 120.0(7) . . ? C1 C2 C66 121.2(8) . . ? C28 O3 Bi1 121.7(4) . 2_666 ? C28 O3 Bi1 124.6(4) . . ? Bi1 O3 Bi1 112.7(2) 2_666 . ? C4 C3 C2 123.9(8) . . ? C4 C3 H3A 118.1 . . ? C2 C3 H3A 118.1 . . ? C3 C4 C5 116.4(8) . . ? C3 C4 C7 124.2(8) . . ? C5 C4 C7 119.3(9) . . ? C39 O4 H4A 109.5 . . ? C50 O5 H5A 109.5 . . ? C4 C5 C6 122.3(8) . . ? C4 C5 H5B 118.9 . . ? C6 C5 H5B 118.9 . . ? C61 O6 H6A 109.5 . . ? C1 C6 C5 120.3(7) . . ? C1 C6 C11 123.4(7) . . ? C5 C6 C11 116.3(8) . . ? C8 C7 C10 108.5(9) . . ? C8 C7 C4 111.1(9) . . ? C10 C7 C4 111.7(8) . . ? C8 C7 C9 108.7(9) . . ? C10 C7 C9 109.8(10) . . ? C4 C7 C9 107.0(8) . . ? 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 H9\A 109.5 . . ? C7 C9 H9\B 109.5 . . ? H9\A C9 H9\B 109.5 . . ? C7 C9 H9\C 109.5 . . ? H9\A C9 H9\C 109.5 . . ? H9\B C9 H9\C 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 . . ? C6 C11 C12 113.8(7) . . ? C6 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C6 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 119.8(8) . . ? C17 C12 C11 118.2(8) . . ? C13 C12 C11 122.0(7) . . ? C12 C13 C14 122.3(8) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 116.1(8) . . ? C15 C14 C18 123.8(8) . . ? C13 C14 C18 120.0(8) . . ? C16 C15 C14 124.0(8) . . ? C16 C15 H15A 118.0 . . ? C14 C15 H15A 118.0 . . ? C15 C16 C17 118.2(8) . . ? C15 C16 C22 121.9(7) . . ? C17 C16 C22 119.5(7) . . ? O2 C17 C12 121.4(7) . . ? O2 C17 C16 119.1(7) . . ? C12 C17 C16 119.4(8) . . ? C19A C18 C20 121.2(13) . . ? C19A C18 C14 114.6(11) . . ? C20 C18 C14 113.4(9) . . ? C19A C18 C21 90.2(15) . . ? C20 C18 C21 104.9(11) . . ? C14 C18 C21 108.4(11) . . ? C19A C18 C19 41.7(12) . . ? C20 C18 C19 95.8(16) . . ? C14 C18 C19 103.2(13) . . ? C21 C18 C19 130.7(17) . . ? 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 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 . . ? C16 C22 C23 107.3(6) . . ? C16 C22 H22A 110.3 . . ? C23 C22 H22A 110.3 . . ? C16 C22 H22B 110.3 . . ? C23 C22 H22B 110.3 . . ? H22A C22 H22B 108.5 . . ? C24 C23 C28 117.6(7) . . ? C24 C23 C22 119.3(7) . . ? C28 C23 C22 122.6(7) . . ? C25 C24 C23 123.1(8) . . ? C25 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? C24 C25 C26 117.4(8) . . ? C24 C25 C29 121.5(8) . . ? C26 C25 C29 121.0(8) . . ? C27 C26 C25 122.7(8) . . ? C27 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C26 C27 C28 118.1(8) . . ? C26 C27 C33 122.9(7) . . ? C28 C27 C33 118.8(7) . . ? O3 C28 C27 118.3(7) . . ? O3 C28 C23 120.9(7) . . ? C27 C28 C23 120.8(7) . . ? C31 C29 C30 108.8(9) . . ? C31 C29 C32 108.4(10) . . ? C30 C29 C32 109.7(9) . . ? C31 C29 C25 112.7(8) . . ? C30 C29 C25 109.1(8) . . ? C32 C29 C25 108.1(8) . . ? 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 113.0(7) . . ? C27 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C27 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C39 120.0(8) . . ? C35 C34 C33 120.1(7) . . ? C39 C34 C33 119.8(8) . . ? C34 C35 C36 121.8(8) . . ? C34 C35 H35A 119.1 . . ? C36 C35 H35A 119.1 . . ? C37 C36 C35 116.6(8) . . ? C37 C36 C40 121.0(9) . . ? C35 C36 C40 122.0(9) . . ? C36 C37 C38 123.6(9) . . ? C36 C37 H37A 118.2 . . ? C38 C37 H37A 118.2 . . ? C37 C38 C39 117.8(8) . . ? C37 C38 C44 121.7(8) . . ? C39 C38 C44 120.4(8) . . ? O4 C39 C34 120.1(8) . . ? O4 C39 C38 119.8(8) . . ? C34 C39 C38 120.1(8) . . ? C36 C40 C41 112.6(8) . . ? C36 C40 C42 108.8(8) . . ? C41 C40 C42 108.1(10) . . ? C36 C40 C43 111.9(8) . . ? C41 C40 C43 107.3(9) . . ? C42 C40 C43 108.0(8) . . ? 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 115.4(8) . . ? C45 C44 H44A 108.4 . . ? C38 C44 H44A 108.4 . . ? C45 C44 H44B 108.4 . . ? C38 C44 H44B 108.4 . . ? H44A C44 H44B 107.5 . . ? C46 C45 C50 118.9(10) . . ? C46 C45 C44 122.2(10) . . ? C50 C45 C44 119.0(9) . . ? C45 C46 C47 124.0(12) . . ? C45 C46 H46A 118.0 . . ? C47 C46 H46A 118.0 . . ? C46 C47 C48 115.9(11) . . ? C46 C47 C51 123.5(13) . . ? C48 C47 C51 120.5(12) . . ? C49 C48 C47 124.0(11) . . ? C49 C48 H48A 118.0 . . ? C47 C48 H48A 118.0 . . ? C48 C49 C50 115.5(11) . . ? C48 C49 C55 121.7(10) . . ? C50 C49 C55 122.8(10) . . ? O5 C50 C45 117.5(9) . . ? O5 C50 C49 120.7(10) . . ? C45 C50 C49 121.6(9) . . ? C54A C51 C52 119.3(18) . . ? C54A C51 C53 55.4(16) . . ? C52 C51 C53 139.7(17) . . ? C54A C51 C47 114.9(17) . . ? C52 C51 C47 109.7(11) . . ? C53 C51 C47 107.0(14) . . ? C54A C51 C54 38.9(15) . . ? C52 C51 C54 91.6(15) . . ? C53 C51 C54 94.3(16) . . ? C47 C51 C54 105.2(15) . . ? C54A C51 C53A 107.5(19) . . ? C52 C51 C53A 92.0(14) . . ? C53 C51 C53A 59.4(15) . . ? C47 C51 C53A 110.8(13) . . ? C54 C51 C53A 140.0(16) . . ? 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 C53A H53D 109.5 . . ? C51 C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C51 C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 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 . . ? C51 C54A H54D 109.5 . . ? C51 C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C51 C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C49 C55 C56 115.7(9) . . ? C49 C55 H55A 108.3 . . ? C56 C55 H55A 108.3 . . ? C49 C55 H55B 108.3 . . ? C56 C55 H55B 108.3 . . ? H55A C55 H55B 107.4 . . ? C57 C56 C61 117.6(10) . . ? C57 C56 C55 121.3(9) . . ? C61 C56 C55 121.0(9) . . ? C56 C57 C58 122.4(10) . . ? C56 C57 H57A 118.8 . . ? C58 C57 H57A 118.8 . . ? C57 C58 C59 116.8(9) . . ? C57 C58 C62 123.2(10) . . ? C59 C58 C62 119.9(10) . . ? C60 C59 C58 122.1(10) . . ? C60 C59 H59A 119.0 . . ? C58 C59 H59A 119.0 . . ? C61 C60 C59 119.4(9) . . ? C61 C60 C66 119.3(8) . . ? C59 C60 C66 121.3(9) . . ? C60 C61 O6 120.1(8) . . ? C60 C61 C56 121.6(8) . . ? O6 C61 C56 118.2(9) . . ? C65 C62 C64 112.7(12) . . ? C65 C62 C58 109.2(9) . . ? C64 C62 C58 110.1(10) . . ? C65 C62 C63 107.9(12) . . ? C64 C62 C63 104.9(11) . . ? C58 C62 C63 112.1(10) . . ? 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 . . ? C2 C66 C60 112.0(7) . . ? C2 C66 H66A 109.2 . . ? C60 C66 H66A 109.2 . . ? C2 C66 H66B 109.2 . . ? C60 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 6.137 _refine_diff_density_min -1.551 _refine_diff_density_rms 0.145 # Attachment '2.CIF' data_tcu177m _database_code_depnum_ccdc_archive 'CCDC 721516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H66 Bi2 O12,7(C4 H8 O), 2(H2O)' _chemical_formula_sum 'C112 H126 Bi2 O21' _chemical_formula_weight 2226.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pccn _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 13.940(3) _cell_length_b 24.307(5) _cell_length_c 29.061(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9847(4) _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 Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 3.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5446 _exptl_absorpt_correction_T_max 0.6296 _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 38534 _diffrn_reflns_av_R_equivalents 0.1790 _diffrn_reflns_av_sigmaI/netI 0.1632 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.30 _reflns_number_total 7102 _reflns_number_gt 3229 _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^)+(0.0309P)^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 7102 _refine_ls_number_parameters 579 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.034 _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 0.15969(3) -0.170722(15) 0.346442(14) 0.04201(14) Uani 1 1 d . . . O1 O 0.1792(5) -0.0938(2) 0.3859(2) 0.043(2) Uani 1 1 d . . . C1 C 0.2142(10) -0.0849(4) 0.4289(5) 0.049(3) Uani 1 1 d . . . O2 O 0.0240(5) -0.1730(3) 0.3790(2) 0.055(2) Uani 1 1 d . . . C2 C 0.3034(9) -0.0587(5) 0.4345(4) 0.050(3) Uani 1 1 d . . . O3 O 0.1050(5) -0.1081(3) 0.3044(3) 0.045(2) Uani 1 1 d . . . C3 C 0.3347(11) -0.0471(4) 0.4783(4) 0.063(3) Uani 1 1 d . . . H3A H 0.3955 -0.0310 0.4822 0.076 Uiso 1 1 calc R . . O4 O 0.2909(4) -0.1760(3) 0.2634(2) 0.0456(18) Uani 1 1 d . . . H4A H 0.3298 -0.1981 0.2746 0.068 Uiso 1 1 calc R . . C4 C 0.2822(11) -0.0580(5) 0.5153(5) 0.068(4) Uani 1 1 d . . . H4B H 0.3060 -0.0494 0.5447 0.082 Uiso 1 1 calc R . . O5 O 0.0935(5) -0.2544(3) 0.3137(3) 0.050(2) Uani 1 1 d . . . H5B H 0.1379 -0.2728 0.3026 0.075 Uiso 1 1 calc R . . C5 C 0.1913(12) -0.0822(5) 0.5108(5) 0.075(5) Uani 1 1 d . . . H5A H 0.1542 -0.0892 0.5372 0.090 Uiso 1 1 calc R . . C6 C 0.1555(10) -0.0959(4) 0.4674(5) 0.051(3) Uani 1 1 d . . . O6 O 0.3913(5) -0.1525(3) 0.3654(2) 0.053(2) Uani 1 1 d . . . H6A H 0.4081 -0.1797 0.3500 0.079 Uiso 1 1 calc R . . C7 C 0.0575(9) -0.1212(5) 0.4631(5) 0.066(4) Uani 1 1 d . . . H7A H 0.0249 -0.1179 0.4928 0.079 Uiso 1 1 calc R . . H7B H 0.0652 -0.1605 0.4565 0.079 Uiso 1 1 calc R . . C8 C -0.0070(9) -0.0962(5) 0.4262(5) 0.057(4) Uani 1 1 d . . . C9 C -0.0528(9) -0.0465(5) 0.4333(5) 0.068(4) Uani 1 1 d . . . H9A H -0.0456 -0.0279 0.4614 0.081 Uiso 1 1 calc R . . C10 C -0.1087(10) -0.0246(6) 0.3993(6) 0.077(5) Uani 1 1 d . . . H10A H -0.1368 0.0102 0.4035 0.093 Uiso 1 1 calc R . . C11 C -0.1243(9) -0.0527(5) 0.3592(6) 0.075(5) Uani 1 1 d . . . H11A H -0.1645 -0.0376 0.3365 0.090 Uiso 1 1 calc R . . C12 C -0.0816(8) -0.1027(4) 0.3519(5) 0.053(3) Uani 1 1 d . . . C13 C -0.0215(9) -0.1239(5) 0.3860(5) 0.053(4) Uani 1 1 d . . . C14 C -0.0995(8) -0.1335(5) 0.3063(5) 0.062(4) Uani 1 1 d . . . H14A H -0.0863 -0.1726 0.3117 0.074 Uiso 1 1 calc R . . H14B H -0.1680 -0.1303 0.2992 0.074 Uiso 1 1 calc R . . C15 C -0.0457(10) -0.1170(5) 0.2646(6) 0.062(4) Uani 1 1 d . . . C16 C -0.0975(10) -0.1119(5) 0.2248(6) 0.073(4) Uani 1 1 d . . . H16A H -0.1638 -0.1188 0.2252 0.088 Uiso 1 1 calc R . . C17 C -0.0540(12) -0.0967(6) 0.1847(6) 0.091(5) Uani 1 1 d . . . H17A H -0.0911 -0.0919 0.1580 0.110 Uiso 1 1 calc R . . C18 C 0.0430(11) -0.0885(5) 0.1830(5) 0.078(4) Uani 1 1 d . . . H18A H 0.0724 -0.0790 0.1550 0.093 Uiso 1 1 calc R . . C19 C 0.0996(10) -0.0943(4) 0.2235(5) 0.055(4) Uani 1 1 d . . . C20 C 0.0527(9) -0.1081(4) 0.2651(5) 0.049(3) Uani 1 1 d . . . C21 C 0.2063(9) -0.0856(4) 0.2211(4) 0.056(4) Uani 1 1 d . . . H21A H 0.2317 -0.0844 0.2525 0.067 Uiso 1 1 calc R . . H21B H 0.2187 -0.0497 0.2069 0.067 Uiso 1 1 calc R . . C22 C 0.2611(9) -0.1291(5) 0.1943(5) 0.053(4) Uani 1 1 d . . . C23 C 0.2710(11) -0.1253(6) 0.1468(5) 0.080(4) Uani 1 1 d . . . H23A H 0.2462 -0.0944 0.1314 0.096 Uiso 1 1 calc R . . C24 C 0.3148(11) -0.1644(6) 0.1228(5) 0.084(5) Uani 1 1 d . . . H24A H 0.3161 -0.1624 0.0906 0.101 Uiso 1 1 calc R . . C25 C 0.3588(10) -0.2085(5) 0.1451(5) 0.080(5) Uani 1 1 d . . . H25A H 0.3921 -0.2351 0.1279 0.096 Uiso 1 1 calc R . . C26 C 0.3537(9) -0.2130(5) 0.1927(4) 0.057(4) Uani 1 1 d . . . C27 C 0.3040(8) -0.1733(5) 0.2168(4) 0.050(3) Uani 1 1 d . . . C28 C 0.4049(9) -0.2603(4) 0.2169(4) 0.054(4) Uani 1 1 d . . . H28A H 0.3603 -0.2782 0.2382 0.064 Uiso 1 1 calc R . . H28B H 0.4248 -0.2876 0.1940 0.064 Uiso 1 1 calc R . . C29 C 0.0106(9) -0.2651(4) 0.2901(6) 0.052(4) Uani 1 1 d . . . C30 C 0.0094(10) -0.2587(4) 0.2429(6) 0.059(4) Uani 1 1 d . . . C31 C -0.0729(13) -0.2722(5) 0.2194(6) 0.085(5) Uani 1 1 d . . . H31A H -0.0745 -0.2700 0.1871 0.102 Uiso 1 1 calc R . . C32 C -0.1554(12) -0.2895(5) 0.2440(8) 0.097(6) Uani 1 1 d . . . H32A H -0.2129 -0.2976 0.2285 0.116 Uiso 1 1 calc R . . C33 C 0.6493(11) -0.2058(5) 0.2905(7) 0.083(5) Uani 1 1 d . . . H33A H 0.7039 -0.1944 0.3070 0.100 Uiso 1 1 calc R . . C34 C 0.5691(11) -0.2166(5) 0.3138(6) 0.061(4) Uani 1 1 d . . . C35 C 0.5719(10) -0.2118(4) 0.3660(6) 0.081(5) Uani 1 1 d . . . H35A H 0.5194 -0.2336 0.3791 0.097 Uiso 1 1 calc R . . H35B H 0.6325 -0.2272 0.3773 0.097 Uiso 1 1 calc R . . C36 C 0.5627(9) -0.1524(4) 0.3823(5) 0.061(4) Uani 1 1 d . . . C37 C 0.6396(9) -0.1213(5) 0.3984(4) 0.075(4) Uani 1 1 d . . . H37A H 0.7002 -0.1379 0.4015 0.089 Uiso 1 1 calc R . . C38 C 0.6289(10) -0.0679(5) 0.4096(5) 0.078(5) Uani 1 1 d . . . H38A H 0.6832 -0.0472 0.4178 0.094 Uiso 1 1 calc R . . C39 C 0.5404(9) -0.0429(5) 0.4095(4) 0.063(4) Uani 1 1 d . . . H39A H 0.5338 -0.0066 0.4202 0.075 Uiso 1 1 calc R . . C40 C 0.4625(9) -0.0709(5) 0.3939(4) 0.050(3) Uani 1 1 d . . . C41 C 0.4717(9) -0.1244(5) 0.3803(4) 0.048(3) Uani 1 1 d . . . C42 C 0.3649(8) -0.0448(4) 0.3942(4) 0.053(4) Uani 1 1 d . . . H42A H 0.3729 -0.0047 0.3932 0.064 Uiso 1 1 calc R . . H42B H 0.3311 -0.0558 0.3661 0.064 Uiso 1 1 calc R . . O43 O 0.5575(8) -0.0297(3) 0.2071(3) 0.084(3) Uani 1 1 d D . . C44 C 0.4702(10) -0.0460(7) 0.2264(6) 0.121(7) Uani 1 1 d D . . H44A H 0.4349 -0.0685 0.2041 0.146 Uiso 1 1 calc R . . H44B H 0.4315 -0.0134 0.2332 0.146 Uiso 1 1 calc R . . C45 C 0.4839(11) -0.0764(6) 0.2670(6) 0.107(6) Uani 1 1 d D . . H45A H 0.4806 -0.1161 0.2611 0.128 Uiso 1 1 calc R . . H45B H 0.4363 -0.0666 0.2904 0.128 Uiso 1 1 calc R . . C46 C 0.5809(12) -0.0598(6) 0.2811(5) 0.102(6) Uani 1 1 d D . . H46A H 0.5790 -0.0267 0.3003 0.122 Uiso 1 1 calc R . . H46B H 0.6131 -0.0893 0.2981 0.122 Uiso 1 1 calc R . . C47 C 0.6283(9) -0.0492(5) 0.2378(6) 0.085(5) Uani 1 1 d D . . H47A H 0.6788 -0.0215 0.2418 0.102 Uiso 1 1 calc R . . H47B H 0.6575 -0.0830 0.2259 0.102 Uiso 1 1 calc R . . O48 O 0.6285(8) -0.0513(4) 0.1047(4) 0.106(4) Uani 1 1 d D . . C49 C 0.610(2) -0.1044(9) 0.1186(7) 0.31(2) Uani 1 1 d D . . H49A H 0.5430 -0.1134 0.1128 0.374 Uiso 1 1 calc R . . H49B H 0.6218 -0.1075 0.1518 0.374 Uiso 1 1 calc R . . C50 C 0.669(3) -0.1415(10) 0.0954(10) 0.41(3) Uani 1 1 d D . . H50A H 0.6414 -0.1786 0.0950 0.495 Uiso 1 1 calc R . . H50B H 0.7336 -0.1428 0.1085 0.495 Uiso 1 1 calc R . . C51 C 0.6687(19) -0.1169(9) 0.0501(7) 0.29(2) Uani 1 1 d D . . H51A H 0.7280 -0.1253 0.0334 0.345 Uiso 1 1 calc R . . H51B H 0.6137 -0.1296 0.0320 0.345 Uiso 1 1 calc R . . C52 C 0.6618(17) -0.0606(7) 0.0597(6) 0.188(11) Uani 1 1 d D . . H52A H 0.6178 -0.0434 0.0377 0.225 Uiso 1 1 calc R . . H52B H 0.7250 -0.0435 0.0559 0.225 Uiso 1 1 calc R . . O53 O 0.9626(19) -0.1863(12) 0.0807(7) 0.378(13) Uiso 1 1 d D . . C54 C 0.909(2) -0.2216(11) 0.0523(11) 0.38(2) Uiso 1 1 d D . . H54A H 0.9382 -0.2583 0.0535 0.453 Uiso 1 1 calc R . . H54B H 0.8442 -0.2246 0.0650 0.453 Uiso 1 1 calc R . . C55 C 0.9018(19) -0.2059(11) 0.0059(9) 0.257(13) Uiso 1 1 d D . . H55A H 0.8358 -0.1970 -0.0029 0.308 Uiso 1 1 calc R . . H55B H 0.9280 -0.2338 -0.0149 0.308 Uiso 1 1 calc R . . C56 C 0.9637(17) -0.1560(9) 0.0086(7) 0.214(10) Uiso 1 1 d D . . H56A H 1.0265 -0.1645 -0.0047 0.257 Uiso 1 1 calc R . . H56B H 0.9347 -0.1266 -0.0098 0.257 Uiso 1 1 calc R . . C57 C 0.977(2) -0.1371(9) 0.0542(10) 0.283(15) Uiso 1 1 d D . . H57A H 0.9290 -0.1090 0.0622 0.339 Uiso 1 1 calc R . . H57B H 1.0410 -0.1221 0.0587 0.339 Uiso 1 1 calc R . . O58 O 0.7500 0.2500 0.0768(5) 0.132(7) Uani 1 2 d S . . C59 C 0.8210(12) 0.2265(5) 0.0484(5) 0.104(6) Uani 1 1 d . . . H59A H 0.8202 0.1863 0.0514 0.125 Uiso 1 1 calc R . . H59B H 0.8846 0.2398 0.0574 0.125 Uiso 1 1 calc R . . C60 C 0.7997(11) 0.2429(9) -0.0011(5) 0.128(9) Uani 1 1 d . . . H60A H 0.8392 0.2743 -0.0104 0.154 Uiso 1 1 calc R . . H60B H 0.8121 0.2122 -0.0221 0.154 Uiso 1 1 calc R . . O61 O 0.5877(3) 0.02658(16) 0.14718(16) 0.0000(11) Uiso 1 1 d . . . 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 0.0389(2) 0.0315(2) 0.0556(2) -0.0014(3) 0.0001(3) 0.0014(3) O1 0.051(6) 0.033(4) 0.044(5) -0.006(4) 0.008(5) -0.005(4) C1 0.067(10) 0.018(7) 0.063(10) -0.006(7) 0.018(9) 0.004(6) O2 0.057(5) 0.043(5) 0.067(5) 0.001(5) 0.011(4) 0.004(5) C2 0.065(10) 0.042(8) 0.043(8) -0.011(7) 0.009(8) -0.004(7) O3 0.035(5) 0.039(5) 0.063(6) -0.006(4) -0.009(4) 0.006(4) C3 0.080(10) 0.055(8) 0.055(9) 0.000(7) -0.007(10) -0.010(9) O4 0.057(5) 0.036(4) 0.043(5) -0.003(4) 0.003(4) 0.007(4) C4 0.091(12) 0.068(10) 0.047(10) -0.012(8) -0.016(9) 0.005(9) O5 0.038(5) 0.044(5) 0.067(6) -0.007(4) -0.001(5) 0.005(4) C5 0.103(15) 0.058(9) 0.065(11) 0.003(8) 0.024(10) 0.015(9) C6 0.058(9) 0.033(6) 0.062(9) -0.001(6) 0.006(10) -0.005(8) O6 0.043(5) 0.040(5) 0.075(6) -0.008(4) -0.006(4) -0.015(4) C7 0.072(10) 0.052(8) 0.072(10) 0.000(8) 0.050(9) -0.005(8) C8 0.045(9) 0.038(8) 0.088(11) 0.009(8) 0.035(9) 0.012(7) C9 0.051(10) 0.058(10) 0.094(12) -0.009(9) 0.032(9) 0.000(8) C10 0.053(10) 0.046(10) 0.133(16) -0.001(10) 0.039(10) 0.010(8) C11 0.053(9) 0.052(9) 0.121(15) 0.000(9) 0.002(9) 0.002(7) C12 0.036(7) 0.029(7) 0.095(11) -0.001(8) 0.020(9) 0.002(6) C13 0.040(8) 0.026(8) 0.094(12) -0.002(8) 0.022(9) 0.002(7) C14 0.023(7) 0.040(8) 0.123(13) 0.001(9) -0.008(8) 0.003(6) C15 0.045(9) 0.044(8) 0.098(12) -0.002(8) -0.026(10) -0.003(7) C16 0.045(10) 0.061(10) 0.114(14) -0.007(10) -0.018(11) -0.003(8) C17 0.082(14) 0.073(11) 0.119(15) 0.015(10) -0.066(12) 0.002(10) C18 0.080(12) 0.053(9) 0.100(12) 0.013(8) -0.033(10) -0.008(9) C19 0.064(11) 0.023(7) 0.077(11) 0.001(7) -0.030(10) -0.009(8) C20 0.052(10) 0.013(6) 0.080(11) 0.009(7) -0.015(9) 0.006(6) C21 0.079(10) 0.038(8) 0.051(9) 0.014(7) -0.016(8) -0.019(8) C22 0.076(10) 0.039(8) 0.044(9) 0.008(7) 0.006(8) -0.007(7) C23 0.109(13) 0.061(10) 0.070(13) 0.013(9) -0.010(10) -0.016(9) C24 0.131(15) 0.072(11) 0.049(9) 0.010(9) 0.014(9) -0.039(11) C25 0.114(14) 0.059(9) 0.067(12) -0.015(8) 0.032(10) -0.021(9) C26 0.074(11) 0.044(8) 0.053(9) -0.003(7) 0.016(9) -0.022(8) C27 0.069(9) 0.034(7) 0.047(8) -0.006(8) 0.008(6) -0.015(7) C28 0.068(10) 0.028(7) 0.065(10) -0.010(7) 0.042(8) -0.011(7) C29 0.042(9) 0.014(7) 0.100(13) 0.011(7) -0.011(9) 0.003(6) C30 0.054(10) 0.022(7) 0.101(13) 0.003(8) -0.031(10) 0.006(7) C31 0.100(14) 0.041(9) 0.115(15) 0.015(9) -0.032(12) 0.002(9) C32 0.061(11) 0.035(8) 0.19(2) 0.019(11) -0.069(16) 0.000(9) C33 0.058(11) 0.031(7) 0.161(17) -0.021(10) 0.022(13) 0.007(8) C34 0.048(10) 0.019(7) 0.115(14) -0.003(8) 0.021(11) 0.001(7) C35 0.068(11) 0.017(8) 0.158(16) 0.006(9) -0.014(11) 0.016(7) C36 0.040(8) 0.042(8) 0.102(11) -0.003(7) -0.013(8) -0.001(6) C37 0.042(10) 0.053(9) 0.128(13) -0.010(8) -0.020(9) -0.007(7) C38 0.070(12) 0.046(9) 0.118(13) -0.027(8) 0.008(10) -0.040(8) C39 0.039(9) 0.056(9) 0.093(11) -0.021(8) 0.009(8) -0.009(8) C40 0.046(9) 0.029(7) 0.076(10) -0.013(7) 0.009(8) -0.006(7) C41 0.047(9) 0.036(8) 0.061(9) 0.001(7) -0.010(7) -0.016(7) C42 0.070(11) 0.027(6) 0.064(9) -0.010(6) -0.006(8) 0.008(6) O43 0.074(7) 0.058(6) 0.120(8) 0.038(6) 0.017(7) 0.003(6) C44 0.070(12) 0.125(15) 0.169(18) 0.068(13) 0.038(13) -0.002(11) C45 0.082(14) 0.092(13) 0.146(18) 0.027(12) 0.041(13) -0.017(11) C46 0.114(16) 0.070(11) 0.122(16) 0.023(10) 0.024(13) -0.008(11) C47 0.067(12) 0.039(8) 0.149(16) -0.001(9) 0.044(12) -0.017(8) O48 0.151(12) 0.049(6) 0.118(9) -0.006(6) 0.028(8) 0.003(6) C49 0.63(7) 0.16(3) 0.14(2) -0.03(2) 0.16(3) 0.01(3) C50 0.81(9) 0.19(3) 0.23(4) -0.01(3) -0.10(5) 0.25(4) C51 0.40(4) 0.21(3) 0.26(3) -0.17(3) -0.24(3) 0.22(3) C52 0.29(3) 0.099(15) 0.17(2) -0.020(15) 0.09(2) -0.079(19) O58 0.186(19) 0.146(15) 0.064(12) 0.000 0.000 0.100(14) C59 0.159(18) 0.062(10) 0.092(13) 0.002(9) -0.002(13) 0.002(11) C60 0.20(3) 0.102(14) 0.081(12) 0.031(11) 0.000(11) -0.015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O3 2.095(7) . ? Bi1 O2 2.116(7) . ? Bi1 O1 2.210(6) . ? Bi1 O5 2.429(7) . ? O1 C1 1.359(13) . ? C1 C2 1.407(15) . ? C1 C6 1.411(15) . ? O2 C13 1.368(12) . ? C2 C3 1.375(14) . ? C2 C42 1.490(14) . ? O3 C20 1.354(13) . ? C3 C4 1.328(15) . ? C3 H3A 0.9400 . ? O4 C27 1.368(11) . ? O4 H4A 0.8300 . ? C4 C5 1.403(16) . ? C4 H4B 0.9400 . ? O5 C29 1.369(13) . ? O5 H5B 0.8300 . ? C5 C6 1.397(16) . ? C5 H5A 0.9400 . ? C6 C7 1.503(16) . ? O6 C41 1.382(11) . ? O6 H6A 0.8300 . ? C7 C8 1.525(16) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.363(16) . ? C8 C9 1.382(15) . ? C9 C10 1.366(17) . ? C9 H9A 0.9400 . ? C10 C11 1.368(17) . ? C10 H10A 0.9400 . ? C11 C12 1.369(15) . ? C11 H11A 0.9400 . ? C12 C13 1.395(16) . ? C12 C14 1.544(16) . ? C14 C15 1.480(17) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.367(16) . ? C15 C20 1.388(15) . ? C16 C17 1.365(18) . ? C16 H16A 0.9400 . ? C17 C18 1.368(17) . ? C17 H17A 0.9400 . ? C18 C19 1.423(16) . ? C18 H18A 0.9400 . ? C19 C20 1.417(16) . ? C19 C21 1.504(15) . ? C21 C22 1.517(15) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.390(16) . ? C22 C27 1.393(15) . ? C23 C24 1.328(16) . ? C23 H23A 0.9400 . ? C24 C25 1.393(17) . ? C24 H24A 0.9400 . ? C25 C26 1.391(15) . ? C25 H25A 0.9400 . ? C26 C27 1.380(15) . ? C26 C28 1.525(15) . ? C28 C30 1.486(16) 2_545 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.381(16) . ? C29 C34 1.381(17) 2_545 ? C30 C31 1.374(17) . ? C30 C28 1.486(16) 2_545 ? C31 C32 1.418(19) . ? C31 H31A 0.9400 . ? C32 C33 1.361(18) 2_545 ? C32 H32A 0.9400 . ? C33 C34 1.333(17) . ? C33 C32 1.361(18) 2_545 ? C33 H33A 0.9400 . ? C34 C29 1.381(17) 2_545 ? C34 C35 1.520(17) . ? C35 C36 1.525(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.393(14) . ? C36 C41 1.441(14) . ? C37 C38 1.347(15) . ? C37 H37A 0.9400 . ? C38 C39 1.375(15) . ? C38 H38A 0.9400 . ? C39 C40 1.359(14) . ? C39 H39A 0.9400 . ? C40 C41 1.367(13) . ? C40 C42 1.502(14) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O43 C44 1.397(13) . ? O43 C47 1.412(13) . ? C44 C45 1.406(15) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.469(15) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.444(14) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? O48 C49 1.377(17) . ? O48 C52 1.407(15) . ? C49 C50 1.39(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.445(19) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.399(16) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? O53 C54 1.405(19) . ? O53 C57 1.435(17) . ? C54 C55 1.40(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.489(18) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.414(17) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? O58 C59 1.411(15) 2_655 ? O58 C59 1.411(15) . ? C59 C60 1.521(16) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 C60 1.43(3) 2_655 ? C60 H60A 0.9800 . ? C60 H60B 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 O2 87.4(3) . . ? O3 Bi1 O1 74.5(3) . . ? O2 Bi1 O1 84.3(3) . . ? O3 Bi1 O5 104.0(3) . . ? O2 Bi1 O5 79.2(3) . . ? O1 Bi1 O5 163.5(2) . . ? C1 O1 Bi1 131.0(6) . . ? O1 C1 C2 119.7(12) . . ? O1 C1 C6 119.4(12) . . ? C2 C1 C6 120.4(13) . . ? C13 O2 Bi1 117.3(6) . . ? C3 C2 C1 118.7(13) . . ? C3 C2 C42 119.9(12) . . ? C1 C2 C42 121.4(11) . . ? C20 O3 Bi1 133.5(6) . . ? C4 C3 C2 122.3(14) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C27 O4 H4A 109.5 . . ? C3 C4 C5 120.4(13) . . ? C3 C4 H4B 119.8 . . ? C5 C4 H4B 119.8 . . ? C29 O5 Bi1 132.6(6) . . ? C29 O5 H5B 109.5 . . ? Bi1 O5 H5B 108.6 . . ? C6 C5 C4 120.5(14) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C1 117.7(13) . . ? C5 C6 C7 119.8(13) . . ? C1 C6 C7 122.5(12) . . ? C41 O6 H6A 109.5 . . ? C6 C7 C8 115.6(10) . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 119.3(14) . . ? C13 C8 C7 119.6(12) . . ? C9 C8 C7 121.0(14) . . ? C10 C9 C8 119.7(15) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 120.8(14) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C12 120.3(15) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C13 118.6(14) . . ? C11 C12 C14 119.5(14) . . ? C13 C12 C14 121.9(11) . . ? C8 C13 O2 119.2(13) . . ? C8 C13 C12 121.1(12) . . ? O2 C13 C12 119.7(12) . . ? C15 C14 C12 119.4(10) . . ? C15 C14 H14A 107.5 . . ? C12 C14 H14A 107.5 . . ? C15 C14 H14B 107.5 . . ? C12 C14 H14B 107.5 . . ? H14A C14 H14B 107.0 . . ? C16 C15 C20 121.1(15) . . ? C16 C15 C14 116.7(13) . . ? C20 C15 C14 122.2(14) . . ? C17 C16 C15 120.8(15) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.6(15) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C19 120.3(15) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C18 118.2(13) . . ? C20 C19 C21 122.0(13) . . ? C18 C19 C21 119.8(14) . . ? O3 C20 C15 122.8(14) . . ? O3 C20 C19 118.1(12) . . ? C15 C20 C19 118.9(14) . . ? C19 C21 C22 115.1(11) . . ? C19 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? C19 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 118.3(12) . . ? C23 C22 C21 120.8(12) . . ? C27 C22 C21 120.8(11) . . ? C24 C23 C22 121.3(13) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 120.6(13) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 120.1(12) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C27 C26 C25 118.3(12) . . ? C27 C26 C28 122.0(12) . . ? C25 C26 C28 119.7(12) . . ? O4 C27 C26 122.3(12) . . ? O4 C27 C22 116.4(11) . . ? C26 C27 C22 121.2(11) . . ? C30 C28 C26 112.0(10) 2_545 . ? C30 C28 H28A 109.2 2_545 . ? C26 C28 H28A 109.2 . . ? C30 C28 H28B 109.2 2_545 . ? C26 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? O5 C29 C30 119.1(13) . . ? O5 C29 C34 119.3(14) . 2_545 ? C30 C29 C34 121.6(14) . 2_545 ? C31 C30 C29 118.4(15) . . ? C31 C30 C28 119.6(15) . 2_545 ? C29 C30 C28 122.0(13) . 2_545 ? C30 C31 C32 119.9(16) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C33 C32 C31 118.4(17) 2_545 . ? C33 C32 H32A 120.8 2_545 . ? C31 C32 H32A 120.8 . . ? C34 C33 C32 122.8(18) . 2_545 ? C34 C33 H33A 118.6 . . ? C32 C33 H33A 118.6 2_545 . ? C33 C34 C29 118.9(16) . 2_545 ? C33 C34 C35 118.0(16) . . ? C29 C34 C35 122.9(14) 2_545 . ? C36 C35 C34 112.4(11) . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C41 115.8(11) . . ? C37 C36 C35 123.7(12) . . ? C41 C36 C35 120.5(11) . . ? C38 C37 C36 121.3(12) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C37 C38 C39 121.7(12) . . ? C37 C38 H38A 119.2 . . ? C39 C38 H38A 119.2 . . ? C40 C39 C38 119.8(12) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C39 C40 C41 119.9(12) . . ? C39 C40 C42 120.7(11) . . ? C41 C40 C42 119.3(11) . . ? C40 C41 O6 119.0(11) . . ? C40 C41 C36 121.3(11) . . ? O6 C41 C36 119.6(10) . . ? C2 C42 C40 115.4(10) . . ? C2 C42 H42A 108.4 . . ? C40 C42 H42A 108.4 . . ? C2 C42 H42B 108.4 . . ? C40 C42 H42B 108.4 . . ? H42A C42 H42B 107.5 . . ? C44 O43 C47 105.1(9) . . ? O43 C44 C45 111.6(12) . . ? O43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? O43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 102.3(12) . . ? C44 C45 H45A 111.3 . . ? C46 C45 H45A 111.3 . . ? C44 C45 H45B 111.3 . . ? C46 C45 H45B 111.3 . . ? H45A C45 H45B 109.2 . . ? C47 C46 C45 103.2(12) . . ? C47 C46 H46A 111.1 . . ? C45 C46 H46A 111.1 . . ? C47 C46 H46B 111.1 . . ? C45 C46 H46B 111.1 . . ? H46A C46 H46B 109.1 . . ? O43 C47 C46 106.9(11) . . ? O43 C47 H47A 110.3 . . ? C46 C47 H47A 110.3 . . ? O43 C47 H47B 110.3 . . ? C46 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? C49 O48 C52 100.6(11) . . ? O48 C49 C50 110.9(19) . . ? O48 C49 H49A 109.5 . . ? C50 C49 H49A 109.5 . . ? O48 C49 H49B 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 108.0 . . ? C49 C50 C51 100.0(18) . . ? C49 C50 H50A 111.8 . . ? C51 C50 H50A 111.8 . . ? C49 C50 H50B 111.8 . . ? C51 C50 H50B 111.8 . . ? H50A C50 H50B 109.5 . . ? C52 C51 C50 103.0(15) . . ? C52 C51 H51A 111.2 . . ? C50 C51 H51A 111.2 . . ? C52 C51 H51B 111.2 . . ? C50 C51 H51B 111.2 . . ? H51A C51 H51B 109.1 . . ? C51 C52 O48 111.4(14) . . ? C51 C52 H52A 109.4 . . ? O48 C52 H52A 109.4 . . ? C51 C52 H52B 109.4 . . ? O48 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 O53 C57 105.3(17) . . ? C55 C54 O53 115.9(19) . . ? C55 C54 H54A 108.3 . . ? O53 C54 H54A 108.3 . . ? C55 C54 H54B 108.3 . . ? O53 C54 H54B 108.3 . . ? H54A C54 H54B 107.4 . . ? C54 C55 C56 97.4(16) . . ? C54 C55 H55A 112.3 . . ? C56 C55 H55A 112.3 . . ? C54 C55 H55B 112.3 . . ? C56 C55 H55B 112.3 . . ? H55A C55 H55B 109.9 . . ? C57 C56 C55 112.7(16) . . ? C57 C56 H56A 109.0 . . ? C55 C56 H56A 109.0 . . ? C57 C56 H56B 109.0 . . ? C55 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? C56 C57 O53 102.5(16) . . ? C56 C57 H57A 111.3 . . ? O53 C57 H57A 111.3 . . ? C56 C57 H57B 111.3 . . ? O53 C57 H57B 111.3 . . ? H57A C57 H57B 109.2 . . ? C59 O58 C59 108.2(17) 2_655 . ? O58 C59 C60 108.2(14) . . ? O58 C59 H59A 110.1 . . ? C60 C59 H59A 110.1 . . ? O58 C59 H59B 110.1 . . ? C60 C59 H59B 110.1 . . ? H59A C59 H59B 108.4 . . ? C60 C60 C59 104.6(10) 2_655 . ? C60 C60 H60A 110.8 2_655 . ? C59 C60 H60A 110.8 . . ? C60 C60 H60B 110.8 2_655 . ? C59 C60 H60B 110.8 . . ? H60A C60 H60B 108.9 . . ? 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 O3 Bi1 O1 C1 177.3(10) . . . . ? O2 Bi1 O1 C1 88.4(10) . . . . ? O5 Bi1 O1 C1 90.3(13) . . . . ? Bi1 O1 C1 C2 110.2(10) . . . . ? Bi1 O1 C1 C6 -77.5(12) . . . . ? O3 Bi1 O2 C13 -38.4(9) . . . . ? O1 Bi1 O2 C13 36.3(9) . . . . ? O5 Bi1 O2 C13 -143.2(9) . . . . ? O1 C1 C2 C3 176.1(10) . . . . ? C6 C1 C2 C3 3.8(17) . . . . ? O1 C1 C2 C42 -5.4(16) . . . . ? C6 C1 C2 C42 -177.7(10) . . . . ? O2 Bi1 O3 C20 -84.1(11) . . . . ? O1 Bi1 O3 C20 -168.9(11) . . . . ? O5 Bi1 O3 C20 -5.9(11) . . . . ? C1 C2 C3 C4 -2.5(18) . . . . ? C42 C2 C3 C4 179.0(11) . . . . ? C2 C3 C4 C5 0(2) . . . . ? O3 Bi1 O5 C29 -29.0(12) . . . . ? O2 Bi1 O5 C29 55.6(11) . . . . ? O1 Bi1 O5 C29 53.6(15) . . . . ? C3 C4 C5 C6 0.9(19) . . . . ? C4 C5 C6 C1 0.4(17) . . . . ? C4 C5 C6 C7 -179.2(11) . . . . ? O1 C1 C6 C5 -175.1(10) . . . . ? C2 C1 C6 C5 -2.8(16) . . . . ? O1 C1 C6 C7 4.5(16) . . . . ? C2 C1 C6 C7 176.9(10) . . . . ? C5 C6 C7 C8 133.2(12) . . . . ? C1 C6 C7 C8 -46.5(16) . . . . ? C6 C7 C8 C13 104.4(14) . . . . ? C6 C7 C8 C9 -77.1(14) . . . . ? C13 C8 C9 C10 -2.8(18) . . . . ? C7 C8 C9 C10 178.7(11) . . . . ? C8 C9 C10 C11 4(2) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C10 C11 C12 C13 -0.6(18) . . . . ? C10 C11 C12 C14 -179.5(12) . . . . ? C9 C8 C13 O2 179.9(10) . . . . ? C7 C8 C13 O2 -1.6(17) . . . . ? C9 C8 C13 C12 0.3(18) . . . . ? C7 C8 C13 C12 178.8(10) . . . . ? Bi1 O2 C13 C8 -91.0(12) . . . . ? Bi1 O2 C13 C12 88.7(11) . . . . ? C11 C12 C13 C8 1.4(18) . . . . ? C14 C12 C13 C8 -179.6(11) . . . . ? C11 C12 C13 O2 -178.2(10) . . . . ? C14 C12 C13 O2 0.7(17) . . . . ? C11 C12 C14 C15 79.7(14) . . . . ? C13 C12 C14 C15 -99.2(14) . . . . ? C12 C14 C15 C16 -134.5(12) . . . . ? C12 C14 C15 C20 46.5(16) . . . . ? C20 C15 C16 C17 -1(2) . . . . ? C14 C15 C16 C17 179.8(13) . . . . ? C15 C16 C17 C18 3(2) . . . . ? C16 C17 C18 C19 -2(2) . . . . ? C17 C18 C19 C20 -0.7(18) . . . . ? C17 C18 C19 C21 179.4(12) . . . . ? Bi1 O3 C20 C15 78.5(14) . . . . ? Bi1 O3 C20 C19 -106.1(11) . . . . ? C16 C15 C20 O3 174.2(11) . . . . ? C14 C15 C20 O3 -6.9(17) . . . . ? C16 C15 C20 C19 -1.1(18) . . . . ? C14 C15 C20 C19 177.8(10) . . . . ? C18 C19 C20 O3 -173.5(9) . . . . ? C21 C19 C20 O3 6.4(16) . . . . ? C18 C19 C20 C15 2.0(16) . . . . ? C21 C19 C20 C15 -178.1(11) . . . . ? C20 C19 C21 C22 111.5(13) . . . . ? C18 C19 C21 C22 -68.7(15) . . . . ? C19 C21 C22 C23 85.3(15) . . . . ? C19 C21 C22 C27 -95.8(15) . . . . ? C27 C22 C23 C24 4(2) . . . . ? C21 C22 C23 C24 -176.8(12) . . . . ? C22 C23 C24 C25 -5(2) . . . . ? C23 C24 C25 C26 3(2) . . . . ? C24 C25 C26 C27 0(2) . . . . ? C24 C25 C26 C28 -178.0(12) . . . . ? C25 C26 C27 O4 176.4(10) . . . . ? C28 C26 C27 O4 -5.4(17) . . . . ? C25 C26 C27 C22 -0.9(18) . . . . ? C28 C26 C27 C22 177.3(10) . . . . ? C23 C22 C27 O4 -178.7(10) . . . . ? C21 C22 C27 O4 2.3(16) . . . . ? C23 C22 C27 C26 -1.2(18) . . . . ? C21 C22 C27 C26 179.8(11) . . . . ? C27 C26 C28 C30 -69.8(16) . . . 2_545 ? C25 C26 C28 C30 108.3(13) . . . 2_545 ? Bi1 O5 C29 C30 87.4(13) . . . . ? Bi1 O5 C29 C34 -94.2(12) . . . 2_545 ? O5 C29 C30 C31 176.9(10) . . . . ? C34 C29 C30 C31 -1.5(17) 2_545 . . . ? O5 C29 C30 C28 -1.1(17) . . . 2_545 ? C34 C29 C30 C28 -179.4(10) 2_545 . . 2_545 ? C29 C30 C31 C32 3.1(18) . . . . ? C28 C30 C31 C32 -178.9(11) 2_545 . . . ? C30 C31 C32 C33 -2(2) . . . 2_545 ? C32 C33 C34 C29 2(2) 2_545 . . 2_545 ? C32 C33 C34 C35 178.0(12) 2_545 . . . ? C33 C34 C35 C36 80.2(15) . . . . ? C29 C34 C35 C36 -103.8(14) 2_545 . . . ? C34 C35 C36 C37 -103.9(16) . . . . ? C34 C35 C36 C41 73.9(17) . . . . ? C41 C36 C37 C38 -2(2) . . . . ? C35 C36 C37 C38 175.7(13) . . . . ? C36 C37 C38 C39 6(2) . . . . ? C37 C38 C39 C40 -6(2) . . . . ? C38 C39 C40 C41 3(2) . . . . ? C38 C39 C40 C42 179.0(12) . . . . ? C39 C40 C41 O6 178.8(11) . . . . ? C42 C40 C41 O6 2.4(17) . . . . ? C39 C40 C41 C36 0.6(19) . . . . ? C42 C40 C41 C36 -175.8(11) . . . . ? C37 C36 C41 C40 -0.8(19) . . . . ? C35 C36 C41 C40 -178.8(12) . . . . ? C37 C36 C41 O6 -179.0(11) . . . . ? C35 C36 C41 O6 3.0(19) . . . . ? C3 C2 C42 C40 58.4(14) . . . . ? C1 C2 C42 C40 -120.1(12) . . . . ? C39 C40 C42 C2 -96.8(14) . . . . ? C41 C40 C42 C2 79.5(14) . . . . ? C47 O43 C44 C45 -2.0(19) . . . . ? O43 C44 C45 C46 21.2(19) . . . . ? C44 C45 C46 C47 -31.4(17) . . . . ? C44 O43 C47 C46 -18.9(15) . . . . ? C45 C46 C47 O43 31.7(15) . . . . ? C52 O48 C49 C50 27(3) . . . . ? O48 C49 C50 C51 -39(4) . . . . ? C49 C50 C51 C52 33(4) . . . . ? C50 C51 C52 O48 -18(3) . . . . ? C49 O48 C52 C51 -4(3) . . . . ? C57 O53 C54 C55 12(5) . . . . ? O53 C54 C55 C56 3(4) . . . . ? C54 C55 C56 C57 -18(4) . . . . ? C55 C56 C57 O53 26(3) . . . . ? C54 O53 C57 C56 -22(4) . . . . ? C59 O58 C59 C60 7.8(10) 2_655 . . . ? O58 C59 C60 C60 -21(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.046 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.107 # Attachment '4.CIF' data_tcu199m _database_code_depnum_ccdc_archive 'CCDC 721517' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H30 O6 Sb2, 2(C4H8O)' _chemical_formula_sum 'C50 H46 O8 Sb2' _chemical_formula_weight 1018.37 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' 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 13.122(7) _cell_length_b 13.766(8) _cell_length_c 14.418(8) _cell_angle_alpha 94.090(10) _cell_angle_beta 115.115(8) _cell_angle_gamma 114.994(8) _cell_volume 2035.2(19) _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 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7595 _exptl_absorpt_correction_T_max 0.8404 _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 8268 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.36 _reflns_number_total 5779 _reflns_number_gt 4539 _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^)+(0.0504P)^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 5779 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.024 _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 Sb1 Sb 0.50646(3) 0.01944(3) 0.24474(3) 0.03308(12) Uani 1 1 d . . . Sb2 Sb 0.77905(3) 0.26865(3) -0.33091(2) 0.02818(11) Uani 1 1 d . . . C11 C 0.8900(6) 0.3865(5) 0.4001(4) 0.0495(15) Uani 1 1 d . . . H11A H 0.9010 0.4563 0.3902 0.059 Uiso 1 1 calc R . . O5 O 0.6106(3) 0.1791(2) -0.3309(2) 0.0289(7) Uani 1 1 d . . . O3 O 0.5729(3) 0.1385(3) 0.1829(2) 0.0318(8) Uani 1 1 d . . . O1 O 0.6022(3) -0.0483(3) 0.2258(3) 0.0354(8) Uani 1 1 d . . . O4 O 0.8636(3) 0.3422(3) -0.1762(2) 0.0348(8) Uani 1 1 d . . . O2 O 0.6421(3) 0.1238(3) 0.3924(3) 0.0377(8) Uani 1 1 d . . . C14 C 0.6641(5) 0.3311(5) 0.3595(4) 0.0451(14) Uani 1 1 d . . . H14A H 0.7013 0.4097 0.3984 0.054 Uiso 1 1 calc R . . H14B H 0.6077 0.2840 0.3848 0.054 Uiso 1 1 calc R . . C40 C 0.1454(4) -0.0762(4) -0.8367(4) 0.0293(11) Uani 1 1 d . . . O7 O 0.7838(4) 0.4877(3) -0.3322(3) 0.0536(10) Uani 1 1 d . . . C26 C 0.6880(5) 0.2696(4) -0.0303(4) 0.0367(12) Uani 1 1 d . . . H26A H 0.6254 0.2805 -0.0230 0.044 Uiso 1 1 calc R . . C36 C 0.3123(4) 0.0517(4) -0.6563(4) 0.0255(10) Uani 1 1 d . . . C35 C 0.3982(4) 0.0725(4) -0.5385(3) 0.0265(11) Uani 1 1 d . . . H35A H 0.4852 0.0927 -0.5258 0.032 Uiso 1 1 calc R . . H35B H 0.3642 0.0017 -0.5222 0.032 Uiso 1 1 calc R . . C1 C 0.7166(5) -0.0301(4) 0.2327(4) 0.0314(11) Uani 1 1 d . . . C9 C 0.9751(5) 0.2625(5) 0.4408(4) 0.0477(15) Uani 1 1 d . . . H9A H 1.0443 0.2485 0.4592 0.057 Uiso 1 1 calc R . . C18 C 0.4174(6) 0.2789(4) 0.0259(5) 0.0462(14) Uani 1 1 d . . . H18A H 0.3629 0.2688 -0.0466 0.055 Uiso 1 1 calc R . . C39 C 0.1690(5) 0.0151(5) -0.8754(4) 0.0367(12) Uani 1 1 d . . . H39A H 0.1207 0.0031 -0.9495 0.044 Uiso 1 1 calc R . . C33 C 0.4122(4) 0.1633(4) -0.4594(4) 0.0250(10) Uani 1 1 d . . . C2 C 0.7168(5) -0.0585(4) 0.1378(4) 0.0322(11) Uani 1 1 d . . . C6 C 0.8301(5) 0.0113(4) 0.3327(4) 0.0345(12) Uani 1 1 d . . . C34 C 0.5215(4) 0.2149(4) -0.3569(4) 0.0267(11) Uani 1 1 d . . . C19 C 0.4498(5) 0.1981(4) 0.0524(4) 0.0336(12) Uani 1 1 d . . . C20 C 0.5334(5) 0.2157(4) 0.1598(4) 0.0344(12) Uani 1 1 d . . . C23 C 0.8670(4) 0.2318(4) -0.0559(4) 0.0296(11) Uani 1 1 d . . . C25 C 0.7430(5) 0.2156(4) 0.0331(4) 0.0399(13) Uani 1 1 d . . . H25A H 0.7218 0.1932 0.0855 0.048 Uiso 1 1 calc R . . C28 C 0.6629(5) 0.3678(4) -0.1719(4) 0.0363(12) Uani 1 1 d . . . H28A H 0.7286 0.4228 -0.1850 0.044 Uiso 1 1 calc R . . H28B H 0.6453 0.4103 -0.1292 0.044 Uiso 1 1 calc R . . C8 C 0.8592(5) 0.1803(5) 0.4295(4) 0.0399(13) Uani 1 1 d . . . C31 C 0.3296(5) 0.2703(4) -0.4081(4) 0.0440(14) Uani 1 1 d . . . H31A H 0.2635 0.2883 -0.4249 0.053 Uiso 1 1 calc R . . C21 C 0.6019(5) -0.0898(4) 0.0296(4) 0.0362(12) Uani 1 1 d . . . H21B H 0.6255 -0.0281 -0.0010 0.043 Uiso 1 1 calc R . . H21C H 0.5309 -0.0953 0.0404 0.043 Uiso 1 1 calc R . . C15 C 0.5809(5) 0.3122(4) 0.2418(4) 0.0421(13) Uani 1 1 d . . . C24 C 0.8305(5) 0.1951(4) 0.0179(4) 0.0369(12) Uani 1 1 d . . . H24A H 0.8657 0.1554 0.0585 0.044 Uiso 1 1 calc R . . C13 C 0.7595(5) 0.2056(4) 0.4052(4) 0.0362(12) Uani 1 1 d . . . C32 C 0.3167(5) 0.1920(4) -0.4845(4) 0.0359(12) Uani 1 1 d . . . H32A H 0.2427 0.1583 -0.5537 0.043 Uiso 1 1 calc R . . C22 C 0.8174(5) 0.2936(4) -0.1121(4) 0.0317(12) Uani 1 1 d . . . C38 C 0.2617(5) 0.1236(5) -0.8082(4) 0.0415(13) Uani 1 1 d . . . H38A H 0.2760 0.1850 -0.8358 0.050 Uiso 1 1 calc R . . C37 C 0.3327(5) 0.1399(4) -0.6996(4) 0.0369(12) Uani 1 1 d . . . H37A H 0.3971 0.2134 -0.6536 0.044 Uiso 1 1 calc R . . C7 C 0.8395(5) 0.0657(5) 0.4329(4) 0.0407(13) Uani 1 1 d . . . H7A H 0.7595 0.0208 0.4346 0.049 Uiso 1 1 calc R . . H7B H 0.9128 0.0714 0.4972 0.049 Uiso 1 1 calc R . . C3 C 0.8311(5) -0.0495(4) 0.1466(4) 0.0411(13) Uani 1 1 d . . . H3A H 0.8333 -0.0677 0.0836 0.049 Uiso 1 1 calc R . . C29 C 0.5388(5) 0.2988(4) -0.2800(4) 0.0313(11) Uani 1 1 d . . . C43 C 0.6758(6) 0.4988(5) -0.4023(5) 0.0557(16) Uani 1 1 d . . . H43A H 0.5937 0.4294 -0.4262 0.067 Uiso 1 1 calc R . . H43B H 0.6811 0.5148 -0.4658 0.067 Uiso 1 1 calc R . . C30 C 0.4382(5) 0.3211(4) -0.3088(4) 0.0411(13) Uani 1 1 d . . . H30A H 0.4449 0.3734 -0.2578 0.049 Uiso 1 1 calc R . . C4 C 0.9394(5) -0.0151(5) 0.2441(4) 0.0468(14) Uani 1 1 d . . . H4A H 1.0140 -0.0125 0.2481 0.056 Uiso 1 1 calc R . . C5 C 0.9386(5) 0.0157(4) 0.3368(4) 0.0438(14) Uani 1 1 d . . . H5A H 1.0135 0.0401 0.4039 0.053 Uiso 1 1 calc R . . C12 C 0.7731(5) 0.3069(4) 0.3892(4) 0.0384(13) Uani 1 1 d . . . C10 C 0.9900(6) 0.3645(5) 0.4252(5) 0.0531(16) Uani 1 1 d . . . H10A H 1.0685 0.4187 0.4318 0.064 Uiso 1 1 calc R . . C45 C 0.8241(8) 0.6670(7) -0.2623(8) 0.120(4) Uani 1 1 d . . . H45A H 0.8394 0.7052 -0.1938 0.144 Uiso 1 1 calc R . . H45B H 0.8636 0.7241 -0.2919 0.144 Uiso 1 1 calc R . . C42 C 0.0530(5) -0.1945(4) -0.9157(4) 0.0369(12) Uani 1 1 d . . . H42A H 0.0114 -0.2459 -0.8830 0.044 Uiso 1 1 calc R . . H42B H -0.0149 -0.1947 -0.9806 0.044 Uiso 1 1 calc R . . C46 C 0.8803(6) 0.5919(5) -0.2463(5) 0.0589(17) Uani 1 1 d . . . H46A H 0.9609 0.6256 -0.2491 0.071 Uiso 1 1 calc R . . H46B H 0.8997 0.5790 -0.1764 0.071 Uiso 1 1 calc R . . C27 C 0.7221(5) 0.3080(4) -0.1042(4) 0.0336(12) Uani 1 1 d . . . C16 C 0.5442(6) 0.3901(5) 0.2103(5) 0.0503(15) Uani 1 1 d . . . H16A H 0.5748 0.4554 0.2630 0.060 Uiso 1 1 calc R . . C44 C 0.6835(7) 0.5946(6) -0.3382(6) 0.072(2) Uani 1 1 d . . . H44A H 0.6488 0.6346 -0.3843 0.087 Uiso 1 1 calc R . . H44B H 0.6357 0.5682 -0.2999 0.087 Uiso 1 1 calc R . . C17 C 0.4641(6) 0.3750(5) 0.1043(5) 0.0553(16) Uani 1 1 d . . . H17C H 0.4412 0.4297 0.0852 0.066 Uiso 1 1 calc R . . O8 O 1.0291(3) 0.3824(3) -0.2692(3) 0.0526(10) Uani 1 1 d . . . C41 C 0.2154(4) -0.0576(4) -0.7260(4) 0.0251(11) Uani 1 1 d . . . C50 C 1.1260(6) 0.4799(5) -0.1763(5) 0.0563(16) Uani 1 1 d . . . H50A H 1.0871 0.4978 -0.1375 0.068 Uiso 1 1 calc R . . H50B H 1.1673 0.5452 -0.1972 0.068 Uiso 1 1 calc R . . C47 C 1.0964(6) 0.3318(6) -0.2868(5) 0.072(2) Uani 1 1 d . . . H47A H 1.0368 0.2510 -0.3245 0.087 Uiso 1 1 calc R . . H47B H 1.1323 0.3660 -0.3310 0.087 Uiso 1 1 calc R . . C49 C 1.2243(7) 0.4477(6) -0.1070(5) 0.074(2) Uani 1 1 d . . . H49A H 1.3135 0.5100 -0.0764 0.089 Uiso 1 1 calc R . . H49B H 1.2104 0.4257 -0.0483 0.089 Uiso 1 1 calc R . . C48 C 1.1980(7) 0.3490(7) -0.1851(6) 0.084(2) Uani 1 1 d . . . H48A H 1.2762 0.3655 -0.1888 0.101 Uiso 1 1 calc R . . H48B H 1.1718 0.2816 -0.1622 0.101 Uiso 1 1 calc R . . O6 O 0.1851(3) -0.1432(2) -0.6835(2) 0.0271(7) Uani 1 1 d . . . 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 0.0270(2) 0.0412(2) 0.0350(2) 0.01258(16) 0.01720(17) 0.01849(17) Sb2 0.02673(19) 0.02830(19) 0.02560(19) 0.00417(14) 0.01153(15) 0.01293(15) C11 0.055(4) 0.050(4) 0.042(3) 0.009(3) 0.023(3) 0.028(3) O5 0.0219(17) 0.0293(18) 0.0296(18) 0.0000(14) 0.0099(14) 0.0126(15) O3 0.0326(19) 0.039(2) 0.0302(18) 0.0121(15) 0.0162(15) 0.0225(17) O1 0.0268(18) 0.040(2) 0.039(2) 0.0095(16) 0.0171(16) 0.0170(16) O4 0.0288(19) 0.0328(19) 0.0264(18) -0.0007(15) 0.0118(15) 0.0060(16) O2 0.032(2) 0.054(2) 0.0306(19) 0.0129(16) 0.0185(16) 0.0223(18) C14 0.046(3) 0.040(3) 0.039(3) -0.002(3) 0.014(3) 0.024(3) C40 0.021(2) 0.036(3) 0.032(3) 0.006(2) 0.013(2) 0.017(2) O7 0.060(3) 0.040(2) 0.057(3) 0.0080(19) 0.023(2) 0.029(2) C26 0.034(3) 0.036(3) 0.033(3) -0.002(2) 0.016(2) 0.016(3) C36 0.023(2) 0.030(3) 0.029(3) 0.009(2) 0.015(2) 0.016(2) C35 0.024(2) 0.028(3) 0.027(3) 0.003(2) 0.011(2) 0.015(2) C1 0.030(3) 0.035(3) 0.038(3) 0.016(2) 0.018(2) 0.021(2) C9 0.026(3) 0.055(4) 0.045(3) 0.003(3) 0.012(3) 0.014(3) C18 0.052(4) 0.043(3) 0.045(3) 0.018(3) 0.020(3) 0.029(3) C39 0.040(3) 0.055(4) 0.029(3) 0.015(3) 0.019(3) 0.034(3) C33 0.027(3) 0.020(2) 0.033(3) 0.008(2) 0.019(2) 0.012(2) C2 0.034(3) 0.036(3) 0.031(3) 0.012(2) 0.016(2) 0.021(2) C6 0.030(3) 0.041(3) 0.039(3) 0.017(2) 0.019(2) 0.021(3) C34 0.024(3) 0.024(3) 0.032(3) 0.004(2) 0.015(2) 0.013(2) C19 0.035(3) 0.033(3) 0.037(3) 0.012(2) 0.020(3) 0.018(2) C20 0.034(3) 0.034(3) 0.045(3) 0.014(2) 0.026(3) 0.019(3) C23 0.021(2) 0.027(3) 0.021(3) -0.006(2) 0.005(2) 0.004(2) C25 0.041(3) 0.039(3) 0.030(3) 0.001(2) 0.018(3) 0.013(3) C28 0.039(3) 0.028(3) 0.035(3) -0.003(2) 0.016(3) 0.016(2) C8 0.036(3) 0.055(4) 0.025(3) 0.006(2) 0.012(2) 0.024(3) C31 0.034(3) 0.050(3) 0.051(4) 0.005(3) 0.018(3) 0.029(3) C21 0.039(3) 0.040(3) 0.031(3) 0.011(2) 0.016(2) 0.023(3) C15 0.040(3) 0.038(3) 0.043(3) 0.006(3) 0.018(3) 0.020(3) C24 0.036(3) 0.037(3) 0.025(3) 0.005(2) 0.010(2) 0.015(3) C13 0.027(3) 0.052(3) 0.022(3) 0.004(2) 0.012(2) 0.015(3) C32 0.025(3) 0.039(3) 0.040(3) 0.004(2) 0.013(2) 0.016(2) C22 0.029(3) 0.030(3) 0.020(3) -0.005(2) 0.009(2) 0.008(2) C38 0.057(4) 0.048(3) 0.048(3) 0.026(3) 0.037(3) 0.037(3) C37 0.038(3) 0.035(3) 0.045(3) 0.011(2) 0.025(3) 0.020(3) C7 0.035(3) 0.064(4) 0.028(3) 0.019(3) 0.011(2) 0.032(3) C3 0.046(3) 0.049(3) 0.044(3) 0.016(3) 0.029(3) 0.028(3) C29 0.032(3) 0.030(3) 0.032(3) 0.007(2) 0.018(2) 0.015(2) C43 0.065(4) 0.055(4) 0.049(4) 0.016(3) 0.025(3) 0.035(3) C30 0.046(3) 0.040(3) 0.044(3) 0.003(3) 0.024(3) 0.027(3) C4 0.033(3) 0.056(4) 0.053(4) 0.012(3) 0.019(3) 0.027(3) C5 0.031(3) 0.052(3) 0.041(3) 0.015(3) 0.009(3) 0.023(3) C12 0.037(3) 0.043(3) 0.034(3) 0.004(2) 0.016(2) 0.023(3) C10 0.041(3) 0.052(4) 0.054(4) 0.005(3) 0.026(3) 0.013(3) C45 0.082(6) 0.067(5) 0.143(8) -0.021(5) 0.001(6) 0.048(5) C42 0.024(3) 0.049(3) 0.029(3) 0.004(2) 0.008(2) 0.018(3) C46 0.051(4) 0.049(4) 0.057(4) 0.005(3) 0.021(3) 0.017(3) C27 0.035(3) 0.026(3) 0.026(3) -0.007(2) 0.010(2) 0.011(2) C16 0.057(4) 0.040(3) 0.050(4) 0.003(3) 0.019(3) 0.030(3) C44 0.081(5) 0.068(5) 0.079(5) 0.016(4) 0.035(4) 0.052(4) C17 0.066(4) 0.045(4) 0.059(4) 0.017(3) 0.024(3) 0.037(3) O8 0.035(2) 0.061(3) 0.047(2) 0.005(2) 0.0121(19) 0.023(2) C41 0.024(3) 0.028(3) 0.031(3) 0.008(2) 0.017(2) 0.016(2) C50 0.045(4) 0.044(4) 0.066(4) 0.003(3) 0.025(3) 0.017(3) C47 0.050(4) 0.091(5) 0.052(4) -0.011(4) 0.015(3) 0.031(4) C49 0.059(5) 0.068(5) 0.062(5) -0.001(4) 0.016(4) 0.024(4) C48 0.074(5) 0.087(6) 0.088(6) 0.021(5) 0.027(5) 0.053(5) O6 0.0248(17) 0.0279(18) 0.0298(18) 0.0070(14) 0.0138(15) 0.0144(15) _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 O1 1.940(3) . ? Sb1 O3 1.975(3) . ? Sb1 O2 1.988(3) . ? Sb2 O4 1.964(3) . ? Sb2 O6 1.975(3) 2_654 ? Sb2 O5 2.026(3) . ? C11 C10 1.376(8) . ? C11 C12 1.390(8) . ? C11 H11A 0.9400 . ? O5 C34 1.376(5) . ? O3 C20 1.370(6) . ? O1 C1 1.371(5) . ? O4 C22 1.376(6) . ? O2 C13 1.391(6) . ? C14 C12 1.497(7) . ? C14 C15 1.505(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C40 C39 1.380(7) . ? C40 C41 1.398(6) . ? C40 C42 1.520(6) . ? O7 C43 1.430(7) . ? O7 C46 1.440(6) . ? C26 C25 1.378(7) . ? C26 C27 1.379(7) . ? C26 H26A 0.9400 . ? C36 C37 1.382(7) . ? C36 C41 1.405(6) . ? C36 C35 1.506(6) . ? C35 C33 1.524(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C1 C2 1.398(7) . ? C1 C6 1.402(7) . ? C9 C10 1.382(8) . ? C9 C8 1.389(8) . ? C9 H9A 0.9400 . ? C18 C19 1.373(7) . ? C18 C17 1.385(7) . ? C18 H18A 0.9400 . ? C39 C38 1.381(7) . ? C39 H39A 0.9400 . ? C33 C32 1.382(6) . ? C33 C34 1.391(6) . ? C2 C3 1.400(7) . ? C2 C21 1.500(7) . ? C6 C5 1.374(7) . ? C6 C7 1.510(7) . ? C34 C29 1.413(6) . ? C19 C20 1.392(7) . ? C19 C21 1.516(6) 2_655 ? C20 C15 1.415(7) . ? C23 C24 1.386(7) . ? C23 C22 1.387(7) . ? C23 C42 1.525(6) 2_654 ? C25 C24 1.387(7) . ? C25 H25A 0.9400 . ? C28 C27 1.499(7) . ? C28 C29 1.520(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C8 C13 1.403(7) . ? C8 C7 1.495(7) . ? C31 C30 1.361(7) . ? C31 C32 1.386(7) . ? C31 H31A 0.9400 . ? C21 C19 1.516(6) 2_655 ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C15 C16 1.381(7) . ? C24 H24A 0.9400 . ? C13 C12 1.379(7) . ? C32 H32A 0.9400 . ? C22 C27 1.393(7) . ? C38 C37 1.380(7) . ? C38 H38A 0.9400 . ? C37 H37A 0.9400 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C3 C4 1.364(7) . ? C3 H3A 0.9400 . ? C29 C30 1.380(7) . ? C43 C44 1.496(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C30 H30A 0.9400 . ? C4 C5 1.379(7) . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C10 H10A 0.9400 . ? C45 C44 1.473(9) . ? C45 C46 1.483(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C42 C23 1.525(6) 2_654 ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C16 C17 1.375(8) . ? C16 H16A 0.9400 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C17 H17C 0.9400 . ? O8 C47 1.419(7) . ? O8 C50 1.438(6) . ? C41 O6 1.355(5) . ? C50 C49 1.520(9) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C47 C48 1.417(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C49 C48 1.513(9) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? O6 Sb2 1.975(3) 2_654 ? 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 O1 Sb1 O3 92.51(14) . . ? O1 Sb1 O2 97.52(13) . . ? O3 Sb1 O2 90.36(14) . . ? O4 Sb2 O6 96.50(13) . 2_654 ? O4 Sb2 O5 88.38(13) . . ? O6 Sb2 O5 90.92(12) 2_654 . ? C10 C11 C12 120.8(6) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C34 O5 Sb2 121.2(3) . . ? C20 O3 Sb1 126.0(3) . . ? C1 O1 Sb1 146.4(3) . . ? C22 O4 Sb2 122.8(3) . . ? C13 O2 Sb1 116.9(3) . . ? C12 C14 C15 116.5(4) . . ? C12 C14 H14A 108.2 . . ? C15 C14 H14A 108.2 . . ? C12 C14 H14B 108.2 . . ? C15 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? C39 C40 C41 118.8(4) . . ? C39 C40 C42 119.4(4) . . ? C41 C40 C42 121.6(4) . . ? C43 O7 C46 109.0(4) . . ? C25 C26 C27 121.8(5) . . ? C25 C26 H26A 119.1 . . ? C27 C26 H26A 119.1 . . ? C37 C36 C41 118.2(4) . . ? C37 C36 C35 120.3(4) . . ? C41 C36 C35 121.4(4) . . ? C36 C35 C33 116.8(4) . . ? C36 C35 H35A 108.1 . . ? C33 C35 H35A 108.1 . . ? C36 C35 H35B 108.1 . . ? C33 C35 H35B 108.1 . . ? H35A C35 H35B 107.3 . . ? O1 C1 C2 118.6(4) . . ? O1 C1 C6 121.1(4) . . ? C2 C1 C6 120.2(4) . . ? C10 C9 C8 121.0(5) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C19 C18 C17 120.9(5) . . ? C19 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C38 C39 C40 121.9(5) . . ? C38 C39 H39A 119.1 . . ? C40 C39 H39A 119.1 . . ? C32 C33 C34 119.0(4) . . ? C32 C33 C35 122.0(4) . . ? C34 C33 C35 118.9(4) . . ? C1 C2 C3 117.9(4) . . ? C1 C2 C21 121.3(4) . . ? C3 C2 C21 120.6(4) . . ? C5 C6 C1 119.3(5) . . ? C5 C6 C7 119.9(5) . . ? C1 C6 C7 120.3(4) . . ? O5 C34 C33 118.1(4) . . ? O5 C34 C29 120.6(4) . . ? C33 C34 C29 121.2(4) . . ? C18 C19 C20 118.8(5) . . ? C18 C19 C21 123.1(5) . 2_655 ? C20 C19 C21 118.1(4) . 2_655 ? O3 C20 C19 117.6(4) . . ? O3 C20 C15 120.9(5) . . ? C19 C20 C15 121.4(5) . . ? C24 C23 C22 118.3(4) . . ? C24 C23 C42 121.1(5) . 2_654 ? C22 C23 C42 120.2(4) . 2_654 ? C26 C25 C24 118.6(5) . . ? C26 C25 H25A 120.7 . . ? C24 C25 H25A 120.7 . . ? C27 C28 C29 118.8(4) . . ? C27 C28 H28A 107.6 . . ? C29 C28 H28A 107.6 . . ? C27 C28 H28B 107.6 . . ? C29 C28 H28B 107.6 . . ? H28A C28 H28B 107.0 . . ? C9 C8 C13 117.8(5) . . ? C9 C8 C7 119.8(5) . . ? C13 C8 C7 122.1(5) . . ? C30 C31 C32 119.8(5) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C2 C21 C19 116.9(4) . 2_655 ? C2 C21 H21B 108.1 . . ? C19 C21 H21B 108.1 2_655 . ? C2 C21 H21C 108.1 . . ? C19 C21 H21C 108.1 2_655 . ? H21B C21 H21C 107.3 . . ? C16 C15 C20 117.1(5) . . ? C16 C15 C14 119.5(5) . . ? C20 C15 C14 123.3(5) . . ? C23 C24 C25 121.4(5) . . ? C23 C24 H24A 119.3 . . ? C25 C24 H24A 119.3 . . ? C12 C13 O2 119.6(4) . . ? C12 C13 C8 121.7(5) . . ? O2 C13 C8 118.7(5) . . ? C33 C32 C31 120.3(5) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? O4 C22 C27 119.4(5) . . ? O4 C22 C23 119.4(4) . . ? C27 C22 C23 121.1(5) . . ? C39 C38 C37 118.4(5) . . ? C39 C38 H38A 120.8 . . ? C37 C38 H38A 120.8 . . ? C38 C37 C36 122.2(5) . . ? C38 C37 H37A 118.9 . . ? C36 C37 H37A 118.9 . . ? C8 C7 C6 107.1(4) . . ? C8 C7 H7A 110.3 . . ? C6 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? C6 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C4 C3 C2 121.8(5) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C30 C29 C34 116.9(4) . . ? C30 C29 C28 119.5(4) . . ? C34 C29 C28 123.6(4) . . ? O7 C43 C44 106.0(5) . . ? O7 C43 H43A 110.5 . . ? C44 C43 H43A 110.5 . . ? O7 C43 H43B 110.5 . . ? C44 C43 H43B 110.5 . . ? H43A C43 H43B 108.7 . . ? C31 C30 C29 122.6(5) . . ? C31 C30 H30A 118.7 . . ? C29 C30 H30A 118.7 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C13 C12 C11 118.7(5) . . ? C13 C12 C14 121.1(5) . . ? C11 C12 C14 120.2(5) . . ? C11 C10 C9 119.9(6) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C44 C45 C46 106.4(6) . . ? C44 C45 H45A 110.4 . . ? C46 C45 H45A 110.4 . . ? C44 C45 H45B 110.4 . . ? C46 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C23 C42 C40 107.5(4) 2_654 . ? C23 C42 H42A 110.2 2_654 . ? C40 C42 H42A 110.2 . . ? C23 C42 H42B 110.2 2_654 . ? C40 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? O7 C46 C45 106.4(5) . . ? O7 C46 H46A 110.5 . . ? C45 C46 H46A 110.5 . . ? O7 C46 H46B 110.5 . . ? C45 C46 H46B 110.5 . . ? H46A C46 H46B 108.6 . . ? C26 C27 C22 118.3(5) . . ? C26 C27 C28 121.4(4) . . ? C22 C27 C28 120.2(5) . . ? C17 C16 C15 122.0(5) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C45 C44 C43 103.2(6) . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44B 111.1 . . ? C43 C44 H44B 111.1 . . ? H44A C44 H44B 109.1 . . ? C16 C17 C18 119.7(5) . . ? C16 C17 H17C 120.2 . . ? C18 C17 H17C 120.2 . . ? C47 O8 C50 105.7(4) . . ? O6 C41 C40 120.6(4) . . ? O6 C41 C36 118.8(4) . . ? C40 C41 C36 120.4(4) . . ? O8 C50 C49 105.0(5) . . ? O8 C50 H50A 110.8 . . ? C49 C50 H50A 110.8 . . ? O8 C50 H50B 110.8 . . ? C49 C50 H50B 110.8 . . ? H50A C50 H50B 108.8 . . ? C48 C47 O8 107.8(5) . . ? C48 C47 H47A 110.1 . . ? O8 C47 H47A 110.1 . . ? C48 C47 H47B 110.1 . . ? O8 C47 H47B 110.1 . . ? H47A C47 H47B 108.5 . . ? C48 C49 C50 103.3(5) . . ? C48 C49 H49A 111.1 . . ? C50 C49 H49A 111.1 . . ? C48 C49 H49B 111.1 . . ? C50 C49 H49B 111.1 . . ? H49A C49 H49B 109.1 . . ? C47 C48 C49 106.9(6) . . ? C47 C48 H48A 110.4 . . ? C49 C48 H48A 110.4 . . ? C47 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.6 . . ? C41 O6 Sb2 136.0(3) . 2_654 ? 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 O4 Sb2 O5 C34 94.3(3) . . . . ? O6 Sb2 O5 C34 -169.2(3) 2_654 . . . ? O1 Sb1 O3 C20 172.8(4) . . . . ? O2 Sb1 O3 C20 -89.7(4) . . . . ? O3 Sb1 O1 C1 40.7(5) . . . . ? O2 Sb1 O1 C1 -50.0(6) . . . . ? O6 Sb2 O4 C22 -66.3(4) 2_654 . . . ? O5 Sb2 O4 C22 24.4(3) . . . . ? O1 Sb1 O2 C13 62.1(3) . . . . ? O3 Sb1 O2 C13 -30.5(3) . . . . ? C37 C36 C35 C33 53.2(6) . . . . ? C41 C36 C35 C33 -130.7(4) . . . . ? Sb1 O1 C1 C2 -112.3(5) . . . . ? Sb1 O1 C1 C6 70.7(7) . . . . ? C41 C40 C39 C38 1.5(7) . . . . ? C42 C40 C39 C38 -173.3(4) . . . . ? C36 C35 C33 C32 26.5(6) . . . . ? C36 C35 C33 C34 -156.7(4) . . . . ? O1 C1 C2 C3 -174.0(4) . . . . ? C6 C1 C2 C3 3.1(7) . . . . ? O1 C1 C2 C21 10.2(7) . . . . ? C6 C1 C2 C21 -172.7(5) . . . . ? O1 C1 C6 C5 172.3(5) . . . . ? C2 C1 C6 C5 -4.8(8) . . . . ? O1 C1 C6 C7 -16.5(7) . . . . ? C2 C1 C6 C7 166.5(4) . . . . ? Sb2 O5 C34 C33 101.7(4) . . . . ? Sb2 O5 C34 C29 -80.6(5) . . . . ? C32 C33 C34 O5 175.2(4) . . . . ? C35 C33 C34 O5 -1.7(6) . . . . ? C32 C33 C34 C29 -2.5(7) . . . . ? C35 C33 C34 C29 -179.4(4) . . . . ? C17 C18 C19 C20 -1.7(8) . . . . ? C17 C18 C19 C21 178.0(5) . . . 2_655 ? Sb1 O3 C20 C19 -103.2(4) . . . . ? Sb1 O3 C20 C15 79.5(5) . . . . ? C18 C19 C20 O3 -174.6(4) . . . . ? C21 C19 C20 O3 5.7(7) 2_655 . . . ? C18 C19 C20 C15 2.7(8) . . . . ? C21 C19 C20 C15 -177.0(5) 2_655 . . . ? C27 C26 C25 C24 -3.1(7) . . . . ? C10 C9 C8 C13 -2.0(8) . . . . ? C10 C9 C8 C7 172.2(5) . . . . ? C1 C2 C21 C19 -129.3(5) . . . 2_655 ? C3 C2 C21 C19 55.1(7) . . . 2_655 ? O3 C20 C15 C16 175.1(5) . . . . ? C19 C20 C15 C16 -2.1(8) . . . . ? O3 C20 C15 C14 -7.1(8) . . . . ? C19 C20 C15 C14 175.7(5) . . . . ? C12 C14 C15 C16 -137.3(6) . . . . ? C12 C14 C15 C20 44.9(8) . . . . ? C22 C23 C24 C25 2.3(7) . . . . ? C42 C23 C24 C25 -170.9(4) 2_654 . . . ? C26 C25 C24 C23 2.8(7) . . . . ? Sb1 O2 C13 C12 86.9(5) . . . . ? Sb1 O2 C13 C8 -90.2(5) . . . . ? C9 C8 C13 C12 2.2(7) . . . . ? C7 C8 C13 C12 -171.8(5) . . . . ? C9 C8 C13 O2 179.2(4) . . . . ? C7 C8 C13 O2 5.2(7) . . . . ? C34 C33 C32 C31 -0.6(7) . . . . ? C35 C33 C32 C31 176.2(5) . . . . ? C30 C31 C32 C33 1.6(8) . . . . ? Sb2 O4 C22 C27 -86.3(5) . . . . ? Sb2 O4 C22 C23 94.1(4) . . . . ? C24 C23 C22 O4 172.4(4) . . . . ? C42 C23 C22 O4 -14.4(6) 2_654 . . . ? C24 C23 C22 C27 -7.2(7) . . . . ? C42 C23 C22 C27 166.1(4) 2_654 . . . ? C40 C39 C38 C37 0.6(7) . . . . ? C39 C38 C37 C36 -1.2(7) . . . . ? C41 C36 C37 C38 -0.3(7) . . . . ? C35 C36 C37 C38 175.9(4) . . . . ? C9 C8 C7 C6 -68.3(6) . . . . ? C13 C8 C7 C6 105.6(5) . . . . ? C5 C6 C7 C8 96.0(6) . . . . ? C1 C6 C7 C8 -75.2(6) . . . . ? C1 C2 C3 C4 0.5(8) . . . . ? C21 C2 C3 C4 176.3(5) . . . . ? O5 C34 C29 C30 -173.1(4) . . . . ? C33 C34 C29 C30 4.5(7) . . . . ? O5 C34 C29 C28 9.9(7) . . . . ? C33 C34 C29 C28 -172.5(5) . . . . ? C27 C28 C29 C30 135.0(5) . . . . ? C27 C28 C29 C34 -48.1(7) . . . . ? C46 O7 C43 C44 -20.7(7) . . . . ? C32 C31 C30 C29 0.6(9) . . . . ? C34 C29 C30 C31 -3.6(8) . . . . ? C28 C29 C30 C31 173.5(5) . . . . ? C2 C3 C4 C5 -2.4(9) . . . . ? C1 C6 C5 C4 2.9(8) . . . . ? C7 C6 C5 C4 -168.4(5) . . . . ? C3 C4 C5 C6 0.7(9) . . . . ? O2 C13 C12 C11 -178.6(4) . . . . ? C8 C13 C12 C11 -1.6(7) . . . . ? O2 C13 C12 C14 0.7(7) . . . . ? C8 C13 C12 C14 177.8(5) . . . . ? C10 C11 C12 C13 0.7(8) . . . . ? C10 C11 C12 C14 -178.6(5) . . . . ? C15 C14 C12 C13 -97.5(6) . . . . ? C15 C14 C12 C11 81.9(6) . . . . ? C12 C11 C10 C9 -0.6(8) . . . . ? C8 C9 C10 C11 1.2(8) . . . . ? C39 C40 C42 C23 88.5(5) . . . 2_654 ? C41 C40 C42 C23 -86.2(5) . . . 2_654 ? C43 O7 C46 C45 3.3(8) . . . . ? C44 C45 C46 O7 15.7(10) . . . . ? C25 C26 C27 C22 -1.6(7) . . . . ? C25 C26 C27 C28 -179.3(4) . . . . ? O4 C22 C27 C26 -172.7(4) . . . . ? C23 C22 C27 C26 6.8(7) . . . . ? O4 C22 C27 C28 5.0(6) . . . . ? C23 C22 C27 C28 -175.4(4) . . . . ? C29 C28 C27 C26 -89.7(6) . . . . ? C29 C28 C27 C22 92.6(6) . . . . ? C20 C15 C16 C17 0.5(9) . . . . ? C14 C15 C16 C17 -177.4(6) . . . . ? C46 C45 C44 C43 -27.5(9) . . . . ? O7 C43 C44 C45 29.6(8) . . . . ? C15 C16 C17 C18 0.5(10) . . . . ? C19 C18 C17 C16 0.1(9) . . . . ? C39 C40 C41 O6 172.6(4) . . . . ? C42 C40 C41 O6 -12.7(6) . . . . ? C39 C40 C41 C36 -3.0(6) . . . . ? C42 C40 C41 C36 171.7(4) . . . . ? C37 C36 C41 O6 -173.2(4) . . . . ? C35 C36 C41 O6 10.6(6) . . . . ? C37 C36 C41 C40 2.4(6) . . . . ? C35 C36 C41 C40 -173.7(4) . . . . ? C47 O8 C50 C49 -32.3(7) . . . . ? C50 O8 C47 C48 33.9(8) . . . . ? O8 C50 C49 C48 19.0(7) . . . . ? O8 C47 C48 C49 -21.0(9) . . . . ? C50 C49 C48 C47 0.8(9) . . . . ? C40 C41 O6 Sb2 80.3(5) . . . 2_654 ? C36 C41 O6 Sb2 -104.1(4) . . . 2_654 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.923 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.088 # Attachment '4a.CIF' data_tcu171m _database_code_depnum_ccdc_archive 'CCDC 721518' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H31 O8 Sb3, 4(C4H8O)' _chemical_formula_sum 'C58 H63 O12 Sb3' _chemical_formula_weight 1317.39 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 13.617(2) _cell_length_b 13.864(2) _cell_length_c 15.698(2) _cell_angle_alpha 69.825(3) _cell_angle_beta 79.972(2) _cell_angle_gamma 69.980(3) _cell_volume 2608.3(7) _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 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.821 _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 14392 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.29 _reflns_number_total 7451 _reflns_number_gt 5348 _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. PLATON/SQUEEZE estimated the solvent-accessible region void to occupy 644.4 \%A^3^ and contain 163 electrons. The electron density was modelled as 4 THF molecules (2 THF molecules per assymetric unit) which accounts for 160 electrons. The THF molecules where added in the formula weight on the structure of assymetric unit. ; _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^)+(0.0534P)^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 7451 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.79477(3) 0.24028(4) 0.34002(3) 0.03367(14) Uani 1 1 d . . . C34 C 1.1006(8) 0.5863(9) 0.3378(6) 0.068(3) Uani 1 1 d . . . Sb2 Sb 0.95843(3) 0.39169(3) 0.21866(3) 0.03060(14) Uani 1 1 d . . . Sb3 Sb 0.97485(4) 0.42812(4) 0.42020(3) 0.04556(16) Uani 1 1 d . . . C13 C 0.7974(7) 0.2280(8) 0.1515(5) 0.066(3) Uani 1 1 d . . . O7 O 0.8799(3) 0.3280(3) 0.3340(3) 0.0320(10) Uani 1 1 d . . . C47 C 1.1164(7) 0.5350(7) 0.0664(7) 0.097(4) Uani 1 1 d . . . H47A H 1.0945 0.5731 0.1120 0.117 Uiso 1 1 calc R . . H47B H 1.0677 0.5726 0.0177 0.117 Uiso 1 1 calc R . . O5 O 1.0339(4) 0.5465(4) 0.4104(3) 0.0571(15) Uani 1 1 d . . . O2 O 0.8161(3) 0.2812(4) 0.2030(3) 0.0448(12) Uani 1 1 d . . . O3 O 1.0672(3) 0.2494(3) 0.2318(3) 0.0388(11) Uani 1 1 d . . . O9 O 0.7436(3) 0.2437(4) 0.5032(3) 0.0418(12) Uani 1 1 d . . . O1 O 0.6627(3) 0.3609(4) 0.3294(3) 0.0487(13) Uani 1 1 d . . . O8 O 1.0230(3) 0.4356(4) 0.2946(3) 0.0417(12) Uani 1 1 d . . . O10 O 1.1150(3) 0.4291(4) 0.1058(3) 0.0500(13) Uani 1 1 d . . . O4 O 1.1046(4) 0.3120(5) 0.4707(3) 0.0694(17) Uani 1 1 d . . . C32 C 1.1296(12) 0.7242(9) 0.2063(8) 0.130(6) Uani 1 1 d . . . H32A H 1.1035 0.7918 0.1629 0.156 Uiso 1 1 calc R . . C19 C 1.0803(6) 0.0871(6) 0.3571(6) 0.062(3) Uani 1 1 d . . . C49 C 1.2869(7) 0.4352(10) 0.0872(6) 0.095(4) Uani 1 1 d . . . H49A H 1.3205 0.4501 0.1296 0.114 Uiso 1 1 calc R . . H49B H 1.3417 0.3957 0.0513 0.114 Uiso 1 1 calc R . . C27 C 1.1890(6) 0.2727(9) 0.4151(5) 0.071(3) Uani 1 1 d . . . C14 C 0.9905(7) 0.1709(6) 0.1165(5) 0.068(3) Uani 1 1 d . . . H14A H 1.0407 0.1399 0.0728 0.081 Uiso 1 1 calc R . . H14B H 0.9921 0.2447 0.1043 0.081 Uiso 1 1 calc R . . C22 C 1.1940(6) 0.1834(8) 0.3891(6) 0.068(3) Uani 1 1 d . . . C23 C 1.2840(5) 0.1412(7) 0.3418(5) 0.076(3) Uani 1 1 d . . . H23A H 1.2916 0.0790 0.3265 0.092 Uiso 1 1 calc R . . C15 C 1.0229(7) 0.1050(6) 0.2115(6) 0.063(3) Uani 1 1 d . . . C20 C 1.0549(5) 0.1488(6) 0.2667(5) 0.047(2) Uani 1 1 d . . . C26 C 1.2662(6) 0.3250(9) 0.3874(5) 0.074(3) Uani 1 1 d . . . C25 C 1.3540(7) 0.2785(11) 0.3393(6) 0.086(4) Uani 1 1 d . . . H25A H 1.4088 0.3095 0.3218 0.103 Uiso 1 1 calc R . . C12 C 0.8815(8) 0.1742(8) 0.1036(5) 0.079(3) Uani 1 1 d . . . C7 C 0.6036(9) 0.2795(15) 0.2056(6) 0.143(7) Uani 1 1 d . . . H7A H 0.5394 0.2715 0.1927 0.172 Uiso 1 1 calc R . . H7B H 0.6159 0.2396 0.2698 0.172 Uiso 1 1 calc R . . C2 C 0.6041(7) 0.5430(13) 0.2335(8) 0.119(6) Uani 1 1 d . . . C21 C 1.1053(6) 0.1347(7) 0.4206(6) 0.065(3) Uani 1 1 d . . . H21A H 1.1220 0.0779 0.4788 0.078 Uiso 1 1 calc R . . H21B H 1.0420 0.1906 0.4319 0.078 Uiso 1 1 calc R . . C10 C 0.7582(16) 0.1312(15) 0.0402(8) 0.198(10) Uani 1 1 d . . . H10A H 0.7445 0.1007 0.0003 0.238 Uiso 1 1 calc R . . C33 C 1.0594(9) 0.6817(9) 0.2747(8) 0.092(4) Uani 1 1 d . . . C1 C 0.6196(5) 0.4333(10) 0.2498(5) 0.074(3) Uani 1 1 d . . . C24 C 1.3640(6) 0.1884(10) 0.3159(7) 0.090(4) Uani 1 1 d . . . H24A H 1.4245 0.1591 0.2827 0.108 Uiso 1 1 calc R . . C43 C 0.6624(7) 0.1933(7) 0.5429(6) 0.069(3) Uani 1 1 d . . . H43A H 0.6465 0.1635 0.5006 0.082 Uiso 1 1 calc R . . H43B H 0.6843 0.1348 0.5993 0.082 Uiso 1 1 calc R . . C31 C 1.2353(14) 0.6689(14) 0.2014(10) 0.145(8) Uani 1 1 d . . . H31A H 1.2805 0.6967 0.1541 0.174 Uiso 1 1 calc R . . C28 C 1.2571(7) 0.4255(13) 0.4092(7) 0.110(5) Uani 1 1 d . . . H28A H 1.3271 0.4236 0.4186 0.132 Uiso 1 1 calc R . . H28B H 1.2145 0.4253 0.4663 0.132 Uiso 1 1 calc R . . C6 C 0.5867(7) 0.3958(13) 0.1912(6) 0.118(6) Uani 1 1 d . . . C18 C 1.0754(8) -0.0174(8) 0.3893(7) 0.097(4) Uani 1 1 d . . . H18A H 1.0920 -0.0592 0.4494 0.117 Uiso 1 1 calc R . . C8 C 0.6960(9) 0.2282(11) 0.1465(5) 0.105(5) Uani 1 1 d . . . C48 C 1.2252(7) 0.5341(9) 0.0285(7) 0.088(3) Uani 1 1 d . . . H48A H 1.2358 0.5338 -0.0348 0.105 Uiso 1 1 calc R . . H48B H 1.2414 0.5963 0.0320 0.105 Uiso 1 1 calc R . . C29 C 1.2093(8) 0.5290(10) 0.3365(7) 0.085(4) Uani 1 1 d . . . C35 C 0.9421(11) 0.7415(8) 0.2795(8) 0.125(6) Uani 1 1 d . . . H35A H 0.9163 0.7287 0.3435 0.150 Uiso 1 1 calc R . . H35B H 0.9314 0.8192 0.2522 0.150 Uiso 1 1 calc R . . C42 C 0.6555(9) 0.5785(8) 0.2835(9) 0.110(5) Uani 1 1 d . . . H42A H 0.6854 0.5165 0.3354 0.132 Uiso 1 1 calc R . . H42B H 0.6017 0.6317 0.3083 0.132 Uiso 1 1 calc R . . C50 C 1.2164(7) 0.3698(11) 0.1383(8) 0.148(7) Uani 1 1 d . . . H50A H 1.2407 0.2994 0.1278 0.177 Uiso 1 1 calc R . . H50B H 1.2150 0.3582 0.2037 0.177 Uiso 1 1 calc R . . O6 O 0.7781(5) 0.6448(5) 0.3695(5) 0.108(3) Uani 1 1 d . . . H6A H 0.7294 0.6179 0.3870 0.162 Uiso 1 1 calc R . . C4 C 0.5045(13) 0.588(2) 0.1091(14) 0.234(19) Uani 1 1 d . . . H4A H 0.4607 0.6420 0.0643 0.281 Uiso 1 1 calc R . . C3 C 0.5445(8) 0.6167(15) 0.1616(10) 0.178(11) Uani 1 1 d . . . H3A H 0.5327 0.6907 0.1509 0.214 Uiso 1 1 calc R . . C41 C 0.7991(10) 0.6625(8) 0.2773(9) 0.105(5) Uani 1 1 d . . . C37 C 0.8927(10) 0.7240(8) 0.1363(8) 0.100(5) Uani 1 1 d . . . H37A H 0.9417 0.7590 0.1026 0.120 Uiso 1 1 calc R . . C39 C 0.7630(7) 0.6460(7) 0.1382(7) 0.089(4) Uani 1 1 d . . . H39A H 0.7238 0.6256 0.1075 0.107 Uiso 1 1 calc R . . C36 C 0.8790(9) 0.7079(7) 0.2321(8) 0.096(4) Uani 1 1 d . . . C30 C 1.2712(9) 0.5762(12) 0.2650(8) 0.102(5) Uani 1 1 d . . . H30A H 1.3434 0.5396 0.2618 0.123 Uiso 1 1 calc R . . C16 C 1.0198(9) -0.0017(7) 0.2482(7) 0.098(4) Uani 1 1 d . . . H16A H 0.9990 -0.0328 0.2126 0.118 Uiso 1 1 calc R . . C40 C 0.7436(9) 0.6291(8) 0.2342(8) 0.100(5) Uani 1 1 d . . . C46 C 0.7213(6) 0.3323(6) 0.5374(5) 0.053(2) Uani 1 1 d . . . H46A H 0.7355 0.3943 0.4894 0.063 Uiso 1 1 calc R . . H46B H 0.7651 0.3125 0.5878 0.063 Uiso 1 1 calc R . . C44 C 0.5731(8) 0.2765(10) 0.5610(9) 0.127(5) Uani 1 1 d . . . H44A H 0.5350 0.2477 0.6178 0.152 Uiso 1 1 calc R . . H44B H 0.5257 0.3070 0.5115 0.152 Uiso 1 1 calc R . . C38 C 0.8396(9) 0.6923(9) 0.0908(9) 0.102(4) Uani 1 1 d . . . H38A H 0.8546 0.7016 0.0283 0.123 Uiso 1 1 calc R . . C5 C 0.5251(9) 0.4773(18) 0.1171(8) 0.170(10) Uani 1 1 d . . . H5A H 0.4997 0.4576 0.0756 0.204 Uiso 1 1 calc R . . C17 C 1.0468(11) -0.0610(8) 0.3352(10) 0.125(6) Uani 1 1 d . . . H17A H 1.0457 -0.1328 0.3581 0.150 Uiso 1 1 calc R . . C11 C 0.8588(13) 0.1274(11) 0.0467(7) 0.145(7) Uani 1 1 d . . . H11A H 0.9137 0.0925 0.0119 0.174 Uiso 1 1 calc R . . C45 C 0.6118(7) 0.3592(9) 0.5684(9) 0.108(4) Uani 1 1 d . . . H45A H 0.5730 0.4308 0.5305 0.129 Uiso 1 1 calc R . . H45B H 0.6037 0.3596 0.6316 0.129 Uiso 1 1 calc R . . C9 C 0.6815(13) 0.1774(15) 0.0899(7) 0.181(9) Uani 1 1 d . . . H9A H 0.6137 0.1760 0.0870 0.217 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 0.0355(3) 0.0409(3) 0.0310(3) -0.0116(2) 0.00282(19) -0.0214(2) C34 0.096(7) 0.096(8) 0.064(6) -0.058(6) 0.038(5) -0.081(7) Sb2 0.0271(2) 0.0302(3) 0.0338(3) -0.0071(2) -0.00220(18) -0.01069(19) Sb3 0.0384(3) 0.0711(4) 0.0425(3) -0.0227(3) 0.0107(2) -0.0368(3) C13 0.101(7) 0.117(8) 0.018(4) -0.023(5) 0.022(4) -0.090(6) O7 0.032(2) 0.039(3) 0.032(3) -0.012(2) 0.0005(19) -0.019(2) C47 0.076(7) 0.056(7) 0.116(9) 0.004(6) 0.029(6) -0.012(5) O5 0.064(3) 0.097(4) 0.046(3) -0.040(3) 0.028(3) -0.066(3) O2 0.044(3) 0.078(4) 0.035(3) -0.028(3) 0.011(2) -0.042(3) O3 0.033(3) 0.028(3) 0.044(3) -0.004(2) 0.010(2) -0.008(2) O9 0.044(3) 0.048(3) 0.034(3) -0.009(2) 0.003(2) -0.021(2) O1 0.023(2) 0.067(4) 0.037(3) -0.002(3) 0.000(2) -0.006(2) O8 0.040(3) 0.054(3) 0.042(3) -0.016(2) 0.001(2) -0.028(2) O10 0.035(3) 0.045(3) 0.058(3) 0.005(3) -0.009(2) -0.015(2) O4 0.032(3) 0.126(5) 0.042(3) -0.005(3) -0.001(2) -0.036(3) C32 0.216(15) 0.086(8) 0.121(10) -0.070(8) 0.112(11) -0.108(10) C19 0.041(5) 0.040(5) 0.057(6) 0.006(5) 0.020(4) 0.012(4) C49 0.058(6) 0.156(11) 0.065(7) -0.005(7) 0.007(5) -0.060(7) C27 0.023(4) 0.132(9) 0.028(5) 0.015(5) -0.005(3) -0.026(5) C14 0.118(8) 0.047(5) 0.047(5) -0.031(4) 0.040(5) -0.041(5) C22 0.029(4) 0.086(7) 0.041(5) 0.024(5) 0.000(4) -0.005(4) C23 0.025(4) 0.082(7) 0.060(6) 0.030(5) 0.004(4) 0.005(4) C15 0.086(6) 0.039(5) 0.057(6) -0.026(4) 0.041(5) -0.021(4) C20 0.040(4) 0.026(4) 0.056(5) -0.012(4) 0.025(4) 0.001(3) C26 0.028(4) 0.159(10) 0.025(4) -0.008(5) -0.011(3) -0.032(5) C25 0.036(5) 0.153(11) 0.039(6) 0.011(6) -0.004(4) -0.031(6) C12 0.134(9) 0.123(8) 0.033(5) -0.041(5) 0.041(5) -0.112(8) C7 0.107(9) 0.35(2) 0.034(6) -0.041(10) 0.025(6) -0.184(14) C2 0.028(5) 0.129(12) 0.082(9) 0.058(9) 0.027(5) 0.012(6) C21 0.036(4) 0.073(6) 0.047(5) 0.015(5) 0.009(4) -0.008(4) C10 0.35(2) 0.35(2) 0.061(8) -0.093(12) 0.077(11) -0.32(2) C33 0.144(10) 0.073(7) 0.099(8) -0.067(7) 0.078(8) -0.085(8) C1 0.016(4) 0.130(9) 0.033(5) 0.019(5) -0.006(3) -0.011(5) C24 0.027(5) 0.128(10) 0.051(6) 0.030(6) 0.000(4) -0.005(6) C43 0.076(6) 0.079(7) 0.060(6) -0.028(5) 0.028(5) -0.045(5) C31 0.217(17) 0.186(16) 0.137(13) -0.135(12) 0.140(13) -0.176(15) C28 0.056(6) 0.282(17) 0.049(6) -0.084(9) 0.026(5) -0.102(9) C6 0.038(5) 0.250(17) 0.032(6) 0.039(8) -0.007(4) -0.083(8) C18 0.103(8) 0.036(7) 0.077(8) 0.016(5) 0.045(6) 0.014(5) C8 0.129(9) 0.223(13) 0.034(5) -0.037(7) 0.019(5) -0.154(10) C48 0.075(7) 0.102(9) 0.085(7) -0.010(7) 0.013(6) -0.053(6) C29 0.085(7) 0.172(11) 0.065(7) -0.077(7) 0.040(6) -0.103(8) C35 0.222(15) 0.032(6) 0.096(9) -0.030(6) 0.104(9) -0.055(8) C42 0.074(8) 0.052(7) 0.114(11) 0.013(6) 0.066(7) 0.018(6) C50 0.041(6) 0.182(13) 0.128(10) 0.081(9) -0.018(6) -0.046(7) O6 0.122(6) 0.068(4) 0.097(5) -0.023(4) 0.082(5) -0.030(4) C4 0.026(8) 0.38(3) 0.102(14) 0.11(2) 0.004(7) -0.014(15) C3 0.022(7) 0.204(16) 0.122(13) 0.097(13) 0.031(7) 0.027(8) C41 0.117(10) 0.029(6) 0.113(10) -0.012(6) 0.090(9) -0.010(6) C37 0.118(10) 0.039(6) 0.082(9) 0.006(6) 0.070(8) -0.012(6) C39 0.052(5) 0.062(6) 0.090(7) 0.008(5) 0.040(5) 0.006(4) C36 0.120(9) 0.025(5) 0.100(9) -0.022(5) 0.070(7) -0.004(5) C30 0.111(9) 0.190(14) 0.093(9) -0.105(9) 0.072(8) -0.130(11) C16 0.162(11) 0.038(6) 0.088(8) -0.031(6) 0.065(7) -0.046(6) C40 0.082(8) 0.026(6) 0.102(10) 0.017(5) 0.068(7) 0.018(5) C46 0.050(5) 0.066(6) 0.057(5) -0.041(5) 0.010(4) -0.020(4) C44 0.073(7) 0.178(13) 0.193(13) -0.130(11) 0.073(8) -0.083(8) C38 0.092(9) 0.066(8) 0.090(9) -0.001(7) 0.048(7) -0.003(6) C5 0.033(7) 0.40(3) 0.040(7) 0.003(13) 0.000(5) -0.098(13) C17 0.172(13) 0.031(6) 0.125(12) -0.015(7) 0.088(10) -0.030(7) C11 0.278(19) 0.190(14) 0.061(7) -0.076(8) 0.072(9) -0.192(14) C45 0.057(6) 0.124(10) 0.182(12) -0.109(9) 0.040(7) -0.037(6) C9 0.246(18) 0.39(2) 0.053(7) -0.089(11) 0.049(9) -0.284(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 O7 1.918(4) . ? Sb1 O1 1.977(4) . ? Sb1 O2 2.021(4) . ? Sb1 O9 2.548(4) . ? C34 C33 1.352(14) . ? C34 O5 1.406(9) . ? C34 C29 1.421(14) . ? Sb2 O8 1.948(4) . ? Sb2 O3 1.989(4) . ? Sb2 O7 2.017(4) . ? Sb3 O8 1.946(4) . ? Sb3 O4 2.001(5) . ? Sb3 O5 2.012(4) . ? C13 O2 1.369(8) . ? C13 C12 1.392(13) . ? C13 C8 1.396(12) . ? C47 O10 1.389(9) . ? C47 C48 1.495(12) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? O3 C20 1.369(8) . ? O9 C46 1.424(8) . ? O9 C43 1.446(8) . ? O1 C1 1.379(9) . ? O10 C50 1.422(10) . ? O4 C27 1.389(10) . ? C32 C31 1.38(2) . ? C32 C33 1.415(13) . ? C32 H32A 0.9400 . ? C19 C18 1.382(12) . ? C19 C20 1.413(11) . ? C19 C21 1.506(12) . ? C49 C48 1.430(13) . ? C49 C50 1.488(12) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C27 C26 1.401(12) . ? C27 C22 1.408(13) . ? C14 C15 1.505(11) . ? C14 C12 1.516(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C22 C23 1.375(11) . ? C22 C21 1.510(11) . ? C23 C24 1.390(13) . ? C23 H23A 0.9400 . ? C15 C16 1.403(11) . ? C15 C20 1.410(11) . ? C26 C25 1.383(13) . ? C26 C28 1.505(15) . ? C25 C24 1.377(14) . ? C25 H25A 0.9400 . ? C12 C11 1.395(12) . ? C7 C6 1.489(19) . ? C7 C8 1.545(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C2 C3 1.390(16) . ? C2 C1 1.398(17) . ? C2 C42 1.429(18) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C10 C9 1.31(2) . ? C10 C11 1.37(2) . ? C10 H10A 0.9400 . ? C33 C35 1.530(16) . ? C1 C6 1.397(16) . ? C24 H24A 0.9400 . ? C43 C44 1.427(13) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C31 C30 1.320(19) . ? C31 H31A 0.9400 . ? C28 C29 1.508(16) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C6 C5 1.455(16) . ? C18 C17 1.367(17) . ? C18 H18A 0.9400 . ? C8 C9 1.383(14) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C29 C30 1.393(12) . ? C35 C36 1.499(17) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C42 C40 1.552(14) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? O6 C41 1.377(13) . ? O6 H6A 0.8300 . ? C4 C3 1.29(4) . ? C4 C5 1.43(3) . ? C4 H4A 0.9400 . ? C3 H3A 0.9400 . ? C41 C40 1.370(17) . ? C41 C36 1.406(14) . ? C37 C38 1.357(15) . ? C37 C36 1.430(14) . ? C37 H37A 0.9400 . ? C39 C38 1.382(13) . ? C39 C40 1.434(14) . ? C39 H39A 0.9400 . ? C30 H30A 0.9400 . ? C16 C17 1.367(16) . ? C16 H16A 0.9400 . ? C46 C45 1.445(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C44 C45 1.460(12) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C38 H38A 0.9400 . ? C5 H5A 0.9400 . ? C17 H17A 0.9400 . ? C11 H11A 0.9400 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C9 H9A 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 O7 Sb1 O1 93.79(19) . . ? O7 Sb1 O2 86.76(16) . . ? O1 Sb1 O2 90.08(19) . . ? O7 Sb1 O9 86.03(15) . . ? O1 Sb1 O9 76.59(17) . . ? O2 Sb1 O9 164.37(17) . . ? C33 C34 O5 118.3(9) . . ? C33 C34 C29 122.4(9) . . ? O5 C34 C29 119.2(10) . . ? O8 Sb2 O3 95.42(19) . . ? O8 Sb2 O7 86.17(16) . . ? O3 Sb2 O7 90.85(17) . . ? O8 Sb3 O4 93.9(2) . . ? O8 Sb3 O5 90.26(18) . . ? O4 Sb3 O5 92.8(2) . . ? O2 C13 C12 118.7(7) . . ? O2 C13 C8 120.8(8) . . ? C12 C13 C8 120.5(8) . . ? Sb1 O7 Sb2 123.0(2) . . ? O10 C47 C48 108.6(8) . . ? O10 C47 H47A 110.0 . . ? C48 C47 H47A 110.0 . . ? O10 C47 H47B 110.0 . . ? C48 C47 H47B 110.0 . . ? H47A C47 H47B 108.3 . . ? C34 O5 Sb3 124.8(4) . . ? C13 O2 Sb1 124.5(4) . . ? C20 O3 Sb2 128.3(4) . . ? C46 O9 C43 106.4(5) . . ? C46 O9 Sb1 128.1(4) . . ? C43 O9 Sb1 110.8(4) . . ? C1 O1 Sb1 126.4(5) . . ? Sb3 O8 Sb2 123.3(2) . . ? C47 O10 C50 105.3(7) . . ? C27 O4 Sb3 122.1(4) . . ? C31 C32 C33 121.8(14) . . ? C31 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? C18 C19 C20 118.7(10) . . ? C18 C19 C21 119.4(9) . . ? C20 C19 C21 121.7(8) . . ? C48 C49 C50 108.1(8) . . ? C48 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? C48 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? O4 C27 C26 117.4(10) . . ? O4 C27 C22 119.6(7) . . ? C26 C27 C22 123.0(9) . . ? C15 C14 C12 111.6(7) . . ? C15 C14 H14A 109.3 . . ? C12 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C12 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C23 C22 C27 117.1(9) . . ? C23 C22 C21 123.9(10) . . ? C27 C22 C21 118.8(8) . . ? C22 C23 C24 121.4(11) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C16 C15 C20 118.1(9) . . ? C16 C15 C14 120.6(9) . . ? C20 C15 C14 121.3(7) . . ? O3 C20 C15 120.3(7) . . ? O3 C20 C19 119.2(8) . . ? C15 C20 C19 120.4(8) . . ? C25 C26 C27 116.4(11) . . ? C25 C26 C28 120.5(9) . . ? C27 C26 C28 123.1(9) . . ? C24 C25 C26 122.3(10) . . ? C24 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? C13 C12 C11 117.2(10) . . ? C13 C12 C14 118.0(7) . . ? C11 C12 C14 124.9(10) . . ? C6 C7 C8 114.3(8) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C3 C2 C1 118.0(17) . . ? C3 C2 C42 120.4(17) . . ? C1 C2 C42 121.3(10) . . ? C19 C21 C22 116.6(7) . . ? C19 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? C19 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C9 C10 C11 119.7(11) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C34 C33 C32 117.3(12) . . ? C34 C33 C35 120.6(8) . . ? C32 C33 C35 122.1(12) . . ? O1 C1 C6 119.2(11) . . ? O1 C1 C2 118.5(10) . . ? C6 C1 C2 122.2(10) . . ? C25 C24 C23 119.5(10) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C44 C43 O9 105.8(7) . . ? C44 C43 H43A 110.6 . . ? O9 C43 H43A 110.6 . . ? C44 C43 H43B 110.6 . . ? O9 C43 H43B 110.6 . . ? H43A C43 H43B 108.7 . . ? C30 C31 C32 118.3(11) . . ? C30 C31 H31A 120.9 . . ? C32 C31 H31A 120.9 . . ? C26 C28 C29 114.1(7) . . ? C26 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? C26 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C1 C6 C5 116.6(15) . . ? C1 C6 C7 123.5(9) . . ? C5 C6 C7 119.6(14) . . ? C17 C18 C19 121.0(11) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C9 C8 C13 118.1(12) . . ? C9 C8 C7 121.0(10) . . ? C13 C8 C7 120.9(8) . . ? C49 C48 C47 102.0(8) . . ? C49 C48 H48A 111.4 . . ? C47 C48 H48A 111.4 . . ? C49 C48 H48B 111.4 . . ? C47 C48 H48B 111.4 . . ? H48A C48 H48B 109.2 . . ? C30 C29 C34 115.9(12) . . ? C30 C29 C28 121.1(11) . . ? C34 C29 C28 122.9(8) . . ? C36 C35 C33 113.4(8) . . ? C36 C35 H35A 108.9 . . ? C33 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C33 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C2 C42 C40 119.0(11) . . ? C2 C42 H42A 107.6 . . ? C40 C42 H42A 107.6 . . ? C2 C42 H42B 107.6 . . ? C40 C42 H42B 107.6 . . ? H42A C42 H42B 107.0 . . ? O10 C50 C49 106.7(8) . . ? O10 C50 H50A 110.4 . . ? C49 C50 H50A 110.4 . . ? O10 C50 H50B 110.4 . . ? C49 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? C41 O6 H6A 109.5 . . ? C3 C4 C5 121.6(18) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C4 C3 C2 123(2) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C40 C41 O6 117.5(10) . . ? C40 C41 C36 122.6(12) . . ? O6 C41 C36 119.8(14) . . ? C38 C37 C36 124.4(11) . . ? C38 C37 H37A 117.8 . . ? C36 C37 H37A 117.8 . . ? C38 C39 C40 119.8(12) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C41 C36 C37 114.8(13) . . ? C41 C36 C35 122.8(11) . . ? C37 C36 C35 122.3(10) . . ? C31 C30 C29 124.3(14) . . ? C31 C30 H30A 117.8 . . ? C29 C30 H30A 117.8 . . ? C17 C16 C15 120.7(11) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C41 C40 C39 119.4(10) . . ? C41 C40 C42 123.0(12) . . ? C39 C40 C42 117.6(13) . . ? O9 C46 C45 107.5(6) . . ? O9 C46 H46A 110.2 . . ? C45 C46 H46A 110.2 . . ? O9 C46 H46B 110.2 . . ? C45 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? C43 C44 C45 106.9(8) . . ? C43 C44 H44A 110.3 . . ? C45 C44 H44A 110.3 . . ? C43 C44 H44B 110.3 . . ? C45 C44 H44B 110.3 . . ? H44A C44 H44B 108.6 . . ? C37 C38 C39 118.8(12) . . ? C37 C38 H38A 120.6 . . ? C39 C38 H38A 120.6 . . ? C4 C5 C6 118.0(18) . . ? C4 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? C18 C17 C16 121.1(10) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C10 C11 C12 121.6(13) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C46 C45 C44 106.4(8) . . ? C46 C45 H45A 110.4 . . ? C44 C45 H45A 110.4 . . ? C46 C45 H45B 110.4 . . ? C44 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C10 C9 C8 122.8(12) . . ? C10 C9 H9A 118.6 . . ? C8 C9 H9A 118.6 . . ? 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 O1 Sb1 O7 Sb2 -98.5(3) . . . . ? O2 Sb1 O7 Sb2 -8.6(3) . . . . ? O9 Sb1 O7 Sb2 -174.7(2) . . . . ? O8 Sb2 O7 Sb1 -172.2(3) . . . . ? O3 Sb2 O7 Sb1 -76.8(3) . . . . ? C33 C34 O5 Sb3 102.6(8) . . . . ? C29 C34 O5 Sb3 -81.5(8) . . . . ? O8 Sb3 O5 C34 -10.9(7) . . . . ? O4 Sb3 O5 C34 83.0(7) . . . . ? C12 C13 O2 Sb1 -114.7(7) . . . . ? C8 C13 O2 Sb1 65.7(11) . . . . ? O7 Sb1 O2 C13 163.4(6) . . . . ? O1 Sb1 O2 C13 -102.8(6) . . . . ? O9 Sb1 O2 C13 -133.9(7) . . . . ? O8 Sb2 O3 C20 120.3(6) . . . . ? O7 Sb2 O3 C20 34.1(6) . . . . ? O7 Sb1 O9 C46 40.5(5) . . . . ? O1 Sb1 O9 C46 -54.3(5) . . . . ? O2 Sb1 O9 C46 -22.2(8) . . . . ? O7 Sb1 O9 C43 173.4(5) . . . . ? O1 Sb1 O9 C43 78.6(5) . . . . ? O2 Sb1 O9 C43 110.7(7) . . . . ? O7 Sb1 O1 C1 86.8(7) . . . . ? O2 Sb1 O1 C1 0.0(7) . . . . ? O9 Sb1 O1 C1 171.8(7) . . . . ? O4 Sb3 O8 Sb2 112.6(3) . . . . ? O5 Sb3 O8 Sb2 -154.6(3) . . . . ? O3 Sb2 O8 Sb3 -101.3(3) . . . . ? O7 Sb2 O8 Sb3 -10.8(3) . . . . ? C48 C47 O10 C50 31.1(12) . . . . ? O8 Sb3 O4 C27 3.2(7) . . . . ? O5 Sb3 O4 C27 -87.3(7) . . . . ? Sb3 O4 C27 C26 89.2(7) . . . . ? Sb3 O4 C27 C22 -91.0(9) . . . . ? O4 C27 C22 C23 -173.6(6) . . . . ? C26 C27 C22 C23 6.2(12) . . . . ? O4 C27 C22 C21 1.8(11) . . . . ? C26 C27 C22 C21 -178.4(7) . . . . ? C27 C22 C23 C24 -3.7(12) . . . . ? C21 C22 C23 C24 -178.9(8) . . . . ? C12 C14 C15 C16 54.3(10) . . . . ? C12 C14 C15 C20 -124.3(8) . . . . ? Sb2 O3 C20 C15 83.7(7) . . . . ? Sb2 O3 C20 C19 -99.8(7) . . . . ? C16 C15 C20 O3 174.8(7) . . . . ? C14 C15 C20 O3 -6.5(11) . . . . ? C16 C15 C20 C19 -1.6(11) . . . . ? C14 C15 C20 C19 177.1(7) . . . . ? C18 C19 C20 O3 -175.0(6) . . . . ? C21 C19 C20 O3 9.2(10) . . . . ? C18 C19 C20 C15 1.5(10) . . . . ? C21 C19 C20 C15 -174.3(7) . . . . ? O4 C27 C26 C25 174.1(7) . . . . ? C22 C27 C26 C25 -5.7(12) . . . . ? O4 C27 C26 C28 -4.9(12) . . . . ? C22 C27 C26 C28 175.3(9) . . . . ? C27 C26 C25 C24 2.7(13) . . . . ? C28 C26 C25 C24 -178.2(9) . . . . ? O2 C13 C12 C11 -175.5(8) . . . . ? C8 C13 C12 C11 4.1(14) . . . . ? O2 C13 C12 C14 4.2(12) . . . . ? C8 C13 C12 C14 -176.2(8) . . . . ? C15 C14 C12 C13 66.9(10) . . . . ? C15 C14 C12 C11 -113.4(10) . . . . ? C18 C19 C21 C22 127.5(8) . . . . ? C20 C19 C21 C22 -56.7(10) . . . . ? C23 C22 C21 C19 -37.5(11) . . . . ? C27 C22 C21 C19 147.4(8) . . . . ? O5 C34 C33 C32 175.2(8) . . . . ? C29 C34 C33 C32 -0.6(13) . . . . ? O5 C34 C33 C35 -3.3(13) . . . . ? C29 C34 C33 C35 -179.1(9) . . . . ? C31 C32 C33 C34 2.5(17) . . . . ? C31 C32 C33 C35 -179.0(11) . . . . ? Sb1 O1 C1 C6 64.3(9) . . . . ? Sb1 O1 C1 C2 -119.9(7) . . . . ? C3 C2 C1 O1 -169.0(8) . . . . ? C42 C2 C1 O1 16.7(13) . . . . ? C3 C2 C1 C6 6.7(13) . . . . ? C42 C2 C1 C6 -167.7(9) . . . . ? C26 C25 C24 C23 -0.5(15) . . . . ? C22 C23 C24 C25 1.0(13) . . . . ? C46 O9 C43 C44 27.1(10) . . . . ? Sb1 O9 C43 C44 -115.9(8) . . . . ? C33 C32 C31 C30 -2.7(19) . . . . ? C25 C26 C28 C29 88.3(10) . . . . ? C27 C26 C28 C29 -92.7(10) . . . . ? O1 C1 C6 C5 169.3(7) . . . . ? C2 C1 C6 C5 -6.4(12) . . . . ? O1 C1 C6 C7 -5.4(12) . . . . ? C2 C1 C6 C7 178.9(8) . . . . ? C8 C7 C6 C1 -101.1(10) . . . . ? C8 C7 C6 C5 84.4(11) . . . . ? C20 C19 C18 C17 0.1(13) . . . . ? C21 C19 C18 C17 176.0(9) . . . . ? O2 C13 C8 C9 177.0(10) . . . . ? C12 C13 C8 C9 -2.6(16) . . . . ? O2 C13 C8 C7 -5.6(16) . . . . ? C12 C13 C8 C7 174.8(10) . . . . ? C6 C7 C8 C9 -124.1(12) . . . . ? C6 C7 C8 C13 58.6(15) . . . . ? C50 C49 C48 C47 14.9(14) . . . . ? O10 C47 C48 C49 -28.7(12) . . . . ? C33 C34 C29 C30 -1.1(12) . . . . ? O5 C34 C29 C30 -176.8(7) . . . . ? C33 C34 C29 C28 176.8(9) . . . . ? O5 C34 C29 C28 1.0(12) . . . . ? C26 C28 C29 C30 -88.9(10) . . . . ? C26 C28 C29 C34 93.4(10) . . . . ? C34 C33 C35 C36 -87.6(12) . . . . ? C32 C33 C35 C36 94.0(11) . . . . ? C3 C2 C42 C40 -64.6(14) . . . . ? C1 C2 C42 C40 109.7(11) . . . . ? C47 O10 C50 C49 -20.7(13) . . . . ? C48 C49 C50 O10 2.7(15) . . . . ? C5 C4 C3 C2 -5(3) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C42 C2 C3 C4 173.4(15) . . . . ? C40 C41 C36 C37 4.5(15) . . . . ? O6 C41 C36 C37 -179.1(8) . . . . ? C40 C41 C36 C35 -178.1(10) . . . . ? O6 C41 C36 C35 -1.7(15) . . . . ? C38 C37 C36 C41 -4.5(16) . . . . ? C38 C37 C36 C35 178.1(11) . . . . ? C33 C35 C36 C41 119.5(10) . . . . ? C33 C35 C36 C37 -63.2(13) . . . . ? C32 C31 C30 C29 0.9(19) . . . . ? C34 C29 C30 C31 0.9(15) . . . . ? C28 C29 C30 C31 -176.9(11) . . . . ? C20 C15 C16 C17 0.3(14) . . . . ? C14 C15 C16 C17 -178.5(9) . . . . ? O6 C41 C40 C39 -180.0(7) . . . . ? C36 C41 C40 C39 -3.5(17) . . . . ? O6 C41 C40 C42 3.3(16) . . . . ? C36 C41 C40 C42 179.8(8) . . . . ? C38 C39 C40 C41 2.2(14) . . . . ? C38 C39 C40 C42 179.0(9) . . . . ? C2 C42 C40 C41 -178.1(12) . . . . ? C2 C42 C40 C39 5.2(15) . . . . ? C43 O9 C46 C45 -20.5(10) . . . . ? Sb1 O9 C46 C45 113.9(8) . . . . ? O9 C43 C44 C45 -23.1(13) . . . . ? C36 C37 C38 C39 3.5(18) . . . . ? C40 C39 C38 C37 -2.1(15) . . . . ? C3 C4 C5 C6 5(3) . . . . ? C1 C6 C5 C4 0.9(17) . . . . ? C7 C6 C5 C4 175.8(13) . . . . ? C19 C18 C17 C16 -1.5(17) . . . . ? C15 C16 C17 C18 1.3(17) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C13 C12 C11 C10 -2.1(18) . . . . ? C14 C12 C11 C10 178.2(12) . . . . ? O9 C46 C45 C44 6.2(13) . . . . ? C43 C44 C45 C46 10.6(14) . . . . ? C11 C10 C9 C8 3(3) . . . . ? C13 C8 C9 C10 -1(2) . . . . ? C7 C8 C9 C10 -178.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.098 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.117 # Attachment '6.cif' data_tcu121 _database_code_depnum_ccdc_archive 'CCDC 721519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C154 H188 Bi4 O16,2(C6H14),5.5 (C4 H10 O2)' _chemical_formula_sum 'C188 H271 Bi4 O27' _chemical_formula_weight 3799.07 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.5399(13) _cell_length_b 30.330(2) _cell_length_c 34.753(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.4290(10) _cell_angle_gamma 90.00 _cell_volume 18055(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(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 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7672 _exptl_absorpt_coefficient_mu 3.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_T_max 0.627 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD Detector' _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 154751 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.1073 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 28.33 _reflns_number_total 42061 _reflns_number_gt 30358 _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. 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 923.2 \%A^3^ and contain 109 electrons. The electron density was modelled as 2 DME molecules (0.5 DME molecules per assymetric unit) which accounts for 100 electrons. The DME molecules where added in the formula weight on the structure of assymetric unit. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+254.2055P] 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 42061 _refine_ls_number_parameters 1932 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.010 _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 Bi4 Bi 1.08976(2) 0.671596(11) 0.211859(10) 0.013 Uani 1 1 d . . . O1 O 0.9133(4) 0.5431(2) 0.23618(19) 0.015 Uani 1 1 d . . . C1 C 0.8648(5) 0.5072(3) 0.2285(3) 0.012 Uani 1 1 d . . . Bi2 Bi 0.88994(2) 0.680864(11) 0.211865(10) 0.013 Uani 1 1 d . . . O2 O 0.8504(4) 0.6194(2) 0.17694(19) 0.015 Uani 1 1 d . . . C2 C 0.8955(5) 0.4647(3) 0.2376(3) 0.018 Uani 1 1 d . . . Bi1 Bi 0.96602(2) 0.572486(11) 0.190581(10) 0.01257(7) Uani 1 1 d . . . O3 O 0.8860(4) 0.7152(2) 0.15542(18) 0.0147(14) Uani 1 1 d . . . C3 C 0.8456(6) 0.4283(3) 0.2301(3) 0.018(2) Uani 1 1 d . . . H3A H 0.8669 0.3997 0.2361 0.022 Uiso 1 1 calc R . . Bi3 Bi 0.98933(2) 0.776841(11) 0.180854(10) 0.01310(8) Uani 1 1 d . . . O4 O 0.9135(4) 0.7991(2) 0.21822(19) 0.0159(14) Uani 1 1 d . . . C4 C 0.7660(6) 0.4323(3) 0.2142(3) 0.019(2) Uani 1 1 d . . . O5 O 0.8912(4) 0.6699(2) 0.2968(2) 0.0225(16) Uani 1 1 d . . . H5A H 0.9077 0.6449 0.3051 0.034 Uiso 1 1 calc R . . C5 C 0.7374(6) 0.4744(3) 0.2071(3) 0.020(2) Uani 1 1 d . . . H5B H 0.6827 0.4782 0.1981 0.023 Uiso 1 1 calc R . . O6 O 0.9396(4) 0.5963(2) 0.3386(2) 0.0232(16) Uani 1 1 d . . . H6A H 0.9598 0.5761 0.3275 0.035 Uiso 1 1 calc R . . C6 C 0.7844(5) 0.5117(3) 0.2124(3) 0.016(2) Uani 1 1 d . . . O7 O 1.0002(4) 0.5313(2) 0.30662(19) 0.0192(15) Uani 1 1 d . . . H7A H 0.9793 0.5486 0.3202 0.029 Uiso 1 1 calc R . . C7 C 0.7129(5) 0.3919(3) 0.2083(3) 0.017(2) Uani 1 1 d . . . O8 O 1.0449(4) 0.6322(2) 0.15905(19) 0.0176(14) Uani 1 1 d . . . C8 C 0.6716(7) 0.3877(4) 0.2417(4) 0.033(3) Uani 1 1 d . . . H8A H 0.7101 0.3840 0.2665 0.049 Uiso 1 1 calc R . . H8B H 0.6370 0.3620 0.2373 0.049 Uiso 1 1 calc R . . H8C H 0.6407 0.4144 0.2431 0.049 Uiso 1 1 calc R . . O9 O 1.0980(4) 0.7296(2) 0.1717(2) 0.0172(14) Uani 1 1 d . . . C9 C 0.7583(6) 0.3492(3) 0.2047(3) 0.026(2) Uani 1 1 d . . . H9A H 0.7982 0.3447 0.2289 0.039 Uiso 1 1 calc R . . H9B H 0.7834 0.3515 0.1822 0.039 Uiso 1 1 calc R . . H9C H 0.7221 0.3241 0.2008 0.039 Uiso 1 1 calc R . . O10 O 1.0778(4) 0.8124(2) 0.22395(19) 0.0145(14) Uani 1 1 d . . . C10 C 0.6506(6) 0.3975(4) 0.1698(4) 0.030(3) Uani 1 1 d . . . H10A H 0.6203 0.4244 0.1714 0.045 Uiso 1 1 calc R . . H10B H 0.6155 0.3720 0.1661 0.045 Uiso 1 1 calc R . . H10C H 0.6762 0.3997 0.1475 0.045 Uiso 1 1 calc R . . O11 O 1.0521(4) 0.8262(2) 0.2941(2) 0.0200(15) Uani 1 1 d . . . H11A H 1.0815 0.8095 0.3100 0.030 Uiso 1 1 calc R . . C11 C 0.7494(5) 0.5563(3) 0.1990(3) 0.017(2) Uani 1 1 d . . . H11B H 0.6947 0.5572 0.2022 0.021 Uiso 1 1 calc R . . H11C H 0.7788 0.5796 0.2160 0.021 Uiso 1 1 calc R . . O12 O 1.1365(4) 0.7633(2) 0.3355(2) 0.0220(16) Uani 1 1 d . . . H12A H 1.1076 0.7817 0.3213 0.033 Uiso 1 1 calc R . . C12 C 0.7512(6) 0.5657(3) 0.1567(3) 0.018(2) Uani 1 1 d . . . C13 C 0.7058(6) 0.5408(3) 0.1258(3) 0.018(2) Uani 1 1 d . . . H13A H 0.6710 0.5192 0.1320 0.022 Uiso 1 1 calc R . . O13 O 1.1609(4) 0.6896(2) 0.2971(2) 0.0224(16) Uani 1 1 d . . . H13B H 1.1473 0.7149 0.3028 0.034 Uiso 1 1 calc R . . C14 C 0.7100(6) 0.5467(3) 0.0866(3) 0.021(2) Uani 1 1 d . . . O14 O 1.0736(4) 0.5535(2) 0.22962(19) 0.0156(14) Uani 1 1 d . . . C15 C 0.7615(6) 0.5790(3) 0.0785(3) 0.018(2) Uani 1 1 d . . . H15A H 0.7656 0.5835 0.0520 0.022 Uiso 1 1 calc R . . O15 O 0.9873(4) 0.6346(2) 0.22228(18) 0.0136(13) Uani 1 1 d . . . C16 C 0.8069(5) 0.6046(3) 0.1078(3) 0.017(2) Uani 1 1 d . . . O16 O 1.0002(4) 0.7188(2) 0.21838(18) 0.0137(13) Uani 1 1 d . . . C17 C 0.8004(5) 0.5974(3) 0.1478(3) 0.016(2) Uani 1 1 d . . . O17 O 0.9517(4) 0.8625(2) 0.1513(2) 0.0218(16) Uani 1 1 d . . . C18 C 0.6553(6) 0.5214(4) 0.0535(3) 0.024(2) Uani 1 1 d . . . O18 O 0.9215(5) 0.8060(2) 0.0862(2) 0.0277(17) Uani 1 1 d . . . C19 C 0.6505(8) 0.4729(4) 0.0651(4) 0.049(4) Uani 1 1 d . . . H19A H 0.6331 0.4710 0.0900 0.074 Uiso 1 1 calc R . . H19B H 0.7020 0.4593 0.0682 0.074 Uiso 1 1 calc R . . H19C H 0.6131 0.4575 0.0445 0.074 Uiso 1 1 calc R . . O19 O 0.9496(4) 0.5297(2) 0.1003(2) 0.0266(17) Uani 1 1 d . . . C20 C 0.6824(7) 0.5236(4) 0.0147(3) 0.036(3) Uani 1 1 d . . . H20A H 0.6856 0.5545 0.0069 0.055 Uiso 1 1 calc R . . H20B H 0.6452 0.5078 -0.0057 0.055 Uiso 1 1 calc R . . H20C H 0.7340 0.5099 0.0181 0.055 Uiso 1 1 calc R . . O20 O 0.9770(4) 0.4824(2) 0.17006(19) 0.0163(14) Uani 1 1 d . . . C21 C 0.5740(7) 0.5420(4) 0.0472(4) 0.040(3) Uani 1 1 d . . . H21A H 0.5766 0.5730 0.0396 0.060 Uiso 1 1 calc R . . H21B H 0.5550 0.5402 0.0717 0.060 Uiso 1 1 calc R . . H21C H 0.5382 0.5260 0.0263 0.060 Uiso 1 1 calc R . . O21 O 0.7621(6) 0.9604(4) 0.1647(4) 0.069(3) Uani 1 1 d . . . C22 C 0.8576(5) 0.6414(3) 0.0986(3) 0.016(2) Uani 1 1 d . . . H22A H 0.8744 0.6350 0.0738 0.020 Uiso 1 1 calc R . . H22B H 0.9049 0.6441 0.1200 0.020 Uiso 1 1 calc R . . O22 O 0.8836(12) 1.0203(8) 0.1848(10) 0.235(14) Uani 1 1 d . . . C23 C 0.8122(6) 0.6844(3) 0.0946(3) 0.0147(19) Uani 1 1 d . . . O23 O 0.5871(6) 0.8446(3) -0.0658(3) 0.049(2) Uani 1 1 d . . . C24 C 0.7501(6) 0.6883(3) 0.0624(3) 0.022(2) Uani 1 1 d . . . H24A H 0.7425 0.6656 0.0430 0.027 Uiso 1 1 calc R . . O24 O 0.6112(6) 0.8598(3) 0.0171(3) 0.055(3) Uani 1 1 d . . . C25 C 0.6992(6) 0.7234(4) 0.0572(3) 0.027(2) Uani 1 1 d . . . O25 O 1.3190(5) 0.8931(3) 0.3307(2) 0.0332(19) Uani 1 1 d . . . C26 C 0.7130(6) 0.7561(3) 0.0857(3) 0.019(2) Uani 1 1 d . . . H26A H 0.6790 0.7809 0.0827 0.023 Uiso 1 1 calc R . . O26 O 1.3948(5) 0.8504(3) 0.2750(3) 0.045(2) Uani 1 1 d . . . C27 C 0.7745(6) 0.7542(3) 0.1186(3) 0.017(2) Uani 1 1 d . . . C28 C 0.8245(5) 0.7169(3) 0.1236(3) 0.0130(19) Uani 1 1 d . . . C29 C 0.6307(7) 0.7256(4) 0.0207(3) 0.039(3) Uani 1 1 d . . . C30 C 0.5615(7) 0.7508(4) 0.0306(4) 0.039(3) Uani 1 1 d . . . H30A H 0.5189 0.7521 0.0071 0.059 Uiso 1 1 calc R . . H30B H 0.5779 0.7808 0.0390 0.059 Uiso 1 1 calc R . . H30C H 0.5434 0.7356 0.0519 0.059 Uiso 1 1 calc R . . C31 C 0.6577(8) 0.7488(5) -0.0122(3) 0.056(4) Uani 1 1 d . . . H31A H 0.6145 0.7504 -0.0353 0.083 Uiso 1 1 calc R . . H31B H 0.7012 0.7324 -0.0189 0.083 Uiso 1 1 calc R . . H31C H 0.6750 0.7787 -0.0038 0.083 Uiso 1 1 calc R . . C32 C 0.6032(9) 0.6788(5) 0.0076(6) 0.083(7) Uani 1 1 d . . . H32A H 0.5599 0.6806 -0.0156 0.124 Uiso 1 1 calc R . . H32B H 0.5855 0.6638 0.0290 0.124 Uiso 1 1 calc R . . H32C H 0.6465 0.6623 0.0008 0.124 Uiso 1 1 calc R . . C33 C 0.7862(5) 0.7908(3) 0.1481(3) 0.0146(19) Uani 1 1 d . . . H33A H 0.7458 0.8136 0.1395 0.018 Uiso 1 1 calc R . . H33B H 0.8378 0.8045 0.1492 0.018 Uiso 1 1 calc R . . C34 C 0.7817(6) 0.7748(3) 0.1882(3) 0.019(2) Uani 1 1 d . . . C35 C 0.7114(6) 0.7569(3) 0.1944(3) 0.018(2) Uani 1 1 d . . . H35A H 0.6675 0.7556 0.1729 0.022 Uiso 1 1 calc R . . C36 C 0.7042(6) 0.7408(3) 0.2311(3) 0.017(2) Uani 1 1 d . . . C37 C 0.7696(6) 0.7431(3) 0.2623(3) 0.0146(19) Uani 1 1 d . . . H37A H 0.7654 0.7322 0.2874 0.018 Uiso 1 1 calc R . . C38 C 0.8401(6) 0.7607(3) 0.2580(3) 0.017(2) Uani 1 1 d . . . C39 C 0.8460(5) 0.7775(3) 0.2207(3) 0.0136(19) Uani 1 1 d . . . C40 C 0.6283(6) 0.7204(4) 0.2384(3) 0.025(2) Uani 1 1 d . . . C41 C 0.5578(6) 0.7307(4) 0.2056(4) 0.042(3) Uani 1 1 d . . . H41A H 0.5513 0.7628 0.2030 0.063 Uiso 1 1 calc R . . H41B H 0.5109 0.7177 0.2120 0.063 Uiso 1 1 calc R . . H41C H 0.5660 0.7184 0.1808 0.063 Uiso 1 1 calc R . . C42 C 0.6405(7) 0.6707(4) 0.2433(5) 0.052(4) Uani 1 1 d . . . H42A H 0.6858 0.6650 0.2648 0.079 Uiso 1 1 calc R . . H42B H 0.6498 0.6582 0.2188 0.079 Uiso 1 1 calc R . . H42C H 0.5939 0.6572 0.2496 0.079 Uiso 1 1 calc R . . C43 C 0.6111(7) 0.7389(5) 0.2765(4) 0.049(4) Uani 1 1 d . . . H43A H 0.6554 0.7330 0.2984 0.074 Uiso 1 1 calc R . . H43B H 0.5641 0.7248 0.2818 0.074 Uiso 1 1 calc R . . H43C H 0.6025 0.7708 0.2737 0.074 Uiso 1 1 calc R . . C44 C 0.9104(5) 0.7608(3) 0.2920(3) 0.0137(19) Uani 1 1 d . . . H44A H 0.9279 0.7915 0.2981 0.016 Uiso 1 1 calc R . . H44B H 0.9536 0.7444 0.2843 0.016 Uiso 1 1 calc R . . C45 C 0.8921(5) 0.7398(3) 0.3287(3) 0.016(2) Uani 1 1 d . . . C46 C 0.8769(6) 0.7648(3) 0.3592(3) 0.020(2) Uani 1 1 d . . . H46A H 0.8892 0.7953 0.3601 0.024 Uiso 1 1 calc R . . C47 C 0.8443(6) 0.7470(3) 0.3890(3) 0.020(2) Uani 1 1 d . . . C48 C 0.8218(6) 0.7027(3) 0.3848(3) 0.021(2) Uani 1 1 d . . . H48A H 0.7962 0.6900 0.4036 0.025 Uiso 1 1 calc R . . C49 C 0.8354(6) 0.6771(3) 0.3547(3) 0.024(2) Uani 1 1 d . . . C50 C 0.8742(6) 0.6946(3) 0.3278(3) 0.020(2) Uani 1 1 d . . . C51 C 0.8301(7) 0.7766(3) 0.4224(3) 0.026(2) Uani 1 1 d . . . C52 C 0.7662(8) 0.8101(4) 0.4064(4) 0.044(3) Uani 1 1 d . . . H52A H 0.7813 0.8275 0.3855 0.066 Uiso 1 1 calc R . . H52B H 0.7591 0.8298 0.4277 0.066 Uiso 1 1 calc R . . H52C H 0.7172 0.7946 0.3958 0.066 Uiso 1 1 calc R . . C53 C 0.9041(7) 0.8019(5) 0.4401(4) 0.042(3) Uani 1 1 d . . . H53A H 0.9199 0.8196 0.4196 0.063 Uiso 1 1 calc R . . H53B H 0.9458 0.7810 0.4511 0.063 Uiso 1 1 calc R . . H53C H 0.8944 0.8213 0.4610 0.063 Uiso 1 1 calc R . . C54 C 0.8067(10) 0.7496(4) 0.4558(4) 0.054(4) Uani 1 1 d . . . H54A H 0.8478 0.7282 0.4662 0.081 Uiso 1 1 calc R . . H54B H 0.7576 0.7340 0.4454 0.081 Uiso 1 1 calc R . . H54C H 0.7997 0.7695 0.4770 0.081 Uiso 1 1 calc R . . C55 C 0.7992(6) 0.6306(3) 0.3497(3) 0.022(2) Uani 1 1 d . . . H55A H 0.7455 0.6321 0.3543 0.026 Uiso 1 1 calc R . . H55B H 0.7955 0.6209 0.3221 0.026 Uiso 1 1 calc R . . C56 C 0.8443(6) 0.5969(3) 0.3767(3) 0.019(2) Uani 1 1 d . . . C57 C 0.8160(6) 0.5819(3) 0.4087(3) 0.019(2) Uani 1 1 d . . . H57A H 0.7682 0.5936 0.4130 0.023 Uiso 1 1 calc R . . C58 C 0.8550(6) 0.5508(3) 0.4345(3) 0.024(2) Uani 1 1 d . . . C59 C 0.9252(7) 0.5339(3) 0.4272(3) 0.025(2) Uani 1 1 d . . . H59A H 0.9527 0.5121 0.4443 0.030 Uiso 1 1 calc R . . C60 C 0.9556(6) 0.5482(3) 0.3956(3) 0.018(2) Uani 1 1 d . . . C61 C 0.9148(6) 0.5794(3) 0.3699(3) 0.023(2) Uani 1 1 d . . . C62 C 0.8220(7) 0.5349(4) 0.4698(3) 0.034(3) Uani 1 1 d . . . C63 C 0.7979(10) 0.5749(5) 0.4914(4) 0.059(4) Uani 1 1 d . . . H63A H 0.7771 0.5648 0.5139 0.089 Uiso 1 1 calc R . . H63B H 0.7577 0.5917 0.4733 0.089 Uiso 1 1 calc R . . H63C H 0.8434 0.5937 0.5008 0.089 Uiso 1 1 calc R . . C64 C 0.8792(8) 0.5083(5) 0.4989(4) 0.048(4) Uani 1 1 d . . . H64A H 0.8953 0.4825 0.4857 0.071 Uiso 1 1 calc R . . H64B H 0.8548 0.4987 0.5203 0.071 Uiso 1 1 calc R . . H64C H 0.9251 0.5265 0.5097 0.071 Uiso 1 1 calc R . . C65 C 0.7501(8) 0.5068(5) 0.4530(5) 0.063(5) Uani 1 1 d . . . H65A H 0.7657 0.4811 0.4393 0.095 Uiso 1 1 calc R . . H65B H 0.7122 0.5244 0.4343 0.095 Uiso 1 1 calc R . . H65C H 0.7262 0.4967 0.4745 0.095 Uiso 1 1 calc R . . C66 C 1.0319(6) 0.5293(3) 0.3892(3) 0.020(2) Uani 1 1 d . . . H66A H 1.0661 0.5227 0.4152 0.024 Uiso 1 1 calc R . . H66B H 1.0585 0.5518 0.3762 0.024 Uiso 1 1 calc R . . C67 C 1.0211(6) 0.4874(3) 0.3642(3) 0.015(2) Uani 1 1 d . . . C68 C 1.0279(6) 0.4459(3) 0.3813(3) 0.021(2) Uani 1 1 d . . . H68A H 1.0392 0.4439 0.4093 0.025 Uiso 1 1 calc R . . C69 C 1.0190(5) 0.4072(3) 0.3597(3) 0.017(2) Uani 1 1 d . . . C70 C 1.0030(6) 0.4119(3) 0.3185(3) 0.019(2) Uani 1 1 d . . . H70A H 0.9948 0.3860 0.3028 0.022 Uiso 1 1 calc R . . C71 C 0.9982(5) 0.4541(3) 0.2986(3) 0.019(2) Uani 1 1 d . . . C72 C 1.0055(6) 0.4903(3) 0.3230(3) 0.018(2) Uani 1 1 d . . . C73 C 1.0247(7) 0.3609(3) 0.3775(3) 0.026(2) Uani 1 1 d . . . C74 C 1.0468(8) 0.3617(4) 0.4221(3) 0.035(3) Uani 1 1 d . . . H74A H 1.0074 0.3784 0.4322 0.053 Uiso 1 1 calc R . . H74B H 1.0978 0.3759 0.4306 0.053 Uiso 1 1 calc R . . H74C H 1.0493 0.3315 0.4322 0.053 Uiso 1 1 calc R . . C75 C 1.0876(7) 0.3344(4) 0.3625(3) 0.031(3) Uani 1 1 d . . . H75A H 1.1379 0.3495 0.3702 0.046 Uiso 1 1 calc R . . H75B H 1.0729 0.3319 0.3338 0.046 Uiso 1 1 calc R . . H75C H 1.0918 0.3048 0.3742 0.046 Uiso 1 1 calc R . . C76 C 0.9453(7) 0.3375(4) 0.3655(3) 0.032(3) Uani 1 1 d . . . H76A H 0.9057 0.3546 0.3750 0.048 Uiso 1 1 calc R . . H76B H 0.9491 0.3079 0.3771 0.048 Uiso 1 1 calc R . . H76C H 0.9306 0.3352 0.3367 0.048 Uiso 1 1 calc R . . C77 C 0.9804(6) 0.4561(3) 0.2559(3) 0.019(2) Uani 1 1 d . . . H77A H 0.9959 0.4278 0.2456 0.023 Uiso 1 1 calc R . . H77B H 1.0123 0.4797 0.2476 0.023 Uiso 1 1 calc R . . C78 C 1.0789(6) 0.6258(3) 0.1272(3) 0.0151(19) Uani 1 1 d . . . C79 C 1.1254(6) 0.5879(3) 0.1257(3) 0.017(2) Uani 1 1 d . . . C80 C 1.1558(5) 0.5801(3) 0.0928(3) 0.018(2) Uani 1 1 d . . . H80A H 1.1865 0.5544 0.0922 0.022 Uiso 1 1 calc R . . C81 C 1.1431(6) 0.6088(4) 0.0605(3) 0.021(2) Uani 1 1 d . . . C82 C 1.0975(6) 0.6463(3) 0.0628(3) 0.019(2) Uani 1 1 d . . . H82A H 1.0873 0.6661 0.0411 0.023 Uiso 1 1 calc R . . C83 C 1.0665(5) 0.6558(3) 0.0954(3) 0.016(2) Uani 1 1 d . . . C84 C 1.1766(7) 0.5984(4) 0.0245(3) 0.028(2) Uani 1 1 d . . . C85 C 1.2650(7) 0.5906(4) 0.0374(4) 0.040(3) Uani 1 1 d . . . H85A H 1.2750 0.5674 0.0574 0.060 Uiso 1 1 calc R . . H85B H 1.2906 0.6179 0.0485 0.060 Uiso 1 1 calc R . . H85C H 1.2858 0.5817 0.0146 0.060 Uiso 1 1 calc R . . C86 C 1.1385(8) 0.5565(4) 0.0049(4) 0.044(3) Uani 1 1 d . . . H86A H 1.0820 0.5610 -0.0036 0.066 Uiso 1 1 calc R . . H86B H 1.1487 0.5320 0.0237 0.066 Uiso 1 1 calc R . . H86C H 1.1603 0.5495 -0.0181 0.066 Uiso 1 1 calc R . . C87 C 1.1623(9) 0.6348(4) -0.0066(4) 0.047(4) Uani 1 1 d . . . H87A H 1.1060 0.6402 -0.0151 0.071 Uiso 1 1 calc R . . H87B H 1.1833 0.6258 -0.0293 0.071 Uiso 1 1 calc R . . H87C H 1.1883 0.6620 0.0047 0.071 Uiso 1 1 calc R . . C88 C 1.0228(6) 0.6987(3) 0.0961(3) 0.0147(19) Uani 1 1 d . . . H88A H 0.9841 0.7023 0.0710 0.018 Uiso 1 1 calc R . . H88B H 0.9944 0.6981 0.1178 0.018 Uiso 1 1 calc R . . C89 C 1.0785(5) 0.7368(3) 0.1018(3) 0.0142(19) Uani 1 1 d . . . C90 C 1.0938(6) 0.7605(3) 0.0698(3) 0.021(2) Uani 1 1 d . . . H90A H 1.0672 0.7523 0.0440 0.025 Uiso 1 1 calc R . . C91 C 1.1457(6) 0.7952(3) 0.0739(3) 0.022(2) Uani 1 1 d . . . C92 C 1.1836(6) 0.8063(3) 0.1126(3) 0.020(2) Uani 1 1 d . . . H92A H 1.2197 0.8300 0.1161 0.024 Uiso 1 1 calc R . . C93 C 1.1714(6) 0.7844(3) 0.1461(3) 0.018(2) Uani 1 1 d . . . C94 C 1.1175(5) 0.7488(3) 0.1392(3) 0.0148(19) Uani 1 1 d . . . C95 C 1.1621(7) 0.8206(4) 0.0385(3) 0.029(3) Uani 1 1 d . . . C96 C 1.1094(9) 0.8063(5) -0.0007(4) 0.060(5) Uani 1 1 d . . . H96A H 1.1165 0.7747 -0.0047 0.090 Uiso 1 1 calc R . . H96B H 1.1234 0.8230 -0.0223 0.090 Uiso 1 1 calc R . . H96C H 1.0548 0.8121 0.0000 0.090 Uiso 1 1 calc R . . C97 C 1.1504(9) 0.8705(4) 0.0445(4) 0.047(4) Uani 1 1 d . . . H97A H 1.1601 0.8868 0.0217 0.071 Uiso 1 1 calc R . . H97B H 1.1869 0.8805 0.0684 0.071 Uiso 1 1 calc R . . H97C H 1.0967 0.8759 0.0473 0.071 Uiso 1 1 calc R . . C98 C 1.2467(7) 0.8132(4) 0.0358(3) 0.033(3) Uani 1 1 d . . . H98A H 1.2553 0.7817 0.0320 0.050 Uiso 1 1 calc R . . H98B H 1.2814 0.8232 0.0602 0.050 Uiso 1 1 calc R . . H98C H 1.2576 0.8299 0.0134 0.050 Uiso 1 1 calc R . . C99 C 1.2099(6) 0.7991(3) 0.1866(3) 0.017(2) Uani 1 1 d . . . H99A H 1.2670 0.8002 0.1888 0.020 Uiso 1 1 calc R . . H99B H 1.1993 0.7772 0.2060 0.020 Uiso 1 1 calc R . . C100 C 1.1815(5) 0.8441(3) 0.1967(3) 0.0145(19) Uani 1 1 d . . . C101 C 1.2212(5) 0.8812(3) 0.1882(3) 0.0129(19) Uiso 1 1 d . . . H10D H 1.2669 0.8778 0.1779 0.015 Uiso 1 1 calc R . . C102 C 1.1945(6) 0.9243(3) 0.1948(3) 0.016(2) Uani 1 1 d . . . C103 C 1.1295(5) 0.9269(3) 0.2115(3) 0.019(2) Uani 1 1 d . . . H10E H 1.1117 0.9555 0.2166 0.023 Uiso 1 1 calc R . . C104 C 1.0891(5) 0.8913(3) 0.2213(3) 0.0135(19) Uani 1 1 d . . . C105 C 1.1158(5) 0.8492(3) 0.2133(3) 0.0136(19) Uani 1 1 d . . . C106 C 1.2423(6) 0.9646(3) 0.1866(3) 0.021(2) Uani 1 1 d . . . C107 C 1.2713(7) 0.9591(4) 0.1489(3) 0.033(3) Uani 1 1 d . . . H10F H 1.3014 0.9852 0.1447 0.049 Uiso 1 1 calc R . . H10G H 1.2266 0.9556 0.1267 0.049 Uiso 1 1 calc R . . H10H H 1.3046 0.9329 0.1510 0.049 Uiso 1 1 calc R . . C108 C 1.1934(6) 1.0066(3) 0.1837(3) 0.027(2) Uani 1 1 d . . . H10I H 1.2247 1.0318 0.1784 0.040 Uiso 1 1 calc R . . H10J H 1.1770 1.0114 0.2086 0.040 Uiso 1 1 calc R . . H10K H 1.1472 1.0037 0.1623 0.040 Uiso 1 1 calc R . . C109 C 1.3108(6) 0.9704(3) 0.2203(3) 0.020(2) Uani 1 1 d . . . H10L H 1.3416 0.9959 0.2152 0.030 Uiso 1 1 calc R . . H10M H 1.3434 0.9439 0.2231 0.030 Uiso 1 1 calc R . . H10N H 1.2923 0.9754 0.2446 0.030 Uiso 1 1 calc R . . C110 C 1.0196(5) 0.8983(3) 0.2395(3) 0.0144(19) Uani 1 1 d . . . H11D H 0.9847 0.8724 0.2336 0.017 Uiso 1 1 calc R . . H11E H 0.9903 0.9244 0.2272 0.017 Uiso 1 1 calc R . . C111 C 1.0412(5) 0.9050(3) 0.2840(3) 0.0128(19) Uani 1 1 d . . . C112 C 1.0459(5) 0.9467(3) 0.3006(3) 0.016(2) Uani 1 1 d . . . H11F H 1.0383 0.9718 0.2839 0.019 Uiso 1 1 calc R . . C113 C 1.0618(6) 0.9526(3) 0.3421(3) 0.023(2) Uani 1 1 d . . . C114 C 1.0683(6) 0.9164(3) 0.3644(3) 0.021(2) Uani 1 1 d . . . H11G H 1.0758 0.9200 0.3921 0.025 Uiso 1 1 calc R . . C115 C 1.0648(6) 0.8740(3) 0.3495(3) 0.020(2) Uani 1 1 d . . . C116 C 1.0553(6) 0.8687(3) 0.3097(3) 0.020(2) Uani 1 1 d . . . C117 C 1.0689(6) 1.0003(3) 0.3572(3) 0.027(2) Uani 1 1 d . . . C118 C 1.1398(7) 1.0230(4) 0.3460(4) 0.033(3) Uani 1 1 d . . . H11H H 1.1333 1.0230 0.3173 0.049 Uiso 1 1 calc R . . H11I H 1.1876 1.0069 0.3579 0.049 Uiso 1 1 calc R . . H11J H 1.1436 1.0534 0.3557 0.049 Uiso 1 1 calc R . . C119 C 0.9947(7) 1.0269(4) 0.3398(4) 0.035(3) Uani 1 1 d . . . H11K H 0.9854 1.0264 0.3110 0.053 Uiso 1 1 calc R . . H11L H 1.0015 1.0575 0.3491 0.053 Uiso 1 1 calc R . . H11M H 0.9499 1.0138 0.3483 0.053 Uiso 1 1 calc R . . C120 C 1.0825(7) 1.0016(4) 0.4026(3) 0.034(3) Uani 1 1 d . . . H12B H 1.1296 0.9848 0.4141 0.050 Uiso 1 1 calc R . . H12C H 1.0375 0.9887 0.4109 0.050 Uiso 1 1 calc R . . H12D H 1.0891 1.0323 0.4116 0.050 Uiso 1 1 calc R . . C121 C 1.0778(6) 0.8343(3) 0.3771(3) 0.020(2) Uani 1 1 d . . . H12E H 1.0629 0.8422 0.4022 0.024 Uiso 1 1 calc R . . H12F H 1.0438 0.8098 0.3650 0.024 Uiso 1 1 calc R . . C122 C 1.1616(6) 0.8194(3) 0.3857(3) 0.018(2) Uani 1 1 d . . . C123 C 1.2165(6) 0.8407(3) 0.4144(3) 0.022(2) Uani 1 1 d . . . H12G H 1.1995 0.8639 0.4290 0.027 Uiso 1 1 calc R . . C124 C 1.2957(6) 0.8295(3) 0.4229(3) 0.018(2) Uani 1 1 d . . . C125 C 1.3167(6) 0.7940(3) 0.4015(3) 0.020(2) Uani 1 1 d . . . H12H H 1.3697 0.7848 0.4070 0.024 Uiso 1 1 calc R . . C126 C 1.2647(6) 0.7720(3) 0.3733(3) 0.022(2) Uani 1 1 d . . . C127 C 1.1873(6) 0.7851(3) 0.3650(3) 0.019(2) Uani 1 1 d . . . C128 C 1.3572(7) 0.8543(4) 0.4533(3) 0.029(3) Uani 1 1 d . . . C129 C 1.3938(8) 0.8236(4) 0.4868(4) 0.044(3) Uani 1 1 d . . . H12I H 1.4326 0.8398 0.5061 0.066 Uiso 1 1 calc R . . H12J H 1.4193 0.7990 0.4763 0.066 Uiso 1 1 calc R . . H12K H 1.3531 0.8122 0.4995 0.066 Uiso 1 1 calc R . . C130 C 1.3211(8) 0.8931(4) 0.4714(4) 0.044(3) Uani 1 1 d . . . H13C H 1.2974 0.9137 0.4505 0.066 Uiso 1 1 calc R . . H13D H 1.3619 0.9083 0.4905 0.066 Uiso 1 1 calc R . . H13E H 1.2810 0.8821 0.4847 0.066 Uiso 1 1 calc R . . C131 C 1.4214(7) 0.8717(4) 0.4335(4) 0.036(3) Uani 1 1 d . . . H13F H 1.3984 0.8917 0.4120 0.054 Uiso 1 1 calc R . . H13G H 1.4463 0.8469 0.4229 0.054 Uiso 1 1 calc R . . H13H H 1.4606 0.8876 0.4529 0.054 Uiso 1 1 calc R . . C132 C 1.2908(6) 0.7346(3) 0.3499(3) 0.019(2) Uani 1 1 d . . . H13I H 1.3485 0.7334 0.3560 0.023 Uiso 1 1 calc R . . H13J H 1.2733 0.7411 0.3214 0.023 Uiso 1 1 calc R . . C133 C 1.2593(6) 0.6896(3) 0.3583(3) 0.022(2) Uani 1 1 d . . . C134 C 1.2927(6) 0.6670(3) 0.3920(3) 0.023(2) Uani 1 1 d . . . H13K H 1.3312 0.6816 0.4112 0.028 Uiso 1 1 calc R . . C135 C 1.2733(6) 0.6242(3) 0.3995(3) 0.021(2) Uani 1 1 d . A . C136 C 1.2218(6) 0.6032(3) 0.3694(3) 0.018(2) Uani 1 1 d . . . H13L H 1.2111 0.5729 0.3728 0.022 Uiso 1 1 calc R . . C137 C 1.1844(5) 0.6235(3) 0.3344(3) 0.017(2) Uani 1 1 d . . . C138 C 1.2007(6) 0.6689(3) 0.3306(3) 0.019(2) Uani 1 1 d . . . C139 C 1.3104(6) 0.6013(3) 0.4383(3) 0.033(3) Uani 1 1 d D . . C140 C 1.3501(19) 0.5587(9) 0.4276(12) 0.071(14) Uiso 0.378(17) 1 d PD A 1 H14A H 1.3671 0.5630 0.4028 0.106 Uiso 0.378(17) 1 calc PR A 1 H14B H 1.3129 0.5342 0.4247 0.106 Uiso 0.378(17) 1 calc PR A 1 H14C H 1.3955 0.5518 0.4487 0.106 Uiso 0.378(17) 1 calc PR A 1 C141 C 1.2460(18) 0.5873(13) 0.4589(12) 0.087(17) Uiso 0.378(17) 1 d PD A 1 H14Q H 1.2525 0.6026 0.4842 0.131 Uiso 0.378(17) 1 calc PR A 1 H14R H 1.2491 0.5554 0.4634 0.131 Uiso 0.378(17) 1 calc PR A 1 H14S H 1.1951 0.5947 0.4423 0.131 Uiso 0.378(17) 1 calc PR A 1 C142 C 1.3726(16) 0.6269(10) 0.4674(9) 0.053(11) Uiso 0.378(17) 1 d PD A 1 H14T H 1.4237 0.6225 0.4608 0.080 Uiso 0.378(17) 1 calc PR A 1 H14U H 1.3744 0.6161 0.4942 0.080 Uiso 0.378(17) 1 calc PR A 1 H14V H 1.3596 0.6583 0.4660 0.080 Uiso 0.378(17) 1 calc PR A 1 C14A C 1.2776(11) 0.5552(5) 0.4414(6) 0.042(6) Uiso 0.622(17) 1 d PD A 2 H14D H 1.2906 0.5363 0.4208 0.063 Uiso 0.622(17) 1 calc PR A 2 H14E H 1.2208 0.5569 0.4381 0.063 Uiso 0.622(17) 1 calc PR A 2 H14F H 1.3005 0.5428 0.4674 0.063 Uiso 0.622(17) 1 calc PR A 2 C14B C 1.2913(11) 0.6289(6) 0.4726(5) 0.039(5) Uiso 0.622(17) 1 d PD A 2 H14N H 1.2346 0.6312 0.4695 0.058 Uiso 0.622(17) 1 calc PR A 2 H14O H 1.3137 0.6585 0.4724 0.058 Uiso 0.622(17) 1 calc PR A 2 H14P H 1.3137 0.6145 0.4978 0.058 Uiso 0.622(17) 1 calc PR A 2 C14C C 1.3983(9) 0.5991(6) 0.4437(6) 0.045(6) Uiso 0.622(17) 1 d PD A 2 H14G H 1.4117 0.5832 0.4216 0.067 Uiso 0.622(17) 1 calc PR A 2 H14H H 1.4205 0.5837 0.4684 0.067 Uiso 0.622(17) 1 calc PR A 2 H14I H 1.4196 0.6291 0.4448 0.067 Uiso 0.622(17) 1 calc PR A 2 C143 C 1.1389(5) 0.5987(3) 0.3013(3) 0.017(2) Uani 1 1 d . . . H14J H 1.0870 0.6127 0.2929 0.021 Uiso 1 1 calc R . . H14K H 1.1309 0.5684 0.3101 0.021 Uiso 1 1 calc R . . C144 C 1.1787(5) 0.5967(3) 0.2658(3) 0.0128(19) Uani 1 1 d . . . C145 C 1.2508(6) 0.6165(3) 0.2678(3) 0.017(2) Uani 1 1 d . . . H14L H 1.2772 0.6290 0.2921 0.020 Uiso 1 1 calc R . . C146 C 1.2858(5) 0.6187(3) 0.2358(3) 0.017(2) Uani 1 1 d . A . C147 C 1.2469(6) 0.5995(3) 0.2007(3) 0.021(2) Uani 1 1 d . . . H14M H 1.2685 0.6021 0.1780 0.025 Uiso 1 1 calc R . . C148 C 1.1778(5) 0.5768(3) 0.1981(2) 0.0091(17) Uani 1 1 d . . . C149 C 1.1408(5) 0.5752(3) 0.2307(3) 0.017(2) Uani 1 1 d . . . C150 C 1.3601(6) 0.6459(3) 0.2378(3) 0.032(3) Uani 1 1 d D . . C151 C 1.4012(15) 0.6595(9) 0.2798(5) 0.020(6) Uiso 0.378(17) 1 d PD A 1 H15Z H 1.3917 0.6909 0.2837 0.030 Uiso 0.378(17) 1 calc PR A 1 H16Y H 1.4575 0.6544 0.2834 0.030 Uiso 0.378(17) 1 calc PR A 1 H16Z H 1.3806 0.6420 0.2989 0.030 Uiso 0.378(17) 1 calc PR A 1 C152 C 1.3318(18) 0.6892(7) 0.2153(8) 0.029(7) Uiso 0.378(17) 1 d PD A 1 H17W H 1.2990 0.6820 0.1895 0.044 Uiso 0.378(17) 1 calc PR A 1 H17X H 1.3770 0.7064 0.2117 0.044 Uiso 0.378(17) 1 calc PR A 1 H17Y H 1.3014 0.7065 0.2305 0.044 Uiso 0.378(17) 1 calc PR A 1 C15A C 1.4126(14) 0.6374(8) 0.2793(5) 0.057(7) Uiso 0.622(17) 1 d PD A 2 H15B H 1.4205 0.6056 0.2834 0.085 Uiso 0.622(17) 1 calc PR A 2 H15C H 1.3872 0.6494 0.2995 0.085 Uiso 0.622(17) 1 calc PR A 2 H15D H 1.4632 0.6519 0.2811 0.085 Uiso 0.622(17) 1 calc PR A 2 C15B C 1.3433(15) 0.6954(6) 0.2351(8) 0.059(7) Uiso 0.622(17) 1 d PD A 2 H15E H 1.3085 0.7021 0.2097 0.089 Uiso 0.622(17) 1 calc PR A 2 H15F H 1.3924 0.7116 0.2374 0.089 Uiso 0.622(17) 1 calc PR A 2 H15G H 1.3182 0.7042 0.2565 0.089 Uiso 0.622(17) 1 calc PR A 2 C153 C 1.4086(7) 0.6289(5) 0.2106(4) 0.050(4) Uani 1 1 d . A . H15H H 1.3767 0.6273 0.1838 0.074 Uiso 1 1 calc R . . H15I H 1.4282 0.5995 0.2191 0.074 Uiso 1 1 calc R . . H15J H 1.4528 0.6489 0.2110 0.074 Uiso 1 1 calc R . . C154 C 1.1397(6) 0.5558(3) 0.1592(3) 0.0152(19) Uani 1 1 d . . . H15K H 1.1736 0.5318 0.1532 0.018 Uiso 1 1 calc R . . H15L H 1.0893 0.5426 0.1616 0.018 Uiso 1 1 calc R . . C155 C 0.8797(7) 0.7869(4) 0.0502(3) 0.035(3) Uani 1 1 d . . . H15M H 0.8679 0.7560 0.0547 0.052 Uiso 1 1 calc R . . H15N H 0.9117 0.7885 0.0303 0.052 Uiso 1 1 calc R . . H15O H 0.8309 0.8031 0.0408 0.052 Uiso 1 1 calc R . . C156 C 0.9383(8) 0.8513(3) 0.0804(3) 0.031(3) Uani 1 1 d . . . H15P H 0.8891 0.8684 0.0731 0.038 Uiso 1 1 calc R . . H15Q H 0.9670 0.8543 0.0590 0.038 Uiso 1 1 calc R . . C157 C 0.9873(7) 0.8686(4) 0.1186(3) 0.026(2) Uani 1 1 d . . . H15R H 1.0384 0.8533 0.1240 0.032 Uiso 1 1 calc R . . H15S H 0.9971 0.9004 0.1156 0.032 Uiso 1 1 calc R . . C158 C 0.8904(7) 0.8939(4) 0.1521(4) 0.031(3) Uani 1 1 d . . . H15T H 0.8675 0.8881 0.1749 0.047 Uiso 1 1 calc R . . H15U H 0.8499 0.8912 0.1279 0.047 Uiso 1 1 calc R . . H15V H 0.9120 0.9238 0.1539 0.047 Uiso 1 1 calc R . . C159 C 0.9592(7) 0.5436(4) 0.0627(3) 0.033(3) Uani 1 1 d . . . H15W H 0.9800 0.5737 0.0645 0.049 Uiso 1 1 calc R . . H15X H 0.9086 0.5430 0.0440 0.049 Uiso 1 1 calc R . . H15Y H 0.9957 0.5238 0.0535 0.049 Uiso 1 1 calc R . . C160 C 0.9197(6) 0.4865(3) 0.0991(3) 0.025(2) Uani 1 1 d . . . H16A H 0.9564 0.4656 0.0908 0.030 Uiso 1 1 calc R . . H16B H 0.8692 0.4849 0.0798 0.030 Uiso 1 1 calc R . . C161 C 0.9083(6) 0.4744(4) 0.1396(3) 0.022(2) Uani 1 1 d . . . H16C H 0.8642 0.4916 0.1454 0.027 Uiso 1 1 calc R . . H16D H 0.8943 0.4427 0.1399 0.027 Uiso 1 1 calc R . . C162 C 1.0387(7) 0.4527(3) 0.1690(3) 0.029(3) Uani 1 1 d . . . H16E H 1.0836 0.4599 0.1901 0.043 Uiso 1 1 calc R . . H16F H 1.0537 0.4551 0.1435 0.043 Uiso 1 1 calc R . . H16G H 1.0214 0.4225 0.1725 0.043 Uiso 1 1 calc R . . C163 C 0.6922(9) 0.9368(6) 0.1518(6) 0.078(6) Uani 1 1 d . . . H16H H 0.7029 0.9099 0.1383 0.117 Uiso 1 1 calc R . . H16I H 0.6549 0.9552 0.1335 0.117 Uiso 1 1 calc R . . H16J H 0.6701 0.9291 0.1745 0.117 Uiso 1 1 calc R . . C164 C 0.7558(10) 0.9993(5) 0.1834(5) 0.065(5) Uani 1 1 d . . . H16K H 0.7249 0.9942 0.2037 0.078 Uiso 1 1 calc R . . H16L H 0.7260 1.0203 0.1639 0.078 Uiso 1 1 calc R . . C165 C 0.830(2) 1.0203(8) 0.2023(8) 0.166(15) Uani 1 1 d . . . H16M H 0.8183 1.0513 0.2079 0.199 Uiso 1 1 calc R . . H16X H 0.8487 1.0056 0.2281 0.199 Uiso 1 1 calc R . . C167 C 0.5610(8) 0.8192(5) -0.1004(4) 0.044(3) Uani 1 1 d . . . H16N H 0.6043 0.8150 -0.1138 0.067 Uiso 1 1 calc R . . H16O H 0.5182 0.8347 -0.1180 0.067 Uiso 1 1 calc R . . H16P H 0.5426 0.7905 -0.0934 0.067 Uiso 1 1 calc R . . C168 C 0.5278(8) 0.8525(4) -0.0455(4) 0.042(3) Uani 1 1 d . . . H16Q H 0.5116 0.8244 -0.0350 0.050 Uiso 1 1 calc R . . H16R H 0.4818 0.8654 -0.0635 0.050 Uiso 1 1 calc R . . C169 C 0.5578(9) 0.8837(4) -0.0121(4) 0.050(4) Uani 1 1 d . . . H16S H 0.5844 0.9091 -0.0215 0.060 Uiso 1 1 calc R . . H16T H 0.5141 0.8951 -0.0010 0.060 Uiso 1 1 calc R . . C170 C 0.6572(10) 0.8870(5) 0.0458(4) 0.062(4) Uani 1 1 d . . . H17A H 0.6930 0.8687 0.0649 0.093 Uiso 1 1 calc R . . H17B H 0.6233 0.9037 0.0595 0.093 Uiso 1 1 calc R . . H17C H 0.6873 0.9075 0.0331 0.093 Uiso 1 1 calc R . . C171 C 1.2675(7) 0.9262(4) 0.3392(4) 0.039(3) Uani 1 1 d . . . H17D H 1.2951 0.9448 0.3609 0.058 Uiso 1 1 calc R . . H17E H 1.2226 0.9122 0.3469 0.058 Uiso 1 1 calc R . . H17F H 1.2492 0.9445 0.3158 0.058 Uiso 1 1 calc R . . C172 C 1.2797(6) 0.8668(4) 0.2992(4) 0.033(3) Uani 1 1 d . . . H17G H 1.2622 0.8851 0.2753 0.039 Uiso 1 1 calc R . . H17H H 1.2334 0.8528 0.3060 0.039 Uiso 1 1 calc R . . C173 C 1.3354(7) 0.8324(4) 0.2918(4) 0.038(3) Uani 1 1 d . . . H17I H 1.3592 0.8177 0.3169 0.045 Uiso 1 1 calc R . . H17J H 1.3066 0.8098 0.2737 0.045 Uiso 1 1 calc R . . C174 C 1.4436(10) 0.8186(5) 0.2639(5) 0.062(5) Uani 1 1 d . . . H17K H 1.4828 0.8331 0.2520 0.094 Uiso 1 1 calc R . . H17L H 1.4124 0.7984 0.2448 0.094 Uiso 1 1 calc R . . H17M H 1.4698 0.8020 0.2872 0.094 Uiso 1 1 calc R . . C175 C 1.0791(15) 0.8732(10) -0.1063(8) 0.157(13) Uani 1 1 d . . . H17N H 1.1270 0.8907 -0.0990 0.235 Uiso 1 1 calc R . . H17O H 1.0478 0.8770 -0.0864 0.235 Uiso 1 1 calc R . . H17P H 1.0490 0.8831 -0.1320 0.235 Uiso 1 1 calc R . . C176 C 1.0970(8) 0.8321(6) -0.1084(5) 0.064(5) Uani 1 1 d . . . H17Q H 1.1499 0.8227 -0.1036 0.076 Uiso 1 1 calc R . . C177 C 1.0365(11) 0.8024(7) -0.1179(6) 0.089(7) Uani 1 1 d . . . H17R H 1.0062 0.8079 -0.1449 0.107 Uiso 1 1 calc R . . H17S H 1.0010 0.8054 -0.0994 0.107 Uiso 1 1 calc R . . C178 C 1.0697(11) 0.7590(8) -0.1152(6) 0.098(8) Uani 1 1 d . . . H17T H 1.1102 0.7572 -0.1310 0.117 Uiso 1 1 calc R . . H17U H 1.0943 0.7520 -0.0874 0.117 Uiso 1 1 calc R . . C179 C 1.0081(8) 0.7283(6) -0.1298(5) 0.061(4) Uani 1 1 d . . . H17V H 0.9544 0.7361 -0.1365 0.073 Uiso 1 1 calc R . . C180 C 1.0359(14) 0.6857(10) -0.1329(7) 0.139(11) Uani 1 1 d . . . H18A H 0.9919 0.6658 -0.1427 0.209 Uiso 1 1 calc R . . H18B H 1.0644 0.6756 -0.1070 0.209 Uiso 1 1 calc R . . H18C H 1.0710 0.6856 -0.1514 0.209 Uiso 1 1 calc R . . C181 C 0.6196(8) 0.6527(5) 0.1223(5) 0.050(4) Uani 1 1 d . . . H18D H 0.6666 0.6703 0.1227 0.075 Uiso 1 1 calc R . . H18E H 0.6147 0.6302 0.1017 0.075 Uiso 1 1 calc R . . H18F H 0.6236 0.6384 0.1479 0.075 Uiso 1 1 calc R . . C182 C 0.5536(5) 0.6803(3) 0.1145(3) 0.0130(18) Uiso 1 1 d . . . H18G H 0.5565 0.7111 0.1101 0.016 Uiso 1 1 calc R . . C183 C 0.4835(7) 0.6583(4) 0.1138(4) 0.034(3) Uani 1 1 d . . . H18H H 0.4865 0.6424 0.1389 0.041 Uiso 1 1 calc R . . H18I H 0.4737 0.6365 0.0921 0.041 Uiso 1 1 calc R . . C184 C 0.4188(7) 0.6908(4) 0.1080(4) 0.036(3) Uani 1 1 d . . . H18J H 0.4308 0.7140 0.1284 0.044 Uiso 1 1 calc R . . H18K H 0.4131 0.7050 0.0818 0.044 Uiso 1 1 calc R . . C185 C 0.3485(5) 0.6695(3) 0.1104(3) 0.018(2) Uani 1 1 d . . . H18L H 0.3457 0.6387 0.1145 0.021 Uiso 1 1 calc R . . C186 C 0.2841(8) 0.6966(5) 0.1064(5) 0.061(4) Uani 1 1 d . . . H18M H 0.2384 0.6789 0.1086 0.092 Uiso 1 1 calc R . . H18N H 0.2746 0.7110 0.0806 0.092 Uiso 1 1 calc R . . H18O H 0.2936 0.7190 0.1272 0.092 Uiso 1 1 calc R . . C166 C 0.9517(15) 1.0406(8) 0.2023(10) 0.173(15) Uani 1 1 d . . . H16U H 0.9908 1.0357 0.1864 0.260 Uiso 1 1 calc R . . H16V H 0.9706 1.0282 0.2287 0.260 Uiso 1 1 calc R . . H16W H 0.9426 1.0723 0.2043 0.260 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 Bi4 0.013 0.009 0.015 0.000 0.002 0.000 O1 0.012 0.015 0.017 -0.002 0.002 0.000 C1 0.015 0.008 0.016 -0.007 0.009 -0.002 Bi2 0.014 0.009 0.015 0.000 0.004 0.000 O2 0.016 0.008 0.021 -0.003 0.006 -0.003 C2 0.006 0.014 0.033 0.000 0.005 -0.003 Bi1 0.01370(16) 0.00926(16) 0.01479(17) -0.00097(13) 0.00316(13) -0.00077(13) O3 0.018(3) 0.009(3) 0.015(3) 0.004(2) 0.002(3) -0.003(3) C3 0.027(5) 0.014(5) 0.018(5) 0.000(4) 0.012(4) 0.001(4) Bi3 0.01332(16) 0.00940(16) 0.01692(17) 0.00110(13) 0.00398(13) -0.00047(13) O4 0.019(3) 0.012(3) 0.019(4) 0.000(3) 0.009(3) 0.003(3) C4 0.018(5) 0.018(5) 0.020(5) -0.004(4) 0.006(4) -0.004(4) O5 0.037(4) 0.012(3) 0.022(4) 0.001(3) 0.013(3) 0.007(3) C5 0.023(5) 0.017(5) 0.023(5) -0.004(4) 0.016(4) -0.009(4) O6 0.035(4) 0.012(3) 0.022(4) 0.007(3) 0.005(3) 0.013(3) C6 0.014(5) 0.016(5) 0.018(5) -0.004(4) 0.006(4) -0.001(4) O7 0.029(4) 0.013(3) 0.018(4) -0.001(3) 0.007(3) 0.000(3) C7 0.015(5) 0.006(4) 0.024(5) 0.008(4) -0.009(4) -0.004(4) O8 0.016(3) 0.018(3) 0.021(4) 0.007(3) 0.008(3) 0.002(3) C8 0.032(6) 0.021(6) 0.052(8) -0.004(5) 0.022(6) -0.016(5) O9 0.019(3) 0.012(3) 0.024(4) -0.001(3) 0.010(3) -0.006(3) C9 0.026(6) 0.017(5) 0.034(6) 0.002(4) 0.004(5) -0.001(4) O10 0.015(3) 0.010(3) 0.021(4) 0.001(3) 0.009(3) -0.002(3) C10 0.017(5) 0.021(6) 0.046(7) 0.003(5) -0.006(5) -0.004(4) O11 0.019(4) 0.012(3) 0.029(4) -0.001(3) 0.004(3) -0.003(3) C11 0.011(5) 0.018(5) 0.021(5) -0.001(4) 0.000(4) 0.011(4) O12 0.027(4) 0.015(3) 0.022(4) -0.002(3) -0.001(3) 0.002(3) C12 0.027(5) 0.012(5) 0.020(5) -0.004(4) 0.012(4) 0.005(4) C13 0.020(5) 0.012(5) 0.022(5) 0.002(4) 0.004(4) -0.003(4) O13 0.031(4) 0.007(3) 0.025(4) -0.002(3) -0.003(3) 0.003(3) C14 0.020(5) 0.013(5) 0.031(6) 0.002(4) 0.008(5) -0.002(4) O14 0.014(3) 0.014(3) 0.018(4) -0.002(3) 0.004(3) -0.001(3) C15 0.018(5) 0.021(5) 0.017(5) -0.004(4) 0.008(4) 0.004(4) O15 0.014(3) 0.009(3) 0.019(3) 0.001(3) 0.005(3) 0.001(3) C16 0.009(4) 0.016(5) 0.028(6) -0.002(4) 0.009(4) 0.005(4) O16 0.016(3) 0.011(3) 0.014(3) 0.001(2) 0.004(3) -0.003(3) C17 0.010(4) 0.013(5) 0.023(5) -0.007(4) -0.001(4) 0.005(4) O17 0.025(4) 0.018(4) 0.026(4) 0.001(3) 0.012(3) 0.004(3) C18 0.021(5) 0.034(6) 0.017(5) -0.012(4) 0.006(4) -0.010(5) O18 0.037(5) 0.023(4) 0.019(4) 0.006(3) 0.000(3) 0.002(3) C19 0.059(9) 0.029(7) 0.049(8) -0.009(6) -0.010(7) -0.027(6) O19 0.034(4) 0.020(4) 0.023(4) -0.002(3) 0.000(3) -0.003(3) C20 0.033(7) 0.050(8) 0.024(6) -0.008(5) 0.003(5) -0.011(6) O20 0.016(3) 0.012(3) 0.020(4) -0.006(3) 0.003(3) -0.001(3) C21 0.022(6) 0.053(8) 0.041(8) -0.012(6) -0.001(5) -0.008(6) O21 0.042(6) 0.067(7) 0.106(9) -0.042(7) 0.035(6) -0.001(5) C22 0.014(5) 0.018(5) 0.018(5) -0.004(4) 0.004(4) -0.004(4) O22 0.129(17) 0.17(2) 0.39(4) -0.15(2) 0.03(2) -0.081(15) C23 0.018(5) 0.010(4) 0.016(5) 0.002(4) 0.004(4) -0.002(4) O23 0.060(6) 0.047(6) 0.041(5) -0.008(4) 0.012(5) -0.011(5) C24 0.032(6) 0.013(5) 0.019(5) 0.001(4) -0.001(4) 0.001(4) O24 0.073(7) 0.045(6) 0.043(6) 0.004(4) 0.002(5) -0.011(5) C25 0.030(6) 0.037(6) 0.014(5) 0.002(5) 0.004(5) 0.003(5) O25 0.029(4) 0.035(5) 0.037(5) -0.006(4) 0.009(4) 0.006(4) C26 0.020(5) 0.017(5) 0.018(5) -0.001(4) -0.003(4) 0.007(4) O26 0.056(6) 0.028(5) 0.059(6) 0.012(4) 0.029(5) 0.005(4) C27 0.015(5) 0.015(5) 0.020(5) 0.002(4) 0.004(4) -0.001(4) C28 0.016(5) 0.012(4) 0.011(4) 0.007(3) 0.002(4) -0.006(4) C29 0.043(7) 0.038(7) 0.025(6) -0.005(5) -0.014(5) 0.014(6) C30 0.027(6) 0.042(8) 0.040(7) 0.007(6) -0.013(6) 0.006(6) C31 0.053(9) 0.093(12) 0.015(6) 0.002(7) -0.007(6) 0.037(8) C32 0.055(10) 0.045(9) 0.117(15) -0.042(10) -0.052(10) 0.026(8) C33 0.010(4) 0.015(5) 0.020(5) 0.001(4) 0.005(4) 0.003(4) C34 0.027(5) 0.016(5) 0.014(5) -0.010(4) 0.004(4) 0.011(4) C35 0.017(5) 0.018(5) 0.018(5) -0.001(4) 0.000(4) -0.006(4) C36 0.021(5) 0.010(4) 0.022(5) 0.001(4) 0.010(4) 0.001(4) C37 0.022(5) 0.011(4) 0.015(5) -0.002(4) 0.012(4) 0.003(4) C38 0.017(5) 0.013(5) 0.021(5) -0.005(4) 0.001(4) 0.000(4) C39 0.018(5) 0.007(4) 0.016(5) -0.003(3) 0.004(4) 0.008(4) C40 0.023(5) 0.027(6) 0.026(6) 0.009(5) 0.011(5) 0.000(5) C41 0.011(5) 0.052(8) 0.058(9) 0.014(7) -0.003(5) -0.009(5) C42 0.027(7) 0.039(8) 0.092(12) 0.015(8) 0.015(7) -0.014(6) C43 0.030(7) 0.079(11) 0.048(8) -0.015(7) 0.029(6) -0.023(7) C44 0.011(4) 0.009(4) 0.023(5) 0.000(4) 0.008(4) -0.001(4) C45 0.015(5) 0.021(5) 0.011(5) -0.008(4) 0.002(4) 0.001(4) C46 0.022(5) 0.015(5) 0.023(5) -0.010(4) 0.006(4) -0.002(4) C47 0.027(6) 0.023(5) 0.010(5) 0.004(4) 0.005(4) 0.007(4) C48 0.016(5) 0.031(6) 0.016(5) 0.004(4) 0.006(4) -0.001(4) C49 0.028(6) 0.025(6) 0.017(5) 0.003(4) 0.005(4) -0.004(5) C50 0.023(5) 0.022(5) 0.014(5) 0.006(4) 0.001(4) 0.005(4) C51 0.037(6) 0.019(5) 0.022(6) -0.002(4) 0.006(5) 0.004(5) C52 0.045(8) 0.049(8) 0.040(8) -0.009(6) 0.015(6) 0.027(7) C53 0.035(7) 0.062(9) 0.027(7) -0.015(6) 0.001(6) -0.012(6) C54 0.090(12) 0.037(8) 0.045(8) -0.002(6) 0.034(8) 0.008(8) C55 0.022(5) 0.026(6) 0.019(5) -0.003(4) 0.006(4) -0.005(4) C56 0.027(6) 0.011(5) 0.015(5) 0.003(4) -0.002(4) -0.002(4) C57 0.024(5) 0.019(5) 0.014(5) 0.004(4) 0.003(4) 0.009(4) C58 0.031(6) 0.018(5) 0.022(6) 0.006(4) 0.005(5) -0.002(4) C59 0.035(6) 0.019(5) 0.022(6) 0.001(4) 0.006(5) 0.003(5) C60 0.022(5) 0.017(5) 0.015(5) 0.001(4) 0.005(4) -0.002(4) C61 0.035(6) 0.013(5) 0.025(6) 0.003(4) 0.012(5) 0.005(4) C62 0.040(7) 0.039(7) 0.030(7) 0.008(5) 0.022(6) 0.014(6) C63 0.080(11) 0.068(10) 0.032(8) 0.014(7) 0.019(8) 0.029(9) C64 0.056(9) 0.054(9) 0.039(8) 0.032(7) 0.025(7) 0.012(7) C65 0.042(8) 0.083(12) 0.065(11) 0.043(9) 0.010(8) -0.005(8) C66 0.025(5) 0.020(5) 0.016(5) -0.002(4) 0.007(4) 0.002(4) C67 0.027(5) 0.012(5) 0.009(4) 0.000(3) 0.007(4) -0.004(4) C68 0.018(5) 0.025(5) 0.019(5) -0.002(4) 0.001(4) 0.003(4) C69 0.014(5) 0.019(5) 0.020(5) 0.006(4) 0.006(4) 0.003(4) C70 0.022(5) 0.011(5) 0.024(5) -0.001(4) 0.007(4) 0.005(4) C71 0.005(4) 0.025(5) 0.025(6) -0.009(4) -0.002(4) 0.008(4) C72 0.018(5) 0.018(5) 0.022(5) -0.005(4) 0.010(4) -0.002(4) C73 0.031(6) 0.018(5) 0.028(6) 0.006(4) 0.007(5) 0.006(5) C74 0.062(9) 0.028(6) 0.020(6) 0.006(5) 0.020(6) 0.000(6) C75 0.039(7) 0.025(6) 0.027(6) 0.010(5) 0.005(5) 0.015(5) C76 0.041(7) 0.020(6) 0.032(6) 0.011(5) 0.002(5) -0.009(5) C77 0.021(5) 0.010(5) 0.032(6) 0.001(4) 0.017(5) -0.003(4) C78 0.022(5) 0.010(4) 0.015(5) 0.001(4) 0.007(4) -0.003(4) C79 0.017(5) 0.017(5) 0.018(5) -0.003(4) 0.006(4) -0.004(4) C80 0.015(5) 0.026(5) 0.013(5) -0.002(4) -0.002(4) 0.002(4) C81 0.019(5) 0.034(6) 0.012(5) -0.001(4) 0.006(4) 0.001(4) C82 0.018(5) 0.022(5) 0.018(5) -0.001(4) 0.003(4) -0.004(4) C83 0.011(5) 0.025(5) 0.011(5) 0.002(4) 0.002(4) -0.005(4) C84 0.029(6) 0.034(6) 0.021(6) -0.003(5) 0.006(5) 0.008(5) C85 0.033(7) 0.048(8) 0.043(8) -0.009(6) 0.017(6) 0.006(6) C86 0.056(9) 0.050(8) 0.027(7) -0.011(6) 0.011(6) 0.009(7) C87 0.065(10) 0.044(8) 0.039(8) 0.009(6) 0.025(7) 0.015(7) C88 0.023(5) 0.006(4) 0.015(5) 0.001(3) 0.003(4) 0.002(4) C89 0.015(5) 0.010(4) 0.020(5) 0.001(4) 0.009(4) 0.005(4) C90 0.026(6) 0.025(5) 0.014(5) 0.002(4) 0.007(4) 0.006(4) C91 0.028(6) 0.016(5) 0.027(6) 0.005(4) 0.014(5) -0.003(4) C92 0.015(5) 0.018(5) 0.030(6) -0.005(4) 0.010(4) -0.008(4) C93 0.018(5) 0.012(5) 0.027(6) -0.001(4) 0.014(4) -0.003(4) C94 0.014(5) 0.019(5) 0.015(5) 0.002(4) 0.011(4) 0.004(4) C95 0.033(6) 0.030(6) 0.027(6) 0.010(5) 0.013(5) -0.012(5) C96 0.078(11) 0.072(11) 0.031(8) 0.015(7) 0.014(7) -0.037(9) C97 0.066(10) 0.031(7) 0.053(9) 0.028(6) 0.030(8) 0.006(7) C98 0.037(7) 0.038(7) 0.027(6) 0.005(5) 0.014(5) -0.006(6) C99 0.017(5) 0.007(4) 0.027(5) 0.006(4) 0.004(4) 0.009(4) C100 0.012(5) 0.010(4) 0.019(5) -0.006(4) -0.001(4) 0.006(4) C102 0.020(5) 0.017(5) 0.011(5) 0.003(4) 0.004(4) -0.001(4) C103 0.013(5) 0.012(5) 0.029(6) -0.010(4) -0.001(4) -0.002(4) C104 0.014(5) 0.008(4) 0.018(5) -0.006(3) 0.001(4) 0.000(4) C105 0.014(5) 0.015(5) 0.012(5) -0.001(4) 0.003(4) -0.003(4) C106 0.024(5) 0.013(5) 0.030(6) -0.004(4) 0.017(5) 0.000(4) C107 0.052(8) 0.019(6) 0.031(6) 0.002(5) 0.019(6) 0.005(5) C108 0.024(6) 0.017(5) 0.037(7) 0.005(5) 0.002(5) -0.006(4) C109 0.018(5) 0.004(4) 0.038(6) -0.003(4) 0.004(4) -0.008(4) C110 0.010(4) 0.016(5) 0.017(5) 0.001(4) 0.002(4) 0.003(4) C111 0.014(5) 0.004(4) 0.023(5) 0.001(3) 0.010(4) -0.003(3) C112 0.011(5) 0.023(5) 0.017(5) -0.007(4) 0.010(4) -0.005(4) C113 0.019(5) 0.018(5) 0.035(6) 0.000(4) 0.009(5) -0.005(4) C114 0.021(5) 0.017(5) 0.025(6) -0.011(4) 0.007(4) -0.007(4) C115 0.021(5) 0.020(5) 0.020(5) 0.000(4) 0.006(4) 0.009(4) C116 0.021(5) 0.014(5) 0.030(6) 0.001(4) 0.018(5) -0.004(4) C117 0.026(6) 0.021(6) 0.034(6) -0.010(5) 0.008(5) -0.004(5) C118 0.027(6) 0.028(6) 0.044(7) -0.009(5) 0.009(5) -0.006(5) C119 0.048(8) 0.022(6) 0.037(7) -0.012(5) 0.010(6) 0.012(5) C120 0.045(7) 0.024(6) 0.034(7) -0.010(5) 0.014(6) 0.002(5) C121 0.029(6) 0.015(5) 0.017(5) -0.007(4) 0.008(4) 0.000(4) C122 0.022(5) 0.008(4) 0.025(5) 0.002(4) 0.007(4) 0.004(4) C123 0.032(6) 0.019(5) 0.014(5) -0.002(4) 0.001(4) 0.002(4) C124 0.023(5) 0.014(5) 0.015(5) -0.001(4) 0.001(4) 0.004(4) C125 0.018(5) 0.019(5) 0.023(5) 0.002(4) 0.007(4) 0.000(4) C126 0.028(6) 0.014(5) 0.021(5) 0.007(4) -0.001(4) 0.005(4) C127 0.022(5) 0.019(5) 0.015(5) -0.008(4) 0.002(4) -0.007(4) C128 0.034(7) 0.028(6) 0.023(6) -0.013(5) 0.002(5) -0.004(5) C129 0.047(8) 0.041(8) 0.037(7) -0.006(6) -0.005(6) 0.011(6) C130 0.046(8) 0.036(7) 0.045(8) -0.025(6) -0.004(6) -0.004(6) C131 0.031(7) 0.034(7) 0.036(7) -0.010(5) -0.010(5) -0.013(5) C132 0.017(5) 0.021(5) 0.018(5) -0.011(4) 0.003(4) 0.000(4) C133 0.030(6) 0.011(5) 0.024(6) -0.003(4) 0.006(5) 0.000(4) C134 0.025(6) 0.024(6) 0.018(5) -0.008(4) 0.001(4) 0.003(4) C135 0.022(5) 0.020(5) 0.021(5) 0.002(4) 0.005(4) 0.002(4) C136 0.017(5) 0.022(5) 0.016(5) -0.002(4) 0.006(4) -0.005(4) C137 0.014(5) 0.024(5) 0.016(5) -0.002(4) 0.007(4) 0.000(4) C138 0.018(5) 0.023(5) 0.018(5) -0.007(4) 0.009(4) 0.000(4) C139 0.051(8) 0.029(6) 0.014(5) 0.009(4) -0.002(5) 0.002(6) C143 0.011(5) 0.024(5) 0.015(5) 0.001(4) -0.002(4) -0.005(4) C144 0.015(5) 0.008(4) 0.015(5) 0.000(3) 0.002(4) 0.007(4) C145 0.017(5) 0.012(5) 0.020(5) 0.001(4) -0.001(4) 0.000(4) C146 0.012(5) 0.017(5) 0.024(5) -0.002(4) 0.005(4) 0.000(4) C147 0.012(5) 0.024(5) 0.027(6) 0.006(4) 0.007(4) 0.006(4) C148 0.008(4) 0.009(4) 0.010(4) 0.006(3) 0.003(3) 0.005(3) C149 0.012(4) 0.017(5) 0.022(5) -0.001(4) 0.005(4) 0.002(4) C150 0.024(6) 0.028(6) 0.047(8) -0.024(5) 0.014(5) -0.009(5) C153 0.027(7) 0.066(10) 0.064(10) -0.032(8) 0.031(7) -0.014(6) C154 0.016(5) 0.010(4) 0.019(5) -0.002(4) 0.002(4) -0.001(4) C155 0.045(7) 0.027(6) 0.037(7) 0.001(5) 0.019(6) 0.003(5) C156 0.053(8) 0.018(5) 0.024(6) 0.012(4) 0.010(5) 0.006(5) C157 0.035(6) 0.021(6) 0.024(6) 0.005(4) 0.009(5) 0.004(5) C158 0.030(6) 0.027(6) 0.038(7) -0.002(5) 0.009(5) 0.016(5) C159 0.038(7) 0.036(7) 0.025(6) -0.004(5) 0.006(5) -0.006(5) C160 0.029(6) 0.015(5) 0.029(6) -0.003(4) 0.003(5) 0.001(4) C161 0.022(5) 0.026(6) 0.016(5) -0.007(4) -0.003(4) -0.007(4) C162 0.032(6) 0.021(6) 0.035(7) -0.001(5) 0.009(5) 0.015(5) C163 0.044(10) 0.105(15) 0.086(14) -0.020(11) 0.018(9) 0.001(10) C164 0.080(12) 0.046(9) 0.062(11) -0.001(8) -0.001(9) 0.036(9) C165 0.30(4) 0.103(18) 0.15(2) -0.078(16) 0.16(3) -0.15(2) C167 0.042(8) 0.063(9) 0.028(7) -0.004(6) 0.007(6) -0.007(7) C168 0.050(8) 0.026(6) 0.048(8) 0.007(6) 0.010(7) 0.004(6) C169 0.067(10) 0.038(8) 0.045(8) 0.010(6) 0.012(7) 0.002(7) C170 0.082(12) 0.058(10) 0.041(9) -0.010(7) 0.002(8) -0.021(9) C171 0.030(7) 0.044(8) 0.045(8) -0.007(6) 0.016(6) 0.000(6) C172 0.021(6) 0.040(7) 0.034(7) -0.006(5) -0.001(5) -0.008(5) C173 0.044(8) 0.026(6) 0.040(7) -0.004(5) 0.005(6) -0.005(6) C174 0.093(13) 0.039(8) 0.067(11) 0.007(7) 0.042(10) 0.019(8) C175 0.10(2) 0.24(4) 0.13(2) 0.05(3) 0.008(18) -0.05(2) C176 0.028(8) 0.069(12) 0.096(14) 0.017(11) 0.019(8) 0.020(8) C177 0.054(12) 0.130(19) 0.074(13) 0.022(13) -0.008(10) -0.003(13) C178 0.064(13) 0.15(2) 0.079(14) 0.040(14) 0.024(11) 0.038(15) C179 0.021(7) 0.081(12) 0.076(12) 0.006(10) 0.002(7) 0.005(8) C180 0.10(2) 0.22(4) 0.10(2) 0.04(2) 0.023(16) -0.01(2) C181 0.038(8) 0.051(9) 0.067(10) -0.001(7) 0.025(7) 0.006(7) C183 0.030(7) 0.031(6) 0.041(7) -0.004(5) 0.010(6) 0.007(5) C184 0.043(7) 0.037(7) 0.027(6) 0.009(5) 0.001(6) 0.011(6) C185 0.003(4) 0.010(4) 0.037(6) -0.008(4) -0.001(4) 0.004(3) C186 0.034(8) 0.066(11) 0.078(12) -0.013(9) -0.002(8) 0.015(7) C166 0.11(2) 0.073(16) 0.30(4) 0.04(2) -0.03(2) -0.041(15) _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 Bi4 O16 2.174(6) . ? Bi4 O8 2.190(7) . ? Bi4 O15 2.214(6) . ? Bi4 O9 2.270(6) . ? Bi4 Bi2 3.5162(6) . ? Bi4 Bi1 3.6882(5) . ? Bi4 Bi3 3.6928(5) . ? O1 C1 1.374(10) . ? O1 Bi1 2.188(6) . ? C1 C2 1.405(13) . ? C1 C6 1.407(13) . ? Bi2 O15 2.180(6) . ? Bi2 O3 2.209(6) . ? Bi2 O16 2.220(6) . ? Bi2 O2 2.251(6) . ? Bi2 Bi3 3.6720(5) . ? Bi2 Bi1 3.6821(5) . ? O2 C17 1.364(11) . ? O2 Bi1 2.439(6) . ? C2 C3 1.400(13) . ? C2 C77 1.511(13) . ? Bi1 O14 2.151(6) . ? Bi1 O15 2.172(6) . ? Bi1 O8 2.655(6) . ? O3 C28 1.369(11) . ? O3 Bi3 2.622(6) . ? C3 C4 1.392(14) . ? C3 H3A 0.9500 . ? Bi3 O4 2.157(6) . ? Bi3 O16 2.174(6) . ? Bi3 O10 2.194(6) . ? Bi3 O9 2.459(7) . ? O4 C39 1.372(11) . ? C4 C5 1.375(14) . ? C4 C7 1.525(13) . ? O5 C50 1.396(12) . ? O5 H5A 0.8400 . ? C5 C6 1.388(13) . ? C5 H5B 0.9500 . ? O6 C61 1.355(12) . ? O6 H6A 0.8400 . ? C6 C11 1.517(13) . ? O7 C72 1.364(11) . ? O7 H7A 0.8400 . ? C7 C8 1.500(15) . ? C7 C9 1.539(13) . ? C7 C10 1.545(13) . ? O8 C78 1.381(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C94 1.377(11) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 C105 1.391(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O11 C116 1.393(11) . ? O11 H11A 0.8400 . ? C11 C12 1.506(13) . ? C11 H11B 0.9900 . ? C11 H11C 0.9900 . ? O12 C127 1.373(11) . ? O12 H12A 0.8400 . ? C12 C17 1.372(13) . ? C12 C13 1.410(13) . ? C13 C14 1.393(14) . ? C13 H13A 0.9500 . ? O13 C138 1.375(12) . ? O13 H13B 0.8400 . ? C14 C15 1.401(13) . ? C14 C18 1.533(14) . ? O14 C149 1.344(11) . ? C15 C16 1.388(14) . ? C15 H15A 0.9500 . ? C16 C17 1.433(14) . ? C16 C22 1.506(13) . ? O17 C157 1.423(12) . ? O17 C158 1.441(12) . ? C18 C20 1.525(15) . ? C18 C21 1.528(15) . ? C18 C19 1.532(16) . ? O18 C155 1.429(13) . ? O18 C156 1.429(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O19 C160 1.408(12) . ? O19 C159 1.418(13) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O20 C162 1.415(11) . ? O20 C161 1.443(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O21 C164 1.364(16) . ? O21 C163 1.406(18) . ? C22 C23 1.517(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O22 C165 1.23(3) . ? O22 C166 1.36(3) . ? C23 C24 1.387(13) . ? C23 C28 1.395(13) . ? O23 C168 1.399(15) . ? O23 C167 1.420(14) . ? C24 C25 1.376(15) . ? C24 H24A 0.9500 . ? O24 C170 1.407(16) . ? O24 C169 1.423(16) . ? C25 C26 1.388(14) . ? C25 C29 1.548(15) . ? O25 C172 1.410(13) . ? O25 C171 1.424(13) . ? C26 C27 1.394(13) . ? C26 H26A 0.9500 . ? O26 C174 1.399(15) . ? O26 C173 1.410(15) . ? C27 C28 1.419(13) . ? C27 C33 1.493(13) . ? C29 C31 1.505(19) . ? C29 C30 1.534(17) . ? C29 C32 1.536(18) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.495(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.405(14) . ? C34 C39 1.415(13) . ? C35 C36 1.398(13) . ? C35 H35A 0.9500 . ? C36 C37 1.399(14) . ? C36 C40 1.538(14) . ? C37 C38 1.384(13) . ? C37 H37A 0.9500 . ? C38 C39 1.419(13) . ? C38 C44 1.513(13) . ? C40 C41 1.523(15) . ? C40 C43 1.524(16) . ? C40 C42 1.526(16) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.517(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.377(12) . ? C45 C50 1.405(14) . ? C46 C47 1.395(14) . ? C46 H46A 0.9500 . ? C47 C48 1.400(14) . ? C47 C51 1.529(14) . ? C48 C49 1.364(14) . ? C48 H48A 0.9500 . ? C49 C50 1.378(14) . ? C49 C55 1.541(14) . ? C51 C53 1.520(16) . ? C51 C52 1.526(15) . ? C51 C54 1.547(16) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.494(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.389(14) . ? C56 C61 1.410(14) . ? C57 C58 1.379(13) . ? C57 H57A 0.9500 . ? C58 C59 1.407(15) . ? C58 C62 1.541(15) . ? C59 C60 1.390(14) . ? C59 H59A 0.9500 . ? C60 C61 1.389(14) . ? C60 C66 1.515(14) . ? C62 C64 1.497(16) . ? C62 C65 1.531(19) . ? C62 C63 1.533(18) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.531(13) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.388(13) . ? C67 C72 1.400(13) . ? C68 C69 1.384(14) . ? C68 H68A 0.9500 . ? C69 C70 1.406(14) . ? C69 C73 1.530(13) . ? C70 C71 1.449(14) . ? C70 H70A 0.9500 . ? C71 C72 1.376(13) . ? C71 C77 1.450(14) . ? C73 C74 1.515(15) . ? C73 C76 1.537(15) . ? C73 C75 1.541(15) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C83 1.409(12) . ? C78 C79 1.417(13) . ? C79 C80 1.381(13) . ? C79 C154 1.495(13) . ? C80 C81 1.401(14) . ? C80 H80A 0.9500 . ? C81 C82 1.402(14) . ? C81 C84 1.526(14) . ? C82 C83 1.389(13) . ? C82 H82A 0.9500 . ? C83 C88 1.515(13) . ? C84 C86 1.526(17) . ? C84 C87 1.529(16) . ? C84 C85 1.537(16) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C89 1.500(13) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C94 1.380(13) . ? C89 C90 1.399(13) . ? C90 C91 1.380(14) . ? C90 H90A 0.9500 . ? C91 C92 1.404(14) . ? C91 C95 1.530(14) . ? C92 C93 1.398(14) . ? C92 H92A 0.9500 . ? C93 C94 1.421(13) . ? C93 C99 1.492(14) . ? C95 C98 1.524(16) . ? C95 C96 1.534(17) . ? C95 C97 1.547(16) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.519(12) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.388(13) . ? C100 C105 1.405(13) . ? C101 C102 1.423(13) . ? C101 H10D 0.9500 . ? C102 C103 1.390(13) . ? C102 C106 1.542(13) . ? C103 C104 1.375(13) . ? C103 H10E 0.9500 . ? C104 C105 1.408(12) . ? C104 C110 1.503(13) . ? C106 C109 1.497(14) . ? C106 C107 1.511(14) . ? C106 C108 1.529(14) . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C108 H10K 0.9800 . ? C109 H10L 0.9800 . ? C109 H10M 0.9800 . ? C109 H10N 0.9800 . ? C110 C111 1.525(13) . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.387(12) . ? C111 C116 1.405(13) . ? C112 C113 1.419(14) . ? C112 H11F 0.9500 . ? C113 C114 1.336(14) . ? C113 C117 1.533(14) . ? C114 C115 1.383(13) . ? C114 H11G 0.9500 . ? C115 C116 1.366(14) . ? C115 C121 1.526(13) . ? C117 C119 1.542(15) . ? C117 C120 1.542(16) . ? C117 C118 1.543(15) . ? C118 H11H 0.9800 . ? C118 H11I 0.9800 . ? C118 H11J 0.9800 . ? C119 H11K 0.9800 . ? C119 H11L 0.9800 . ? C119 H11M 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C120 H12D 0.9800 . ? C121 C122 1.505(14) . ? C121 H12E 0.9900 . ? C121 H12F 0.9900 . ? C122 C123 1.388(14) . ? C122 C127 1.394(13) . ? C123 C124 1.398(14) . ? C123 H12G 0.9500 . ? C124 C125 1.404(13) . ? C124 C128 1.533(14) . ? C125 C126 1.360(14) . ? C125 H12H 0.9500 . ? C126 C127 1.385(14) . ? C126 C132 1.524(13) . ? C128 C129 1.520(16) . ? C128 C130 1.534(15) . ? C128 C131 1.536(17) . ? C129 H12I 0.9800 . ? C129 H12J 0.9800 . ? C129 H12K 0.9800 . ? C130 H13C 0.9800 . ? C130 H13D 0.9800 . ? C130 H13E 0.9800 . ? C131 H13F 0.9800 . ? C131 H13G 0.9800 . ? C131 H13H 0.9800 . ? C132 C133 1.524(14) . ? C132 H13I 0.9900 . ? C132 H13J 0.9900 . ? C133 C134 1.375(14) . ? C133 C138 1.395(14) . ? C134 C135 1.382(14) . ? C134 H13K 0.9500 . ? C135 C136 1.381(14) . ? C135 C139 1.532(14) . ? C136 C137 1.395(13) . ? C136 H13L 0.9500 . ? C137 C138 1.419(14) . ? C137 C143 1.459(13) . ? C139 C14C 1.513(15) . ? C139 C141 1.523(17) . ? C139 C14A 1.525(14) . ? C139 C142 1.530(16) . ? C139 C140 1.551(17) . ? C139 C14B 1.553(14) . ? C140 H14A 0.9800 . ? C140 H14B 0.9800 . ? C140 H14C 0.9800 . ? C141 H14Q 0.9800 . ? C141 H14R 0.9800 . ? C141 H14S 0.9800 . ? C142 H14T 0.9800 . ? C142 H14U 0.9800 . ? C142 H14V 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C14B H14N 0.9800 . ? C14B H14O 0.9800 . ? C14B H14P 0.9800 . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C14C H14I 0.9800 . ? C143 C144 1.545(13) . ? C143 H14J 0.9900 . ? C143 H14K 0.9900 . ? C144 C145 1.388(13) . ? C144 C149 1.415(13) . ? C145 C146 1.381(14) . ? C145 H14L 0.9500 . ? C146 C147 1.390(14) . ? C146 C150 1.533(14) . ? C147 C148 1.380(13) . ? C147 H14M 0.9500 . ? C148 C149 1.424(12) . ? C148 C154 1.514(12) . ? C150 C153 1.493(15) . ? C150 C15B 1.528(16) . ? C150 C151 1.537(16) . ? C150 C152 1.554(17) . ? C150 C15A 1.556(16) . ? C151 H15Z 0.9800 . ? C151 H16Y 0.9800 . ? C151 H16Z 0.9800 . ? C152 H17W 0.9800 . ? C152 H17X 0.9800 . ? C152 H17Y 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C15A H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C15B H15G 0.9800 . ? C153 H15H 0.9800 . ? C153 H15I 0.9800 . ? C153 H15J 0.9800 . ? C154 H15K 0.9900 . ? C154 H15L 0.9900 . ? C155 H15M 0.9800 . ? C155 H15N 0.9800 . ? C155 H15O 0.9800 . ? C156 C157 1.511(15) . ? C156 H15P 0.9900 . ? C156 H15Q 0.9900 . ? C157 H15R 0.9900 . ? C157 H15S 0.9900 . ? C158 H15T 0.9800 . ? C158 H15U 0.9800 . ? C158 H15V 0.9800 . ? C159 H15W 0.9800 . ? C159 H15X 0.9800 . ? C159 H15Y 0.9800 . ? C160 C161 1.510(14) . ? C160 H16A 0.9900 . ? C160 H16B 0.9900 . ? C161 H16C 0.9900 . ? C161 H16D 0.9900 . ? C162 H16E 0.9800 . ? C162 H16F 0.9800 . ? C162 H16G 0.9800 . ? C163 H16H 0.9800 . ? C163 H16I 0.9800 . ? C163 H16J 0.9800 . ? C164 C165 1.47(3) . ? C164 H16K 0.9900 . ? C164 H16L 0.9900 . ? C165 H16M 0.9900 . ? C165 H16X 0.9900 . ? C167 H16N 0.9800 . ? C167 H16O 0.9800 . ? C167 H16P 0.9800 . ? C168 C169 1.503(18) . ? C168 H16Q 0.9900 . ? C168 H16R 0.9900 . ? C169 H16S 0.9900 . ? C169 H16T 0.9900 . ? C170 H17A 0.9800 . ? C170 H17B 0.9800 . ? C170 H17C 0.9800 . ? C171 H17D 0.9800 . ? C171 H17E 0.9800 . ? C171 H17F 0.9800 . ? C172 C173 1.489(16) . ? C172 H17G 0.9900 . ? C172 H17H 0.9900 . ? C173 H17I 0.9900 . ? C173 H17J 0.9900 . ? C174 H17K 0.9800 . ? C174 H17L 0.9800 . ? C174 H17M 0.9800 . ? C175 C176 1.29(3) . ? C175 H17N 0.9800 . ? C175 H17O 0.9800 . ? C175 H17P 0.9800 . ? C176 C177 1.38(2) . ? C176 H17Q 0.9500 . ? C177 C178 1.44(3) . ? C177 H17R 0.9900 . ? C177 H17S 0.9900 . ? C178 C179 1.43(3) . ? C178 H17T 0.9900 . ? C178 H17U 0.9900 . ? C179 C180 1.39(3) . ? C179 H17V 0.9500 . ? C180 H18A 0.9800 . ? C180 H18B 0.9800 . ? C180 H18C 0.9800 . ? C181 C182 1.407(15) . ? C181 H18D 0.9800 . ? C181 H18E 0.9800 . ? C181 H18F 0.9800 . ? C182 C183 1.394(14) . ? C182 H18G 0.9500 . ? C183 C184 1.482(16) . ? C183 H18H 0.9900 . ? C183 H18I 0.9900 . ? C184 C185 1.411(15) . ? C184 H18J 0.9900 . ? C184 H18K 0.9900 . ? C185 C186 1.377(15) . ? C185 H18L 0.9500 . ? C186 H18M 0.9800 . ? C186 H18N 0.9800 . ? C186 H18O 0.9800 . ? C166 H16U 0.9800 . ? C166 H16V 0.9800 . ? C166 H16W 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 O16 Bi4 O8 108.0(2) . . ? O16 Bi4 O15 71.8(2) . . ? O8 Bi4 O15 72.7(2) . . ? O16 Bi4 O9 72.3(2) . . ? O8 Bi4 O9 88.1(2) . . ? O15 Bi4 O9 130.9(2) . . ? O16 Bi4 Bi2 37.29(16) . . ? O8 Bi4 Bi2 82.24(17) . . ? O15 Bi4 Bi2 36.53(16) . . ? O9 Bi4 Bi2 97.65(16) . . ? O16 Bi4 Bi1 98.66(16) . . ? O8 Bi4 Bi1 45.35(16) . . ? O15 Bi4 Bi1 32.43(16) . . ? O9 Bi4 Bi1 128.39(17) . . ? Bi2 Bi4 Bi1 61.419(10) . . ? O16 Bi4 Bi3 31.86(16) . . ? O8 Bi4 Bi3 99.45(17) . . ? O15 Bi4 Bi3 97.66(16) . . ? O9 Bi4 Bi3 40.52(16) . . ? Bi2 Bi4 Bi3 61.184(9) . . ? Bi1 Bi4 Bi3 115.014(13) . . ? C1 O1 Bi1 121.5(5) . . ? O1 C1 C2 119.5(8) . . ? O1 C1 C6 121.7(8) . . ? C2 C1 C6 118.8(8) . . ? O15 Bi2 O3 109.0(2) . . ? O15 Bi2 O16 71.5(2) . . ? O3 Bi2 O16 72.9(2) . . ? O15 Bi2 O2 72.3(2) . . ? O3 Bi2 O2 88.0(2) . . ? O16 Bi2 O2 130.2(2) . . ? O15 Bi2 Bi4 37.20(16) . . ? O3 Bi2 Bi4 83.02(17) . . ? O16 Bi2 Bi4 36.41(16) . . ? O2 Bi2 Bi4 97.18(16) . . ? O15 Bi2 Bi3 98.92(16) . . ? O3 Bi2 Bi3 44.91(16) . . ? O16 Bi2 Bi3 32.91(16) . . ? O2 Bi2 Bi3 127.50(16) . . ? Bi4 Bi2 Bi3 61.781(10) . . ? O15 Bi2 Bi1 32.16(16) . . ? O3 Bi2 Bi1 100.71(16) . . ? O16 Bi2 Bi1 97.95(16) . . ? O2 Bi2 Bi1 40.11(16) . . ? Bi4 Bi2 Bi1 61.593(10) . . ? Bi3 Bi2 Bi1 115.676(13) . . ? C17 O2 Bi2 151.6(6) . . ? C17 O2 Bi1 103.6(5) . . ? Bi2 O2 Bi1 103.4(2) . . ? C3 C2 C1 119.2(8) . . ? C3 C2 C77 117.5(8) . . ? C1 C2 C77 123.3(8) . . ? O14 Bi1 O15 83.1(2) . . ? O14 Bi1 O1 83.3(2) . . ? O15 Bi1 O1 92.2(2) . . ? O14 Bi1 O2 149.1(2) . . ? O15 Bi1 O2 68.8(2) . . ? O1 Bi1 O2 85.1(2) . . ? O14 Bi1 O8 88.8(2) . . ? O15 Bi1 O8 64.5(2) . . ? O1 Bi1 O8 156.3(2) . . ? O2 Bi1 O8 90.4(2) . . ? O14 Bi1 Bi2 114.74(17) . . ? O15 Bi1 Bi2 32.29(16) . . ? O1 Bi1 Bi2 89.42(16) . . ? O2 Bi1 Bi2 36.49(14) . . ? O8 Bi1 Bi2 73.58(14) . . ? O14 Bi1 Bi4 72.14(17) . . ? O15 Bi1 Bi4 33.14(16) . . ? O1 Bi1 Bi4 120.56(16) . . ? O2 Bi1 Bi4 89.55(14) . . ? O8 Bi1 Bi4 35.93(15) . . ? Bi2 Bi1 Bi4 56.988(10) . . ? C28 O3 Bi2 127.2(5) . . ? C28 O3 Bi3 127.7(5) . . ? Bi2 O3 Bi3 98.6(2) . . ? C4 C3 C2 122.6(9) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? O4 Bi3 O16 83.0(2) . . ? O4 Bi3 O10 82.7(2) . . ? O16 Bi3 O10 91.8(2) . . ? O4 Bi3 O9 148.8(2) . . ? O16 Bi3 O9 68.7(2) . . ? O10 Bi3 O9 85.5(2) . . ? O4 Bi3 O3 87.4(2) . . ? O16 Bi3 O3 65.8(2) . . ? O10 Bi3 O3 156.5(2) . . ? O9 Bi3 O3 92.3(2) . . ? O4 Bi3 Bi2 71.22(17) . . ? O16 Bi3 Bi2 33.69(16) . . ? O10 Bi3 Bi2 120.01(16) . . ? O9 Bi3 Bi2 90.35(14) . . ? O3 Bi3 Bi2 36.50(13) . . ? O4 Bi3 Bi4 114.31(17) . . ? O16 Bi3 Bi4 31.87(16) . . ? O10 Bi3 Bi4 90.17(16) . . ? O9 Bi3 Bi4 36.85(15) . . ? O3 Bi3 Bi4 74.56(14) . . ? Bi2 Bi3 Bi4 57.035(10) . . ? C39 O4 Bi3 122.8(5) . . ? C5 C4 C3 116.6(9) . . ? C5 C4 C7 122.2(9) . . ? C3 C4 C7 121.0(9) . . ? C50 O5 H5A 109.5 . . ? C4 C5 C6 123.4(10) . . ? C4 C5 H5B 118.3 . . ? C6 C5 H5B 118.3 . . ? C61 O6 H6A 109.5 . . ? C5 C6 C1 119.3(9) . . ? C5 C6 C11 119.8(9) . . ? C1 C6 C11 120.9(8) . . ? C72 O7 H7A 109.5 . . ? C8 C7 C4 110.3(8) . . ? C8 C7 C9 109.6(8) . . ? C4 C7 C9 112.1(8) . . ? C8 C7 C10 108.0(9) . . ? C4 C7 C10 109.0(8) . . ? C9 C7 C10 107.7(8) . . ? C78 O8 Bi4 127.6(6) . . ? C78 O8 Bi1 126.1(5) . . ? Bi4 O8 Bi1 98.7(2) . . ? 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 . . ? C94 O9 Bi4 153.1(6) . . ? C94 O9 Bi3 101.3(5) . . ? Bi4 O9 Bi3 102.6(2) . . ? 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 . . ? C105 O10 Bi3 121.5(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 . . ? C116 O11 H11A 109.5 . . ? C12 C11 C6 112.1(8) . . ? C12 C11 H11B 109.2 . . ? C6 C11 H11B 109.2 . . ? C12 C11 H11C 109.2 . . ? C6 C11 H11C 109.2 . . ? H11B C11 H11C 107.9 . . ? C127 O12 H12A 109.5 . . ? C17 C12 C13 118.9(9) . . ? C17 C12 C11 120.0(9) . . ? C13 C12 C11 121.1(9) . . ? C14 C13 C12 122.5(9) . . ? C14 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C138 O13 H13B 109.5 . . ? C13 C14 C15 117.2(9) . . ? C13 C14 C18 120.8(9) . . ? C15 C14 C18 121.8(9) . . ? C149 O14 Bi1 122.1(6) . . ? C16 C15 C14 122.5(9) . . ? C16 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? Bi1 O15 Bi2 115.5(3) . . ? Bi1 O15 Bi4 114.4(3) . . ? Bi2 O15 Bi4 106.3(2) . . ? C15 C16 C17 118.3(9) . . ? C15 C16 C22 122.1(9) . . ? C17 C16 C22 119.5(9) . . ? Bi3 O16 Bi4 116.3(3) . . ? Bi3 O16 Bi2 113.4(3) . . ? Bi4 O16 Bi2 106.3(3) . . ? O2 C17 C12 120.7(9) . . ? O2 C17 C16 118.3(8) . . ? C12 C17 C16 120.7(9) . . ? C157 O17 C158 112.7(8) . . ? C20 C18 C21 108.4(10) . . ? C20 C18 C19 108.6(10) . . ? C21 C18 C19 109.1(10) . . ? C20 C18 C14 112.0(9) . . ? C21 C18 C14 108.6(9) . . ? C19 C18 C14 110.1(9) . . ? C155 O18 C156 110.5(8) . . ? 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 . . ? C160 O19 C159 111.6(8) . . ? 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 . . ? C162 O20 C161 113.2(8) . . ? 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 . . ? C164 O21 C163 116.0(12) . . ? C16 C22 C23 109.5(8) . . ? C16 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? C16 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C165 O22 C166 118(3) . . ? C24 C23 C28 119.7(9) . . ? C24 C23 C22 117.0(8) . . ? C28 C23 C22 122.9(8) . . ? C168 O23 C167 112.5(10) . . ? C25 C24 C23 123.2(10) . . ? C25 C24 H24A 118.4 . . ? C23 C24 H24A 118.4 . . ? C170 O24 C169 113.3(11) . . ? C24 C25 C26 116.8(10) . . ? C24 C25 C29 120.7(10) . . ? C26 C25 C29 122.6(10) . . ? C172 O25 C171 109.6(9) . . ? C25 C26 C27 122.8(9) . . ? C25 C26 H26A 118.6 . . ? C27 C26 H26A 118.6 . . ? C174 O26 C173 113.3(10) . . ? C26 C27 C28 118.8(9) . . ? C26 C27 C33 120.0(9) . . ? C28 C27 C33 121.2(8) . . ? O3 C28 C23 121.9(8) . . ? O3 C28 C27 119.2(8) . . ? C23 C28 C27 118.7(8) . . ? C31 C29 C30 109.3(10) . . ? C31 C29 C32 109.6(13) . . ? C30 C29 C32 108.3(12) . . ? C31 C29 C25 109.1(11) . . ? C30 C29 C25 110.6(10) . . ? C32 C29 C25 110.0(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 . . ? C27 C33 C34 111.9(8) . . ? C27 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? C27 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C39 118.4(9) . . ? C35 C34 C33 119.5(9) . . ? C39 C34 C33 122.2(9) . . ? C36 C35 C34 122.0(9) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C35 C36 C37 117.9(9) . . ? C35 C36 C40 122.9(9) . . ? C37 C36 C40 119.2(9) . . ? C38 C37 C36 122.7(9) . . ? C38 C37 H37A 118.7 . . ? C36 C37 H37A 118.7 . . ? C37 C38 C39 118.6(9) . . ? C37 C38 C44 120.9(9) . . ? C39 C38 C44 120.5(8) . . ? O4 C39 C34 121.9(9) . . ? O4 C39 C38 117.5(8) . . ? C34 C39 C38 120.4(9) . . ? C41 C40 C43 107.1(10) . . ? C41 C40 C42 111.0(10) . . ? C43 C40 C42 108.4(11) . . ? C41 C40 C36 112.7(9) . . ? C43 C40 C36 109.6(9) . . ? C42 C40 C36 108.0(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 111.8(8) . . ? C38 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? C38 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C50 118.3(9) . . ? C46 C45 C44 121.9(9) . . ? C50 C45 C44 118.5(8) . . ? C45 C46 C47 122.7(9) . . ? C45 C46 H46A 118.7 . . ? C47 C46 H46A 118.7 . . ? C46 C47 C48 116.4(9) . . ? C46 C47 C51 119.8(9) . . ? C48 C47 C51 123.7(9) . . ? C49 C48 C47 122.4(9) . . ? C49 C48 H48A 118.8 . . ? C47 C48 H48A 118.8 . . ? C48 C49 C50 119.7(10) . . ? C48 C49 C55 118.3(9) . . ? C50 C49 C55 121.8(9) . . ? C49 C50 O5 122.4(9) . . ? C49 C50 C45 120.2(10) . . ? O5 C50 C45 117.2(9) . . ? C53 C51 C52 107.9(10) . . ? C53 C51 C47 109.8(9) . . ? C52 C51 C47 110.0(9) . . ? C53 C51 C54 107.8(10) . . ? C52 C51 C54 109.5(11) . . ? C47 C51 C54 111.8(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 . . ? C56 C55 C49 113.9(8) . . ? C56 C55 H55A 108.8 . . ? C49 C55 H55A 108.8 . . ? C56 C55 H55B 108.8 . . ? C49 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? C57 C56 C61 119.3(9) . . ? C57 C56 C55 119.6(9) . . ? C61 C56 C55 121.0(9) . . ? C58 C57 C56 122.2(10) . . ? C58 C57 H57A 118.9 . . ? C56 C57 H57A 118.9 . . ? C57 C58 C59 117.4(10) . . ? C57 C58 C62 120.9(10) . . ? C59 C58 C62 121.6(9) . . ? C60 C59 C58 122.1(10) . . ? C60 C59 H59A 119.0 . . ? C58 C59 H59A 119.0 . . ? C61 C60 C59 119.2(10) . . ? C61 C60 C66 120.9(9) . . ? C59 C60 C66 119.9(9) . . ? O6 C61 C60 124.2(9) . . ? O6 C61 C56 115.9(9) . . ? C60 C61 C56 119.8(9) . . ? C64 C62 C65 109.7(11) . . ? C64 C62 C63 108.1(11) . . ? C65 C62 C63 109.6(12) . . ? C64 C62 C58 113.1(10) . . ? C65 C62 C58 106.8(10) . . ? C63 C62 C58 109.4(10) . . ? 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 . . ? C60 C66 C67 113.1(8) . . ? C60 C66 H66A 109.0 . . ? C67 C66 H66A 109.0 . . ? C60 C66 H66B 109.0 . . ? C67 C66 H66B 109.0 . . ? H66A C66 H66B 107.8 . . ? C68 C67 C72 118.4(9) . . ? C68 C67 C66 121.4(8) . . ? C72 C67 C66 120.2(8) . . ? C69 C68 C67 123.1(9) . . ? C69 C68 H68A 118.5 . . ? C67 C68 H68A 118.5 . . ? C68 C69 C70 116.2(9) . . ? C68 C69 C73 124.7(9) . . ? C70 C69 C73 119.1(9) . . ? C69 C70 C71 123.7(9) . . ? C69 C70 H70A 118.2 . . ? C71 C70 H70A 118.2 . . ? C72 C71 C70 114.9(9) . . ? C72 C71 C77 124.6(10) . . ? C70 C71 C77 120.2(9) . . ? O7 C72 C71 118.8(9) . . ? O7 C72 C67 117.6(8) . . ? C71 C72 C67 123.5(9) . . ? C74 C73 C69 112.1(9) . . ? C74 C73 C76 107.6(9) . . ? C69 C73 C76 109.8(9) . . ? C74 C73 C75 108.0(9) . . ? C69 C73 C75 109.4(9) . . ? C76 C73 C75 109.9(9) . . ? 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 . . ? C71 C77 C2 114.5(8) . . ? C71 C77 H77A 108.6 . . ? C2 C77 H77A 108.6 . . ? C71 C77 H77B 108.6 . . ? C2 C77 H77B 108.6 . . ? H77A C77 H77B 107.6 . . ? O8 C78 C83 121.2(8) . . ? O8 C78 C79 119.6(8) . . ? C83 C78 C79 119.2(9) . . ? C80 C79 C78 119.7(9) . . ? C80 C79 C154 120.1(9) . . ? C78 C79 C154 120.1(8) . . ? C79 C80 C81 122.3(9) . . ? C79 C80 H80A 118.9 . . ? C81 C80 H80A 118.9 . . ? C80 C81 C82 117.0(9) . . ? C80 C81 C84 120.4(9) . . ? C82 C81 C84 122.6(9) . . ? C83 C82 C81 122.8(9) . . ? C83 C82 H82A 118.6 . . ? C81 C82 H82A 118.6 . . ? C82 C83 C78 119.0(9) . . ? C82 C83 C88 118.6(9) . . ? C78 C83 C88 122.3(8) . . ? C86 C84 C81 109.3(10) . . ? C86 C84 C87 107.3(10) . . ? C81 C84 C87 113.3(9) . . ? C86 C84 C85 108.7(10) . . ? C81 C84 C85 109.5(9) . . ? C87 C84 C85 108.6(10) . . ? 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 C83 110.3(8) . . ? C89 C88 H88A 109.6 . . ? C83 C88 H88A 109.6 . . ? C89 C88 H88B 109.6 . . ? C83 C88 H88B 109.6 . . ? H88A C88 H88B 108.1 . . ? C94 C89 C90 118.3(9) . . ? C94 C89 C88 120.3(8) . . ? C90 C89 C88 121.4(9) . . ? C91 C90 C89 123.0(10) . . ? C91 C90 H90A 118.5 . . ? C89 C90 H90A 118.5 . . ? C90 C91 C92 116.5(9) . . ? C90 C91 C95 122.3(10) . . ? C92 C91 C95 121.2(9) . . ? C93 C92 C91 124.0(9) . . ? C93 C92 H92A 118.0 . . ? C91 C92 H92A 118.0 . . ? C92 C93 C94 115.8(9) . . ? C92 C93 C99 121.7(8) . . ? C94 C93 C99 122.4(9) . . ? O9 C94 C89 120.0(8) . . ? O9 C94 C93 117.2(8) . . ? C89 C94 C93 122.4(9) . . ? C98 C95 C91 109.2(9) . . ? C98 C95 C96 108.1(11) . . ? C91 C95 C96 113.0(9) . . ? C98 C95 C97 108.2(10) . . ? C91 C95 C97 109.3(9) . . ? C96 C95 C97 109.0(11) . . ? C95 C96 H96A 109.5 . . ? 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 H97A 109.5 . . ? C95 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C95 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 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 . . ? C93 C99 C100 112.4(8) . . ? C93 C99 H99A 109.1 . . ? C100 C99 H99A 109.1 . . ? C93 C99 H99B 109.1 . . ? C100 C99 H99B 109.1 . . ? H99A C99 H99B 107.9 . . ? C101 C100 C105 119.4(8) . . ? C101 C100 C99 118.4(8) . . ? C105 C100 C99 122.2(8) . . ? C100 C101 C102 120.9(8) . . ? C100 C101 H10D 119.6 . . ? C102 C101 H10D 119.6 . . ? C103 C102 C101 116.6(9) . . ? C103 C102 C106 124.0(8) . . ? C101 C102 C106 119.2(8) . . ? C104 C103 C102 124.8(9) . . ? C104 C103 H10E 117.6 . . ? C102 C103 H10E 117.6 . . ? C103 C104 C105 116.9(9) . . ? C103 C104 C110 120.1(8) . . ? C105 C104 C110 123.0(8) . . ? O10 C105 C100 120.2(8) . . ? O10 C105 C104 118.4(8) . . ? C100 C105 C104 121.3(8) . . ? C109 C106 C107 109.1(9) . . ? C109 C106 C108 107.2(8) . . ? C107 C106 C108 108.9(9) . . ? C109 C106 C102 109.0(8) . . ? C107 C106 C102 111.8(8) . . ? C108 C106 C102 110.7(8) . . ? C106 C107 H10F 109.5 . . ? C106 C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C106 C107 H10H 109.5 . . ? H10F C107 H10H 109.5 . . ? H10G C107 H10H 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 H10L 109.5 . . ? C106 C109 H10M 109.5 . . ? H10L C109 H10M 109.5 . . ? C106 C109 H10N 109.5 . . ? H10L C109 H10N 109.5 . . ? H10M C109 H10N 109.5 . . ? C104 C110 C111 113.6(8) . . ? C104 C110 H11D 108.9 . . ? C111 C110 H11D 108.9 . . ? C104 C110 H11E 108.9 . . ? C111 C110 H11E 108.9 . . ? H11D C110 H11E 107.7 . . ? C112 C111 C116 117.8(9) . . ? C112 C111 C110 121.5(8) . . ? C116 C111 C110 120.7(8) . . ? C111 C112 C113 121.2(9) . . ? C111 C112 H11F 119.4 . . ? C113 C112 H11F 119.4 . . ? C114 C113 C112 117.3(9) . . ? C114 C113 C117 125.8(10) . . ? C112 C113 C117 116.9(9) . . ? C113 C114 C115 123.8(10) . . ? C113 C114 H11G 118.1 . . ? C115 C114 H11G 118.1 . . ? C116 C115 C114 118.4(9) . . ? C116 C115 C121 120.8(9) . . ? C114 C115 C121 120.6(9) . . ? C115 C116 O11 119.4(9) . . ? C115 C116 C111 121.1(9) . . ? O11 C116 C111 119.3(9) . . ? C113 C117 C119 111.1(9) . . ? C113 C117 C120 111.1(9) . . ? C119 C117 C120 108.6(9) . . ? C113 C117 C118 110.1(9) . . ? C119 C117 C118 109.0(10) . . ? C120 C117 C118 106.9(9) . . ? C117 C118 H11H 109.5 . . ? C117 C118 H11I 109.5 . . ? H11H C118 H11I 109.5 . . ? C117 C118 H11J 109.5 . . ? H11H C118 H11J 109.5 . . ? H11I C118 H11J 109.5 . . ? C117 C119 H11K 109.5 . . ? C117 C119 H11L 109.5 . . ? H11K C119 H11L 109.5 . . ? C117 C119 H11M 109.5 . . ? H11K C119 H11M 109.5 . . ? H11L C119 H11M 109.5 . . ? C117 C120 H12B 109.5 . . ? C117 C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C117 C120 H12D 109.5 . . ? H12B C120 H12D 109.5 . . ? H12C C120 H12D 109.5 . . ? C122 C121 C115 111.6(8) . . ? C122 C121 H12E 109.3 . . ? C115 C121 H12E 109.3 . . ? C122 C121 H12F 109.3 . . ? C115 C121 H12F 109.3 . . ? H12E C121 H12F 108.0 . . ? C123 C122 C127 117.9(9) . . ? C123 C122 C121 120.0(9) . . ? C127 C122 C121 122.2(9) . . ? C122 C123 C124 122.9(9) . . ? C122 C123 H12G 118.6 . . ? C124 C123 H12G 118.6 . . ? C123 C124 C125 115.9(9) . . ? C123 C124 C128 123.1(9) . . ? C125 C124 C128 121.0(9) . . ? C126 C125 C124 123.1(10) . . ? C126 C125 H12H 118.4 . . ? C124 C125 H12H 118.4 . . ? C125 C126 C127 119.0(9) . . ? C125 C126 C132 121.2(9) . . ? C127 C126 C132 119.7(9) . . ? O12 C127 C126 117.9(9) . . ? O12 C127 C122 120.9(9) . . ? C126 C127 C122 121.2(9) . . ? C129 C128 C124 110.2(9) . . ? C129 C128 C130 107.5(10) . . ? C124 C128 C130 111.5(9) . . ? C129 C128 C131 108.9(10) . . ? C124 C128 C131 109.6(9) . . ? C130 C128 C131 109.1(10) . . ? C128 C129 H12I 109.5 . . ? C128 C129 H12J 109.5 . . ? H12I C129 H12J 109.5 . . ? C128 C129 H12K 109.5 . . ? H12I C129 H12K 109.5 . . ? H12J C129 H12K 109.5 . . ? C128 C130 H13C 109.5 . . ? C128 C130 H13D 109.5 . . ? H13C C130 H13D 109.5 . . ? C128 C130 H13E 109.5 . . ? H13C C130 H13E 109.5 . . ? H13D C130 H13E 109.5 . . ? C128 C131 H13F 109.5 . . ? C128 C131 H13G 109.5 . . ? H13F C131 H13G 109.5 . . ? C128 C131 H13H 109.5 . . ? H13F C131 H13H 109.5 . . ? H13G C131 H13H 109.5 . . ? C126 C132 C133 113.7(8) . . ? C126 C132 H13I 108.8 . . ? C133 C132 H13I 108.8 . . ? C126 C132 H13J 108.8 . . ? C133 C132 H13J 108.8 . . ? H13I C132 H13J 107.7 . . ? C134 C133 C138 118.6(9) . . ? C134 C133 C132 120.3(9) . . ? C138 C133 C132 120.9(9) . . ? C133 C134 C135 123.4(10) . . ? C133 C134 H13K 118.3 . . ? C135 C134 H13K 118.3 . . ? C136 C135 C134 116.1(9) . . ? C136 C135 C139 122.8(9) . . ? C134 C135 C139 121.0(9) . . ? C135 C136 C137 124.3(9) . . ? C135 C136 H13L 117.9 . . ? C137 C136 H13L 117.9 . . ? C136 C137 C138 116.3(9) . . ? C136 C137 C143 122.3(9) . . ? C138 C137 C143 120.9(9) . . ? O13 C138 C133 122.9(9) . . ? O13 C138 C137 116.5(8) . . ? C133 C138 C137 120.4(9) . . ? C14C C139 C141 140(2) . . ? C14C C139 C14A 109.9(10) . . ? C141 C139 C14A 51.7(15) . . ? C14C C139 C142 51.5(13) . . ? C141 C139 C142 109.0(13) . . ? C14A C139 C142 130.0(18) . . ? C14C C139 C135 111.1(11) . . ? C141 C139 C135 108.8(19) . . ? C14A C139 C135 112.5(11) . . ? C142 C139 C135 117.5(16) . . ? C14C C139 C140 59.7(13) . . ? C141 C139 C140 107.1(13) . . ? C14A C139 C140 56.5(14) . . ? C142 C139 C140 106.7(13) . . ? C135 C139 C140 107.2(17) . . ? C14C C139 C14B 108.0(10) . . ? C141 C139 C14B 59.0(14) . . ? C14A C139 C14B 107.0(9) . . ? C142 C139 C14B 57.2(13) . . ? C135 C139 C14B 108.2(11) . . ? C140 C139 C14B 144.6(19) . . ? C139 C140 H14A 109.5 . . ? C139 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? C139 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? C139 C141 H14Q 109.5 . . ? C139 C141 H14R 109.5 . . ? H14Q C141 H14R 109.5 . . ? C139 C141 H14S 109.5 . . ? H14Q C141 H14S 109.5 . . ? H14R C141 H14S 109.5 . . ? C139 C142 H14T 109.5 . . ? C139 C142 H14U 109.5 . . ? H14T C142 H14U 109.5 . . ? C139 C142 H14V 109.5 . . ? H14T C142 H14V 109.5 . . ? H14U C142 H14V 109.5 . . ? C139 C14A H14D 109.5 . . ? C139 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C139 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C139 C14B H14N 109.5 . . ? C139 C14B H14O 109.5 . . ? H14N C14B H14O 109.5 . . ? C139 C14B H14P 109.5 . . ? H14N C14B H14P 109.5 . . ? H14O C14B H14P 109.5 . . ? C139 C14C H14G 109.5 . . ? C139 C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? C139 C14C H14I 109.5 . . ? H14G C14C H14I 109.5 . . ? H14H C14C H14I 109.5 . . ? C137 C143 C144 112.7(8) . . ? C137 C143 H14J 109.0 . . ? C144 C143 H14J 109.0 . . ? C137 C143 H14K 109.0 . . ? C144 C143 H14K 109.0 . . ? H14J C143 H14K 107.8 . . ? C145 C144 C149 119.7(9) . . ? C145 C144 C143 120.4(8) . . ? C149 C144 C143 119.8(8) . . ? C146 C145 C144 122.6(9) . . ? C146 C145 H14L 118.7 . . ? C144 C145 H14L 118.7 . . ? C145 C146 C147 117.8(9) . . ? C145 C146 C150 120.6(9) . . ? C147 C146 C150 121.2(9) . . ? C148 C147 C146 121.7(9) . . ? C148 C147 H14M 119.2 . . ? C146 C147 H14M 119.2 . . ? C147 C148 C149 120.6(9) . . ? C147 C148 C154 118.8(8) . . ? C149 C148 C154 120.5(8) . . ? O14 C149 C144 119.8(8) . . ? O14 C149 C148 122.8(8) . . ? C144 C149 C148 117.4(8) . . ? C153 C150 C15B 115.4(15) . . ? C153 C150 C146 112.3(9) . . ? C15B C150 C146 112.0(13) . . ? C153 C150 C151 118.6(14) . . ? C15B C150 C151 80.8(16) . . ? C146 C150 C151 114.1(13) . . ? C153 C150 C152 97.9(15) . . ? C15B C150 C152 26.3(12) . . ? C146 C150 C152 104.8(14) . . ? C151 C150 C152 106.6(16) . . ? C153 C150 C15A 103.0(13) . . ? C15B C150 C15A 106.7(15) . . ? C146 C150 C15A 106.3(12) . . ? C151 C150 C15A 26.2(11) . . ? C152 C150 C15A 131.9(18) . . ? C150 C151 H15Z 109.5 . . ? C150 C151 H16Y 109.5 . . ? H15Z C151 H16Y 109.5 . . ? C150 C151 H16Z 109.5 . . ? H15Z C151 H16Z 109.5 . . ? H16Y C151 H16Z 109.5 . . ? C150 C152 H17W 109.5 . . ? C150 C152 H17X 109.5 . . ? H17W C152 H17X 109.5 . . ? C150 C152 H17Y 109.5 . . ? H17W C152 H17Y 109.5 . . ? H17X C152 H17Y 109.5 . . ? C150 C15A H15B 109.5 . . ? C150 C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C150 C15A H15D 109.5 . . ? H15B C15A H15D 109.5 . . ? H15C C15A H15D 109.5 . . ? C150 C15B H15E 109.5 . . ? C150 C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C150 C15B H15G 109.5 . . ? H15E C15B H15G 109.5 . . ? H15F C15B H15G 109.5 . . ? C150 C153 H15H 109.5 . . ? C150 C153 H15I 109.5 . . ? H15H C153 H15I 109.5 . . ? C150 C153 H15J 109.5 . . ? H15H C153 H15J 109.5 . . ? H15I C153 H15J 109.5 . . ? C79 C154 C148 112.9(7) . . ? C79 C154 H15K 109.0 . . ? C148 C154 H15K 109.0 . . ? C79 C154 H15L 109.0 . . ? C148 C154 H15L 109.0 . . ? H15K C154 H15L 107.8 . . ? O18 C155 H15M 109.5 . . ? O18 C155 H15N 109.5 . . ? H15M C155 H15N 109.5 . . ? O18 C155 H15O 109.5 . . ? H15M C155 H15O 109.5 . . ? H15N C155 H15O 109.5 . . ? O18 C156 C157 107.8(8) . . ? O18 C156 H15P 110.2 . . ? C157 C156 H15P 110.2 . . ? O18 C156 H15Q 110.2 . . ? C157 C156 H15Q 110.2 . . ? H15P C156 H15Q 108.5 . . ? O17 C157 C156 113.1(9) . . ? O17 C157 H15R 109.0 . . ? C156 C157 H15R 109.0 . . ? O17 C157 H15S 109.0 . . ? C156 C157 H15S 109.0 . . ? H15R C157 H15S 107.8 . . ? O17 C158 H15T 109.5 . . ? O17 C158 H15U 109.5 . . ? H15T C158 H15U 109.5 . . ? O17 C158 H15V 109.5 . . ? H15T C158 H15V 109.5 . . ? H15U C158 H15V 109.5 . . ? O19 C159 H15W 109.5 . . ? O19 C159 H15X 109.5 . . ? H15W C159 H15X 109.5 . . ? O19 C159 H15Y 109.5 . . ? H15W C159 H15Y 109.5 . . ? H15X C159 H15Y 109.5 . . ? O19 C160 C161 108.8(8) . . ? O19 C160 H16A 109.9 . . ? C161 C160 H16A 109.9 . . ? O19 C160 H16B 109.9 . . ? C161 C160 H16B 109.9 . . ? H16A C160 H16B 108.3 . . ? O20 C161 C160 112.6(8) . . ? O20 C161 H16C 109.1 . . ? C160 C161 H16C 109.1 . . ? O20 C161 H16D 109.1 . . ? C160 C161 H16D 109.1 . . ? H16C C161 H16D 107.8 . . ? O20 C162 H16E 109.5 . . ? O20 C162 H16F 109.5 . . ? H16E C162 H16F 109.5 . . ? O20 C162 H16G 109.5 . . ? H16E C162 H16G 109.5 . . ? H16F C162 H16G 109.5 . . ? O21 C163 H16H 109.5 . . ? O21 C163 H16I 109.5 . . ? H16H C163 H16I 109.5 . . ? O21 C163 H16J 109.5 . . ? H16H C163 H16J 109.5 . . ? H16I C163 H16J 109.5 . . ? O21 C164 C165 115.8(16) . . ? O21 C164 H16K 108.3 . . ? C165 C164 H16K 108.3 . . ? O21 C164 H16L 108.3 . . ? C165 C164 H16L 108.3 . . ? H16K C164 H16L 107.4 . . ? O22 C165 C164 119(2) . . ? O22 C165 H16M 107.7 . . ? C164 C165 H16M 107.7 . . ? O22 C165 H16X 107.7 . . ? C164 C165 H16X 107.7 . . ? H16M C165 H16X 107.1 . . ? O23 C167 H16N 109.5 . . ? O23 C167 H16O 109.5 . . ? H16N C167 H16O 109.5 . . ? O23 C167 H16P 109.5 . . ? H16N C167 H16P 109.5 . . ? H16O C167 H16P 109.5 . . ? O23 C168 C169 108.8(11) . . ? O23 C168 H16Q 109.9 . . ? C169 C168 H16Q 109.9 . . ? O23 C168 H16R 109.9 . . ? C169 C168 H16R 109.9 . . ? H16Q C168 H16R 108.3 . . ? O24 C169 C168 107.2(11) . . ? O24 C169 H16S 110.3 . . ? C168 C169 H16S 110.3 . . ? O24 C169 H16T 110.3 . . ? C168 C169 H16T 110.3 . . ? H16S C169 H16T 108.5 . . ? O24 C170 H17A 109.5 . . ? O24 C170 H17B 109.5 . . ? H17A C170 H17B 109.5 . . ? O24 C170 H17C 109.5 . . ? H17A C170 H17C 109.5 . . ? H17B C170 H17C 109.5 . . ? O25 C171 H17D 109.5 . . ? O25 C171 H17E 109.5 . . ? H17D C171 H17E 109.5 . . ? O25 C171 H17F 109.5 . . ? H17D C171 H17F 109.5 . . ? H17E C171 H17F 109.5 . . ? O25 C172 C173 107.6(9) . . ? O25 C172 H17G 110.2 . . ? C173 C172 H17G 110.2 . . ? O25 C172 H17H 110.2 . . ? C173 C172 H17H 110.2 . . ? H17G C172 H17H 108.5 . . ? O26 C173 C172 111.7(10) . . ? O26 C173 H17I 109.3 . . ? C172 C173 H17I 109.3 . . ? O26 C173 H17J 109.3 . . ? C172 C173 H17J 109.3 . . ? H17I C173 H17J 107.9 . . ? O26 C174 H17K 109.5 . . ? O26 C174 H17L 109.5 . . ? H17K C174 H17L 109.5 . . ? O26 C174 H17M 109.5 . . ? H17K C174 H17M 109.5 . . ? H17L C174 H17M 109.5 . . ? C176 C175 H17N 109.5 . . ? C176 C175 H17O 109.5 . . ? H17N C175 H17O 109.5 . . ? C176 C175 H17P 109.5 . . ? H17N C175 H17P 109.5 . . ? H17O C175 H17P 109.5 . . ? C175 C176 C177 117.4(19) . . ? C175 C176 H17Q 121.3 . . ? C177 C176 H17Q 121.3 . . ? C176 C177 C178 107.7(17) . . ? C176 C177 H17R 110.2 . . ? C178 C177 H17R 110.2 . . ? C176 C177 H17S 110.2 . . ? C178 C177 H17S 110.2 . . ? H17R C177 H17S 108.5 . . ? C179 C178 C177 108.0(17) . . ? C179 C178 H17T 110.1 . . ? C177 C178 H17T 110.1 . . ? C179 C178 H17U 110.1 . . ? C177 C178 H17U 110.1 . . ? H17T C178 H17U 108.4 . . ? C180 C179 C178 112.3(17) . . ? C180 C179 H17V 123.8 . . ? C178 C179 H17V 123.8 . . ? C179 C180 H18A 109.5 . . ? C179 C180 H18B 109.5 . . ? H18A C180 H18B 109.5 . . ? C179 C180 H18C 109.5 . . ? H18A C180 H18C 109.5 . . ? H18B C180 H18C 109.5 . . ? C182 C181 H18D 109.5 . . ? C182 C181 H18E 109.5 . . ? H18D C181 H18E 109.5 . . ? C182 C181 H18F 109.5 . . ? H18D C181 H18F 109.5 . . ? H18E C181 H18F 109.5 . . ? C183 C182 C181 114.0(10) . . ? C183 C182 H18G 123.0 . . ? C181 C182 H18G 123.0 . . ? C182 C183 C184 109.4(10) . . ? C182 C183 H18H 109.8 . . ? C184 C183 H18H 109.8 . . ? C182 C183 H18I 109.8 . . ? C184 C183 H18I 109.8 . . ? H18H C183 H18I 108.2 . . ? C185 C184 C183 110.0(10) . . ? C185 C184 H18J 109.7 . . ? C183 C184 H18J 109.7 . . ? C185 C184 H18K 109.7 . . ? C183 C184 H18K 109.7 . . ? H18J C184 H18K 108.2 . . ? C186 C185 C184 115.4(11) . . ? C186 C185 H18L 122.3 . . ? C184 C185 H18L 122.3 . . ? C185 C186 H18M 109.5 . . ? C185 C186 H18N 109.5 . . ? H18M C186 H18N 109.5 . . ? C185 C186 H18O 109.5 . . ? H18M C186 H18O 109.5 . . ? H18N C186 H18O 109.5 . . ? O22 C166 H16U 109.5 . . ? O22 C166 H16V 109.5 . . ? H16U C166 H16V 109.5 . . ? O22 C166 H16W 109.5 . . ? H16U C166 H16W 109.5 . . ? H16V C166 H16W 109.5 . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.342 _refine_diff_density_min -1.955 _refine_diff_density_rms 0.219 # Attachment '7.CIF' data_tcu174m _database_code_depnum_ccdc_archive 'CCDC 721520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C112 H80 Bi8 O20' _chemical_formula_sum 'C112 H80 Bi8 O20' _chemical_formula_weight 3417.60 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 m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 30.287(6) _cell_length_b 21.769(4) _cell_length_c 22.432(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14790(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 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6304 _exptl_absorpt_coefficient_mu 9.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.183 _exptl_absorpt_correction_T_max 0.265 _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 97048 _diffrn_reflns_av_R_equivalents 0.1938 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.25 _reflns_number_total 10925 _reflns_number_gt 7525 _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^)+(0.0911P)^2^+2043.5316P] 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 10925 _refine_ls_number_parameters 313 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1569 _refine_ls_R_factor_gt 0.1159 _refine_ls_wR_factor_ref 0.2805 _refine_ls_wR_factor_gt 0.2590 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.028 _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 -0.27970(6) -0.7500 0.20198(7) 0.0319(4) Uani 1 2 d S . . C1 C -0.2400(11) -0.6610(14) 0.1227(12) 0.045(9) Uiso 1 1 d D . . C2 C -0.2603(9) -0.6061(12) 0.1203(11) 0.024(7) Uiso 1 1 d D . . C3 C -0.2721(12) -0.5858(15) 0.0629(14) 0.053(10) Uiso 1 1 d D . . H26A H -0.2889 -0.5500 0.0576 0.063 Uiso 1 1 calc R . . C4 C -0.2589(14) -0.6187(17) 0.0170(15) 0.077(13) Uiso 1 1 d D . . H1CA H -0.2588 -0.5984 -0.0200 0.093 Uiso 1 1 calc R . . C5 C -0.2439(13) -0.6850(16) 0.0160(15) 0.073(13) Uiso 1 1 d D . . H31A H -0.2465 -0.7136 -0.0152 0.088 Uiso 1 1 calc R . . C6 C -0.2256(9) -0.6937(12) 0.0712(11) 0.026(7) Uiso 1 1 d D . . C7 C -0.2735(12) -0.5710(18) 0.1800(17) 0.053(10) Uiso 1 1 d . . . H10A H -0.2517 -0.5831 0.2100 0.064 Uiso 1 1 calc R . . H10C H -0.2687 -0.5272 0.1722 0.064 Uiso 1 1 calc R . . C8 C -0.3161(12) -0.5758(17) 0.2083(17) 0.046(9) Uiso 1 1 d . . . C9 C -0.3496(11) -0.5348(16) 0.1917(16) 0.043(9) Uiso 1 1 d . . . H87A H -0.3448 -0.5085 0.1591 0.052 Uiso 1 1 calc R . . C10 C -0.3888(14) -0.532(2) 0.2209(19) 0.064(12) Uiso 1 1 d . . . H74A H -0.4097 -0.5023 0.2087 0.077 Uiso 1 1 calc R . . C11 C -0.3983(15) -0.567(2) 0.264(2) 0.068(12) Uiso 1 1 d . . . H35A H -0.4264 -0.5649 0.2815 0.082 Uiso 1 1 calc R . . C12 C -0.3649(9) -0.6097(13) 0.2856(13) 0.024(7) Uiso 1 1 d . . . C13 C -0.3271(12) -0.6210(17) 0.2587(17) 0.047(9) Uiso 1 1 d . . . C14 C -0.3742(10) -0.6497(14) 0.3419(12) 0.033(8) Uiso 1 1 d D . . H42A H -0.3565 -0.6874 0.3406 0.039 Uiso 1 1 calc R . . H42B H -0.4055 -0.6613 0.3432 0.039 Uiso 1 1 calc R . . C15 C -0.3618(8) -0.6108(12) 0.3990(11) 0.021(6) Uiso 1 1 d D . . C16 C -0.3929(10) -0.5753(15) 0.4235(15) 0.052(10) Uiso 1 1 d D . . H68A H -0.4219 -0.5753 0.4086 0.062 Uiso 1 1 calc R . . C17 C -0.3813(10) -0.5384(16) 0.4716(16) 0.059(11) Uiso 1 1 d D . . H21A H -0.4030 -0.5171 0.4933 0.070 Uiso 1 1 calc R . . C18 C -0.3395(9) -0.5340(13) 0.4859(13) 0.033(8) Uiso 1 1 d D . . H96A H -0.3316 -0.5011 0.5109 0.039 Uiso 1 1 calc R . . C19 C -0.3033(9) -0.5757(15) 0.4669(15) 0.049(9) Uiso 1 1 d D . . C20 C -0.3186(8) -0.6159(12) 0.4242(11) 0.024(7) Uiso 1 1 d D . . C21 C -0.2612(9) -0.5742(14) 0.4828(13) 0.031(7) Uiso 1 1 d D . . H3A H -0.2523 -0.5309 0.4824 0.037 Uiso 1 1 calc R . . H3B H -0.2445 -0.5944 0.4509 0.037 Uiso 1 1 calc R . . C22 C -0.2424(11) -0.6042(15) 0.5481(15) 0.036(8) Uiso 1 1 d . . . C23 C -0.2556(10) -0.5785(15) 0.5989(14) 0.034(8) Uiso 1 1 d . . . H16A H -0.2731 -0.5429 0.5990 0.040 Uiso 1 1 calc R . . C24 C -0.2416(12) -0.6080(17) 0.6545(17) 0.050(10) Uiso 1 1 d . . . H25A H -0.2469 -0.5885 0.6913 0.060 Uiso 1 1 calc R . . C25 C -0.2210(9) -0.6637(12) 0.6528(12) 0.020(6) Uiso 1 1 d . . . H13A H -0.2149 -0.6845 0.6885 0.023 Uiso 1 1 calc R . . C26 C -0.2075(12) -0.6932(17) 0.5915(17) 0.048(9) Uiso 1 1 d . . . C27 C -0.2233(10) -0.6614(15) 0.5431(15) 0.035(8) Uiso 1 1 d . . . C28 C -0.1800(17) -0.7500 0.585(2) 0.049(13) Uiso 1 2 d S . . H19A H -0.1568 -0.7500 0.6156 0.059 Uiso 1 2 calc SR . . H19B H -0.1657 -0.7500 0.5460 0.059 Uiso 1 2 calc SR . . C29 C -0.2004(16) -0.7500 0.065(2) 0.039(12) Uiso 1 2 d S . . H1JA H -0.1863 -0.7500 0.0256 0.047 Uiso 1 2 calc SR . . H1JB H -0.1769 -0.7500 0.0949 0.047 Uiso 1 2 calc SR . . C30 C -0.0633(13) -0.6643(18) 0.4426(18) 0.054(10) Uiso 1 1 d . . . C31 C -0.0223(13) -0.6962(19) 0.4395(18) 0.056(10) Uiso 1 1 d . . . C32 C 0.012(2) -0.677(3) 0.483(3) 0.14(3) Uiso 1 1 d . . . H54A H 0.0375 -0.7012 0.4879 0.171 Uiso 1 1 calc R . . C33 C 0.007(3) -0.619(4) 0.518(3) 0.15(3) Uiso 1 1 d . . . H1BA H 0.0310 -0.6034 0.5392 0.182 Uiso 1 1 calc R . . C34 C -0.036(2) -0.587(3) 0.519(3) 0.11(2) Uiso 1 1 d . . . H2BA H -0.0397 -0.5489 0.5371 0.136 Uiso 1 1 calc R . . C35 C -0.0714(14) -0.619(2) 0.4906(19) 0.063(11) Uiso 1 1 d . . . C36 C -0.1198(16) -0.594(2) 0.497(2) 0.088(15) Uiso 1 1 d . . . H28A H -0.1256 -0.5883 0.5398 0.105 Uiso 1 1 calc R . . H28B H -0.1399 -0.6260 0.4830 0.105 Uiso 1 1 calc R . . C37 C -0.1329(15) -0.531(2) 0.464(2) 0.072(13) Uiso 1 1 d . . . C38 C -0.1154(15) -0.474(2) 0.492(2) 0.071(13) Uiso 1 1 d . . . H89A H -0.0973 -0.4734 0.5259 0.085 Uiso 1 1 calc R . . C39 C -0.1280(18) -0.428(3) 0.464(3) 0.099(17) Uiso 1 1 d . . . H88A H -0.1219 -0.3921 0.4850 0.118 Uiso 1 1 calc R . . C40 C -0.149(2) -0.415(4) 0.410(3) 0.14(2) Uiso 1 1 d . . . H47A H -0.1523 -0.3759 0.3933 0.162 Uiso 1 1 calc R . . C41 C -0.1648(13) -0.4740(18) 0.3819(17) 0.052(10) Uiso 1 1 d . . . C42 C -0.1535(13) -0.527(2) 0.4108(19) 0.059(11) Uiso 1 1 d . . . C43 C -0.1923(15) -0.475(2) 0.3316(16) 0.081(14) Uiso 1 1 d D . . H40A H -0.2113 -0.4385 0.3334 0.097 Uiso 1 1 calc R . . H40D H -0.2115 -0.5110 0.3347 0.097 Uiso 1 1 calc R . . C44 C -0.1696(16) -0.4762(17) 0.2682(16) 0.090(16) Uiso 1 1 d D . . C45 C -0.1544(17) -0.4214(17) 0.2486(19) 0.107(19) Uiso 1 1 d D . . H50A H -0.1542 -0.3861 0.2728 0.128 Uiso 1 1 calc R . . C46 C -0.1389(18) -0.4210(18) 0.1901(19) 0.108(19) Uiso 1 1 d D . . H42C H -0.1331 -0.3830 0.1717 0.129 Uiso 1 1 calc R . . C47 C -0.1323(18) -0.4715(18) 0.1599(19) 0.111(19) Uiso 1 1 d D . . H1GA H -0.1168 -0.4677 0.1238 0.133 Uiso 1 1 calc R . . C48 C -0.1469(15) -0.5348(17) 0.1771(17) 0.080(14) Uiso 1 1 d D . . C49 C -0.1623(14) -0.5303(15) 0.2342(15) 0.070(12) Uiso 1 1 d D . . C50 C -0.1361(18) -0.587(2) 0.150(2) 0.11(2) Uiso 1 1 d D . . H70A H -0.1468 -0.5814 0.1095 0.136 Uiso 1 1 calc R . . H70C H -0.1560 -0.6172 0.1684 0.136 Uiso 1 1 calc R . . C51 C -0.0923(19) -0.623(3) 0.143(3) 0.096(17) Uiso 1 1 d . . . C52 C -0.059(3) -0.606(4) 0.099(4) 0.15(3) Uiso 1 1 d . . . H5BA H -0.0681 -0.5758 0.0714 0.183 Uiso 1 1 calc R . . C53 C -0.022(2) -0.623(3) 0.092(3) 0.13(2) Uiso 1 1 d . . . H3BA H -0.0034 -0.6052 0.0641 0.159 Uiso 1 1 calc R . . C54 C -0.0081(19) -0.674(3) 0.129(3) 0.099(17) Uiso 1 1 d . . . H4BA H 0.0193 -0.6923 0.1216 0.118 Uiso 1 1 calc R . . C55 C -0.0351(17) -0.698(2) 0.179(2) 0.087(15) Uiso 1 1 d . . . C56 C -0.0798(15) -0.661(2) 0.188(2) 0.071(13) Uiso 1 1 d . . . C57 C -0.027(2) -0.7500 0.218(3) 0.077(19) Uiso 1 2 d S . . H39A H 0.0036 -0.7500 0.2327 0.092 Uiso 1 2 calc SR . . H39B H -0.0472 -0.7500 0.2521 0.092 Uiso 1 2 calc SR . . C58 C -0.014(2) -0.7500 0.408(3) 0.065(17) Uiso 1 2 d S . . H1KA H 0.0164 -0.7500 0.3946 0.078 Uiso 1 2 calc SR . . H1KB H -0.0331 -0.7500 0.3722 0.078 Uiso 1 2 calc SR . . O1 O -0.2288(7) -0.6874(9) 0.1755(9) 0.033(5) Uiso 1 1 d . . . O2 O -0.2965(6) -0.6638(9) 0.2692(9) 0.029(5) Uiso 1 1 d . . . O3 O -0.2916(6) -0.6635(9) 0.4079(9) 0.032(5) Uiso 1 1 d . . . O4 O -0.2146(6) -0.6865(8) 0.4882(8) 0.022(4) Uiso 1 1 d . . . O5 O -0.0960(6) -0.6803(9) 0.4047(9) 0.031(5) Uiso 1 1 d . . . O6 O -0.1669(8) -0.5840(12) 0.3909(12) 0.056(7) Uiso 1 1 d . . . O7 O -0.1754(9) -0.5824(13) 0.2677(12) 0.064(8) Uiso 1 1 d . . . O8 O -0.1049(7) -0.6758(10) 0.2363(10) 0.039(6) Uiso 1 1 d . . . O9 O -0.2374(8) -0.7500 0.2760(11) 0.016(6) Uiso 1 2 d S . . O10 O -0.2317(7) -0.7500 0.3883(10) 0.011(5) Uiso 1 2 d S . . O11 O -0.1605(5) -0.6914(7) 0.3259(8) 0.016(4) Uiso 1 1 d . . . Bi2 Bi -0.24050(4) -0.66326(4) 0.33304(5) 0.0222(3) Uani 1 1 d . . . Bi3 Bi -0.26810(6) -0.7500 0.46926(7) 0.0250(4) Uani 1 2 d S . . Bi4 Bi -0.14995(5) -0.7500 0.40997(7) 0.0248(4) Uani 1 2 d S . . Bi5 Bi -0.12015(4) -0.61183(5) 0.32288(6) 0.0361(4) Uani 1 1 d . . . Bi6 Bi -0.15853(6) -0.7500 0.24089(7) 0.0298(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0380(10) 0.0416(10) 0.0160(9) 0.000 -0.0048(8) 0.000 Bi2 0.0341(6) 0.0078(5) 0.0246(6) 0.0027(4) -0.0005(5) 0.0006(4) Bi3 0.0411(10) 0.0170(8) 0.0167(8) 0.000 0.0024(7) 0.000 Bi4 0.0358(10) 0.0119(8) 0.0266(9) 0.000 -0.0055(8) 0.000 Bi5 0.0349(7) 0.0160(6) 0.0574(9) 0.0061(6) 0.0009(6) -0.0061(5) Bi6 0.0346(10) 0.0328(10) 0.0221(9) 0.000 0.0017(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O9 2.10(2) . ? Bi1 O1 2.14(2) . ? Bi1 O1 2.14(2) 8_545 ? Bi1 O2 2.46(2) . ? Bi1 O2 2.46(2) 8_545 ? Bi1 Bi2 3.6902(18) . ? Bi1 Bi2 3.6902(18) 8_545 ? C1 C2 1.34(3) . ? C1 O1 1.36(3) . ? C1 C6 1.43(3) . ? C2 C3 1.41(3) . ? C2 C7 1.59(4) . ? C3 C4 1.32(3) . ? C3 H26A 0.9400 . ? C4 C5 1.51(4) . ? C4 H1CA 0.9400 . ? C5 C6 1.37(3) . ? C5 H31A 0.9400 . ? C6 C29 1.45(3) . ? C7 C8 1.44(5) . ? C7 H10A 0.9800 . ? C7 H10C 0.9800 . ? C8 C9 1.40(5) . ? C8 C13 1.53(5) . ? C9 C10 1.36(5) . ? C9 H87A 0.9400 . ? C10 C11 1.26(6) . ? C10 H74A 0.9400 . ? C11 C12 1.47(5) . ? C11 H35A 0.9400 . ? C12 C13 1.32(4) . ? C12 C14 1.56(4) . ? C13 O2 1.34(4) . ? C14 C15 1.58(3) . ? C14 H42A 0.9800 . ? C14 H42B 0.9800 . ? C15 C16 1.34(3) . ? C15 C20 1.43(3) . ? C16 C17 1.39(3) . ? C16 H68A 0.9400 . ? C17 C18 1.31(3) . ? C17 H21A 0.9400 . ? C18 C19 1.49(3) . ? C18 H96A 0.9400 . ? C19 C21 1.33(4) . ? C19 C20 1.38(3) . ? C20 O3 1.37(3) . ? C21 C22 1.70(4) . ? C21 H3A 0.9800 . ? C21 H3B 0.9800 . ? C22 C23 1.33(4) . ? C22 C27 1.38(5) . ? C23 C24 1.47(5) . ? C23 H16A 0.9400 . ? C24 C25 1.36(4) . ? C24 H25A 0.9400 . ? C25 C26 1.57(4) . ? C25 H13A 0.9400 . ? C26 C27 1.37(5) . ? C26 C28 1.50(5) . ? C27 O4 1.37(4) . ? C28 C26 1.50(5) 8_545 ? C28 H19A 0.9800 . ? C28 H19B 0.9800 . ? C29 C6 1.45(3) 8_545 ? C29 H1JA 0.9800 . ? C29 H1JB 0.9800 . ? C30 O5 1.35(4) . ? C30 C31 1.43(5) . ? C30 C35 1.48(6) . ? C31 C58 1.39(5) . ? C31 C32 1.48(8) . ? C32 C33 1.49(9) . ? C32 H54A 0.9400 . ? C33 C34 1.47(9) . ? C33 H1BA 0.9400 . ? C34 C35 1.42(7) . ? C34 H2BA 0.9400 . ? C35 C36 1.57(6) . ? C36 C37 1.61(6) . ? C36 H28A 0.9800 . ? C36 H28B 0.9800 . ? C37 C42 1.35(6) . ? C37 C38 1.48(6) . ? C38 C39 1.24(6) . ? C38 H89A 0.9400 . ? C39 C40 1.39(8) . ? C39 H88A 0.9400 . ? C40 C41 1.50(8) . ? C40 H47A 0.9400 . ? C41 C42 1.36(5) . ? C41 C43 1.40(5) . ? C42 O6 1.39(5) . ? C43 C44 1.58(3) . ? C43 H40A 0.9800 . ? C43 H40D 0.9800 . ? C44 C45 1.35(3) . ? C44 C49 1.42(3) . ? C45 C46 1.39(3) . ? C45 H50A 0.9400 . ? C46 C47 1.31(3) . ? C46 H42C 0.9400 . ? C47 C48 1.50(4) . ? C47 H1GA 0.9400 . ? C48 C50 1.32(4) . ? C48 C49 1.37(3) . ? C49 O7 1.42(4) . ? C50 C51 1.55(7) . ? C50 H70A 0.9800 . ? C50 H70C 0.9800 . ? C51 C56 1.38(7) . ? C51 C52 1.45(8) . ? C52 C53 1.18(9) . ? C52 H5BA 0.9400 . ? C53 C54 1.45(8) . ? C53 H3BA 0.9400 . ? C54 C55 1.47(7) . ? C54 H4BA 0.9400 . ? C55 C57 1.46(6) . ? C55 C56 1.58(6) . ? C56 O8 1.36(5) . ? C57 C55 1.46(6) 8_545 ? C57 H39A 0.9800 . ? C57 H39B 0.9800 . ? C58 C31 1.39(5) 8_545 ? C58 H1KA 0.9800 . ? C58 H1KB 0.9800 . ? O2 Bi2 2.220(19) . ? O3 Bi2 2.28(2) . ? O3 Bi3 2.44(2) . ? O4 Bi3 2.171(18) . ? O5 Bi4 2.23(2) . ? O5 Bi5 2.47(2) . ? O6 Bi5 2.17(3) . ? O7 Bi5 2.18(3) . ? O8 Bi6 2.29(2) . ? O8 Bi5 2.43(2) . ? O9 Bi2 2.283(14) . ? O9 Bi2 2.283(14) 8_545 ? O9 Bi6 2.52(2) . ? O10 Bi3 2.13(2) . ? O10 Bi2 2.274(13) 8_545 ? O10 Bi2 2.274(13) . ? O10 Bi4 2.52(2) . ? O11 Bi5 2.121(16) . ? O11 Bi6 2.296(17) . ? O11 Bi4 2.298(17) . ? O11 Bi2 2.504(16) . ? Bi2 Bi3 3.6880(17) . ? Bi3 O4 2.171(18) 8_545 ? Bi3 O3 2.44(2) 8_545 ? Bi3 Bi2 3.6880(17) 8_545 ? Bi4 O5 2.23(2) 8_545 ? Bi4 O11 2.298(17) 8_545 ? Bi4 Bi5 3.6984(16) 8_545 ? Bi4 Bi5 3.6984(16) . ? Bi6 O8 2.29(2) 8_545 ? Bi6 O11 2.296(17) 8_545 ? 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 O9 Bi1 O1 77.3(7) . . ? O9 Bi1 O1 77.3(7) . 8_545 ? O1 Bi1 O1 79.1(11) . 8_545 ? O9 Bi1 O2 69.0(6) . . ? O1 Bi1 O2 80.4(7) . . ? O1 Bi1 O2 143.5(7) 8_545 . ? O9 Bi1 O2 69.0(6) . 8_545 ? O1 Bi1 O2 143.5(7) . 8_545 ? O1 Bi1 O2 80.4(7) 8_545 8_545 ? O2 Bi1 O2 99.5(9) . 8_545 ? O9 Bi1 Bi2 34.2(3) . . ? O1 Bi1 Bi2 70.3(6) . . ? O1 Bi1 Bi2 108.4(5) 8_545 . ? O2 Bi1 Bi2 35.7(4) . . ? O2 Bi1 Bi2 88.2(5) 8_545 . ? O9 Bi1 Bi2 34.2(3) . 8_545 ? O1 Bi1 Bi2 108.4(6) . 8_545 ? O1 Bi1 Bi2 70.3(6) 8_545 8_545 ? O2 Bi1 Bi2 88.2(5) . 8_545 ? O2 Bi1 Bi2 35.7(4) 8_545 8_545 ? Bi2 Bi1 Bi2 61.55(4) . 8_545 ? C2 C1 O1 122(2) . . ? C2 C1 C6 123(2) . . ? O1 C1 C6 115(2) . . ? C1 C2 C3 116(2) . . ? C1 C2 C7 120(2) . . ? C3 C2 C7 124(3) . . ? C4 C3 C2 118(3) . . ? C4 C3 H26A 121.0 . . ? C2 C3 H26A 121.0 . . ? C3 C4 C5 128(3) . . ? C3 C4 H1CA 115.8 . . ? C5 C4 H1CA 115.8 . . ? C6 C5 C4 104(2) . . ? C6 C5 H31A 128.0 . . ? C4 C5 H31A 128.1 . . ? C5 C6 C1 123(2) . . ? C5 C6 C29 104(3) . . ? C1 C6 C29 131(3) . . ? C8 C7 C2 124(3) . . ? C8 C7 H10A 106.3 . . ? C2 C7 H10A 106.3 . . ? C8 C7 H10C 106.3 . . ? C2 C7 H10C 106.3 . . ? H10A C7 H10C 106.4 . . ? C9 C8 C7 119(3) . . ? C9 C8 C13 116(3) . . ? C7 C8 C13 125(3) . . ? C10 C9 C8 122(4) . . ? C10 C9 H87A 118.7 . . ? C8 C9 H87A 118.8 . . ? C11 C10 C9 123(5) . . ? C11 C10 H74A 118.7 . . ? C9 C10 H74A 118.7 . . ? C10 C11 C12 119(4) . . ? C10 C11 H35A 120.5 . . ? C12 C11 H35A 120.5 . . ? C13 C12 C11 124(3) . . ? C13 C12 C14 115(3) . . ? C11 C12 C14 120(3) . . ? C12 C13 O2 131(3) . . ? C12 C13 C8 114(3) . . ? O2 C13 C8 115(3) . . ? C12 C14 C15 108(2) . . ? C12 C14 H42A 110.0 . . ? C15 C14 H42A 110.0 . . ? C12 C14 H42B 110.0 . . ? C15 C14 H42B 110.0 . . ? H42A C14 H42B 108.4 . . ? C16 C15 C20 122(2) . . ? C16 C15 C14 118(2) . . ? C20 C15 C14 120(2) . . ? C15 C16 C17 119(3) . . ? C15 C16 H68A 120.7 . . ? C17 C16 H68A 120.7 . . ? C18 C17 C16 118(3) . . ? C18 C17 H21A 120.8 . . ? C16 C17 H21A 120.8 . . ? C17 C18 C19 127(3) . . ? C17 C18 H96A 116.6 . . ? C19 C18 H96A 116.6 . . ? C21 C19 C20 122(3) . . ? C21 C19 C18 128(3) . . ? C20 C19 C18 110(2) . . ? O3 C20 C19 118(2) . . ? O3 C20 C15 120(2) . . ? C19 C20 C15 122(2) . . ? C19 C21 C22 123(3) . . ? C19 C21 H3A 106.6 . . ? C22 C21 H3A 106.6 . . ? C19 C21 H3B 106.6 . . ? C22 C21 H3B 106.6 . . ? H3A C21 H3B 106.5 . . ? C23 C22 C27 125(3) . . ? C23 C22 C21 118(3) . . ? C27 C22 C21 115(3) . . ? C22 C23 C24 117(3) . . ? C22 C23 H16A 121.3 . . ? C24 C23 H16A 121.3 . . ? C25 C24 C23 120(3) . . ? C25 C24 H25A 120.1 . . ? C23 C24 H25A 120.1 . . ? C24 C25 C26 121(3) . . ? C24 C25 H13A 119.7 . . ? C26 C25 H13A 119.7 . . ? C27 C26 C28 122(4) . . ? C27 C26 C25 113(3) . . ? C28 C26 C25 125(3) . . ? O4 C27 C26 116(3) . . ? O4 C27 C22 121(3) . . ? C26 C27 C22 122(3) . . ? C26 C28 C26 111(4) . 8_545 ? C26 C28 H19A 109.4 . . ? C26 C28 H19A 109.4 8_545 . ? C26 C28 H19B 109.4 . . ? C26 C28 H19B 109.4 8_545 . ? H19A C28 H19B 108.0 . . ? C6 C29 C6 115(4) 8_545 . ? C6 C29 H1JA 108.4 8_545 . ? C6 C29 H1JA 108.4 . . ? C6 C29 H1JB 108.4 8_545 . ? C6 C29 H1JB 108.4 . . ? H1JA C29 H1JB 107.5 . . ? O5 C30 C31 119(3) . . ? O5 C30 C35 121(3) . . ? C31 C30 C35 120(4) . . ? C58 C31 C30 126(4) . . ? C58 C31 C32 117(5) . . ? C30 C31 C32 116(4) . . ? C31 C32 C33 121(7) . . ? C31 C32 H54A 119.7 . . ? C33 C32 H54A 119.7 . . ? C34 C33 C32 120(7) . . ? C34 C33 H1BA 120.0 . . ? C32 C33 H1BA 120.0 . . ? C35 C34 C33 115(6) . . ? C35 C34 H2BA 122.3 . . ? C33 C34 H2BA 122.3 . . ? C34 C35 C30 121(4) . . ? C34 C35 C36 120(4) . . ? C30 C35 C36 117(4) . . ? C35 C36 C37 119(4) . . ? C35 C36 H28A 107.6 . . ? C37 C36 H28A 107.6 . . ? C35 C36 H28B 107.6 . . ? C37 C36 H28B 107.6 . . ? H28A C36 H28B 107.1 . . ? C42 C37 C38 119(4) . . ? C42 C37 C36 126(4) . . ? C38 C37 C36 115(4) . . ? C39 C38 C37 110(5) . . ? C39 C38 H89A 124.9 . . ? C37 C38 H89A 124.9 . . ? C38 C39 C40 138(7) . . ? C38 C39 H88A 111.0 . . ? C40 C39 H88A 111.0 . . ? C39 C40 C41 109(6) . . ? C39 C40 H47A 125.2 . . ? C41 C40 H47A 125.3 . . ? C42 C41 C43 122(4) . . ? C42 C41 C40 116(4) . . ? C43 C41 C40 122(4) . . ? C37 C42 C41 127(4) . . ? C37 C42 O6 111(4) . . ? C41 C42 O6 122(4) . . ? C41 C43 C44 118(4) . . ? C41 C43 H40A 107.8 . . ? C44 C43 H40A 107.8 . . ? C41 C43 H40D 107.8 . . ? C44 C43 H40D 107.8 . . ? H40A C43 H40D 107.2 . . ? C45 C44 C49 120(3) . . ? C45 C44 C43 115(3) . . ? C49 C44 C43 124(3) . . ? C44 C45 C46 115(3) . . ? C44 C45 H50A 122.3 . . ? C46 C45 H50A 122.3 . . ? C47 C46 C45 122(3) . . ? C47 C46 H42C 118.9 . . ? C45 C46 H42C 118.9 . . ? C46 C47 C48 127(3) . . ? C46 C47 H1GA 116.7 . . ? C48 C47 H1GA 116.7 . . ? C50 C48 C49 125(3) . . ? C50 C48 C47 127(3) . . ? C49 C48 C47 106(3) . . ? C48 C49 O7 122(3) . . ? C48 C49 C44 128(3) . . ? O7 C49 C44 110(3) . . ? C48 C50 C51 134(5) . . ? C48 C50 H70A 103.7 . . ? C51 C50 H70A 103.7 . . ? C48 C50 H70C 103.7 . . ? C51 C50 H70C 103.7 . . ? H70A C50 H70C 105.4 . . ? C56 C51 C52 118(6) . . ? C56 C51 C50 117(5) . . ? C52 C51 C50 123(6) . . ? C53 C52 C51 131(9) . . ? C53 C52 H5BA 114.5 . . ? C51 C52 H5BA 114.5 . . ? C52 C53 C54 117(8) . . ? C52 C53 H3BA 121.6 . . ? C54 C53 H3BA 121.6 . . ? C53 C54 C55 122(6) . . ? C53 C54 H4BA 118.8 . . ? C55 C54 H4BA 118.8 . . ? C57 C55 C54 129(5) . . ? C57 C55 C56 117(5) . . ? C54 C55 C56 114(5) . . ? O8 C56 C51 125(4) . . ? O8 C56 C55 118(4) . . ? C51 C56 C55 116(4) . . ? C55 C57 C55 102(6) 8_545 . ? C55 C57 H39A 111.3 8_545 . ? C55 C57 H39A 111.3 . . ? C55 C57 H39B 111.3 8_545 . ? C55 C57 H39B 111.3 . . ? H39A C57 H39B 109.2 . . ? C31 C58 C31 115(6) . 8_545 ? C31 C58 H1KA 108.5 . . ? C31 C58 H1KA 108.5 8_545 . ? C31 C58 H1KB 108.5 . . ? C31 C58 H1KB 108.5 8_545 . ? H1KA C58 H1KB 107.5 . . ? C1 O1 Bi1 109.4(19) . . ? C13 O2 Bi2 130(2) . . ? C13 O2 Bi1 125(2) . . ? Bi2 O2 Bi1 104.0(8) . . ? C20 O3 Bi2 126.8(17) . . ? C20 O3 Bi3 127.5(17) . . ? Bi2 O3 Bi3 102.6(8) . . ? C27 O4 Bi3 106.7(17) . . ? C30 O5 Bi4 133(2) . . ? C30 O5 Bi5 122(2) . . ? Bi4 O5 Bi5 103.4(8) . . ? C42 O6 Bi5 107(2) . . ? C49 O7 Bi5 109(2) . . ? C56 O8 Bi6 126(2) . . ? C56 O8 Bi5 128(2) . . ? Bi6 O8 Bi5 103.4(8) . . ? Bi1 O9 Bi2 114.7(7) . . ? Bi1 O9 Bi2 114.7(7) . 8_545 ? Bi2 O9 Bi2 111.6(10) . 8_545 ? Bi1 O9 Bi6 109.4(10) . . ? Bi2 O9 Bi6 102.4(7) . . ? Bi2 O9 Bi6 102.4(7) 8_545 . ? Bi3 O10 Bi2 113.9(6) . 8_545 ? Bi3 O10 Bi2 113.9(6) . . ? Bi2 O10 Bi2 112.3(10) 8_545 . ? Bi3 O10 Bi4 110.1(9) . . ? Bi2 O10 Bi4 102.7(6) 8_545 . ? Bi2 O10 Bi4 102.7(6) . . ? Bi5 O11 Bi6 114.3(7) . . ? Bi5 O11 Bi4 113.6(7) . . ? Bi6 O11 Bi4 111.7(7) . . ? Bi5 O11 Bi2 111.1(7) . . ? Bi6 O11 Bi2 102.4(6) . . ? Bi4 O11 Bi2 102.6(6) . . ? O2 Bi2 O10 115.9(7) . . ? O2 Bi2 O9 70.5(8) . . ? O10 Bi2 O9 67.3(7) . . ? O2 Bi2 O3 87.5(7) . . ? O10 Bi2 O3 71.2(7) . . ? O9 Bi2 O3 116.0(7) . . ? O2 Bi2 O11 134.2(6) . . ? O10 Bi2 O11 73.6(7) . . ? O9 Bi2 O11 73.9(7) . . ? O3 Bi2 O11 134.6(6) . . ? O2 Bi2 Bi3 111.0(5) . . ? O10 Bi2 Bi3 31.8(5) . . ? O9 Bi2 Bi3 92.9(5) . . ? O3 Bi2 Bi3 40.2(5) . . ? O11 Bi2 Bi3 98.4(4) . . ? O2 Bi2 Bi1 40.3(5) . . ? O10 Bi2 Bi1 92.7(5) . . ? O9 Bi2 Bi1 31.1(6) . . ? O3 Bi2 Bi1 111.5(5) . . ? O11 Bi2 Bi1 97.8(4) . . ? Bi3 Bi2 Bi1 108.98(4) . . ? O10 Bi3 O4 77.3(7) . . ? O10 Bi3 O4 77.3(7) . 8_545 ? O4 Bi3 O4 79.1(9) . 8_545 ? O10 Bi3 O3 70.7(6) . 8_545 ? O4 Bi3 O3 145.1(7) . 8_545 ? O4 Bi3 O3 80.6(7) 8_545 8_545 ? O10 Bi3 O3 70.7(6) . . ? O4 Bi3 O3 80.6(7) . . ? O4 Bi3 O3 145.1(7) 8_545 . ? O3 Bi3 O3 101.1(10) 8_545 . ? O10 Bi3 Bi2 34.3(3) . 8_545 ? O4 Bi3 Bi2 108.6(5) . 8_545 ? O4 Bi3 Bi2 70.6(5) 8_545 8_545 ? O3 Bi3 Bi2 37.2(5) 8_545 8_545 ? O3 Bi3 Bi2 89.7(5) . 8_545 ? O10 Bi3 Bi2 34.3(3) . . ? O4 Bi3 Bi2 70.6(5) . . ? O4 Bi3 Bi2 108.6(5) 8_545 . ? O3 Bi3 Bi2 89.7(5) 8_545 . ? O3 Bi3 Bi2 37.2(5) . . ? Bi2 Bi3 Bi2 61.59(4) 8_545 . ? O5 Bi4 O5 85.6(10) . 8_545 ? O5 Bi4 O11 115.8(7) . 8_545 ? O5 Bi4 O11 71.4(7) 8_545 8_545 ? O5 Bi4 O11 71.4(7) . . ? O5 Bi4 O11 115.8(7) 8_545 . ? O11 Bi4 O11 67.4(8) 8_545 . ? O5 Bi4 O10 135.1(5) . . ? O5 Bi4 O10 135.1(5) 8_545 . ? O11 Bi4 O10 72.9(6) 8_545 . ? O11 Bi4 O10 72.9(6) . . ? O5 Bi4 Bi5 110.2(5) . 8_545 ? O5 Bi4 Bi5 40.6(5) 8_545 8_545 ? O11 Bi4 Bi5 31.7(4) 8_545 8_545 ? O11 Bi4 Bi5 93.0(4) . 8_545 ? O10 Bi4 Bi5 97.9(3) . 8_545 ? O5 Bi4 Bi5 40.6(5) . . ? O5 Bi4 Bi5 110.2(5) 8_545 . ? O11 Bi4 Bi5 93.0(4) 8_545 . ? O11 Bi4 Bi5 31.7(4) . . ? O10 Bi4 Bi5 97.9(3) . . ? Bi5 Bi4 Bi5 108.83(6) 8_545 . ? O11 Bi5 O6 80.1(8) . . ? O11 Bi5 O7 79.4(9) . . ? O6 Bi5 O7 79.4(10) . . ? O11 Bi5 O8 70.6(7) . . ? O6 Bi5 O8 147.7(8) . . ? O7 Bi5 O8 81.9(9) . . ? O11 Bi5 O5 69.8(7) . . ? O6 Bi5 O5 80.8(8) . . ? O7 Bi5 O5 145.7(9) . . ? O8 Bi5 O5 101.0(7) . . ? O11 Bi5 Bi4 34.7(5) . . ? O6 Bi5 Bi4 72.3(7) . . ? O7 Bi5 Bi4 110.6(7) . . ? O8 Bi5 Bi4 90.2(5) . . ? O5 Bi5 Bi4 36.0(5) . . ? O8 Bi6 O8 89.6(11) 8_545 . ? O8 Bi6 O11 116.6(7) 8_545 . ? O8 Bi6 O11 70.4(7) . . ? O8 Bi6 O11 70.4(7) 8_545 8_545 ? O8 Bi6 O11 116.6(7) . 8_545 ? O11 Bi6 O11 67.5(8) . 8_545 ? O8 Bi6 O9 133.4(6) 8_545 . ? O8 Bi6 O9 133.4(6) . . ? O11 Bi6 O9 73.4(6) . . ? O11 Bi6 O9 73.4(6) 8_545 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.783 _refine_diff_density_min -7.362 _refine_diff_density_rms 0.416 # Attachment '8.CIF' data_tcu219m _database_code_depnum_ccdc_archive 'CCDC 721521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C228 H184 Bi8 N2 O21, 4(C6H6)' _chemical_formula_sum 'C252 H208 Bi8 N2 O21' _chemical_formula_weight 5272.19 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' N N 0.0061 0.0033 '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 19.468(4) _cell_length_b 22.096(4) _cell_length_c 27.093(6) _cell_angle_alpha 92.148(4) _cell_angle_beta 90.463(4) _cell_angle_gamma 112.019(3) _cell_volume 10794(4) _cell_formula_units_Z 2 _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 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5026 _exptl_absorpt_coefficient_mu 6.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3687 _exptl_absorpt_correction_T_max 0.4200 _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 51430 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.1469 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.31 _reflns_number_total 30715 _reflns_number_gt 18277 _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. Most of the benzyl groups were positionally disordered. Geometry of the disordered moities was restrained using SADI or SAME instructions. Due to the high disorder present the carbon atoms in the benzylic groups were modeled using isotropic displacement parameters. Due to the low quality of the crystal one benzyl group was very disordered and could not be located in the densiry map. The Hydrogen atoms of the water molecule O(21) could not be located on density map. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^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 30715 _refine_ls_number_parameters 1775 _refine_ls_number_restraints 605 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.009 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 0.79359(3) 0.66521(3) 0.31700(2) 0.03214(14) Uani 1 1 d U . . O1 O 0.7226(5) 0.7265(5) 0.3309(3) 0.030(2) Uani 1 1 d U . . O2 O 0.8423(5) 0.7000(5) 0.3951(3) 0.040(3) Uani 1 1 d U . . O3 O 0.9576(5) 0.6383(5) 0.3782(4) 0.038(3) Uani 1 1 d U . . O4 O 1.0759(5) 0.7506(5) 0.3443(4) 0.046(3) Uani 1 1 d U . . O5 O 0.9963(5) 0.8462(5) 0.3400(4) 0.037(3) Uani 1 1 d U . . O6 O 0.8785(5) 0.8707(5) 0.2788(3) 0.034(2) Uani 1 1 d U . . O7 O 0.7946(5) 0.8106(5) 0.1880(4) 0.043(3) Uiso 1 1 d U . . O8 O 0.6809(5) 0.7075(5) 0.2243(3) 0.035(3) Uani 1 1 d U . . O9 O 0.7252(5) 0.5736(4) 0.1621(3) 0.035(2) Uani 1 1 d U . . O10 O 0.6792(5) 0.5629(5) 0.2667(4) 0.045(3) Uani 1 1 d U . . O11 O 0.7944(6) 0.5343(6) 0.3086(4) 0.049(3) Uani 1 1 d U . . O12 O 0.8825(5) 0.5345(5) 0.2209(4) 0.042(3) Uani 1 1 d U . . O13 O 1.0010(6) 0.6378(5) 0.1669(4) 0.049(3) Uani 1 1 d U . . O14 O 1.0808(6) 0.7853(6) 0.1662(4) 0.056(3) Uani 1 1 d U . . O15 O 0.9638(6) 0.8203(5) 0.1307(4) 0.049(3) Uani 1 1 d U . . O16 O 0.8458(5) 0.6828(5) 0.1053(4) 0.041(3) Uani 1 1 d U . . O17 O 0.9176(4) 0.7197(5) 0.3139(3) 0.030(2) Uani 1 1 d U . . O18 O 0.8212(4) 0.7434(4) 0.2630(3) 0.024(2) Uiso 1 1 d U . . O19 O 0.8229(5) 0.6197(4) 0.2352(3) 0.030(2) Uani 1 1 d U . . O20 O 0.9206(5) 0.7103(5) 0.1895(3) 0.038(3) Uani 1 1 d U . . O21 O 1.0479(5) 0.7583(5) 0.2552(4) 0.041(3) Uani 1 1 d U . . C1 C 0.6665(8) 0.7256(8) 0.3621(6) 0.036(4) Uani 1 1 d U . . C2 C 0.5925(9) 0.6970(8) 0.3442(6) 0.045(4) Uani 1 1 d U . . C3 C 0.5382(8) 0.7015(9) 0.3739(5) 0.048(5) Uani 1 1 d U . . H3A H 0.4885 0.6805 0.3632 0.057 Uiso 1 1 calc R . . C4 C 0.5529(9) 0.7351(9) 0.4187(6) 0.050(5) Uani 1 1 d U . . C5 C 0.6213(9) 0.7584(9) 0.4358(6) 0.054(5) Uani 1 1 d U . . H5A H 0.6311 0.7787 0.4676 0.065 Uiso 1 1 calc R . . C6 C 0.6805(8) 0.7546(8) 0.4087(5) 0.036(4) Uani 1 1 d U . . C7 C 0.4908(10) 0.7416(10) 0.4520(8) 0.076(6) Uiso 1 1 d U . . H7A H 0.5110 0.7535 0.4858 0.091 Uiso 1 1 calc R . . H7B H 0.4782 0.7778 0.4405 0.091 Uiso 1 1 calc R . . C8 C 0.4212(11) 0.6825(11) 0.4535(8) 0.076(6) Uiso 1 1 d U . . C9 C 0.3633(14) 0.6750(13) 0.4200(10) 0.108(8) Uiso 1 1 d U . . H9A H 0.3697 0.7062 0.3959 0.129 Uiso 1 1 calc R . . C10 C 0.2937(13) 0.6200(12) 0.4218(9) 0.097(8) Uiso 1 1 d U . . H10A H 0.2546 0.6146 0.3994 0.117 Uiso 1 1 calc R . . C11 C 0.2868(15) 0.5759(13) 0.4576(9) 0.106(8) Uiso 1 1 d U . . H11A H 0.2403 0.5424 0.4615 0.127 Uiso 1 1 calc R . . C12 C 0.3435(15) 0.5785(14) 0.4872(10) 0.113(9) Uiso 1 1 d U . . H12A H 0.3373 0.5440 0.5082 0.136 Uiso 1 1 calc R . . C13 C 0.4123(16) 0.6320(14) 0.4876(11) 0.123(10) Uiso 1 1 d U . . H13A H 0.4511 0.6344 0.5095 0.148 Uiso 1 1 calc R . . C14 C 0.7612(8) 0.7767(9) 0.4318(6) 0.050(5) Uani 1 1 d U . . H14A H 0.7975 0.7879 0.4055 0.060 Uiso 1 1 calc R . . H14B H 0.7714 0.8156 0.4537 0.060 Uiso 1 1 calc R . . C15 C 0.7680(7) 0.7227(7) 0.4604(5) 0.028(3) Uiso 1 1 d U . . C16 C 0.7415(8) 0.7101(9) 0.5076(6) 0.047(4) Uani 1 1 d U . . H16A H 0.7208 0.7379 0.5230 0.056 Uiso 1 1 calc R . . C17 C 0.7444(9) 0.6580(8) 0.5330(5) 0.045(4) Uani 1 1 d U . . C18 C 0.7739(10) 0.6173(9) 0.5100(6) 0.057(5) Uani 1 1 d U . . H18A H 0.7731 0.5805 0.5267 0.068 Uiso 1 1 calc R . . C19 C 0.8054(8) 0.6272(9) 0.4628(6) 0.046(4) Uani 1 1 d U . . C20 C 0.8050(8) 0.6844(8) 0.4383(5) 0.038(4) Uani 1 1 d U . . C21 C 0.7106(10) 0.6432(10) 0.5858(7) 0.074(6) Uiso 1 1 d U . . H21A H 0.7481 0.6392 0.6084 0.089 Uiso 1 1 calc R . . H21B H 0.6983 0.6802 0.5980 0.089 Uiso 1 1 calc R . . C22 C 0.6417(12) 0.5814(11) 0.5863(8) 0.080(6) Uiso 1 1 d U . . C23 C 0.5761(12) 0.5741(12) 0.5583(9) 0.091(7) Uiso 1 1 d U . . H23A H 0.5772 0.6081 0.5381 0.109 Uiso 1 1 calc R . . C246 C 1.1086(13) 0.5154(12) 0.2314(8) 0.101(8) Uani 1 1 d U . . H24A H 1.0930 0.4763 0.2503 0.152 Uiso 1 1 calc R . . H24B H 1.1623 0.5345 0.2310 0.152 Uiso 1 1 calc R . . H24C H 1.0890 0.5041 0.1978 0.152 Uiso 1 1 calc R . . C24 C 0.5075(16) 0.5164(15) 0.5597(11) 0.128(10) Uiso 1 1 d U . . H24D H 0.4651 0.5111 0.5405 0.154 Uiso 1 1 calc R . . C25 C 0.5106(18) 0.4701(17) 0.5920(12) 0.143(12) Uiso 1 1 d U . . H25A H 0.4690 0.4309 0.5934 0.172 Uiso 1 1 calc R . . C26 C 0.5778(17) 0.4790(17) 0.6256(12) 0.143(11) Uiso 1 1 d U . . H26A H 0.5767 0.4477 0.6485 0.171 Uiso 1 1 calc R . . C27 C 0.6425(17) 0.5370(16) 0.6204(11) 0.134(11) Uiso 1 1 d U . . H27A H 0.6852 0.5447 0.6402 0.160 Uiso 1 1 calc R . . C28 C 0.8368(9) 0.5793(8) 0.4384(6) 0.046(4) Uani 1 1 d U . . H28A H 0.8046 0.5347 0.4459 0.055 Uiso 1 1 calc R . . H28B H 0.8353 0.5829 0.4025 0.055 Uiso 1 1 calc R . . C29 C 0.9147(9) 0.5905(8) 0.4546(5) 0.039(4) Uani 1 1 d U . . C30 C 0.9320(10) 0.5721(9) 0.4998(7) 0.056(5) Uani 1 1 d U . . H30A H 0.8930 0.5515 0.5211 0.067 Uiso 1 1 calc R . . C31 C 1.0028(11) 0.5821(9) 0.5154(7) 0.055(5) Uani 1 1 d U . . C32 C 1.0608(11) 0.6122(9) 0.4840(6) 0.059(5) Uani 1 1 d U . . H32A H 1.1099 0.6204 0.4943 0.071 Uiso 1 1 calc R . . C33 C 1.0463(9) 0.6309(7) 0.4358(5) 0.037(4) Uani 1 1 d U . . C34 C 0.9755(9) 0.6212(7) 0.4222(5) 0.034(4) Uani 1 1 d U . . C35 C 1.0223(11) 0.5626(11) 0.5668(7) 0.080(6) Uiso 1 1 d U . . H35A H 1.0170 0.5167 0.5650 0.096 Uiso 1 1 calc R . . H35B H 1.0740 0.5893 0.5759 0.096 Uiso 1 1 calc R . . C36 C 0.9719(11) 0.5725(11) 0.6060(8) 0.070(6) Uiso 1 1 d U . . C37 C 0.9109(12) 0.5230(12) 0.6186(8) 0.085(7) Uiso 1 1 d U . . H37A H 0.9025 0.4809 0.6051 0.101 Uiso 1 1 calc R . . C38 C 0.8562(19) 0.5312(18) 0.6527(12) 0.155(13) Uiso 1 1 d U . . H38A H 0.8139 0.4960 0.6619 0.186 Uiso 1 1 calc R . . C39 C 0.8720(16) 0.5959(15) 0.6706(10) 0.121(10) Uiso 1 1 d U . . H39A H 0.8381 0.6048 0.6912 0.145 Uiso 1 1 calc R . . C40 C 0.9327(14) 0.6436(14) 0.6591(9) 0.102(8) Uiso 1 1 d U . . H40A H 0.9440 0.6851 0.6745 0.123 Uiso 1 1 calc R . . C41 C 0.9812(12) 0.6348(12) 0.6248(8) 0.085(7) Uiso 1 1 d U . . H41A H 1.0207 0.6714 0.6140 0.102 Uiso 1 1 calc R . . C42 C 1.1133(9) 0.6610(9) 0.4026(6) 0.053(5) Uani 1 1 d U . . H42A H 1.1488 0.6405 0.4098 0.064 Uiso 1 1 calc R . . H42B H 1.0961 0.6486 0.3683 0.064 Uiso 1 1 calc R . . C43 C 1.1542(9) 0.7326(9) 0.4057(7) 0.062(6) Uani 1 1 d U . . C44 C 1.2147(10) 0.7592(11) 0.4365(8) 0.065(6) Uani 1 1 d U . . H44A H 1.2267 0.7314 0.4574 0.078 Uiso 1 1 calc R . . C45 C 1.2602(11) 0.8259(15) 0.4386(8) 0.089(8) Uani 1 1 d U . . C46 C 1.2387(9) 0.8638(9) 0.4085(6) 0.056(5) Uani 1 1 d U . . H46A H 1.2697 0.9082 0.4085 0.067 Uiso 1 1 calc R . . C47 C 1.1767(8) 0.8442(9) 0.3780(6) 0.049(4) Uani 1 1 d U . . C48 C 1.1359(9) 0.7758(8) 0.3763(6) 0.044(4) Uiso 1 1 d U . . C49 C 1.3295(11) 0.8569(11) 0.4710(8) 0.082(6) Uiso 1 1 d U . . H49A H 1.3388 0.8229 0.4888 0.098 Uiso 1 1 calc R . . H49B H 1.3216 0.8873 0.4955 0.098 Uiso 1 1 calc R . . C50 C 1.3986(12) 0.8945(12) 0.4402(8) 0.078(6) Uiso 1 1 d U . . C51 C 1.4203(16) 0.8692(15) 0.4028(11) 0.121(10) Uiso 1 1 d U . . H51A H 1.3914 0.8248 0.3961 0.145 Uiso 1 1 calc R . . C52 C 1.4749(19) 0.8934(19) 0.3721(14) 0.166(14) Uiso 1 1 d U . . H52A H 1.4850 0.8699 0.3453 0.199 Uiso 1 1 calc R . . C53 C 1.5165(18) 0.9605(18) 0.3854(12) 0.143(12) Uiso 1 1 d U . . H53A H 1.5588 0.9829 0.3672 0.171 Uiso 1 1 calc R . . C54 C 1.499(2) 0.993(2) 0.4220(14) 0.173(14) Uiso 1 1 d U . . H54A H 1.5263 1.0373 0.4283 0.207 Uiso 1 1 calc R . . C55 C 1.4349(17) 0.9579(17) 0.4528(12) 0.145(12) Uiso 1 1 d U . . H55A H 1.4207 0.9788 0.4794 0.174 Uiso 1 1 calc R . . C56 C 1.1553(7) 0.8871(8) 0.3415(6) 0.043(4) Uani 1 1 d U . . H56A H 1.2002 0.9182 0.3272 0.052 Uiso 1 1 calc R . . H56B H 1.1242 0.8593 0.3144 0.052 Uiso 1 1 calc R . . C57 C 1.1139(6) 0.9235(7) 0.3677(6) 0.042(4) Uani 1 1 d DU . . C58 C 1.1550(8) 0.9790(8) 0.3942(6) 0.060(5) Uani 1 1 d DU . . H58A H 1.2064 0.9902 0.3974 0.072 Uiso 1 1 calc R . . C59 C 1.1227(8) 1.0213(7) 0.4175(6) 0.058(5) Uani 1 1 d DU . . C60 C 1.0449(7) 1.0015(7) 0.4101(5) 0.048(4) Uani 1 1 d DU . . H60A H 1.0215 1.0286 0.4232 0.057 Uiso 1 1 calc R . . C61 C 1.0018(8) 0.9441(8) 0.3845(6) 0.049(5) Uani 1 1 d DU . . C62 C 1.0365(8) 0.9034(7) 0.3639(6) 0.039(4) Uani 1 1 d DU . . C63 C 1.1678(11) 1.0816(11) 0.4468(8) 0.079(6) Uiso 1 1 d U . . H63A H 1.1351 1.0978 0.4658 0.095 Uiso 1 1 calc R . . H63B H 1.1961 1.1156 0.4245 0.095 Uiso 1 1 calc R . . C64 C 1.2195(17) 1.067(2) 0.4809(17) 0.200(17) Uiso 1 1 d DU . . C65 C 1.230(3) 1.043(4) 0.526(3) 0.52(6) Uiso 1 1 d DU . . H65A H 1.1921 1.0275 0.5488 0.629 Uiso 1 1 calc R . . C66 C 1.305(3) 1.042(3) 0.5342(16) 0.30(3) Uiso 1 1 d DU . . H66A H 1.3142 1.0155 0.5578 0.359 Uiso 1 1 calc R . . C67 C 1.361(2) 1.083(3) 0.5039(19) 0.27(3) Uiso 1 1 d DU . . H67A H 1.4105 1.0946 0.5153 0.327 Uiso 1 1 calc R . . C68 C 1.351(2) 1.109(3) 0.459(2) 0.35(3) Uiso 1 1 d DU . . H68A H 1.3888 1.1255 0.4360 0.414 Uiso 1 1 calc R . . C69 C 1.278(2) 1.1068(19) 0.4530(12) 0.180(15) Uiso 1 1 d DU . . H69A H 1.2684 1.1329 0.4294 0.216 Uiso 1 1 calc R . . C70 C 0.9201(8) 0.9313(8) 0.3750(6) 0.046(4) Uani 1 1 d U . . H70A H 0.8923 0.8843 0.3692 0.055 Uiso 1 1 calc R . . H70B H 0.8999 0.9460 0.4040 0.055 Uiso 1 1 calc R . . C71 C 0.9119(8) 0.9672(8) 0.3306(6) 0.043(4) Uani 1 1 d U . . C72 C 0.9219(8) 1.0330(8) 0.3352(6) 0.043(4) Uani 1 1 d U . . H72A H 0.9272 1.0533 0.3669 0.052 Uiso 1 1 calc R . . C73 C 0.9243(9) 1.0691(9) 0.2944(7) 0.054(5) Uani 1 1 d U . . C74 C 0.9137(9) 1.0393(8) 0.2485(6) 0.048(4) Uani 1 1 d U . . H74A H 0.9152 1.0641 0.2208 0.058 Uiso 1 1 calc R . . C75 C 0.9013(8) 0.9752(8) 0.2418(6) 0.043(4) Uani 1 1 d U . . C76 C 0.8953(8) 0.9353(7) 0.2833(7) 0.044(4) Uani 1 1 d U . . C77 C 0.9423(10) 1.1436(9) 0.3012(7) 0.068(6) Uiso 1 1 d U . . H77A H 0.9217 1.1585 0.2732 0.081 Uiso 1 1 calc R . . H77B H 0.9196 1.1525 0.3314 0.081 Uiso 1 1 calc R . . C78 C 1.0255(11) 1.1801(10) 0.3047(8) 0.070(6) Uiso 1 1 d U . . C79 C 1.0617(12) 1.1861(11) 0.3515(8) 0.087(7) Uiso 1 1 d U . . H79A H 1.0347 1.1687 0.3796 0.104 Uiso 1 1 calc R . . C80 C 1.1405(13) 1.2193(12) 0.3545(9) 0.096(8) Uiso 1 1 d U . . H80A H 1.1648 1.2232 0.3852 0.115 Uiso 1 1 calc R . . C81 C 1.1841(16) 1.2469(14) 0.3124(10) 0.121(10) Uiso 1 1 d U . . H81A H 1.2359 1.2684 0.3137 0.145 Uiso 1 1 calc R . . C82 C 1.1432(12) 1.2388(12) 0.2718(9) 0.093(7) Uiso 1 1 d U . . H82A H 1.1682 1.2578 0.2434 0.111 Uiso 1 1 calc R . . C245 C 1.0796(13) 0.5642(13) 0.2548(8) 0.097(8) Uani 1 1 d U . . C83 C 1.0672(11) 1.2050(10) 0.2664(8) 0.075(6) Uiso 1 1 d U . . H83A H 1.0447 1.1997 0.2349 0.090 Uiso 1 1 calc R . . C84 C 0.8953(8) 0.9424(8) 0.1890(6) 0.047(4) Uani 1 1 d U . . H84A H 0.9321 0.9735 0.1685 0.057 Uiso 1 1 calc R . . H84B H 0.9096 0.9046 0.1918 0.057 Uiso 1 1 calc R . . C85 C 0.8214(9) 0.9195(8) 0.1615(6) 0.051(5) Uani 1 1 d DU . . C86 C 0.8005(11) 0.9640(9) 0.1337(6) 0.068(6) Uani 1 1 d DU . . H86A H 0.8299 1.0089 0.1344 0.081 Uiso 1 1 calc R . . C87 C 0.7345(12) 0.9380(9) 0.1055(6) 0.066(6) Uani 1 1 d DU . . C88 C 0.6893(11) 0.8759(10) 0.1080(7) 0.071(6) Uani 1 1 d DU . . H88A H 0.6439 0.8613 0.0902 0.085 Uiso 1 1 calc R . . C89 C 0.7060(9) 0.8323(9) 0.1353(5) 0.052(5) Uani 1 1 d DU . . C90 C 0.7740(8) 0.8535(8) 0.1609(5) 0.041(4) Uani 1 1 d DU . . C91 C 0.7184(13) 0.9833(12) 0.0736(8) 0.091(7) Uiso 1 1 d U . . H91A H 0.7568 1.0269 0.0795 0.109 Uiso 1 1 calc R . . H91B H 0.6711 0.9857 0.0832 0.109 Uiso 1 1 calc R . . C92 C 0.7141(11) 0.9652(11) 0.0172(7) 0.080(6) Uiso 1 1 d DU . . C93 C 0.6579(13) 0.9716(13) -0.0146(9) 0.117(9) Uiso 1 1 d DU . . H93A H 0.6203 0.9849 -0.0029 0.140 Uiso 1 1 calc R . . C94 C 0.6643(13) 0.9561(13) -0.0650(9) 0.111(9) Uiso 1 1 d DU . . H94A H 0.6316 0.9619 -0.0883 0.133 Uiso 1 1 calc R . . C95 C 0.7150(13) 0.9338(12) -0.0801(8) 0.106(8) Uiso 1 1 d DU . . H95A H 0.7175 0.9258 -0.1142 0.127 Uiso 1 1 calc R . . C96 C 0.7635(11) 0.9218(11) -0.0500(7) 0.088(7) Uiso 1 1 d DU . . H96A H 0.7974 0.9044 -0.0626 0.106 Uiso 1 1 calc R . . C97 C 0.7616(11) 0.9359(11) 0.0005(7) 0.088(7) Uiso 1 1 d DU . . H97A H 0.7923 0.9256 0.0229 0.105 Uiso 1 1 calc R . . C98 C 0.6558(9) 0.7586(9) 0.1319(6) 0.054(5) Uani 1 1 d U . . H98A H 0.6290 0.7491 0.1000 0.065 Uiso 1 1 calc R . . H98B H 0.6877 0.7333 0.1322 0.065 Uiso 1 1 calc R . . C99 C 0.5990(8) 0.7344(8) 0.1727(6) 0.047(4) Uani 1 1 d DU . . C100 C 0.5282(9) 0.7347(9) 0.1641(6) 0.053(5) Uiso 1 1 d DU . . H10B H 0.5184 0.7493 0.1337 0.064 Uiso 1 1 calc R . . C101 C 0.4728(9) 0.7154(11) 0.1970(7) 0.071(6) Uani 1 1 d DU . . C102 C 0.4870(8) 0.6879(10) 0.2406(6) 0.063(6) Uani 1 1 d DU . . H10C H 0.4484 0.6721 0.2631 0.075 Uiso 1 1 calc R . . C103 C 0.5553(7) 0.6827(7) 0.2522(5) 0.035(4) Uani 1 1 d DU . . C104 C 0.6111(8) 0.7072(8) 0.2165(5) 0.037(4) Uani 1 1 d DU . . C105 C 0.3954(13) 0.7109(13) 0.1863(9) 0.106(8) Uiso 1 1 d U . . H10D H 0.3978 0.7436 0.1622 0.127 Uiso 1 1 calc R . . H10E H 0.3679 0.6678 0.1705 0.127 Uiso 1 1 calc R . . C106 C 0.3597(15) 0.7806(12) 0.2466(10) 0.134(11) Uiso 1 1 d DU . . H10F H 0.3920 0.8199 0.2340 0.161 Uiso 1 1 calc R . . C107 C 0.3141(19) 0.7790(15) 0.2868(12) 0.191(16) Uiso 1 1 d DU . . H10G H 0.3132 0.8185 0.3003 0.229 Uiso 1 1 calc R . . C108 C 0.2721(16) 0.7231(15) 0.3065(10) 0.140(11) Uiso 1 1 d DU . . H10H H 0.2479 0.7250 0.3360 0.168 Uiso 1 1 calc R . . C109 C 0.2623(18) 0.6606(15) 0.2846(12) 0.186(16) Uiso 1 1 d DU . . H10I H 0.2278 0.6218 0.2966 0.224 Uiso 1 1 calc R . . C110 C 0.3071(17) 0.6601(13) 0.2440(11) 0.170(14) Uiso 1 1 d DU . . H11B H 0.3054 0.6204 0.2290 0.203 Uiso 1 1 calc R . . C111 C 0.3538(10) 0.7196(10) 0.2266(7) 0.069(6) Uiso 1 1 d DU . . C112 C 0.5704(9) 0.6540(8) 0.2963(6) 0.044(4) Uiso 1 1 d U . . H11C H 0.6102 0.6383 0.2890 0.053 Uiso 1 1 calc R . . H11H H 0.5260 0.6156 0.3029 0.053 Uiso 1 1 calc R . . C113 C 0.6678(6) 0.5433(7) 0.1287(4) 0.031(4) Uani 1 1 d DU . . C114 C 0.6837(7) 0.5281(8) 0.0798(5) 0.044(4) Uani 1 1 d DU . . C115 C 0.6247(7) 0.4895(8) 0.0496(5) 0.052(5) Uani 1 1 d DU . . H11D H 0.6352 0.4771 0.0178 0.062 Uiso 1 1 calc R . . C116 C 0.5527(7) 0.4686(8) 0.0626(5) 0.046(4) Uani 1 1 d DU . . C117 C 0.5396(7) 0.4896(7) 0.1089(5) 0.044(4) Uani 1 1 d DU . . H11E H 0.4901 0.4786 0.1181 0.053 Uiso 1 1 calc R . . C118 C 0.5951(6) 0.5259(7) 0.1426(5) 0.038(4) Uani 1 1 d DU . . C119 C 0.4915(9) 0.4282(9) 0.0279(7) 0.058(5) Uiso 1 1 d U . . H11F H 0.5080 0.4385 -0.0059 0.069 Uiso 1 1 calc R . . H11G H 0.4493 0.4415 0.0330 0.069 Uiso 1 1 calc R . . C120 C 0.4645(9) 0.3558(9) 0.0318(6) 0.051(4) Uiso 1 1 d U . . C121 C 0.4060(10) 0.3132(10) 0.0016(7) 0.063(5) Uiso 1 1 d U . . H12B H 0.3811 0.3300 -0.0207 0.075 Uiso 1 1 calc R . . C122 C 0.3861(13) 0.2489(12) 0.0047(9) 0.092(7) Uiso 1 1 d U . . H12C H 0.3454 0.2221 -0.0151 0.111 Uiso 1 1 calc R . . C123 C 0.4178(15) 0.2197(15) 0.0327(10) 0.115(9) Uiso 1 1 d U . . H12D H 0.4045 0.1742 0.0304 0.138 Uiso 1 1 calc R . . C124 C 0.474(2) 0.261(2) 0.0674(14) 0.186(16) Uiso 1 1 d U . . H12E H 0.4929 0.2423 0.0924 0.223 Uiso 1 1 calc R . . C125 C 0.5007(16) 0.3299(15) 0.0625(10) 0.125(10) Uiso 1 1 d U . . H12F H 0.5431 0.3574 0.0806 0.149 Uiso 1 1 calc R . . C126 C 0.5772(8) 0.5492(7) 0.1918(5) 0.038(4) Uani 1 1 d U . . H12G H 0.5354 0.5629 0.1867 0.046 Uiso 1 1 calc R . . H12I H 0.6198 0.5882 0.2028 0.046 Uiso 1 1 calc R . . C127 C 0.5582(7) 0.5021(7) 0.2334(5) 0.030(4) Uani 1 1 d DU . . C128 C 0.4899(8) 0.4537(8) 0.2392(6) 0.050(5) Uani 1 1 d DU . . H12H H 0.4525 0.4484 0.2153 0.061 Uiso 1 1 calc R . . C129 C 0.4724(9) 0.4105(9) 0.2798(7) 0.058(5) Uani 1 1 d DU . . C130 C 0.5262(9) 0.4260(9) 0.3159(6) 0.056(5) Uani 1 1 d DU . . H13B H 0.5146 0.4015 0.3444 0.067 Uiso 1 1 calc R . . C131 C 0.5966(8) 0.4745(9) 0.3145(6) 0.048(5) Uani 1 1 d DU . . C132 C 0.6110(8) 0.5137(8) 0.2721(5) 0.040(4) Uani 1 1 d DU . . C133 C 0.4004(11) 0.3569(10) 0.2831(8) 0.076(6) Uiso 1 1 d U . . H13C H 0.3915 0.3467 0.3180 0.091 Uiso 1 1 calc R . . H13D H 0.3619 0.3719 0.2717 0.091 Uiso 1 1 calc R . . C134 C 0.3924(13) 0.2978(11) 0.2555(8) 0.088(7) Uiso 1 1 d DU . . C135 C 0.3601(16) 0.2795(15) 0.2094(11) 0.153(12) Uiso 1 1 d DU . . H13E H 0.3371 0.3054 0.1952 0.183 Uiso 1 1 calc R . . C136 C 0.360(2) 0.2225(18) 0.1818(11) 0.187(16) Uiso 1 1 d DU . . H13F H 0.3336 0.2090 0.1515 0.224 Uiso 1 1 calc R . . C137 C 0.398(2) 0.1893(18) 0.2012(15) 0.24(2) Uiso 1 1 d DU . . H13G H 0.4096 0.1596 0.1803 0.285 Uiso 1 1 calc R . . C138 C 0.422(3) 0.197(2) 0.2506(18) 0.42(5) Uiso 1 1 d DU . . H13H H 0.4286 0.1636 0.2689 0.502 Uiso 1 1 calc R . . C139 C 0.4351(19) 0.2618(18) 0.2695(12) 0.200(17) Uiso 1 1 d DU . . H13J H 0.4743 0.2814 0.2925 0.239 Uiso 1 1 calc R . . C140 C 0.6519(9) 0.4889(9) 0.3576(6) 0.052(5) Uani 1 1 d U . . H14C H 0.6242 0.4789 0.3882 0.062 Uiso 1 1 calc R . . H14D H 0.6819 0.5359 0.3591 0.062 Uiso 1 1 calc R . . C141 C 0.7048(9) 0.4515(9) 0.3558(6) 0.053(5) Uani 1 1 d DU . . C142 C 0.6852(11) 0.3933(9) 0.3816(7) 0.066(6) Uani 1 1 d DU . . H14E H 0.6395 0.3760 0.3974 0.079 Uiso 1 1 calc R . . C143 C 0.7356(12) 0.3623(10) 0.3832(7) 0.073(6) Uani 1 1 d DU . . C144 C 0.8004(11) 0.3853(10) 0.3602(7) 0.067(6) Uani 1 1 d DU . . H14F H 0.8326 0.3626 0.3618 0.081 Uiso 1 1 calc R . . C145 C 0.8215(10) 0.4431(10) 0.3335(6) 0.059(5) Uani 1 1 d DU . . C146 C 0.7729(9) 0.4772(7) 0.3341(6) 0.041(4) Uani 1 1 d DU . . C147 C 0.7129(14) 0.3018(13) 0.4143(9) 0.109(9) Uiso 1 1 d U . . H14G H 0.7491 0.3104 0.4415 0.131 Uiso 1 1 calc R . . H14H H 0.6649 0.2956 0.4288 0.131 Uiso 1 1 calc R . . C148 C 0.7066(18) 0.2388(14) 0.3872(11) 0.126(10) Uiso 1 1 d DU . . C149 C 0.761(2) 0.214(2) 0.4030(15) 0.24(2) Uiso 1 1 d DU . . H14I H 0.7956 0.2348 0.4285 0.286 Uiso 1 1 calc R . . C150 C 0.759(2) 0.156(2) 0.3775(16) 0.22(2) Uiso 1 1 d DU . . H15A H 0.7942 0.1380 0.3837 0.270 Uiso 1 1 calc R . . C151 C 0.703(2) 0.1292(17) 0.3441(14) 0.190(16) Uiso 1 1 d DU . . H15B H 0.7018 0.0905 0.3278 0.228 Uiso 1 1 calc R . . C152 C 0.647(3) 0.152(3) 0.330(2) 0.37(4) Uiso 1 1 d DU . . H15C H 0.6108 0.1289 0.3061 0.441 Uiso 1 1 calc R . . C153 C 0.647(2) 0.210(2) 0.3552(15) 0.222(19) Uiso 1 1 d DU . . H15D H 0.6104 0.2271 0.3500 0.266 Uiso 1 1 calc R . . C154 C 0.8993(8) 0.4747(8) 0.3114(7) 0.055(5) Uani 1 1 d U . . H15F H 0.9110 0.5217 0.3092 0.066 Uiso 1 1 calc R . . H15G H 0.9358 0.4694 0.3341 0.066 Uiso 1 1 calc R . . C155 C 0.9070(10) 0.4470(8) 0.2612(7) 0.052(5) Uani 1 1 d U . . C157 C 0.9395(12) 0.3700(10) 0.2112(7) 0.070(6) Uani 1 1 d U . . C158 C 0.9377(10) 0.4023(10) 0.1695(8) 0.071(6) Uani 1 1 d U . . H15H H 0.9478 0.3862 0.1389 0.085 Uiso 1 1 calc R . . C159 C 0.9207(8) 0.4604(9) 0.1712(7) 0.059(6) Uani 1 1 d U . . C160 C 0.9036(9) 0.4800(8) 0.2209(7) 0.050(5) Uani 1 1 d U . . C161 C 0.9545(13) 0.3070(12) 0.2065(9) 0.101(8) Uiso 1 1 d U . . H16B H 0.9944 0.3135 0.1831 0.121 Uiso 1 1 calc R . . H16C H 0.9724 0.2994 0.2387 0.121 Uiso 1 1 calc R . . C162 C 0.8927(11) 0.2495(11) 0.1907(9) 0.092(7) Uiso 1 1 d DU . . C163 C 0.8365(13) 0.2222(13) 0.2245(8) 0.119(9) Uiso 1 1 d DU . . H16D H 0.8374 0.2437 0.2552 0.143 Uiso 1 1 calc R . . C164 C 0.7797(15) 0.1632(14) 0.2123(11) 0.152(12) Uiso 1 1 d DU . . H16E H 0.7478 0.1411 0.2372 0.182 Uiso 1 1 calc R . . C165 C 0.7681(16) 0.1359(15) 0.1656(12) 0.178(15) Uiso 1 1 d DU . . H16F H 0.7251 0.0999 0.1561 0.213 Uiso 1 1 calc R . . C166 C 0.824(2) 0.165(2) 0.1334(12) 0.26(2) Uiso 1 1 d DU . . H16G H 0.8176 0.1479 0.1006 0.316 Uiso 1 1 calc R . . C167 C 0.8882(16) 0.2168(15) 0.1456(9) 0.155(13) Uiso 1 1 d DU . . H16H H 0.9281 0.2297 0.1239 0.186 Uiso 1 1 calc R . . C168 C 0.9307(9) 0.5029(8) 0.1291(7) 0.058(5) Uani 1 1 d U . . H16I H 0.9022 0.5309 0.1342 0.070 Uiso 1 1 calc R . . H16J H 0.9118 0.4759 0.0988 0.070 Uiso 1 1 calc R . . C169 C 1.0107(8) 0.5446(8) 0.1235(6) 0.049(4) Uani 1 1 d DU . . C170 C 1.0567(9) 0.5192(9) 0.0966(7) 0.065(6) Uani 1 1 d DU . . H17A H 1.0345 0.4789 0.0791 0.078 Uiso 1 1 calc R . . C171 C 1.1331(9) 0.5511(9) 0.0950(7) 0.065(6) Uani 1 1 d DU . . C172 C 1.1610(9) 0.6105(9) 0.1225(7) 0.067(6) Uani 1 1 d DU . . H17B H 1.2128 0.6317 0.1242 0.080 Uiso 1 1 calc R . . C173 C 1.1229(8) 0.6401(8) 0.1461(6) 0.050(5) Uani 1 1 d DU . . C174 C 1.0439(7) 0.6077(7) 0.1456(6) 0.047(4) Uani 1 1 d DU . . C175 C 1.1810(11) 0.5233(11) 0.0638(8) 0.083(7) Uiso 1 1 d U . . H17C H 1.1783 0.4822 0.0778 0.100 Uiso 1 1 calc R . . H17D H 1.1592 0.5128 0.0303 0.100 Uiso 1 1 calc R . . C176 C 1.2577(10) 0.5646(10) 0.0601(7) 0.079(6) Uiso 1 1 d DU . . C177 C 1.2802(14) 0.6158(14) 0.0265(10) 0.140(11) Uiso 1 1 d DU . . H17E H 1.2436 0.6212 0.0063 0.168 Uiso 1 1 calc R . . C178 C 1.3536(16) 0.6587(16) 0.0217(12) 0.175(14) Uiso 1 1 d DU . . H17F H 1.3690 0.6922 -0.0009 0.210 Uiso 1 1 calc R . . C179 C 1.4013(13) 0.6456(13) 0.0548(10) 0.122(10) Uiso 1 1 d DU . . H17G H 1.4510 0.6747 0.0541 0.146 Uiso 1 1 calc R . . C180 C 1.3881(11) 0.5994(13) 0.0864(10) 0.133(11) Uiso 1 1 d DU . . H18B H 1.4259 0.5952 0.1062 0.159 Uiso 1 1 calc R . . C181 C 1.3121(8) 0.5555(11) 0.0890(9) 0.134(11) Uiso 1 1 d DU . . H18C H 1.2992 0.5205 0.1103 0.160 Uiso 1 1 calc R . . C182 C 1.1615(9) 0.7046(8) 0.1716(6) 0.047(4) Uiso 1 1 d U . . H18D H 1.1287 0.7104 0.1970 0.056 Uiso 1 1 calc R . . H18E H 1.2055 0.7034 0.1886 0.056 Uiso 1 1 calc R . . C183 C 1.1851(10) 0.7626(9) 0.1416(7) 0.058(5) Uiso 1 1 d U . . C184 C 1.2525(11) 0.7819(11) 0.1117(8) 0.081(6) Uiso 1 1 d U . . H18F H 1.2816 0.7564 0.1127 0.097 Uiso 1 1 calc R . . C185 C 1.2752(17) 0.8353(16) 0.0822(11) 0.138(11) Uiso 1 1 d U . . H18G H 1.3184 0.8466 0.0636 0.166 Uiso 1 1 calc R . . C186 C 1.2273(13) 0.8730(13) 0.0820(9) 0.100(8) Uiso 1 1 d U . . H18H H 1.2397 0.9093 0.0620 0.121 Uiso 1 1 calc R . . C187 C 1.1600(10) 0.8558(9) 0.1123(7) 0.057(5) Uiso 1 1 d U . . C188 C 1.1417(8) 0.8004(8) 0.1387(6) 0.041(4) Uiso 1 1 d U . . C196 C 1.1204(10) 0.9020(10) 0.1142(7) 0.069(6) Uani 1 1 d U . . H19A H 1.1569 0.9463 0.1102 0.083 Uiso 1 1 calc R . . H19B H 1.0999 0.9013 0.1472 0.083 Uiso 1 1 calc R . . C197 C 1.0574(12) 0.8891(9) 0.0759(7) 0.066(6) Uani 1 1 d U . . C198 C 1.0739(12) 0.9195(10) 0.0298(8) 0.075(6) Uani 1 1 d U . . H19C H 1.1233 0.9447 0.0226 0.090 Uiso 1 1 calc R . . C199 C 1.0177(13) 0.9127(11) -0.0049(8) 0.081(7) Uani 1 1 d U . . C200 C 0.9447(12) 0.8744(9) 0.0072(7) 0.075(6) Uani 1 1 d U . . H20A H 0.9069 0.8670 -0.0168 0.090 Uiso 1 1 calc R . . C201 C 0.9247(10) 0.8462(9) 0.0540(6) 0.057(5) Uani 1 1 d U . . C202 C 0.9817(9) 0.8503(7) 0.0875(6) 0.044(4) Uani 1 1 d U . . C203 C 1.0366(12) 0.9432(12) -0.0556(8) 0.095(7) Uiso 1 1 d U . . H20B H 1.0481 0.9903 -0.0511 0.114 Uiso 1 1 calc R . . H20C H 1.0816 0.9377 -0.0671 0.114 Uiso 1 1 calc R . . C204 C 0.9795(11) 0.9170(11) -0.0939(8) 0.075(6) Uiso 1 1 d U . . C205 C 0.9443(13) 0.9548(13) -0.1138(9) 0.093(7) Uiso 1 1 d U . . H20D H 0.9594 0.9992 -0.1038 0.112 Uiso 1 1 calc R . . C206 C 0.8896(15) 0.9290(15) -0.1468(10) 0.120(9) Uiso 1 1 d U . . H20E H 0.8686 0.9567 -0.1607 0.144 Uiso 1 1 calc R . . C207 C 0.8621(16) 0.8652(15) -0.1617(11) 0.123(10) Uiso 1 1 d U . . H20F H 0.8199 0.8470 -0.1825 0.148 Uiso 1 1 calc R . . C208 C 0.8995(15) 0.8294(15) -0.1445(10) 0.115(9) Uiso 1 1 d U . . H20G H 0.8858 0.7861 -0.1569 0.138 Uiso 1 1 calc R . . C209 C 0.9547(15) 0.8518(15) -0.1108(10) 0.124(10) Uiso 1 1 d U . . H20H H 0.9766 0.8239 -0.0986 0.149 Uiso 1 1 calc R . . C210 C 0.8458(8) 0.8040(9) 0.0641(6) 0.050(5) Uani 1 1 d U . . H21C H 0.8143 0.8281 0.0560 0.060 Uiso 1 1 calc R . . H21D H 0.8418 0.7965 0.0995 0.060 Uiso 1 1 calc R . . C211 C 0.8152(9) 0.7380(9) 0.0362(5) 0.050(5) Uani 1 1 d U . . C212 C 0.7862(10) 0.7317(10) -0.0120(6) 0.059(5) Uani 1 1 d U . . H21E H 0.7886 0.7696 -0.0278 0.071 Uiso 1 1 calc R . . C213 C 0.7548(10) 0.6728(11) -0.0370(6) 0.060(5) Uani 1 1 d U . . C214 C 0.7468(9) 0.6177(10) -0.0134(6) 0.058(5) Uani 1 1 d U . . H21F H 0.7214 0.5771 -0.0299 0.069 Uiso 1 1 calc R . . C215 C 0.7749(7) 0.6185(9) 0.0348(5) 0.042(4) Uani 1 1 d U . . C216 C 0.8111(8) 0.6777(8) 0.0597(5) 0.039(4) Uani 1 1 d U . . C217 C 0.7203(11) 0.6704(11) -0.0894(7) 0.074(6) Uiso 1 1 d U . . H21G H 0.6662 0.6513 -0.0874 0.089 Uiso 1 1 calc R . . H21H H 0.7339 0.7152 -0.1002 0.089 Uiso 1 1 calc R . . C218 C 0.8179(14) 0.6390(13) -0.1332(9) 0.104(8) Uiso 1 1 d U . . H21I H 0.8574 0.6657 -0.1124 0.125 Uiso 1 1 calc R . . C219 C 0.8258(17) 0.5991(15) -0.1760(11) 0.124(10) Uiso 1 1 d U . . H21K H 0.8735 0.6020 -0.1846 0.148 Uiso 1 1 calc R . . C220 C 0.7695(19) 0.5602(17) -0.2020(13) 0.152(13) Uiso 1 1 d U . . H22A H 0.7791 0.5364 -0.2288 0.183 Uiso 1 1 calc R . . C221 C 0.699(2) 0.5512(18) -0.1940(13) 0.161(13) Uiso 1 1 d U . . H22B H 0.6610 0.5192 -0.2127 0.194 Uiso 1 1 calc R . . C222 C 0.6834(16) 0.5887(15) -0.1586(11) 0.125(10) Uiso 1 1 d U . . H22C H 0.6347 0.5866 -0.1544 0.149 Uiso 1 1 calc R . . C223 C 0.7442(11) 0.6320(10) -0.1276(7) 0.065(5) Uiso 1 1 d U . . C224 C 0.7620(8) 0.5561(8) 0.0602(6) 0.043(4) Uani 1 1 d U . . H22D H 0.7979 0.5645 0.0877 0.052 Uiso 1 1 calc R . . H22E H 0.7695 0.5243 0.0369 0.052 Uiso 1 1 calc R . . C225 C 1.0884(14) 0.8199(13) 0.5051(9) 0.097(8) Uiso 1 1 d U . . H22G H 1.1389 0.8262 0.5039 0.116 Uiso 1 1 calc R . . C226 C 1.0415(14) 0.7661(14) 0.5176(9) 0.109(8) Uiso 1 1 d U . . H22F H 1.0587 0.7324 0.5230 0.130 Uiso 1 1 calc R . . C227 C 0.9690(14) 0.7525(13) 0.5239(9) 0.103(8) Uiso 1 1 d U . . H22H H 0.9364 0.7123 0.5350 0.124 Uiso 1 1 calc R . . C228 C 0.9453(13) 0.8048(12) 0.5123(8) 0.086(7) Uiso 1 1 d U . . H22I H 0.8956 0.7993 0.5169 0.103 Uiso 1 1 calc R . . C229 C 0.9888(14) 0.8566(14) 0.4966(9) 0.112(9) Uiso 1 1 d U . . H22J H 0.9708 0.8883 0.4867 0.134 Uiso 1 1 calc R . . C230 C 1.0654(14) 0.8690(13) 0.4933(9) 0.101(8) Uiso 1 1 d U . . H23E H 1.0992 0.9094 0.4833 0.121 Uiso 1 1 calc R . . C231 C 0.7029(14) 0.9215(13) 0.3346(10) 0.107(8) Uiso 1 1 d U . . H23F H 0.7310 0.9321 0.3643 0.129 Uiso 1 1 calc R . . C232 C 0.6375(12) 0.8713(12) 0.3294(9) 0.087(7) Uiso 1 1 d U . . H23G H 0.6183 0.8486 0.3580 0.105 Uiso 1 1 calc R . . C233 C 0.5971(14) 0.8502(13) 0.2880(9) 0.102(8) Uiso 1 1 d U . . H23H H 0.5531 0.8129 0.2872 0.122 Uiso 1 1 calc R . . C234 C 0.6211(14) 0.8835(13) 0.2480(10) 0.107(8) Uiso 1 1 d U . . H23I H 0.5920 0.8702 0.2187 0.128 Uiso 1 1 calc R . . C235 C 0.6826(13) 0.9336(13) 0.2472(10) 0.102(8) Uiso 1 1 d U . . H23J H 0.6990 0.9546 0.2176 0.123 Uiso 1 1 calc R . . C236 C 0.7255(12) 0.9569(12) 0.2920(8) 0.088(7) Uiso 1 1 d U . . H23K H 0.7683 0.9953 0.2927 0.106 Uiso 1 1 calc R . . C237 C 0.9849(8) 0.7193(10) -0.0177(9) 0.109(9) Uiso 1 1 d DU . . H23B H 0.9567 0.7424 -0.0295 0.131 Uiso 1 1 calc R . . C238 C 0.9529(10) 0.6536(9) -0.0111(8) 0.096(7) Uiso 1 1 d DU . . H23C H 0.9027 0.6308 -0.0199 0.115 Uiso 1 1 calc R . . C239 C 0.9923(10) 0.6221(9) 0.0076(8) 0.085(7) Uiso 1 1 d DU . . H23D H 0.9688 0.5777 0.0143 0.102 Uiso 1 1 calc R . . C240 C 1.0694(10) 0.6543(7) 0.0176(8) 0.099(8) Uiso 1 1 d DU . . H24E H 1.0992 0.6323 0.0287 0.119 Uiso 1 1 calc R . . C241 C 1.0971(13) 0.7202(12) 0.0099(9) 0.107(8) Uiso 1 1 d DU . . H24G H 1.1475 0.7446 0.0174 0.129 Uiso 1 1 calc R . . C242 C 1.0567(14) 0.7498(13) -0.0071(10) 0.113(9) Uiso 1 1 d DU . . H24H H 1.0790 0.7948 -0.0123 0.136 Uiso 1 1 calc R . . C243 C 1.0810(11) 0.9827(12) 0.2635(7) 0.070(6) Uani 1 1 d U . . C244 C 1.1083(11) 1.0508(10) 0.2825(9) 0.086(7) Uani 1 1 d U . . C301 C 0.6965(14) 0.3319(13) 0.2370(9) 0.114(9) Uiso 1 1 d DU . . H30B H 0.7100 0.3128 0.2640 0.137 Uiso 1 1 calc R . . C304 C 0.6472(14) 0.3765(13) 0.1589(9) 0.111(9) Uiso 1 1 d DU . . H30C H 0.6279 0.3911 0.1319 0.133 Uiso 1 1 calc R . . C302 C 0.7380(12) 0.3449(12) 0.1960(8) 0.092(7) Uiso 1 1 d DU . . H30D H 0.7831 0.3385 0.1956 0.110 Uiso 1 1 calc R . . C305 C 0.6100(14) 0.3654(14) 0.1988(10) 0.118(9) Uiso 1 1 d DU . . H30E H 0.5643 0.3706 0.1993 0.142 Uiso 1 1 calc R . . C303 C 0.7136(12) 0.3685(11) 0.1531(8) 0.091 Uiso 1 1 d DU . . H30F H 0.7405 0.3776 0.1238 0.109 Uiso 1 1 calc R . . C300 C 0.6339(14) 0.3473(14) 0.2384(10) 0.121 Uiso 1 1 d DU . . H30H H 0.6084 0.3446 0.2681 0.145 Uiso 1 1 calc R . . N1 N 1.0609(9) 0.9317(9) 0.2452(6) 0.069 Uani 1 1 d U . . Bi2 Bi 0.97332(3) 0.74022(3) 0.38357(2) 0.037 Uani 1 1 d U . . Bi3 Bi 0.94660(3) 0.80830(3) 0.26536(2) 0.035 Uani 1 1 d U . . Bi4 Bi 0.75138(3) 0.79853(3) 0.26278(2) 0.034 Uani 1 1 d U . . Bi5 Bi 0.79521(3) 0.68142(3) 0.17974(2) 0.032 Uani 1 1 d U . . Bi6 Bi 0.75331(3) 0.51977(3) 0.23248(2) 0.038 Uani 1 1 d U . . N2 N 1.0610(9) 0.6046(9) 0.2691(6) 0.073 Uani 1 1 d U . . Bi7 Bi 0.94784(3) 0.64057(3) 0.23864(2) 0.039 Uani 1 1 d U . . Bi8 Bi 0.97938(3) 0.72923(3) 0.12288(2) 0.043 Uani 1 1 d U . . C156 C 0.9254(10) 0.3925(9) 0.2568(7) 0.061 Uani 1 1 d U . . H15I H 0.9284 0.3704 0.2852 0.073 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 0.0320(3) 0.0361(3) 0.0300(3) -0.0046(3) 0.0039(2) 0.0152(3) O1 0.041(6) 0.034(6) 0.022(5) -0.006(5) 0.011(4) 0.023(5) O2 0.034(6) 0.058(7) 0.023(6) 0.003(5) 0.011(5) 0.011(5) O3 0.044(6) 0.039(6) 0.039(6) 0.012(5) 0.008(5) 0.024(5) O4 0.039(6) 0.052(7) 0.058(7) -0.025(6) -0.021(5) 0.032(5) O5 0.035(5) 0.039(6) 0.040(6) -0.009(5) 0.000(5) 0.018(5) O6 0.029(5) 0.040(6) 0.038(6) -0.010(5) 0.004(5) 0.021(5) O8 0.045(6) 0.057(7) 0.014(5) -0.014(5) 0.004(4) 0.032(5) O9 0.044(6) 0.022(6) 0.029(6) -0.007(5) 0.014(5) 0.000(5) O10 0.037(6) 0.050(7) 0.052(7) -0.025(6) -0.009(5) 0.023(5) O11 0.054(7) 0.058(8) 0.049(7) -0.009(6) 0.007(6) 0.037(6) O12 0.038(6) 0.034(6) 0.056(7) -0.017(5) -0.008(5) 0.017(5) O13 0.060(7) 0.053(8) 0.041(7) -0.015(6) -0.001(6) 0.031(6) O14 0.045(6) 0.070(9) 0.048(7) -0.022(6) 0.016(6) 0.019(6) O15 0.077(8) 0.029(6) 0.039(7) 0.008(5) 0.032(6) 0.018(6) O16 0.033(6) 0.030(6) 0.051(7) -0.022(5) -0.003(5) 0.004(5) O17 0.018(5) 0.045(6) 0.026(5) -0.011(5) 0.000(4) 0.013(4) O19 0.048(6) 0.020(5) 0.022(5) -0.002(4) 0.006(4) 0.014(5) O20 0.029(5) 0.045(7) 0.038(6) -0.017(5) 0.001(5) 0.012(5) O21 0.048(6) 0.037(6) 0.044(6) -0.016(5) 0.002(5) 0.024(5) C1 0.029(8) 0.045(10) 0.041(10) -0.010(8) 0.001(7) 0.023(7) C2 0.059(11) 0.041(10) 0.033(9) 0.001(8) 0.009(8) 0.015(9) C3 0.034(9) 0.082(14) 0.033(9) -0.014(9) 0.004(7) 0.029(9) C4 0.035(9) 0.080(14) 0.042(10) -0.004(10) 0.021(8) 0.030(9) C5 0.059(11) 0.079(14) 0.031(10) -0.017(9) 0.009(9) 0.035(10) C6 0.038(8) 0.056(11) 0.029(9) 0.004(8) 0.010(7) 0.034(8) C14 0.029(8) 0.066(13) 0.042(10) -0.019(9) 0.013(7) 0.006(8) C16 0.036(9) 0.063(12) 0.040(10) -0.006(9) 0.010(8) 0.019(9) C17 0.059(11) 0.049(11) 0.024(9) 0.006(8) 0.025(8) 0.015(9) C18 0.082(13) 0.068(13) 0.042(11) 0.027(10) 0.011(10) 0.050(11) C19 0.036(9) 0.057(12) 0.037(10) 0.007(9) 0.004(8) 0.007(8) C20 0.029(8) 0.054(11) 0.030(9) -0.001(8) -0.007(7) 0.015(8) C246 0.12(2) 0.11(2) 0.089(17) -0.039(15) -0.012(15) 0.068(17) C28 0.060(11) 0.041(10) 0.037(10) -0.004(8) 0.015(8) 0.020(9) C29 0.057(10) 0.043(10) 0.032(9) 0.013(8) -0.004(8) 0.037(8) C30 0.071(12) 0.051(12) 0.061(12) 0.008(10) 0.005(10) 0.040(10) C31 0.078(13) 0.043(11) 0.052(12) -0.011(9) -0.007(10) 0.033(10) C32 0.077(13) 0.065(13) 0.047(11) 0.004(10) 0.000(10) 0.041(11) C33 0.068(11) 0.038(10) 0.027(9) 0.000(7) 0.006(8) 0.045(9) C34 0.067(11) 0.013(8) 0.033(9) 0.004(7) 0.012(8) 0.026(8) C42 0.049(10) 0.077(14) 0.056(11) 0.009(10) -0.007(9) 0.049(10) C43 0.040(10) 0.053(12) 0.090(15) -0.049(11) -0.008(10) 0.021(9) C44 0.047(11) 0.078(15) 0.083(15) 0.027(13) 0.002(11) 0.034(11) C45 0.055(13) 0.17(3) 0.064(14) -0.004(16) -0.029(11) 0.064(16) C46 0.049(11) 0.063(13) 0.050(11) -0.020(10) 0.005(9) 0.017(10) C47 0.035(9) 0.051(11) 0.063(12) -0.002(9) -0.005(9) 0.020(8) C56 0.020(7) 0.043(10) 0.057(11) -0.023(9) 0.022(7) 0.003(7) C57 0.028(8) 0.038(10) 0.054(11) -0.013(8) 0.007(8) 0.008(7) C58 0.053(11) 0.056(12) 0.079(14) -0.027(11) -0.015(10) 0.031(10) C59 0.070(12) 0.041(11) 0.054(12) -0.003(9) -0.002(10) 0.010(9) C60 0.043(9) 0.067(12) 0.043(10) -0.011(9) 0.001(8) 0.035(9) C61 0.032(9) 0.046(11) 0.055(11) -0.023(9) 0.010(8) 0.001(8) C62 0.041(9) 0.028(9) 0.053(10) 0.014(8) 0.020(8) 0.017(7) C70 0.054(10) 0.035(10) 0.045(10) 0.004(8) 0.024(8) 0.011(8) C71 0.033(9) 0.047(11) 0.050(11) -0.018(9) -0.001(8) 0.015(8) C72 0.049(10) 0.044(11) 0.041(10) -0.004(9) 0.017(8) 0.024(8) C73 0.059(11) 0.057(12) 0.065(13) -0.002(11) 0.006(10) 0.044(10) C74 0.061(11) 0.045(11) 0.047(11) 0.012(9) 0.019(9) 0.028(9) C75 0.039(9) 0.044(11) 0.049(10) 0.006(9) 0.007(8) 0.019(8) C76 0.027(8) 0.029(9) 0.081(13) 0.001(9) 0.010(8) 0.018(7) C245 0.104(18) 0.11(2) 0.082(17) -0.006(15) -0.011(14) 0.042(15) C84 0.049(10) 0.044(11) 0.042(10) -0.007(8) 0.018(8) 0.010(8) C85 0.059(11) 0.049(12) 0.050(11) -0.017(9) 0.011(9) 0.028(10) C86 0.110(17) 0.057(13) 0.044(12) 0.014(10) 0.002(11) 0.040(12) C87 0.134(19) 0.045(12) 0.035(11) 0.011(10) 0.000(12) 0.050(13) C88 0.084(14) 0.092(18) 0.046(12) -0.009(12) -0.028(11) 0.045(13) C89 0.072(12) 0.075(14) 0.022(9) 0.012(9) 0.026(9) 0.041(11) C90 0.041(9) 0.068(13) 0.023(8) 0.000(8) 0.002(7) 0.030(9) C98 0.063(11) 0.083(15) 0.030(10) 0.009(10) 0.013(9) 0.042(11) C99 0.037(9) 0.048(11) 0.063(12) -0.023(9) -0.018(8) 0.025(8) C101 0.053(12) 0.113(18) 0.053(12) -0.031(12) -0.016(10) 0.042(12) C102 0.021(8) 0.109(17) 0.057(12) 0.004(12) 0.008(8) 0.023(10) C103 0.027(8) 0.048(10) 0.022(8) -0.027(7) 0.007(6) 0.008(7) C104 0.054(10) 0.057(11) 0.015(8) -0.022(7) -0.022(7) 0.040(9) C113 0.025(8) 0.024(8) 0.032(9) -0.009(7) -0.005(6) -0.004(6) C114 0.034(8) 0.051(11) 0.038(10) -0.016(8) 0.004(7) 0.005(8) C115 0.061(11) 0.076(13) 0.026(9) -0.034(9) -0.014(8) 0.037(10) C116 0.037(9) 0.058(12) 0.036(10) -0.002(9) -0.004(8) 0.012(8) C117 0.042(9) 0.036(10) 0.045(10) 0.001(8) 0.000(8) 0.003(8) C118 0.033(9) 0.034(9) 0.036(9) -0.007(8) 0.005(7) 0.000(7) C126 0.037(8) 0.032(9) 0.053(10) -0.016(8) -0.022(8) 0.024(7) C127 0.032(8) 0.032(9) 0.017(8) -0.018(7) 0.006(6) 0.003(7) C128 0.047(10) 0.053(12) 0.043(11) 0.005(9) 0.021(8) 0.008(9) C129 0.038(10) 0.058(13) 0.065(13) -0.013(10) 0.004(9) 0.004(9) C130 0.066(12) 0.055(12) 0.044(11) 0.003(9) 0.019(10) 0.021(10) C131 0.032(9) 0.059(12) 0.047(11) -0.019(9) 0.004(8) 0.011(8) C132 0.048(9) 0.044(10) 0.027(9) 0.014(8) 0.035(8) 0.013(8) C140 0.046(10) 0.047(11) 0.054(11) 0.004(9) 0.012(9) 0.009(9) C141 0.054(11) 0.055(12) 0.029(10) -0.005(9) 0.012(8) -0.004(9) C142 0.076(14) 0.058(14) 0.051(12) -0.013(11) 0.004(10) 0.013(11) C143 0.094(16) 0.079(16) 0.059(14) 0.031(12) 0.008(12) 0.043(14) C144 0.090(15) 0.065(14) 0.059(13) 0.020(11) -0.001(12) 0.042(12) C145 0.067(12) 0.072(14) 0.042(11) -0.012(10) -0.012(9) 0.034(11) C146 0.071(11) 0.009(8) 0.039(10) 0.001(7) -0.005(9) 0.010(8) C154 0.033(9) 0.040(11) 0.093(14) -0.028(10) -0.026(9) 0.017(8) C155 0.074(12) 0.044(11) 0.061(12) -0.002(10) -0.010(10) 0.048(10) C157 0.106(16) 0.085(16) 0.059(13) -0.030(12) -0.028(12) 0.084(14) C158 0.067(13) 0.073(15) 0.084(15) -0.040(13) -0.006(12) 0.042(12) C159 0.033(9) 0.056(12) 0.080(14) -0.062(11) -0.021(9) 0.013(9) C160 0.046(10) 0.023(9) 0.085(14) -0.007(9) 0.011(9) 0.017(8) C168 0.069(13) 0.038(11) 0.069(13) -0.026(10) -0.029(10) 0.024(10) C169 0.050(10) 0.043(11) 0.057(11) -0.003(9) 0.002(9) 0.022(9) C170 0.056(11) 0.059(13) 0.081(14) -0.044(11) -0.002(10) 0.029(10) C171 0.063(12) 0.055(13) 0.087(15) -0.016(11) 0.016(11) 0.035(10) C172 0.044(10) 0.075(15) 0.065(13) -0.030(11) 0.004(9) 0.007(10) C173 0.054(10) 0.060(12) 0.048(10) -0.034(9) -0.014(8) 0.041(9) C174 0.040(9) 0.050(11) 0.056(11) -0.028(9) -0.014(8) 0.025(8) C196 0.061(12) 0.073(15) 0.067(14) 0.007(12) 0.024(11) 0.019(11) C197 0.104(16) 0.035(11) 0.060(13) -0.010(10) 0.021(12) 0.028(11) C198 0.088(16) 0.065(15) 0.056(14) -0.005(12) 0.015(12) 0.011(12) C199 0.097(17) 0.067(15) 0.074(16) 0.024(13) 0.051(14) 0.020(13) C200 0.094(16) 0.055(13) 0.065(14) 0.001(11) 0.029(12) 0.015(12) C201 0.073(13) 0.049(12) 0.045(11) 0.024(9) 0.039(10) 0.015(10) C202 0.049(10) 0.023(9) 0.049(11) 0.003(8) 0.023(9) 0.002(8) C210 0.044(10) 0.064(12) 0.049(11) 0.020(10) 0.015(8) 0.025(9) C211 0.059(11) 0.066(13) 0.020(9) -0.018(9) 0.004(8) 0.019(10) C212 0.077(13) 0.076(15) 0.035(10) -0.002(10) 0.017(9) 0.039(11) C213 0.072(13) 0.082(16) 0.035(11) 0.002(11) 0.003(9) 0.040(12) C214 0.040(10) 0.076(15) 0.040(11) -0.014(10) 0.012(8) 0.004(10) C215 0.015(7) 0.074(13) 0.026(9) -0.013(9) 0.013(6) 0.004(8) C216 0.032(8) 0.063(12) 0.023(8) 0.002(8) 0.020(7) 0.020(8) C224 0.035(9) 0.047(11) 0.050(10) -0.026(9) 0.002(8) 0.020(8) C243 0.072(13) 0.096(17) 0.050(12) 0.012(12) 0.030(10) 0.041(12) C244 0.073(14) 0.053(13) 0.115(19) -0.044(13) 0.025(13) 0.006(11) N1 0.069 0.069 0.069 0.003 0.002 0.026 Bi2 0.036 0.044 0.035 -0.009 -0.001 0.021 Bi3 0.034 0.037 0.036 -0.007 0.005 0.016 Bi4 0.035 0.040 0.033 -0.007 0.004 0.021 Bi5 0.033 0.039 0.028 -0.008 0.003 0.016 Bi6 0.040 0.035 0.039 -0.009 0.002 0.015 N2 0.073 0.073 0.073 0.003 0.002 0.027 Bi7 0.036 0.042 0.042 -0.012 0.000 0.021 Bi8 0.040 0.049 0.037 -0.011 0.011 0.014 C156 0.061 0.061 0.061 0.003 0.001 0.023 _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 O18 2.218(9) . ? Bi1 O17 2.263(8) . ? Bi1 O1 2.294(9) . ? Bi1 O2 2.294(9) . ? Bi1 O19 2.556(9) . ? Bi1 Bi2 3.6836(10) . ? Bi1 Bi4 3.6920(10) . ? O1 C1 1.380(16) . ? O1 Bi4 2.414(9) . ? O2 C20 1.368(17) . ? O2 Bi2 2.394(9) . ? O3 C34 1.344(17) . ? O3 Bi2 2.156(10) . ? O4 C48 1.374(18) . ? O4 Bi2 2.210(10) . ? O5 C62 1.348(17) . ? O5 Bi3 2.227(10) . ? O5 Bi2 2.552(10) . ? O6 C76 1.339(17) . ? O6 Bi3 2.266(9) . ? O6 Bi4 2.414(9) . ? O7 C90 1.390(17) . ? O7 Bi4 2.187(10) . ? O8 C104 1.372(15) . ? O8 Bi4 2.182(10) . ? O9 C113 1.375(15) . ? O9 Bi5 2.287(9) . ? O9 Bi6 2.447(10) . ? O10 C132 1.378(17) . ? O10 Bi6 2.200(10) . ? O11 C146 1.386(17) . ? O11 Bi6 2.173(11) . ? O12 C160 1.411(18) . ? O12 Bi7 2.239(10) . ? O12 Bi6 2.436(10) . ? O13 C174 1.368(17) . ? O13 Bi7 2.219(10) . ? O13 Bi8 2.547(11) . ? O14 C188 1.345(18) . ? O14 Bi8 2.197(11) . ? O15 C202 1.351(18) . ? O15 Bi8 2.148(11) . ? O16 C216 1.384(17) . ? O16 Bi5 2.248(10) . ? O16 Bi8 2.446(9) . ? O17 Bi2 2.115(8) . ? O17 Bi3 2.294(10) . ? O18 Bi4 2.138(9) . ? O18 Bi3 2.322(8) . ? O18 Bi5 2.540(9) . ? O19 Bi6 2.112(9) . ? O19 Bi5 2.257(9) . ? O19 Bi7 2.300(9) . ? O20 Bi8 2.116(10) . ? O20 Bi7 2.275(11) . ? O20 Bi5 2.290(9) . ? O21 Bi3 2.609(10) . ? O21 Bi7 2.621(10) . ? C1 C6 1.37(2) . ? C1 C2 1.41(2) . ? C2 C3 1.36(2) . ? C2 C112 1.54(2) . ? C3 C4 1.37(2) . ? C3 H3A 0.9400 . ? C4 C5 1.31(2) . ? C4 C7 1.56(2) . ? C5 C6 1.40(2) . ? C5 H5A 0.9400 . ? C6 C14 1.58(2) . ? C7 C8 1.49(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.40(3) . ? C8 C13 1.44(3) . ? C9 C10 1.45(3) . ? C9 H9A 0.9400 . ? C10 C11 1.37(3) . ? C10 H10A 0.9400 . ? C11 C12 1.34(3) . ? C11 H11A 0.9400 . ? C12 C13 1.42(3) . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C14 C15 1.49(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.38(2) . ? C15 C20 1.42(2) . ? C16 C17 1.38(2) . ? C16 H16A 0.9400 . ? C17 C18 1.37(2) . ? C17 C21 1.57(2) . ? C18 C19 1.41(2) . ? C18 H18A 0.9400 . ? C19 C20 1.45(2) . ? C19 C28 1.54(2) . ? C21 C22 1.51(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C27 1.38(3) . ? C22 C23 1.43(3) . ? C23 C24 1.46(3) . ? C23 H23A 0.9400 . ? C246 C245 1.51(3) . ? C246 H24A 0.9700 . ? C246 H24B 0.9700 . ? C246 H24C 0.9700 . ? C24 C25 1.39(4) . ? C24 H24D 0.9400 . ? C25 C26 1.53(4) . ? C25 H25A 0.9400 . ? C26 C27 1.43(4) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 C29 1.50(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.38(2) . ? C29 C34 1.45(2) . ? C30 C31 1.37(2) . ? C30 H30A 0.9400 . ? C31 C32 1.39(2) . ? C31 C35 1.56(3) . ? C32 C33 1.44(2) . ? C32 H32A 0.9400 . ? C33 C34 1.36(2) . ? C33 C42 1.54(2) . ? C35 C36 1.52(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.34(3) . ? C36 C41 1.40(3) . ? C37 C38 1.47(4) . ? C37 H37A 0.9400 . ? C38 C39 1.41(4) . ? C38 H38A 0.9400 . ? C39 C40 1.30(3) . ? C39 H39A 0.9400 . ? C40 C41 1.39(3) . ? C40 H40A 0.9400 . ? C41 H41A 0.9400 . ? C42 C43 1.48(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.36(2) . ? C43 C48 1.41(2) . ? C44 C45 1.40(3) . ? C44 H44A 0.9400 . ? C45 C46 1.36(3) . ? C45 C49 1.52(3) . ? C46 C47 1.38(2) . ? C46 H46A 0.9400 . ? C47 C48 1.42(2) . ? C47 C56 1.55(2) . ? C49 C50 1.56(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.29(3) . ? C50 C55 1.34(4) . ? C51 C52 1.32(4) . ? C51 H51A 0.9400 . ? C52 C53 1.43(4) . ? C52 H52A 0.9400 . ? C53 C54 1.32(4) . ? C53 H53A 0.9400 . ? C54 C55 1.48(4) . ? C54 H54A 0.9400 . ? C55 H55A 0.9400 . ? C56 C57 1.50(2) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.36(2) . ? C57 C62 1.406(19) . ? C58 C59 1.44(2) . ? C58 H58A 0.9400 . ? C59 C60 1.42(2) . ? C59 C63 1.49(3) . ? C60 C61 1.39(2) . ? C60 H60A 0.9400 . ? C61 C62 1.41(2) . ? C61 C70 1.53(2) . ? C63 C64 1.49(4) . ? C63 C69 2.01(5) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C64 C65 1.39(3) . ? C64 C69 1.39(2) . ? C65 C66 1.48(4) . ? C65 H65A 0.9400 . ? C66 C67 1.43(3) . ? C66 H66A 0.9400 . ? C67 C68 1.40(3) . ? C67 H67A 0.9400 . ? C68 C69 1.42(3) . ? C68 H68A 0.9400 . ? C69 H69A 0.9400 . ? C70 C71 1.50(2) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C71 C72 1.39(2) . ? C71 C76 1.41(2) . ? C72 C73 1.38(2) . ? C72 H72A 0.9400 . ? C73 C74 1.36(2) . ? C73 C77 1.55(3) . ? C74 C75 1.35(2) . ? C74 H74A 0.9400 . ? C75 C76 1.43(2) . ? C75 C84 1.56(2) . ? C77 C78 1.51(3) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C78 C83 1.33(3) . ? C78 C79 1.42(3) . ? C79 C80 1.43(3) . ? C79 H79A 0.9400 . ? C80 C81 1.44(3) . ? C80 H80A 0.9400 . ? C81 C82 1.32(3) . ? C81 H81A 0.9400 . ? C82 C83 1.39(3) . ? C82 H82A 0.9400 . ? C245 N2 1.14(3) . ? C83 H83A 0.9400 . ? C84 C85 1.51(2) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C85 C90 1.403(19) . ? C85 C86 1.43(2) . ? C86 C87 1.40(2) . ? C86 H86A 0.9400 . ? C87 C88 1.33(2) . ? C87 C91 1.46(3) . ? C88 C89 1.37(2) . ? C88 H88A 0.9400 . ? C89 C90 1.395(18) . ? C89 C98 1.55(2) . ? C91 C92 1.56(3) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C92 C97 1.38(2) . ? C92 C93 1.44(2) . ? C93 C94 1.41(2) . ? C93 H93A 0.9400 . ? C94 C95 1.32(2) . ? C94 H94A 0.9400 . ? C95 C96 1.35(2) . ? C95 H95A 0.9400 . ? C96 C97 1.40(2) . ? C96 H96A 0.9400 . ? C97 H97A 0.9400 . ? C98 C99 1.53(2) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C99 C100 1.399(19) . ? C99 C104 1.407(19) . ? C100 C101 1.36(2) . ? C100 H10B 0.9400 . ? C101 C102 1.42(2) . ? C101 C105 1.50(3) . ? C102 C103 1.413(19) . ? C102 H10C 0.9400 . ? C103 C104 1.422(18) . ? C103 C112 1.45(2) . ? C105 C111 1.41(3) . ? C105 H10D 0.9800 . ? C105 H10E 0.9800 . ? C106 C111 1.40(2) . ? C106 C107 1.41(2) . ? C106 H10F 0.9400 . ? C107 C108 1.33(2) . ? C107 H10G 0.9400 . ? C108 C109 1.43(3) . ? C108 H10H 0.9400 . ? C109 C110 1.41(2) . ? C109 H10I 0.9400 . ? C110 C111 1.39(2) . ? C110 H11B 0.9400 . ? C112 H11C 0.9800 . ? C112 H11H 0.9800 . ? C113 C118 1.381(18) . ? C113 C114 1.422(18) . ? C114 C115 1.383(18) . ? C114 C224 1.52(2) . ? C115 C116 1.354(19) . ? C115 H11D 0.9400 . ? C116 C117 1.38(2) . ? C116 C119 1.49(2) . ? C117 C118 1.387(19) . ? C117 H11E 0.9400 . ? C118 C126 1.50(2) . ? C119 C120 1.49(2) . ? C119 H11F 0.9800 . ? C119 H11G 0.9800 . ? C120 C125 1.36(3) . ? C120 C121 1.41(2) . ? C121 C122 1.33(3) . ? C121 H12B 0.9400 . ? C122 C123 1.30(3) . ? C122 H12C 0.9400 . ? C123 C124 1.44(4) . ? C123 H12D 0.9400 . ? C124 C125 1.43(4) . ? C124 H12E 0.9400 . ? C125 H12F 0.9400 . ? C126 C127 1.51(2) . ? C126 H12G 0.9800 . ? C126 H12I 0.9800 . ? C127 C128 1.374(18) . ? C127 C132 1.410(19) . ? C128 C129 1.44(2) . ? C128 H12H 0.9400 . ? C129 C130 1.36(2) . ? C129 C133 1.46(2) . ? C130 C131 1.39(2) . ? C130 H13B 0.9400 . ? C131 C132 1.43(2) . ? C131 C140 1.52(2) . ? C133 C134 1.44(3) . ? C133 H13C 0.9800 . ? C133 H13D 0.9800 . ? C134 C135 1.37(2) . ? C134 C139 1.41(2) . ? C135 C136 1.44(3) . ? C135 H13E 0.9400 . ? C136 C137 1.35(3) . ? C136 H13F 0.9400 . ? C137 C138 1.40(3) . ? C137 H13G 0.9400 . ? C138 C139 1.44(3) . ? C138 H13H 0.9400 . ? C139 H13J 0.9400 . ? C140 C141 1.54(2) . ? C140 H14C 0.9800 . ? C140 H14D 0.9800 . ? C141 C146 1.38(2) . ? C141 C142 1.41(2) . ? C142 C143 1.39(2) . ? C142 H14E 0.9400 . ? C143 C144 1.34(2) . ? C143 C147 1.53(3) . ? C144 C145 1.41(2) . ? C144 H14F 0.9400 . ? C145 C146 1.41(2) . ? C145 C154 1.55(2) . ? C147 C148 1.51(3) . ? C147 H14G 0.9800 . ? C147 H14H 0.9800 . ? C148 C153 1.37(2) . ? C148 C149 1.43(3) . ? C149 C150 1.41(3) . ? C149 H14I 0.9400 . ? C150 C151 1.34(3) . ? C150 H15A 0.9400 . ? C151 C152 1.41(3) . ? C151 H15B 0.9400 . ? C152 C153 1.43(3) . ? C152 H15C 0.9400 . ? C153 H15D 0.9400 . ? C154 C155 1.50(2) . ? C154 H15F 0.9800 . ? C154 H15G 0.9800 . ? C155 C160 1.35(2) . ? C155 C156 1.38(2) . ? C157 C158 1.37(3) . ? C157 C156 1.38(2) . ? C157 C161 1.53(3) . ? C158 C159 1.44(3) . ? C158 H15H 0.9400 . ? C159 C168 1.47(3) . ? C159 C160 1.48(2) . ? C161 C162 1.43(3) . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? C162 C167 1.38(2) . ? C162 C163 1.40(2) . ? C163 C164 1.38(2) . ? C163 H16D 0.9400 . ? C164 C165 1.36(2) . ? C164 H16E 0.9400 . ? C165 C166 1.37(3) . ? C165 H16F 0.9400 . ? C166 C167 1.37(2) . ? C166 H16G 0.9400 . ? C167 H16H 0.9400 . ? C168 C169 1.50(2) . ? C168 H16I 0.9800 . ? C168 H16J 0.9800 . ? C169 C174 1.406(19) . ? C169 C170 1.41(2) . ? C170 C171 1.39(2) . ? C170 H17A 0.9400 . ? C171 C172 1.40(2) . ? C171 C175 1.54(3) . ? C172 C173 1.31(2) . ? C172 H17B 0.9400 . ? C173 C174 1.432(19) . ? C173 C182 1.48(2) . ? C175 C176 1.44(3) . ? C175 H17C 0.9800 . ? C175 H17D 0.9800 . ? C176 C181 1.39(2) . ? C176 C177 1.42(2) . ? C177 C178 1.40(2) . ? C177 H17E 0.9400 . ? C178 C179 1.40(2) . ? C178 H17F 0.9400 . ? C179 C180 1.31(2) . ? C179 H17G 0.9400 . ? C180 C181 1.44(2) . ? C180 H18B 0.9400 . ? C181 H18C 0.9400 . ? C182 C183 1.47(2) . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C183 C188 1.40(2) . ? C183 C184 1.48(3) . ? C184 C185 1.38(3) . ? C184 H18F 0.9400 . ? C185 C186 1.47(4) . ? C185 H18G 0.9400 . ? C186 C187 1.48(3) . ? C186 H18H 0.9400 . ? C187 C188 1.37(2) . ? C187 C196 1.49(3) . ? C196 C197 1.54(3) . ? C196 H19A 0.9800 . ? C196 H19B 0.9800 . ? C197 C198 1.42(3) . ? C197 C202 1.45(2) . ? C198 C199 1.40(3) . ? C198 H19C 0.9400 . ? C199 C200 1.40(3) . ? C199 C203 1.54(3) . ? C200 C201 1.43(2) . ? C200 H20A 0.9400 . ? C201 C202 1.40(2) . ? C201 C210 1.50(2) . ? C202 Bi8 2.861(16) . ? C203 C204 1.45(3) . ? C203 H20B 0.9800 . ? C203 H20C 0.9800 . ? C204 C205 1.38(3) . ? C204 C209 1.39(3) . ? C205 C206 1.32(3) . ? C205 H20D 0.9400 . ? C206 C207 1.35(4) . ? C206 H20E 0.9400 . ? C207 C208 1.35(4) . ? C207 H20F 0.9400 . ? C208 C209 1.33(3) . ? C208 H20G 0.9400 . ? C209 H20H 0.9400 . ? C210 C211 1.52(2) . ? C210 H21C 0.9800 . ? C210 H21D 0.9800 . ? C211 C212 1.40(2) . ? C211 C216 1.47(2) . ? C212 C213 1.36(3) . ? C212 H21E 0.9400 . ? C213 C214 1.36(3) . ? C213 C217 1.56(2) . ? C214 C215 1.41(2) . ? C214 H21F 0.9400 . ? C215 C216 1.38(2) . ? C215 C224 1.50(2) . ? C217 C223 1.50(3) . ? C217 H21G 0.9800 . ? C217 H21H 0.9800 . ? C218 C223 1.39(3) . ? C218 C219 1.47(4) . ? C218 H21I 0.9400 . ? C219 C220 1.29(4) . ? C219 H21K 0.9400 . ? C220 C221 1.33(4) . ? C220 H22A 0.9400 . ? C221 C222 1.36(4) . ? C221 H22B 0.9400 . ? C222 C223 1.45(3) . ? C222 H22C 0.9400 . ? C224 H22D 0.9800 . ? C224 H22E 0.9800 . ? C225 C226 1.26(3) . ? C225 C230 1.37(3) . ? C225 H22G 0.9400 . ? C226 C227 1.34(3) . ? C226 H22F 0.9400 . ? C227 C228 1.44(3) . ? C227 H22H 0.9400 . ? C228 C229 1.24(3) . ? C228 H22I 0.9400 . ? C229 C230 1.42(3) . ? C229 H22J 0.9400 . ? C230 H23E 0.9400 . ? C231 C232 1.34(3) . ? C231 C236 1.40(3) . ? C231 H23F 0.9400 . ? C232 C233 1.33(3) . ? C232 H23G 0.9400 . ? C233 C234 1.32(3) . ? C233 H23H 0.9400 . ? C234 C235 1.29(3) . ? C234 H23I 0.9400 . ? C235 C236 1.43(3) . ? C235 H23J 0.9400 . ? C236 H23K 0.9400 . ? C237 C242 1.33(2) . ? C237 C238 1.37(3) . ? C237 H23B 0.9400 . ? C238 C239 1.32(2) . ? C238 H23C 0.9400 . ? C239 C240 1.42(2) . ? C239 H23D 0.9400 . ? C240 C241 1.37(2) . ? C240 H24E 0.9400 . ? C241 C242 1.29(3) . ? C241 H24G 0.9400 . ? C242 H24H 0.9400 . ? C243 N1 1.14(2) . ? C243 C244 1.47(3) . ? C301 C302 1.35(2) . ? C301 C300 1.38(3) . ? C301 H30B 0.9400 . ? C304 C305 1.29(2) . ? C304 C303 1.38(2) . ? C304 H30C 0.9400 . ? C302 C303 1.44(2) . ? C302 H30D 0.9400 . ? C305 C300 1.30(2) . ? C305 H30E 0.9400 . ? C303 H30F 0.9400 . ? C300 H30H 0.9400 . ? Bi5 Bi6 3.6989(11) . ? N2 Bi7 2.740(17) . ? Bi7 Bi8 3.6933(11) . ? C156 H15I 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 O18 Bi1 O17 69.1(3) . . ? O18 Bi1 O1 70.5(3) . . ? O17 Bi1 O1 117.1(3) . . ? O18 Bi1 O2 114.6(3) . . ? O17 Bi1 O2 69.9(3) . . ? O1 Bi1 O2 86.2(3) . . ? O18 Bi1 O19 72.0(3) . . ? O17 Bi1 O19 78.6(3) . . ? O1 Bi1 O19 129.1(3) . . ? O2 Bi1 O19 141.3(3) . . ? O18 Bi1 Bi2 93.4(2) . . ? O17 Bi1 Bi2 31.5(2) . . ? O1 Bi1 Bi2 110.3(2) . . ? O2 Bi1 Bi2 39.2(2) . . ? O19 Bi1 Bi2 105.1(2) . . ? O18 Bi1 Bi4 31.4(2) . . ? O17 Bi1 Bi4 93.5(3) . . ? O1 Bi1 Bi4 39.5(2) . . ? O2 Bi1 Bi4 107.8(3) . . ? O19 Bi1 Bi4 95.6(2) . . ? Bi2 Bi1 Bi4 107.33(2) . . ? C1 O1 Bi1 137.0(9) . . ? C1 O1 Bi4 119.1(8) . . ? Bi1 O1 Bi4 103.3(3) . . ? C20 O2 Bi1 126.2(8) . . ? C20 O2 Bi2 128.1(8) . . ? Bi1 O2 Bi2 103.6(3) . . ? C34 O3 Bi2 108.6(8) . . ? C48 O4 Bi2 109.9(9) . . ? C62 O5 Bi3 139.7(9) . . ? C62 O5 Bi2 118.7(9) . . ? Bi3 O5 Bi2 101.4(4) . . ? C76 O6 Bi3 133.6(8) . . ? C76 O6 Bi4 119.3(8) . . ? Bi3 O6 Bi4 105.4(4) . . ? C90 O7 Bi4 113.7(9) . . ? C104 O8 Bi4 110.3(8) . . ? C113 O9 Bi5 132.0(9) . . ? C113 O9 Bi6 123.7(8) . . ? Bi5 O9 Bi6 102.7(4) . . ? C132 O10 Bi6 108.1(9) . . ? C146 O11 Bi6 113.7(9) . . ? C160 O12 Bi7 130.8(9) . . ? C160 O12 Bi6 119.9(9) . . ? Bi7 O12 Bi6 105.6(4) . . ? C174 O13 Bi7 138.5(11) . . ? C174 O13 Bi8 119.7(10) . . ? Bi7 O13 Bi8 101.4(4) . . ? C188 O14 Bi8 111.9(9) . . ? C202 O15 Bi8 107.5(9) . . ? C216 O16 Bi5 126.8(8) . . ? C216 O16 Bi8 126.5(8) . . ? Bi5 O16 Bi8 104.1(4) . . ? Bi2 O17 Bi1 114.5(4) . . ? Bi2 O17 Bi3 114.2(4) . . ? Bi1 O17 Bi3 111.4(4) . . ? Bi4 O18 Bi1 115.9(4) . . ? Bi4 O18 Bi3 113.2(4) . . ? Bi1 O18 Bi3 112.0(3) . . ? Bi4 O18 Bi5 104.5(3) . . ? Bi1 O18 Bi5 103.8(3) . . ? Bi3 O18 Bi5 106.2(3) . . ? Bi6 O19 Bi5 115.7(4) . . ? Bi6 O19 Bi7 115.1(4) . . ? Bi5 O19 Bi7 111.7(4) . . ? Bi6 O19 Bi1 104.6(3) . . ? Bi5 O19 Bi1 102.1(3) . . ? Bi7 O19 Bi1 106.0(3) . . ? Bi8 O20 Bi7 114.4(4) . . ? Bi8 O20 Bi5 114.3(4) . . ? Bi7 O20 Bi5 111.4(4) . . ? Bi3 O21 Bi7 91.9(3) . . ? C6 C1 O1 122.3(12) . . ? C6 C1 C2 119.1(14) . . ? O1 C1 C2 118.5(13) . . ? C3 C2 C1 117.8(15) . . ? C3 C2 C112 119.1(14) . . ? C1 C2 C112 122.6(14) . . ? C2 C3 C4 122.8(15) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 118.3(14) . . ? C5 C4 C7 118.8(16) . . ? C3 C4 C7 122.7(15) . . ? C4 C5 C6 122.8(16) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C1 C6 C5 118.8(14) . . ? C1 C6 C14 119.0(12) . . ? C5 C6 C14 122.0(14) . . ? C8 C7 C4 116.1(18) . . ? C8 C7 H7A 108.3 . . ? C4 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C4 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C13 119(2) . . ? C9 C8 C7 119(2) . . ? C13 C8 C7 122(2) . . ? C8 C9 C10 121(3) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 118(3) . . ? C11 C10 H10A 121.2 . . ? C9 C10 H10A 121.2 . . ? C12 C11 C10 123(3) . . ? C12 C11 H11A 118.5 . . ? C10 C11 H11A 118.5 . . ? C11 C12 C13 122(3) . . ? C11 C12 H12A 119.2 . . ? C13 C12 H12A 119.2 . . ? C12 C13 C8 118(3) . . ? C12 C13 H13A 121.0 . . ? C8 C13 H13A 121.0 . . ? C15 C14 C6 109.7(13) . . ? C15 C14 H14A 109.7 . . ? C6 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C6 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C20 119.5(14) . . ? C16 C15 C14 122.4(14) . . ? C20 C15 C14 118.1(13) . . ? C15 C16 C17 122.3(16) . . ? C15 C16 H16A 118.9 . . ? C17 C16 H16A 118.9 . . ? C18 C17 C16 118.3(15) . . ? C18 C17 C21 120.6(16) . . ? C16 C17 C21 121.0(16) . . ? C17 C18 C19 124.1(16) . . ? C17 C18 H18A 118.0 . . ? C19 C18 H18A 118.0 . . ? C18 C19 C20 116.1(16) . . ? C18 C19 C28 121.9(15) . . ? C20 C19 C28 122.0(14) . . ? O2 C20 C15 122.6(14) . . ? O2 C20 C19 118.1(14) . . ? C15 C20 C19 119.2(14) . . ? C22 C21 C17 113.1(17) . . ? C22 C21 H21A 109.0 . . ? C17 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C17 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 122(2) . . ? C27 C22 C21 116(2) . . ? C23 C22 C21 122(2) . . ? C22 C23 C24 123(2) . . ? C22 C23 H23A 118.4 . . ? C24 C23 H23A 118.4 . . ? C245 C246 H24A 109.5 . . ? C245 C246 H24B 109.5 . . ? H24A C246 H24B 109.5 . . ? C245 C246 H24C 109.5 . . ? H24A C246 H24C 109.5 . . ? H24B C246 H24C 109.5 . . ? C25 C24 C23 114(3) . . ? C25 C24 H24D 123.0 . . ? C23 C24 H24D 123.0 . . ? C24 C25 C26 124(3) . . ? C24 C25 H25A 118.0 . . ? C26 C25 H25A 118.0 . . ? C27 C26 C25 117(3) . . ? C27 C26 H26A 121.5 . . ? C25 C26 H26A 121.5 . . ? C22 C27 C26 119(3) . . ? C22 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C29 C28 C19 114.3(13) . . ? C29 C28 H28A 108.7 . . ? C19 C28 H28A 108.7 . . ? C29 C28 H28B 108.7 . . ? C19 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C34 117.1(15) . . ? C30 C29 C28 122.9(15) . . ? C34 C29 C28 120.0(12) . . ? C31 C30 C29 123.8(18) . . ? C31 C30 H30A 118.1 . . ? C29 C30 H30A 118.1 . . ? C30 C31 C32 118.3(17) . . ? C30 C31 C35 123.8(18) . . ? C32 C31 C35 117.9(17) . . ? C31 C32 C33 120.6(17) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 119.2(15) . . ? C34 C33 C42 123.8(13) . . ? C32 C33 C42 117.1(15) . . ? O3 C34 C33 122.7(14) . . ? O3 C34 C29 116.3(13) . . ? C33 C34 C29 121.0(13) . . ? C36 C35 C31 110.7(17) . . ? C36 C35 H35A 109.5 . . ? C31 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C37 C36 C41 117(2) . . ? C37 C36 C35 121(2) . . ? C41 C36 C35 121(2) . . ? C36 C37 C38 123(3) . . ? C36 C37 H37A 118.5 . . ? C38 C37 H37A 118.5 . . ? C39 C38 C37 115(3) . . ? C39 C38 H38A 122.5 . . ? C37 C38 H38A 122.5 . . ? C40 C39 C38 121(3) . . ? C40 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? C39 C40 C41 122(3) . . ? C39 C40 H40A 119.0 . . ? C41 C40 H40A 119.0 . . ? C40 C41 C36 121(2) . . ? C40 C41 H41A 119.6 . . ? C36 C41 H41A 119.6 . . ? C43 C42 C33 118.9(15) . . ? C43 C42 H42A 107.6 . . ? C33 C42 H42A 107.6 . . ? C43 C42 H42B 107.6 . . ? C33 C42 H42B 107.6 . . ? H42A C42 H42B 107.0 . . ? C44 C43 C48 116.9(17) . . ? C44 C43 C42 119.9(19) . . ? C48 C43 C42 123.1(15) . . ? C43 C44 C45 123.6(18) . . ? C43 C44 H44A 118.2 . . ? C45 C44 H44A 118.2 . . ? C46 C45 C44 115.3(17) . . ? C46 C45 C49 119(2) . . ? C44 C45 C49 125(2) . . ? C45 C46 C47 127(2) . . ? C45 C46 H46A 116.4 . . ? C47 C46 H46A 116.4 . . ? C46 C47 C48 113.6(16) . . ? C46 C47 C56 126.7(16) . . ? C48 C47 C56 119.1(14) . . ? O4 C48 C43 118.5(15) . . ? O4 C48 C47 118.3(14) . . ? C43 C48 C47 123.1(15) . . ? C45 C49 C50 112.0(18) . . ? C45 C49 H49A 109.2 . . ? C50 C49 H49A 109.2 . . ? C45 C49 H49B 109.2 . . ? C50 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C51 C50 C55 119(3) . . ? C51 C50 C49 124(3) . . ? C55 C50 C49 117(3) . . ? C50 C51 C52 133(4) . . ? C50 C51 H51A 113.7 . . ? C52 C51 H51A 113.7 . . ? C51 C52 C53 110(4) . . ? C51 C52 H52A 125.0 . . ? C53 C52 H52A 125.0 . . ? C54 C53 C52 123(4) . . ? C54 C53 H53A 118.4 . . ? C52 C53 H53A 118.4 . . ? C53 C54 C55 120(4) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.1 . . ? C50 C55 C54 115(3) . . ? C50 C55 H55A 122.3 . . ? C54 C55 H55A 122.3 . . ? C57 C56 C47 110.2(14) . . ? C57 C56 H56A 109.6 . . ? C47 C56 H56A 109.6 . . ? C57 C56 H56B 109.6 . . ? C47 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C58 C57 C62 120.6(15) . . ? C58 C57 C56 117.1(13) . . ? C62 C57 C56 122.3(14) . . ? C57 C58 C59 122.5(16) . . ? C57 C58 H58A 118.7 . . ? C59 C58 H58A 118.7 . . ? C60 C59 C58 115.1(16) . . ? C60 C59 C63 122.6(17) . . ? C58 C59 C63 122.3(17) . . ? C61 C60 C59 123.1(15) . . ? C61 C60 H60A 118.5 . . ? C59 C60 H60A 118.5 . . ? C60 C61 C62 119.1(14) . . ? C60 C61 C70 118.1(14) . . ? C62 C61 C70 122.5(14) . . ? O5 C62 C57 119.7(13) . . ? O5 C62 C61 120.9(13) . . ? C57 C62 C61 119.4(14) . . ? C59 C63 C64 110(3) . . ? C59 C63 C69 119.4(19) . . ? C64 C63 C69 44.0(15) . . ? C59 C63 H63A 109.7 . . ? C64 C63 H63A 109.7 . . ? C69 C63 H63A 129.6 . . ? C59 C63 H63B 109.7 . . ? C64 C63 H63B 109.7 . . ? C69 C63 H63B 66.2 . . ? H63A C63 H63B 108.2 . . ? C65 C64 C69 123(3) . . ? C65 C64 C63 148(4) . . ? C69 C64 C63 88(3) . . ? C64 C65 C66 115(3) . . ? C64 C65 H65A 122.4 . . ? C66 C65 H65A 122.4 . . ? C67 C66 C65 115(3) . . ? C67 C66 H66A 122.4 . . ? C65 C66 H66A 122.4 . . ? C68 C67 C66 127(3) . . ? C68 C67 H67A 116.5 . . ? C66 C67 H67A 116.5 . . ? C67 C68 C69 112(3) . . ? C67 C68 H68A 124.1 . . ? C69 C68 H68A 124.1 . . ? C64 C69 C68 122(3) . . ? C64 C69 C63 48(2) . . ? C68 C69 C63 167(4) . . ? C64 C69 H69A 118.9 . . ? C68 C69 H69A 118.9 . . ? C63 C69 H69A 71.8 . . ? C71 C70 C61 109.7(13) . . ? C71 C70 H70A 109.7 . . ? C61 C70 H70A 109.7 . . ? C71 C70 H70B 109.7 . . ? C61 C70 H70B 109.7 . . ? H70A C70 H70B 108.2 . . ? C72 C71 C76 118.7(16) . . ? C72 C71 C70 120.6(15) . . ? C76 C71 C70 120.7(15) . . ? C73 C72 C71 121.7(16) . . ? C73 C72 H72A 119.2 . . ? C71 C72 H72A 119.2 . . ? C74 C73 C72 119.3(17) . . ? C74 C73 C77 121.0(17) . . ? C72 C73 C77 119.6(16) . . ? C75 C74 C73 121.7(17) . . ? C75 C74 H74A 119.1 . . ? C73 C74 H74A 119.1 . . ? C74 C75 C76 120.7(16) . . ? C74 C75 C84 121.6(15) . . ? C76 C75 C84 117.7(15) . . ? O6 C76 C71 119.5(15) . . ? O6 C76 C75 123.1(15) . . ? C71 C76 C75 117.3(15) . . ? C78 C77 C73 109.7(16) . . ? C78 C77 H77A 109.7 . . ? C73 C77 H77A 109.7 . . ? C78 C77 H77B 109.7 . . ? C73 C77 H77B 109.7 . . ? H77A C77 H77B 108.2 . . ? C83 C78 C79 118(2) . . ? C83 C78 C77 124.0(19) . . ? C79 C78 C77 118.3(19) . . ? C78 C79 C80 118(2) . . ? C78 C79 H79A 120.9 . . ? C80 C79 H79A 120.9 . . ? C79 C80 C81 123(2) . . ? C79 C80 H80A 118.6 . . ? C81 C80 H80A 118.6 . . ? C82 C81 C80 112(3) . . ? C82 C81 H81A 123.8 . . ? C80 C81 H81A 123.8 . . ? C81 C82 C83 127(3) . . ? C81 C82 H82A 116.5 . . ? C83 C82 H82A 116.5 . . ? N2 C245 C246 174(3) . . ? C78 C83 C82 122(2) . . ? C78 C83 H83A 119.2 . . ? C82 C83 H83A 119.2 . . ? C85 C84 C75 118.3(13) . . ? C85 C84 H84A 107.7 . . ? C75 C84 H84A 107.7 . . ? C85 C84 H84B 107.7 . . ? C75 C84 H84B 107.7 . . ? H84A C84 H84B 107.1 . . ? C90 C85 C86 119.0(15) . . ? C90 C85 C84 120.3(14) . . ? C86 C85 C84 120.7(16) . . ? C87 C86 C85 117.3(16) . . ? C87 C86 H86A 121.3 . . ? C85 C86 H86A 121.3 . . ? C88 C87 C86 121.6(15) . . ? C88 C87 C91 122.3(19) . . ? C86 C87 C91 116.1(18) . . ? C87 C88 C89 122.7(17) . . ? C87 C88 H88A 118.6 . . ? C89 C88 H88A 118.6 . . ? C88 C89 C90 118.7(16) . . ? C88 C89 C98 120.5(16) . . ? C90 C89 C98 120.2(14) . . ? O7 C90 C89 120.9(14) . . ? O7 C90 C85 118.7(13) . . ? C89 C90 C85 120.3(14) . . ? C87 C91 C92 115(2) . . ? C87 C91 H91A 108.5 . . ? C92 C91 H91A 108.5 . . ? C87 C91 H91B 108.5 . . ? C92 C91 H91B 108.5 . . ? H91A C91 H91B 107.5 . . ? C97 C92 C93 121.7(19) . . ? C97 C92 C91 116.4(18) . . ? C93 C92 C91 121.6(19) . . ? C94 C93 C92 114.1(19) . . ? C94 C93 H93A 122.9 . . ? C92 C93 H93A 122.9 . . ? C95 C94 C93 122(2) . . ? C95 C94 H94A 119.1 . . ? C93 C94 H94A 119.1 . . ? C94 C95 C96 125(2) . . ? C94 C95 H95A 117.7 . . ? C96 C95 H95A 117.7 . . ? C95 C96 C97 118(2) . . ? C95 C96 H96A 121.1 . . ? C97 C96 H96A 121.1 . . ? C92 C97 C96 119.2(18) . . ? C92 C97 H97A 120.4 . . ? C96 C97 H97A 120.4 . . ? C99 C98 C89 116.3(14) . . ? C99 C98 H98A 108.2 . . ? C89 C98 H98A 108.2 . . ? C99 C98 H98B 108.2 . . ? C89 C98 H98B 108.2 . . ? H98A C98 H98B 107.4 . . ? C100 C99 C104 117.4(15) . . ? C100 C99 C98 117.7(14) . . ? C104 C99 C98 124.7(13) . . ? C101 C100 C99 124.1(17) . . ? C101 C100 H10B 117.9 . . ? C99 C100 H10B 117.9 . . ? C100 C101 C102 116.5(16) . . ? C100 C101 C105 124.1(18) . . ? C102 C101 C105 118.6(18) . . ? C103 C102 C101 124.1(15) . . ? C103 C102 H10C 118.0 . . ? C101 C102 H10C 118.0 . . ? C102 C103 C104 115.1(13) . . ? C102 C103 C112 124.7(13) . . ? C104 C103 C112 120.2(13) . . ? O8 C104 C99 116.6(13) . . ? O8 C104 C103 120.8(12) . . ? C99 C104 C103 122.6(13) . . ? C111 C105 C101 118(2) . . ? C111 C105 H10D 107.9 . . ? C101 C105 H10D 107.9 . . ? C111 C105 H10E 107.9 . . ? C101 C105 H10E 107.9 . . ? H10D C105 H10E 107.2 . . ? C111 C106 C107 115(2) . . ? C111 C106 H10F 122.3 . . ? C107 C106 H10F 122.3 . . ? C108 C107 C106 122(3) . . ? C108 C107 H10G 119.1 . . ? C106 C107 H10G 119.1 . . ? C107 C108 C109 123(2) . . ? C107 C108 H10H 118.5 . . ? C109 C108 H10H 118.5 . . ? C110 C109 C108 116(2) . . ? C110 C109 H10I 121.8 . . ? C108 C109 H10I 121.8 . . ? C111 C110 C109 118(2) . . ? C111 C110 H11B 120.8 . . ? C109 C110 H11B 120.8 . . ? C110 C111 C106 124(2) . . ? C110 C111 C105 112(2) . . ? C106 C111 C105 124(2) . . ? C103 C112 C2 118.1(14) . . ? C103 C112 H11C 107.8 . . ? C2 C112 H11C 107.8 . . ? C103 C112 H11H 107.8 . . ? C2 C112 H11H 107.8 . . ? H11C C112 H11H 107.1 . . ? O9 C113 C118 120.8(12) . . ? O9 C113 C114 119.4(12) . . ? C118 C113 C114 119.7(12) . . ? C115 C114 C113 117.4(13) . . ? C115 C114 C224 121.1(13) . . ? C113 C114 C224 121.4(12) . . ? C116 C115 C114 124.5(14) . . ? C116 C115 H11D 117.8 . . ? C114 C115 H11D 117.8 . . ? C115 C116 C117 115.9(14) . . ? C115 C116 C119 121.9(14) . . ? C117 C116 C119 122.2(15) . . ? C116 C117 C118 124.0(15) . . ? C116 C117 H11E 118.0 . . ? C118 C117 H11E 118.0 . . ? C113 C118 C117 118.1(13) . . ? C113 C118 C126 120.4(12) . . ? C117 C118 C126 121.4(13) . . ? C116 C119 C120 116.9(15) . . ? C116 C119 H11F 108.1 . . ? C120 C119 H11F 108.1 . . ? C116 C119 H11G 108.1 . . ? C120 C119 H11G 108.1 . . ? H11F C119 H11G 107.3 . . ? C125 C120 C121 119(2) . . ? C125 C120 C119 119(2) . . ? C121 C120 C119 121.6(16) . . ? C122 C121 C120 120(2) . . ? C122 C121 H12B 120.2 . . ? C120 C121 H12B 120.2 . . ? C123 C122 C121 126(3) . . ? C123 C122 H12C 117.0 . . ? C121 C122 H12C 117.0 . . ? C122 C123 C124 117(3) . . ? C122 C123 H12D 121.6 . . ? C124 C123 H12D 121.6 . . ? C125 C124 C123 118(4) . . ? C125 C124 H12E 121.0 . . ? C123 C124 H12E 121.0 . . ? C120 C125 C124 120(3) . . ? C120 C125 H12F 120.1 . . ? C124 C125 H12F 120.1 . . ? C118 C126 C127 118.1(13) . . ? C118 C126 H12G 107.8 . . ? C127 C126 H12G 107.8 . . ? C118 C126 H12I 107.8 . . ? C127 C126 H12I 107.8 . . ? H12G C126 H12I 107.1 . . ? C128 C127 C132 117.1(13) . . ? C128 C127 C126 124.5(13) . . ? C132 C127 C126 117.8(11) . . ? C127 C128 C129 123.7(15) . . ? C127 C128 H12H 118.2 . . ? C129 C128 H12H 118.2 . . ? C130 C129 C128 114.7(14) . . ? C130 C129 C133 123.0(18) . . ? C128 C129 C133 122.1(16) . . ? C129 C130 C131 126.3(17) . . ? C129 C130 H13B 116.9 . . ? C131 C130 H13B 116.9 . . ? C130 C131 C132 115.5(15) . . ? C130 C131 C140 122.0(16) . . ? C132 C131 C140 122.2(14) . . ? O10 C132 C127 117.2(12) . . ? O10 C132 C131 120.5(14) . . ? C127 C132 C131 122.2(13) . . ? C134 C133 C129 115.5(19) . . ? C134 C133 H13C 108.4 . . ? C129 C133 H13C 108.4 . . ? C134 C133 H13D 108.4 . . ? C129 C133 H13D 108.4 . . ? H13C C133 H13D 107.5 . . ? C135 C134 C139 113(2) . . ? C135 C134 C133 126(2) . . ? C139 C134 C133 119(2) . . ? C134 C135 C136 123(2) . . ? C134 C135 H13E 118.4 . . ? C136 C135 H13E 118.4 . . ? C137 C136 C135 117(2) . . ? C137 C136 H13F 121.4 . . ? C135 C136 H13F 121.4 . . ? C136 C137 C138 124(3) . . ? C136 C137 H13G 118.2 . . ? C138 C137 H13G 118.2 . . ? C137 C138 C139 110(3) . . ? C137 C138 H13H 125.0 . . ? C139 C138 H13H 125.0 . . ? C134 C139 C138 124(3) . . ? C134 C139 H13J 118.1 . . ? C138 C139 H13J 118.1 . . ? C131 C140 C141 116.0(14) . . ? C131 C140 H14C 108.3 . . ? C141 C140 H14C 108.3 . . ? C131 C140 H14D 108.3 . . ? C141 C140 H14D 108.3 . . ? H14C C140 H14D 107.4 . . ? C146 C141 C142 120.2(17) . . ? C146 C141 C140 121.3(16) . . ? C142 C141 C140 118.2(15) . . ? C143 C142 C141 118.1(18) . . ? C143 C142 H14E 121.0 . . ? C141 C142 H14E 121.0 . . ? C144 C143 C142 122.0(18) . . ? C144 C143 C147 123(2) . . ? C142 C143 C147 115(2) . . ? C143 C144 C145 121.4(18) . . ? C143 C144 H14F 119.3 . . ? C145 C144 H14F 119.3 . . ? C146 C145 C144 117.2(17) . . ? C146 C145 C154 119.7(17) . . ? C144 C145 C154 122.4(17) . . ? C141 C146 O11 122.0(15) . . ? C141 C146 C145 120.9(15) . . ? O11 C146 C145 117.0(15) . . ? C148 C147 C143 116(2) . . ? C148 C147 H14G 108.3 . . ? C143 C147 H14G 108.3 . . ? C148 C147 H14H 108.3 . . ? C143 C147 H14H 108.3 . . ? H14G C147 H14H 107.4 . . ? C153 C148 C149 129(3) . . ? C153 C148 C147 117(3) . . ? C149 C148 C147 113(3) . . ? C150 C149 C148 115(3) . . ? C150 C149 H14I 122.3 . . ? C148 C149 H14I 122.3 . . ? C151 C150 C149 116(3) . . ? C151 C150 H15A 121.8 . . ? C149 C150 H15A 121.8 . . ? C150 C151 C152 128(3) . . ? C150 C151 H15B 115.9 . . ? C152 C151 H15B 115.9 . . ? C151 C152 C153 117(3) . . ? C151 C152 H15C 121.4 . . ? C153 C152 H15C 121.4 . . ? C148 C153 C152 114(2) . . ? C148 C153 H15D 123.2 . . ? C152 C153 H15D 123.2 . . ? C155 C154 C145 114.4(14) . . ? C155 C154 H15F 108.7 . . ? C145 C154 H15F 108.7 . . ? C155 C154 H15G 108.7 . . ? C145 C154 H15G 108.7 . . ? H15F C154 H15G 107.6 . . ? C160 C155 C156 120.3(17) . . ? C160 C155 C154 119.1(15) . . ? C156 C155 C154 120.2(16) . . ? C158 C157 C156 120.8(18) . . ? C158 C157 C161 118.9(18) . . ? C156 C157 C161 120(2) . . ? C157 C158 C159 121.6(18) . . ? C157 C158 H15H 119.2 . . ? C159 C158 H15H 119.2 . . ? C158 C159 C168 123.1(17) . . ? C158 C159 C160 114.5(19) . . ? C168 C159 C160 121.7(16) . . ? C155 C160 O12 125.0(16) . . ? C155 C160 C159 121.9(16) . . ? O12 C160 C159 113.1(16) . . ? C162 C161 C157 116(2) . . ? C162 C161 H16B 108.3 . . ? C157 C161 H16B 108.3 . . ? C162 C161 H16C 108.3 . . ? C157 C161 H16C 108.3 . . ? H16B C161 H16C 107.4 . . ? C167 C162 C163 118(2) . . ? C167 C162 C161 124(2) . . ? C163 C162 C161 118(2) . . ? C164 C163 C162 119(2) . . ? C164 C163 H16D 120.3 . . ? C162 C163 H16D 120.3 . . ? C165 C164 C163 123(2) . . ? C165 C164 H16E 118.7 . . ? C163 C164 H16E 118.7 . . ? C164 C165 C166 115(2) . . ? C164 C165 H16F 122.5 . . ? C166 C165 H16F 122.5 . . ? C167 C166 C165 125(3) . . ? C167 C166 H16G 117.6 . . ? C165 C166 H16G 117.6 . . ? C166 C167 C162 118(2) . . ? C166 C167 H16H 120.9 . . ? C162 C167 H16H 120.9 . . ? C159 C168 C169 110.9(14) . . ? C159 C168 H16I 109.5 . . ? C169 C168 H16I 109.5 . . ? C159 C168 H16J 109.5 . . ? C169 C168 H16J 109.5 . . ? H16I C168 H16J 108.1 . . ? C174 C169 C170 117.6(14) . . ? C174 C169 C168 122.9(14) . . ? C170 C169 C168 119.4(15) . . ? C171 C170 C169 123.1(15) . . ? C171 C170 H17A 118.5 . . ? C169 C170 H17A 118.5 . . ? C170 C171 C172 114.2(15) . . ? C170 C171 C175 121.7(16) . . ? C172 C171 C175 124.1(16) . . ? C173 C172 C171 127.4(16) . . ? C173 C172 H17B 116.3 . . ? C171 C172 H17B 116.3 . . ? C172 C173 C174 117.5(15) . . ? C172 C173 C182 120.2(15) . . ? C174 C173 C182 122.3(13) . . ? O13 C174 C169 120.2(13) . . ? O13 C174 C173 120.2(13) . . ? C169 C174 C173 119.7(13) . . ? C176 C175 C171 116(2) . . ? C176 C175 H17C 108.2 . . ? C171 C175 H17C 108.2 . . ? C176 C175 H17D 108.2 . . ? C171 C175 H17D 108.2 . . ? H17C C175 H17D 107.4 . . ? C181 C176 C177 118.0(18) . . ? C181 C176 C175 121(2) . . ? C177 C176 C175 121(2) . . ? C178 C177 C176 124(2) . . ? C178 C177 H17E 118.1 . . ? C176 C177 H17E 118.1 . . ? C177 C178 C179 112(2) . . ? C177 C178 H17F 124.2 . . ? C179 C178 H17F 124.2 . . ? C180 C179 C178 131(2) . . ? C180 C179 H17G 114.7 . . ? C178 C179 H17G 114.7 . . ? C179 C180 C181 116(2) . . ? C179 C180 H18B 122.2 . . ? C181 C180 H18B 122.2 . . ? C176 C181 C180 120(2) . . ? C176 C181 H18C 119.9 . . ? C180 C181 H18C 119.9 . . ? C183 C182 C173 118.0(15) . . ? C183 C182 H18D 107.8 . . ? C173 C182 H18D 107.8 . . ? C183 C182 H18E 107.8 . . ? C173 C182 H18E 107.8 . . ? H18D C182 H18E 107.1 . . ? C188 C183 C182 120.2(16) . . ? C188 C183 C184 117.1(17) . . ? C182 C183 C184 122.6(18) . . ? C185 C184 C183 124(2) . . ? C185 C184 H18F 118.0 . . ? C183 C184 H18F 118.0 . . ? C184 C185 C186 115(3) . . ? C184 C185 H18G 122.3 . . ? C186 C185 H18G 122.3 . . ? C185 C186 C187 122(2) . . ? C185 C186 H18H 118.9 . . ? C187 C186 H18H 119.0 . . ? C188 C187 C186 117.0(19) . . ? C188 C187 C196 125.1(17) . . ? C186 C187 C196 117.7(18) . . ? O14 C188 C187 116.6(16) . . ? O14 C188 C183 119.0(15) . . ? C187 C188 C183 124.2(16) . . ? C187 C196 C197 116.4(17) . . ? C187 C196 H19A 108.2 . . ? C197 C196 H19A 108.2 . . ? C187 C196 H19B 108.2 . . ? C197 C196 H19B 108.2 . . ? H19A C196 H19B 107.3 . . ? C198 C197 C202 120(2) . . ? C198 C197 C196 119.0(18) . . ? C202 C197 C196 120.8(17) . . ? C199 C198 C197 121(2) . . ? C199 C198 H19C 119.5 . . ? C197 C198 H19C 119.5 . . ? C198 C199 C200 118(2) . . ? C198 C199 C203 120.6(19) . . ? C200 C199 C203 122(2) . . ? C199 C200 C201 123(2) . . ? C199 C200 H20A 118.3 . . ? C201 C200 H20A 118.3 . . ? C202 C201 C200 118.1(16) . . ? C202 C201 C210 120.3(14) . . ? C200 C201 C210 120.9(18) . . ? O15 C202 C201 118.9(13) . . ? O15 C202 C197 121.9(16) . . ? C201 C202 C197 119.1(16) . . ? O15 C202 Bi8 45.7(7) . . ? C201 C202 Bi8 116.2(11) . . ? C197 C202 Bi8 107.5(12) . . ? C204 C203 C199 116(2) . . ? C204 C203 H20B 108.3 . . ? C199 C203 H20B 108.3 . . ? C204 C203 H20C 108.3 . . ? C199 C203 H20C 108.3 . . ? H20B C203 H20C 107.4 . . ? C205 C204 C209 117(2) . . ? C205 C204 C203 121(2) . . ? C209 C204 C203 122(2) . . ? C206 C205 C204 120(3) . . ? C206 C205 H20D 119.8 . . ? C204 C205 H20D 119.8 . . ? C205 C206 C207 124(3) . . ? C205 C206 H20E 118.1 . . ? C207 C206 H20E 118.1 . . ? C206 C207 C208 115(3) . . ? C206 C207 H20F 122.4 . . ? C208 C207 H20F 122.3 . . ? C209 C208 C207 124(3) . . ? C209 C208 H20G 118.0 . . ? C207 C208 H20G 118.1 . . ? C208 C209 C204 119(3) . . ? C208 C209 H20H 120.3 . . ? C204 C209 H20H 120.3 . . ? C201 C210 C211 116.0(15) . . ? C201 C210 H21C 108.3 . . ? C211 C210 H21C 108.3 . . ? C201 C210 H21D 108.3 . . ? C211 C210 H21D 108.3 . . ? H21C C210 H21D 107.4 . . ? C212 C211 C216 117.3(16) . . ? C212 C211 C210 121.2(17) . . ? C216 C211 C210 121.4(14) . . ? C213 C212 C211 122.7(19) . . ? C213 C212 H21E 118.7 . . ? C211 C212 H21E 118.7 . . ? C214 C213 C212 118.9(17) . . ? C214 C213 C217 121.8(19) . . ? C212 C213 C217 118.8(19) . . ? C213 C214 C215 123.0(18) . . ? C213 C214 H21F 118.5 . . ? C215 C214 H21F 118.5 . . ? C216 C215 C214 119.0(17) . . ? C216 C215 C224 119.9(14) . . ? C214 C215 C224 121.0(15) . . ? C215 C216 O16 122.4(15) . . ? C215 C216 C211 118.8(14) . . ? O16 C216 C211 118.7(14) . . ? C223 C217 C213 114.0(17) . . ? C223 C217 H21G 108.7 . . ? C213 C217 H21G 108.8 . . ? C223 C217 H21H 108.8 . . ? C213 C217 H21H 108.8 . . ? H21G C217 H21H 107.6 . . ? C223 C218 C219 111(2) . . ? C223 C218 H21I 124.5 . . ? C219 C218 H21I 124.4 . . ? C220 C219 C218 123(3) . . ? C220 C219 H21K 118.8 . . ? C218 C219 H21K 118.7 . . ? C219 C220 C221 125(4) . . ? C219 C220 H22A 117.4 . . ? C221 C220 H22A 117.5 . . ? C220 C221 C222 119(4) . . ? C220 C221 H22B 120.3 . . ? C222 C221 H22B 120.3 . . ? C221 C222 C223 118(3) . . ? C221 C222 H22C 121.3 . . ? C223 C222 H22C 121.2 . . ? C218 C223 C222 124(2) . . ? C218 C223 C217 123(2) . . ? C222 C223 C217 113(2) . . ? C215 C224 C114 110.7(13) . . ? C215 C224 H22D 109.5 . . ? C114 C224 H22D 109.5 . . ? C215 C224 H22E 109.5 . . ? C114 C224 H22E 109.5 . . ? H22D C224 H22E 108.1 . . ? C226 C225 C230 119(3) . . ? C226 C225 H22G 120.3 . . ? C230 C225 H22G 120.3 . . ? C225 C226 C227 126(3) . . ? C225 C226 H22F 117.1 . . ? C227 C226 H22F 117.1 . . ? C226 C227 C228 114(3) . . ? C226 C227 H22H 122.9 . . ? C228 C227 H22H 122.8 . . ? C229 C228 C227 122(3) . . ? C229 C228 H22I 119.1 . . ? C227 C228 H22I 119.2 . . ? C228 C229 C230 121(3) . . ? C228 C229 H22J 119.5 . . ? C230 C229 H22J 119.5 . . ? C225 C230 C229 117(3) . . ? C225 C230 H23E 121.3 . . ? C229 C230 H23E 121.2 . . ? C232 C231 C236 114(3) . . ? C232 C231 H23F 122.9 . . ? C236 C231 H23F 123.0 . . ? C233 C232 C231 127(3) . . ? C233 C232 H23G 116.7 . . ? C231 C232 H23G 116.7 . . ? C234 C233 C232 118(3) . . ? C234 C233 H23H 121.1 . . ? C232 C233 H23H 121.2 . . ? C235 C234 C233 123(3) . . ? C235 C234 H23I 118.5 . . ? C233 C234 H23I 118.6 . . ? C234 C235 C236 119(3) . . ? C234 C235 H23J 120.3 . . ? C236 C235 H23J 120.3 . . ? C231 C236 C235 119(2) . . ? C231 C236 H23K 120.5 . . ? C235 C236 H23K 120.5 . . ? C242 C237 C238 119(2) . . ? C242 C237 H23B 120.7 . . ? C238 C237 H23B 120.7 . . ? C239 C238 C237 120(2) . . ? C239 C238 H23C 119.9 . . ? C237 C238 H23C 119.9 . . ? C238 C239 C240 121(2) . . ? C238 C239 H23D 119.5 . . ? C240 C239 H23D 119.5 . . ? C241 C240 C239 115(2) . . ? C241 C240 H24E 122.6 . . ? C239 C240 H24E 122.6 . . ? C242 C241 C240 122(2) . . ? C242 C241 H24G 118.8 . . ? C240 C241 H24G 118.8 . . ? C241 C242 C237 123(3) . . ? C241 C242 H24H 118.6 . . ? C237 C242 H24H 118.6 . . ? N1 C243 C244 175(2) . . ? C302 C301 C300 119(2) . . ? C302 C301 H30B 120.7 . . ? C300 C301 H30B 120.7 . . ? C305 C304 C303 124(2) . . ? C305 C304 H30C 117.9 . . ? C303 C304 H30C 117.9 . . ? C301 C302 C303 120(2) . . ? C301 C302 H30D 119.8 . . ? C303 C302 H30D 119.8 . . ? C304 C305 C300 122(3) . . ? C304 C305 H30E 119.0 . . ? C300 C305 H30E 119.0 . . ? C304 C303 C302 114(2) . . ? C304 C303 H30F 123.0 . . ? C302 C303 H30F 123.0 . . ? C305 C300 C301 120(2) . . ? C305 C300 H30H 119.8 . . ? C301 C300 H30H 119.8 . . ? O17 Bi2 O3 83.8(4) . . ? O17 Bi2 O4 87.6(3) . . ? O3 Bi2 O4 82.1(4) . . ? O17 Bi2 O2 70.5(3) . . ? O3 Bi2 O2 84.5(4) . . ? O4 Bi2 O2 155.4(3) . . ? O17 Bi2 O5 70.0(3) . . ? O3 Bi2 O5 148.4(3) . . ? O4 Bi2 O5 79.6(4) . . ? O2 Bi2 O5 102.2(3) . . ? O17 Bi2 Bi1 34.0(2) . . ? O3 Bi2 Bi1 77.3(3) . . ? O4 Bi2 Bi1 119.1(2) . . ? O2 Bi2 Bi1 37.3(2) . . ? O5 Bi2 Bi1 89.5(2) . . ? O5 Bi3 O6 85.1(3) . . ? O5 Bi3 O17 73.3(3) . . ? O6 Bi3 O17 114.8(3) . . ? O5 Bi3 O18 115.9(3) . . ? O6 Bi3 O18 69.8(3) . . ? O17 Bi3 O18 66.8(3) . . ? O5 Bi3 O21 87.3(3) . . ? O6 Bi3 O21 168.2(3) . . ? O17 Bi3 O21 71.3(3) . . ? O18 Bi3 O21 121.8(3) . . ? O18 Bi4 O8 78.4(3) . . ? O18 Bi4 O7 77.8(4) . . ? O8 Bi4 O7 77.5(4) . . ? O18 Bi4 O6 70.1(3) . . ? O8 Bi4 O6 143.8(3) . . ? O7 Bi4 O6 78.8(3) . . ? O18 Bi4 O1 69.5(3) . . ? O8 Bi4 O1 80.2(3) . . ? O7 Bi4 O1 143.4(4) . . ? O6 Bi4 O1 104.2(3) . . ? O18 Bi4 Bi1 32.7(2) . . ? O8 Bi4 Bi1 72.7(3) . . ? O7 Bi4 Bi1 107.7(3) . . ? O6 Bi4 Bi1 89.1(2) . . ? O1 Bi4 Bi1 37.2(2) . . ? O16 Bi5 O19 115.1(4) . . ? O16 Bi5 O9 87.2(3) . . ? O19 Bi5 O9 70.7(3) . . ? O16 Bi5 O20 70.6(3) . . ? O19 Bi5 O20 68.3(4) . . ? O9 Bi5 O20 117.5(4) . . ? O16 Bi5 O18 140.9(3) . . ? O19 Bi5 O18 71.7(3) . . ? O9 Bi5 O18 128.6(3) . . ? O20 Bi5 O18 77.9(3) . . ? O16 Bi5 Bi6 109.4(3) . . ? O19 Bi5 Bi6 31.0(2) . . ? O9 Bi5 Bi6 40.2(3) . . ? O20 Bi5 Bi6 93.0(3) . . ? O18 Bi5 Bi6 94.6(2) . . ? O19 Bi6 O11 78.4(4) . . ? O19 Bi6 O10 79.6(4) . . ? O11 Bi6 O10 79.3(4) . . ? O19 Bi6 O12 68.6(3) . . ? O11 Bi6 O12 79.1(4) . . ? O10 Bi6 O12 144.4(3) . . ? O19 Bi6 O9 69.9(3) . . ? O11 Bi6 O9 144.4(4) . . ? O10 Bi6 O9 79.3(4) . . ? O12 Bi6 O9 103.2(3) . . ? O19 Bi6 Bi5 33.4(2) . . ? O11 Bi6 Bi5 108.7(3) . . ? O10 Bi6 Bi5 72.5(3) . . ? O12 Bi6 Bi5 88.2(3) . . ? O9 Bi6 Bi5 37.1(2) . . ? C245 N2 Bi7 131.1(18) . . ? O13 Bi7 O12 84.8(4) . . ? O13 Bi7 O20 73.3(4) . . ? O12 Bi7 O20 114.7(4) . . ? O13 Bi7 O19 116.2(4) . . ? O12 Bi7 O19 69.1(3) . . ? O20 Bi7 O19 67.8(3) . . ? O13 Bi7 O21 87.6(4) . . ? O12 Bi7 O21 168.2(3) . . ? O20 Bi7 O21 71.5(3) . . ? O19 Bi7 O21 122.6(3) . . ? O13 Bi7 N2 80.0(5) . . ? O12 Bi7 N2 87.3(4) . . ? O20 Bi7 N2 143.1(4) . . ? O19 Bi7 N2 148.8(4) . . ? O21 Bi7 N2 82.5(4) . . ? O13 Bi7 Bi8 42.5(3) . . ? O12 Bi7 Bi8 108.7(3) . . ? O20 Bi7 Bi8 31.4(2) . . ? O19 Bi7 Bi8 92.1(2) . . ? O21 Bi7 Bi8 70.8(2) . . ? N2 Bi7 Bi8 115.4(4) . . ? O20 Bi8 O15 82.7(4) . . ? O20 Bi8 O14 88.8(4) . . ? O15 Bi8 O14 81.5(5) . . ? O20 Bi8 O16 69.7(3) . . ? O15 Bi8 O16 84.4(4) . . ? O14 Bi8 O16 155.6(3) . . ? O20 Bi8 O13 69.6(4) . . ? O15 Bi8 O13 146.4(4) . . ? O14 Bi8 O13 79.3(4) . . ? O16 Bi8 O13 102.6(4) . . ? O20 Bi8 C202 108.8(4) . . ? O15 Bi8 C202 26.7(4) . . ? O14 Bi8 C202 88.0(5) . . ? O16 Bi8 C202 88.3(4) . . ? O13 Bi8 C202 167.2(4) . . ? O20 Bi8 Bi7 34.1(3) . . ? O15 Bi8 Bi7 112.7(3) . . ? O14 Bi8 Bi7 78.1(3) . . ? O16 Bi8 Bi7 89.3(3) . . ? O13 Bi8 Bi7 36.1(2) . . ? C202 Bi8 Bi7 139.4(3) . . ? C155 C156 C157 121.0(18) . . ? C155 C156 H15I 119.5 . . ? C157 C156 H15I 119.5 . . ? 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 O18 Bi1 O1 C1 176.8(13) . . . . ? O17 Bi1 O1 C1 -130.5(12) . . . . ? O2 Bi1 O1 C1 -65.4(12) . . . . ? O19 Bi1 O1 C1 132.0(11) . . . . ? Bi2 Bi1 O1 C1 -96.8(12) . . . . ? Bi4 Bi1 O1 C1 170.3(14) . . . . ? O18 Bi1 O1 Bi4 6.5(3) . . . . ? O17 Bi1 O1 Bi4 59.2(4) . . . . ? O2 Bi1 O1 Bi4 124.3(4) . . . . ? O19 Bi1 O1 Bi4 -38.3(5) . . . . ? Bi2 Bi1 O1 Bi4 92.9(3) . . . . ? O18 Bi1 O2 C20 133.1(11) . . . . ? O17 Bi1 O2 C20 -172.7(12) . . . . ? O1 Bi1 O2 C20 66.6(12) . . . . ? O19 Bi1 O2 C20 -135.2(11) . . . . ? Bi2 Bi1 O2 C20 -164.1(14) . . . . ? Bi4 Bi1 O2 C20 100.2(11) . . . . ? O18 Bi1 O2 Bi2 -62.8(5) . . . . ? O17 Bi1 O2 Bi2 -8.6(4) . . . . ? O1 Bi1 O2 Bi2 -129.3(4) . . . . ? O19 Bi1 O2 Bi2 28.8(7) . . . . ? Bi4 Bi1 O2 Bi2 -95.8(3) . . . . ? O18 Bi1 O17 Bi2 138.3(5) . . . . ? O1 Bi1 O17 Bi2 84.9(5) . . . . ? O2 Bi1 O17 Bi2 10.4(4) . . . . ? O19 Bi1 O17 Bi2 -146.8(5) . . . . ? Bi4 Bi1 O17 Bi2 118.1(4) . . . . ? O18 Bi1 O17 Bi3 6.8(3) . . . . ? O1 Bi1 O17 Bi3 -46.6(5) . . . . ? O2 Bi1 O17 Bi3 -121.1(5) . . . . ? O19 Bi1 O17 Bi3 81.7(4) . . . . ? Bi2 Bi1 O17 Bi3 -131.5(7) . . . . ? Bi4 Bi1 O17 Bi3 -13.4(3) . . . . ? O17 Bi1 O18 Bi4 -138.7(5) . . . . ? O1 Bi1 O18 Bi4 -7.9(4) . . . . ? O2 Bi1 O18 Bi4 -84.1(5) . . . . ? O19 Bi1 O18 Bi4 137.0(5) . . . . ? Bi2 Bi1 O18 Bi4 -118.3(3) . . . . ? O17 Bi1 O18 Bi3 -6.7(3) . . . . ? O1 Bi1 O18 Bi3 124.0(4) . . . . ? O2 Bi1 O18 Bi3 47.9(5) . . . . ? O19 Bi1 O18 Bi3 -91.1(4) . . . . ? Bi2 Bi1 O18 Bi3 13.6(3) . . . . ? Bi4 Bi1 O18 Bi3 132.0(6) . . . . ? O17 Bi1 O18 Bi5 107.4(4) . . . . ? O1 Bi1 O18 Bi5 -121.9(4) . . . . ? O2 Bi1 O18 Bi5 162.0(3) . . . . ? O19 Bi1 O18 Bi5 23.1(3) . . . . ? Bi2 Bi1 O18 Bi5 127.8(2) . . . . ? Bi4 Bi1 O18 Bi5 -113.9(5) . . . . ? O18 Bi1 O19 Bi6 -146.9(4) . . . . ? O17 Bi1 O19 Bi6 141.6(4) . . . . ? O1 Bi1 O19 Bi6 -102.6(4) . . . . ? O2 Bi1 O19 Bi6 106.0(5) . . . . ? Bi2 Bi1 O19 Bi6 124.4(3) . . . . ? Bi4 Bi1 O19 Bi6 -126.0(3) . . . . ? O18 Bi1 O19 Bi5 -26.0(3) . . . . ? O17 Bi1 O19 Bi5 -97.5(4) . . . . ? O1 Bi1 O19 Bi5 18.3(5) . . . . ? O2 Bi1 O19 Bi5 -133.1(5) . . . . ? Bi2 Bi1 O19 Bi5 -114.7(3) . . . . ? Bi4 Bi1 O19 Bi5 -5.1(3) . . . . ? O18 Bi1 O19 Bi7 91.1(4) . . . . ? O17 Bi1 O19 Bi7 19.6(4) . . . . ? O1 Bi1 O19 Bi7 135.4(4) . . . . ? O2 Bi1 O19 Bi7 -16.0(7) . . . . ? Bi2 Bi1 O19 Bi7 2.4(3) . . . . ? Bi4 Bi1 O19 Bi7 112.1(3) . . . . ? Bi1 O1 C1 C6 85.9(18) . . . . ? Bi4 O1 C1 C6 -104.9(15) . . . . ? Bi1 O1 C1 C2 -97.7(16) . . . . ? Bi4 O1 C1 C2 71.5(16) . . . . ? C6 C1 C2 C3 2(2) . . . . ? O1 C1 C2 C3 -174.5(15) . . . . ? C6 C1 C2 C112 -169.7(15) . . . . ? O1 C1 C2 C112 14(2) . . . . ? C1 C2 C3 C4 4(3) . . . . ? C112 C2 C3 C4 175.6(17) . . . . ? C2 C3 C4 C5 -7(3) . . . . ? C2 C3 C4 C7 178.4(18) . . . . ? C3 C4 C5 C6 5(3) . . . . ? C7 C4 C5 C6 179.7(18) . . . . ? O1 C1 C6 C5 172.4(15) . . . . ? C2 C1 C6 C5 -4(2) . . . . ? O1 C1 C6 C14 -13(2) . . . . ? C2 C1 C6 C14 170.6(15) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C4 C5 C6 C14 -173.9(18) . . . . ? C5 C4 C7 C8 -136(2) . . . . ? C3 C4 C7 C8 39(3) . . . . ? C4 C7 C8 C9 -92(3) . . . . ? C4 C7 C8 C13 87(3) . . . . ? C13 C8 C9 C10 5(4) . . . . ? C7 C8 C9 C10 -177(2) . . . . ? C8 C9 C10 C11 0(4) . . . . ? C9 C10 C11 C12 -6(4) . . . . ? C10 C11 C12 C13 8(5) . . . . ? C11 C12 C13 C8 -3(5) . . . . ? C9 C8 C13 C12 -3(4) . . . . ? C7 C8 C13 C12 178(2) . . . . ? C1 C6 C14 C15 -91.4(17) . . . . ? C5 C6 C14 C15 83.0(19) . . . . ? C6 C14 C15 C16 -79.7(17) . . . . ? C6 C14 C15 C20 102.0(15) . . . . ? C20 C15 C16 C17 -5(2) . . . . ? C14 C15 C16 C17 176.5(14) . . . . ? C15 C16 C17 C18 -1(3) . . . . ? C15 C16 C17 C21 -177.3(14) . . . . ? C16 C17 C18 C19 4(3) . . . . ? C21 C17 C18 C19 -179.8(16) . . . . ? C17 C18 C19 C20 0(3) . . . . ? C17 C18 C19 C28 -179.1(17) . . . . ? Bi1 O2 C20 C15 -90.8(16) . . . . ? Bi2 O2 C20 C15 109.0(13) . . . . ? Bi1 O2 C20 C19 91.0(14) . . . . ? Bi2 O2 C20 C19 -69.2(16) . . . . ? C16 C15 C20 O2 -169.9(13) . . . . ? C14 C15 C20 O2 8(2) . . . . ? C16 C15 C20 C19 8(2) . . . . ? C14 C15 C20 C19 -173.3(13) . . . . ? C18 C19 C20 O2 172.8(13) . . . . ? C28 C19 C20 O2 -9(2) . . . . ? C18 C19 C20 C15 -6(2) . . . . ? C28 C19 C20 C15 173.2(14) . . . . ? C18 C17 C21 C22 -66(2) . . . . ? C16 C17 C21 C22 110(2) . . . . ? C17 C21 C22 C27 128(2) . . . . ? C17 C21 C22 C23 -61(3) . . . . ? C27 C22 C23 C24 -7(4) . . . . ? C21 C22 C23 C24 -177(2) . . . . ? C22 C23 C24 C25 2(4) . . . . ? C23 C24 C25 C26 3(5) . . . . ? C24 C25 C26 C27 -4(5) . . . . ? C23 C22 C27 C26 5(5) . . . . ? C21 C22 C27 C26 176(3) . . . . ? C25 C26 C27 C22 0(5) . . . . ? C18 C19 C28 C29 -83.2(19) . . . . ? C20 C19 C28 C29 98.2(17) . . . . ? C19 C28 C29 C30 76(2) . . . . ? C19 C28 C29 C34 -104.4(17) . . . . ? C34 C29 C30 C31 1(3) . . . . ? C28 C29 C30 C31 -179.7(16) . . . . ? C29 C30 C31 C32 0(3) . . . . ? C29 C30 C31 C35 178.7(18) . . . . ? C30 C31 C32 C33 -1(3) . . . . ? C35 C31 C32 C33 179.4(16) . . . . ? C31 C32 C33 C34 3(2) . . . . ? C31 C32 C33 C42 -177.4(16) . . . . ? Bi2 O3 C34 C33 -84.1(14) . . . . ? Bi2 O3 C34 C29 96.8(12) . . . . ? C32 C33 C34 O3 178.8(14) . . . . ? C42 C33 C34 O3 -1(2) . . . . ? C32 C33 C34 C29 -2(2) . . . . ? C42 C33 C34 C29 177.9(14) . . . . ? C30 C29 C34 O3 179.5(14) . . . . ? C28 C29 C34 O3 0(2) . . . . ? C30 C29 C34 C33 0(2) . . . . ? C28 C29 C34 C33 -179.0(14) . . . . ? C30 C31 C35 C36 -36(3) . . . . ? C32 C31 C35 C36 143.5(18) . . . . ? C31 C35 C36 C37 95(2) . . . . ? C31 C35 C36 C41 -75(3) . . . . ? C41 C36 C37 C38 -3(4) . . . . ? C35 C36 C37 C38 -174(2) . . . . ? C36 C37 C38 C39 1(4) . . . . ? C37 C38 C39 C40 -3(5) . . . . ? C38 C39 C40 C41 7(5) . . . . ? C39 C40 C41 C36 -9(4) . . . . ? C37 C36 C41 C40 7(3) . . . . ? C35 C36 C41 C40 177(2) . . . . ? C34 C33 C42 C43 91(2) . . . . ? C32 C33 C42 C43 -89.3(19) . . . . ? C33 C42 C43 C44 93.3(19) . . . . ? C33 C42 C43 C48 -90(2) . . . . ? C48 C43 C44 C45 -2(3) . . . . ? C42 C43 C44 C45 174.5(19) . . . . ? C43 C44 C45 C46 2(3) . . . . ? C43 C44 C45 C49 -178(2) . . . . ? C44 C45 C46 C47 2(3) . . . . ? C49 C45 C46 C47 -178.0(18) . . . . ? C45 C46 C47 C48 -5(3) . . . . ? C45 C46 C47 C56 -176.1(18) . . . . ? Bi2 O4 C48 C43 84.7(16) . . . . ? Bi2 O4 C48 C47 -95.3(15) . . . . ? C44 C43 C48 O4 179.0(15) . . . . ? C42 C43 C48 O4 2(3) . . . . ? C44 C43 C48 C47 -1(3) . . . . ? C42 C43 C48 C47 -177.7(16) . . . . ? C46 C47 C48 O4 -175.5(14) . . . . ? C56 C47 C48 O4 -4(2) . . . . ? C46 C47 C48 C43 4(3) . . . . ? C56 C47 C48 C43 175.9(15) . . . . ? C46 C45 C49 C50 -56(3) . . . . ? C44 C45 C49 C50 124(2) . . . . ? C45 C49 C50 C51 -54(3) . . . . ? C45 C49 C50 C55 123(3) . . . . ? C55 C50 C51 C52 1(6) . . . . ? C49 C50 C51 C52 178(3) . . . . ? C50 C51 C52 C53 1(6) . . . . ? C51 C52 C53 C54 -3(5) . . . . ? C52 C53 C54 C55 3(6) . . . . ? C51 C50 C55 C54 -1(4) . . . . ? C49 C50 C55 C54 -178(2) . . . . ? C53 C54 C55 C50 -1(5) . . . . ? C46 C47 C56 C57 -86(2) . . . . ? C48 C47 C56 C57 104.1(17) . . . . ? C47 C56 C57 C58 80.9(19) . . . . ? C47 C56 C57 C62 -101.6(18) . . . . ? C62 C57 C58 C59 -3(3) . . . . ? C56 C57 C58 C59 174.5(18) . . . . ? C57 C58 C59 C60 -1(3) . . . . ? C57 C58 C59 C63 179.5(18) . . . . ? C58 C59 C60 C61 3(3) . . . . ? C63 C59 C60 C61 -177.5(18) . . . . ? C59 C60 C61 C62 -1(3) . . . . ? C59 C60 C61 C70 -174.6(15) . . . . ? Bi3 O5 C62 C57 -95.3(17) . . . . ? Bi2 O5 C62 C57 76.6(16) . . . . ? Bi3 O5 C62 C61 83.5(19) . . . . ? Bi2 O5 C62 C61 -104.6(15) . . . . ? C58 C57 C62 O5 -176.0(16) . . . . ? C56 C57 C62 O5 7(2) . . . . ? C58 C57 C62 C61 5(3) . . . . ? C56 C57 C62 C61 -172.2(16) . . . . ? C60 C61 C62 O5 178.0(15) . . . . ? C70 C61 C62 O5 -9(3) . . . . ? C60 C61 C62 C57 -3(3) . . . . ? C70 C61 C62 C57 170.1(15) . . . . ? C60 C59 C63 C64 135(3) . . . . ? C58 C59 C63 C64 -46(3) . . . . ? C60 C59 C63 C69 -177.9(17) . . . . ? C58 C59 C63 C69 1(3) . . . . ? C59 C63 C64 C65 -81(12) . . . . ? C69 C63 C64 C65 166(14) . . . . ? C59 C63 C64 C69 112(3) . . . . ? C69 C64 C65 C66 -19(12) . . . . ? C63 C64 C65 C66 177(7) . . . . ? C64 C65 C66 C67 18(12) . . . . ? C65 C66 C67 C68 -20(12) . . . . ? C66 C67 C68 C69 19(11) . . . . ? C65 C64 C69 C68 20(10) . . . . ? C63 C64 C69 C68 -169(5) . . . . ? C65 C64 C69 C63 -171(9) . . . . ? C67 C68 C69 C64 -17(9) . . . . ? C67 C68 C69 C63 -56(22) . . . . ? C59 C63 C69 C64 -88(4) . . . . ? C59 C63 C69 C68 -43(19) . . . . ? C64 C63 C69 C68 45(18) . . . . ? C60 C61 C70 C71 82.0(19) . . . . ? C62 C61 C70 C71 -91(2) . . . . ? C61 C70 C71 C72 -82.8(18) . . . . ? C61 C70 C71 C76 95.8(17) . . . . ? C76 C71 C72 C73 -7(2) . . . . ? C70 C71 C72 C73 171.3(15) . . . . ? C71 C72 C73 C74 3(3) . . . . ? C71 C72 C73 C77 -174.9(15) . . . . ? C72 C73 C74 C75 0(3) . . . . ? C77 C73 C74 C75 177.1(16) . . . . ? C73 C74 C75 C76 3(3) . . . . ? C73 C74 C75 C84 -175.1(15) . . . . ? Bi3 O6 C76 C71 -91.3(16) . . . . ? Bi4 O6 C76 C71 105.5(13) . . . . ? Bi3 O6 C76 C75 85.4(17) . . . . ? Bi4 O6 C76 C75 -77.8(15) . . . . ? C72 C71 C76 O6 -173.7(13) . . . . ? C70 C71 C76 O6 8(2) . . . . ? C72 C71 C76 C75 9(2) . . . . ? C70 C71 C76 C75 -169.2(13) . . . . ? C74 C75 C76 O6 175.8(14) . . . . ? C84 C75 C76 O6 -6(2) . . . . ? C74 C75 C76 C71 -7(2) . . . . ? C84 C75 C76 C71 170.7(13) . . . . ? C74 C73 C77 C78 -94(2) . . . . ? C72 C73 C77 C78 84(2) . . . . ? C73 C77 C78 C83 94(2) . . . . ? C73 C77 C78 C79 -84(2) . . . . ? C83 C78 C79 C80 1(3) . . . . ? C77 C78 C79 C80 179(2) . . . . ? C78 C79 C80 C81 0(4) . . . . ? C79 C80 C81 C82 1(4) . . . . ? C80 C81 C82 C83 -3(4) . . . . ? C79 C78 C83 C82 -3(3) . . . . ? C77 C78 C83 C82 179(2) . . . . ? C81 C82 C83 C78 5(4) . . . . ? C74 C75 C84 C85 -84(2) . . . . ? C76 C75 C84 C85 98.0(18) . . . . ? C75 C84 C85 C90 -99.0(19) . . . . ? C75 C84 C85 C86 84(2) . . . . ? C90 C85 C86 C87 -3(3) . . . . ? C84 C85 C86 C87 174.2(16) . . . . ? C85 C86 C87 C88 6(3) . . . . ? C85 C86 C87 C91 -173.9(18) . . . . ? C86 C87 C88 C89 -4(3) . . . . ? C91 C87 C88 C89 175.9(19) . . . . ? C87 C88 C89 C90 -1(3) . . . . ? C87 C88 C89 C98 -172.6(18) . . . . ? Bi4 O7 C90 C89 -84.5(15) . . . . ? Bi4 O7 C90 C85 92.7(14) . . . . ? C88 C89 C90 O7 -178.0(15) . . . . ? C98 C89 C90 O7 -7(2) . . . . ? C88 C89 C90 C85 5(2) . . . . ? C98 C89 C90 C85 176.2(14) . . . . ? C86 C85 C90 O7 -179.9(15) . . . . ? C84 C85 C90 O7 3(2) . . . . ? C86 C85 C90 C89 -3(2) . . . . ? C84 C85 C90 C89 -179.7(14) . . . . ? C88 C87 C91 C92 -63(3) . . . . ? C86 C87 C91 C92 118(2) . . . . ? C87 C91 C92 C97 -35(3) . . . . ? C87 C91 C92 C93 138(2) . . . . ? C97 C92 C93 C94 -10(4) . . . . ? C91 C92 C93 C94 177(2) . . . . ? C92 C93 C94 C95 4(4) . . . . ? C93 C94 C95 C96 2(5) . . . . ? C94 C95 C96 C97 -2(4) . . . . ? C93 C92 C97 C96 11(4) . . . . ? C91 C92 C97 C96 -176(2) . . . . ? C95 C96 C97 C92 -4(4) . . . . ? C88 C89 C98 C99 -98.1(19) . . . . ? C90 C89 C98 C99 90.8(18) . . . . ? C89 C98 C99 C100 91.8(19) . . . . ? C89 C98 C99 C104 -93(2) . . . . ? C104 C99 C100 C101 5(3) . . . . ? C98 C99 C100 C101 -179.2(18) . . . . ? C99 C100 C101 C102 -6(3) . . . . ? C99 C100 C101 C105 -175(2) . . . . ? C100 C101 C102 C103 3(3) . . . . ? C105 C101 C102 C103 173(2) . . . . ? C101 C102 C103 C104 0(3) . . . . ? C101 C102 C103 C112 -179.3(18) . . . . ? Bi4 O8 C104 C99 88.3(13) . . . . ? Bi4 O8 C104 C103 -89.5(14) . . . . ? C100 C99 C104 O8 -179.8(14) . . . . ? C98 C99 C104 O8 5(2) . . . . ? C100 C99 C104 C103 -2(2) . . . . ? C98 C99 C104 C103 -177.1(15) . . . . ? C102 C103 C104 O8 177.3(14) . . . . ? C112 C103 C104 O8 -4(2) . . . . ? C102 C103 C104 C99 0(2) . . . . ? C112 C103 C104 C99 178.8(15) . . . . ? C100 C101 C105 C111 -152(2) . . . . ? C102 C101 C105 C111 39(3) . . . . ? C111 C106 C107 C108 4(5) . . . . ? C106 C107 C108 C109 -9(6) . . . . ? C107 C108 C109 C110 8(6) . . . . ? C108 C109 C110 C111 -4(5) . . . . ? C109 C110 C111 C106 0(5) . . . . ? C109 C110 C111 C105 179(3) . . . . ? C107 C106 C111 C110 0(5) . . . . ? C107 C106 C111 C105 -180(3) . . . . ? C101 C105 C111 C110 -98(3) . . . . ? C101 C105 C111 C106 82(3) . . . . ? C102 C103 C112 C2 -83(2) . . . . ? C104 C103 C112 C2 97.8(17) . . . . ? C3 C2 C112 C103 86(2) . . . . ? C1 C2 C112 C103 -102.2(19) . . . . ? Bi5 O9 C113 C118 -94.1(15) . . . . ? Bi6 O9 C113 C118 68.8(17) . . . . ? Bi5 O9 C113 C114 87.6(17) . . . . ? Bi6 O9 C113 C114 -109.5(14) . . . . ? O9 C113 C114 C115 171.1(15) . . . . ? C118 C113 C114 C115 -7(2) . . . . ? O9 C113 C114 C224 -12(2) . . . . ? C118 C113 C114 C224 169.4(15) . . . . ? C113 C114 C115 C116 4(3) . . . . ? C224 C114 C115 C116 -172.8(17) . . . . ? C114 C115 C116 C117 2(3) . . . . ? C114 C115 C116 C119 178.8(18) . . . . ? C115 C116 C117 C118 -5(3) . . . . ? C119 C116 C117 C118 178.5(16) . . . . ? O9 C113 C118 C117 -173.5(14) . . . . ? C114 C113 C118 C117 5(2) . . . . ? O9 C113 C118 C126 10(2) . . . . ? C114 C113 C118 C126 -171.9(15) . . . . ? C116 C117 C118 C113 1(3) . . . . ? C116 C117 C118 C126 178.0(16) . . . . ? C115 C116 C119 C120 95(2) . . . . ? C117 C116 C119 C120 -89(2) . . . . ? C116 C119 C120 C125 -6(3) . . . . ? C116 C119 C120 C121 178.7(16) . . . . ? C125 C120 C121 C122 2(3) . . . . ? C119 C120 C121 C122 176.9(19) . . . . ? C120 C121 C122 C123 -3(4) . . . . ? C121 C122 C123 C124 7(5) . . . . ? C122 C123 C124 C125 -11(5) . . . . ? C121 C120 C125 C124 -6(4) . . . . ? C119 C120 C125 C124 179(3) . . . . ? C123 C124 C125 C120 11(5) . . . . ? C113 C118 C126 C127 -100.4(18) . . . . ? C117 C118 C126 C127 83.0(19) . . . . ? C118 C126 C127 C128 -80.5(19) . . . . ? C118 C126 C127 C132 107.7(15) . . . . ? C132 C127 C128 C129 -6(2) . . . . ? C126 C127 C128 C129 -178.3(15) . . . . ? C127 C128 C129 C130 8(3) . . . . ? C127 C128 C129 C133 -176.2(18) . . . . ? C128 C129 C130 C131 -6(3) . . . . ? C133 C129 C130 C131 177.5(19) . . . . ? C129 C130 C131 C132 4(3) . . . . ? C129 C130 C131 C140 178.4(18) . . . . ? Bi6 O10 C132 C127 -92.1(14) . . . . ? Bi6 O10 C132 C131 85.2(15) . . . . ? C128 C127 C132 O10 -179.0(14) . . . . ? C126 C127 C132 O10 -7(2) . . . . ? C128 C127 C132 C131 4(2) . . . . ? C126 C127 C132 C131 176.1(14) . . . . ? C130 C131 C132 O10 -179.5(15) . . . . ? C140 C131 C132 O10 6(2) . . . . ? C130 C131 C132 C127 -2(2) . . . . ? C140 C131 C132 C127 -176.9(15) . . . . ? C130 C129 C133 C134 -101(3) . . . . ? C128 C129 C133 C134 83(3) . . . . ? C129 C133 C134 C135 -97(3) . . . . ? C129 C133 C134 C139 67(3) . . . . ? C139 C134 C135 C136 10(5) . . . . ? C133 C134 C135 C136 174(3) . . . . ? C134 C135 C136 C137 -5(6) . . . . ? C135 C136 C137 C138 17(8) . . . . ? C136 C137 C138 C139 -30(8) . . . . ? C135 C134 C139 C138 -26(6) . . . . ? C133 C134 C139 C138 168(4) . . . . ? C137 C138 C139 C134 35(8) . . . . ? C130 C131 C140 C141 91(2) . . . . ? C132 C131 C140 C141 -94.4(19) . . . . ? C131 C140 C141 C146 91.3(19) . . . . ? C131 C140 C141 C142 -95.4(18) . . . . ? C146 C141 C142 C143 -2(3) . . . . ? C140 C141 C142 C143 -175.2(16) . . . . ? C141 C142 C143 C144 -1(3) . . . . ? C141 C142 C143 C147 176.5(18) . . . . ? C142 C143 C144 C145 1(3) . . . . ? C147 C143 C144 C145 -177(2) . . . . ? C143 C144 C145 C146 3(3) . . . . ? C143 C144 C145 C154 173.3(18) . . . . ? C142 C141 C146 O11 -179.8(15) . . . . ? C140 C141 C146 O11 -7(2) . . . . ? C142 C141 C146 C145 6(2) . . . . ? C140 C141 C146 C145 178.8(15) . . . . ? Bi6 O11 C146 C141 -83.0(15) . . . . ? Bi6 O11 C146 C145 91.8(14) . . . . ? C144 C145 C146 C141 -6(2) . . . . ? C154 C145 C146 C141 -176.8(15) . . . . ? C144 C145 C146 O11 179.1(15) . . . . ? C154 C145 C146 O11 8(2) . . . . ? C144 C143 C147 C148 -61(3) . . . . ? C142 C143 C147 C148 121(3) . . . . ? C143 C147 C148 C153 -73(4) . . . . ? C143 C147 C148 C149 113(3) . . . . ? C153 C148 C149 C150 9(7) . . . . ? C147 C148 C149 C150 -178(4) . . . . ? C148 C149 C150 C151 -4(7) . . . . ? C149 C150 C151 C152 1(9) . . . . ? C150 C151 C152 C153 -1(10) . . . . ? C149 C148 C153 C152 -9(8) . . . . ? C147 C148 C153 C152 179(4) . . . . ? C151 C152 C153 C148 4(9) . . . . ? C146 C145 C154 C155 -104.5(18) . . . . ? C144 C145 C154 C155 85(2) . . . . ? C145 C154 C155 C160 101(2) . . . . ? C145 C154 C155 C156 -87(2) . . . . ? C156 C157 C158 C159 0(3) . . . . ? C161 C157 C158 C159 177.3(18) . . . . ? C157 C158 C159 C168 169.1(18) . . . . ? C157 C158 C159 C160 -2(3) . . . . ? C156 C155 C160 O12 177.3(16) . . . . ? C154 C155 C160 O12 -10(3) . . . . ? C156 C155 C160 C159 -1(3) . . . . ? C154 C155 C160 C159 171.6(15) . . . . ? Bi7 O12 C160 C155 83(2) . . . . ? Bi6 O12 C160 C155 -72.0(19) . . . . ? Bi7 O12 C160 C159 -98.4(15) . . . . ? Bi6 O12 C160 C159 106.7(13) . . . . ? C158 C159 C160 C155 3(2) . . . . ? C168 C159 C160 C155 -168.3(16) . . . . ? C158 C159 C160 O12 -176.1(13) . . . . ? C168 C159 C160 O12 13(2) . . . . ? C158 C157 C161 C162 -79(3) . . . . ? C156 C157 C161 C162 98(3) . . . . ? C157 C161 C162 C167 112(3) . . . . ? C157 C161 C162 C163 -73(3) . . . . ? C167 C162 C163 C164 1(4) . . . . ? C161 C162 C163 C164 -174(3) . . . . ? C162 C163 C164 C165 -12(5) . . . . ? C163 C164 C165 C166 11(6) . . . . ? C164 C165 C166 C167 1(8) . . . . ? C165 C166 C167 C162 -11(8) . . . . ? C163 C162 C167 C166 10(5) . . . . ? C161 C162 C167 C166 -176(4) . . . . ? C158 C159 C168 C169 -77(2) . . . . ? C160 C159 C168 C169 93.6(19) . . . . ? C159 C168 C169 C174 -92(2) . . . . ? C159 C168 C169 C170 85(2) . . . . ? C174 C169 C170 C171 6(3) . . . . ? C168 C169 C170 C171 -171.5(19) . . . . ? C169 C170 C171 C172 0(3) . . . . ? C169 C170 C171 C175 -178(2) . . . . ? C170 C171 C172 C173 -5(3) . . . . ? C175 C171 C172 C173 173(2) . . . . ? C171 C172 C173 C174 2(3) . . . . ? C171 C172 C173 C182 -177.1(19) . . . . ? Bi7 O13 C174 C169 84.3(19) . . . . ? Bi8 O13 C174 C169 -105.0(16) . . . . ? Bi7 O13 C174 C173 -95(2) . . . . ? Bi8 O13 C174 C173 75.6(18) . . . . ? C170 C169 C174 O13 172.1(17) . . . . ? C168 C169 C174 O13 -10(3) . . . . ? C170 C169 C174 C173 -9(3) . . . . ? C168 C169 C174 C173 168.9(17) . . . . ? C172 C173 C174 O13 -175.9(18) . . . . ? C182 C173 C174 O13 3(3) . . . . ? C172 C173 C174 C169 5(3) . . . . ? C182 C173 C174 C169 -175.9(16) . . . . ? C170 C171 C175 C176 172(2) . . . . ? C172 C171 C175 C176 -5(3) . . . . ? C171 C175 C176 C181 100(3) . . . . ? C171 C175 C176 C177 -80(3) . . . . ? C181 C176 C177 C178 -2(5) . . . . ? C175 C176 C177 C178 179(3) . . . . ? C176 C177 C178 C179 -1(5) . . . . ? C177 C178 C179 C180 3(6) . . . . ? C178 C179 C180 C181 -2(6) . . . . ? C177 C176 C181 C180 3(4) . . . . ? C175 C176 C181 C180 -177(3) . . . . ? C179 C180 C181 C176 -2(5) . . . . ? C172 C173 C182 C183 80(2) . . . . ? C174 C173 C182 C183 -99(2) . . . . ? C173 C182 C183 C188 98(2) . . . . ? C173 C182 C183 C184 -79(2) . . . . ? C188 C183 C184 C185 1(3) . . . . ? C182 C183 C184 C185 178(2) . . . . ? C183 C184 C185 C186 0(4) . . . . ? C184 C185 C186 C187 1(4) . . . . ? C185 C186 C187 C188 -4(3) . . . . ? C185 C186 C187 C196 173(2) . . . . ? Bi8 O14 C188 C187 85.2(16) . . . . ? Bi8 O14 C188 C183 -99.7(15) . . . . ? C186 C187 C188 O14 179.8(16) . . . . ? C196 C187 C188 O14 4(3) . . . . ? C186 C187 C188 C183 5(3) . . . . ? C196 C187 C188 C183 -170.8(18) . . . . ? C182 C183 C188 O14 4(2) . . . . ? C184 C183 C188 O14 -178.6(15) . . . . ? C182 C183 C188 C187 178.9(17) . . . . ? C184 C183 C188 C187 -4(3) . . . . ? C188 C187 C196 C197 -92(2) . . . . ? C186 C187 C196 C197 92(2) . . . . ? C187 C196 C197 C198 -91(2) . . . . ? C187 C196 C197 C202 93(2) . . . . ? C202 C197 C198 C199 0(3) . . . . ? C196 C197 C198 C199 -176(2) . . . . ? C197 C198 C199 C200 0(3) . . . . ? C197 C198 C199 C203 -177(2) . . . . ? C198 C199 C200 C201 4(3) . . . . ? C203 C199 C200 C201 -179(2) . . . . ? C199 C200 C201 C202 -8(3) . . . . ? C199 C200 C201 C210 -178.0(19) . . . . ? Bi8 O15 C202 C201 99.6(16) . . . . ? Bi8 O15 C202 C197 -83.4(16) . . . . ? C200 C201 C202 O15 -175.8(15) . . . . ? C210 C201 C202 O15 -6(3) . . . . ? C200 C201 C202 C197 7(3) . . . . ? C210 C201 C202 C197 177.4(16) . . . . ? C200 C201 C202 Bi8 -124.0(15) . . . . ? C210 C201 C202 Bi8 46(2) . . . . ? C198 C197 C202 O15 179.5(16) . . . . ? C196 C197 C202 O15 -5(3) . . . . ? C198 C197 C202 C201 -4(3) . . . . ? C196 C197 C202 C201 172.3(17) . . . . ? C198 C197 C202 Bi8 131.3(16) . . . . ? C196 C197 C202 Bi8 -52.9(18) . . . . ? C198 C199 C203 C204 161(2) . . . . ? C200 C199 C203 C204 -16(3) . . . . ? C199 C203 C204 C205 114(3) . . . . ? C199 C203 C204 C209 -62(3) . . . . ? C209 C204 C205 C206 1(4) . . . . ? C203 C204 C205 C206 -176(2) . . . . ? C204 C205 C206 C207 3(4) . . . . ? C205 C206 C207 C208 -7(5) . . . . ? C206 C207 C208 C209 7(5) . . . . ? C207 C208 C209 C204 -4(5) . . . . ? C205 C204 C209 C208 0(4) . . . . ? C203 C204 C209 C208 177(2) . . . . ? C202 C201 C210 C211 -101(2) . . . . ? C200 C201 C210 C211 69(2) . . . . ? C201 C210 C211 C212 -84(2) . . . . ? C201 C210 C211 C216 99.7(19) . . . . ? C216 C211 C212 C213 0(3) . . . . ? C210 C211 C212 C213 -176.3(16) . . . . ? C211 C212 C213 C214 4(3) . . . . ? C211 C212 C213 C217 176.8(16) . . . . ? C212 C213 C214 C215 -5(3) . . . . ? C217 C213 C214 C215 -177.4(15) . . . . ? C213 C214 C215 C216 1(2) . . . . ? C213 C214 C215 C224 177.5(16) . . . . ? C214 C215 C216 O16 -174.2(13) . . . . ? C224 C215 C216 O16 9(2) . . . . ? C214 C215 C216 C211 4(2) . . . . ? C224 C215 C216 C211 -172.8(13) . . . . ? Bi5 O16 C216 C215 -90.6(15) . . . . ? Bi8 O16 C216 C215 110.7(13) . . . . ? Bi5 O16 C216 C211 91.6(14) . . . . ? Bi8 O16 C216 C211 -67.1(16) . . . . ? C212 C211 C216 C215 -4(2) . . . . ? C210 C211 C216 C215 172.3(13) . . . . ? C212 C211 C216 O16 173.6(13) . . . . ? C210 C211 C216 O16 -10(2) . . . . ? C214 C213 C217 C223 -57(3) . . . . ? C212 C213 C217 C223 131.3(19) . . . . ? C223 C218 C219 C220 -4(4) . . . . ? C218 C219 C220 C221 0(6) . . . . ? C219 C220 C221 C222 6(6) . . . . ? C220 C221 C222 C223 -7(5) . . . . ? C219 C218 C223 C222 3(4) . . . . ? C219 C218 C223 C217 -175(2) . . . . ? C221 C222 C223 C218 2(4) . . . . ? C221 C222 C223 C217 -179(3) . . . . ? C213 C217 C223 C218 -47(3) . . . . ? C213 C217 C223 C222 135(2) . . . . ? C216 C215 C224 C114 98.5(15) . . . . ? C214 C215 C224 C114 -77.8(17) . . . . ? C115 C114 C224 C215 84.1(19) . . . . ? C113 C114 C224 C215 -92.4(19) . . . . ? C230 C225 C226 C227 -5(5) . . . . ? C225 C226 C227 C228 3(4) . . . . ? C226 C227 C228 C229 2(4) . . . . ? C227 C228 C229 C230 -5(4) . . . . ? C226 C225 C230 C229 1(4) . . . . ? C228 C229 C230 C225 4(4) . . . . ? C236 C231 C232 C233 5(4) . . . . ? C231 C232 C233 C234 -4(4) . . . . ? C232 C233 C234 C235 2(5) . . . . ? C233 C234 C235 C236 -3(5) . . . . ? C232 C231 C236 C235 -6(4) . . . . ? C234 C235 C236 C231 5(4) . . . . ? C242 C237 C238 C239 3(4) . . . . ? C237 C238 C239 C240 -5(4) . . . . ? C238 C239 C240 C241 5(4) . . . . ? C239 C240 C241 C242 -3(4) . . . . ? C240 C241 C242 C237 1(5) . . . . ? C238 C237 C242 C241 -1(5) . . . . ? C300 C301 C302 C303 -6(4) . . . . ? C303 C304 C305 C300 2(5) . . . . ? C305 C304 C303 C302 1(4) . . . . ? C301 C302 C303 C304 1(4) . . . . ? C304 C305 C300 C301 -8(5) . . . . ? C302 C301 C300 C305 9(4) . . . . ? Bi1 O17 Bi2 O3 76.4(5) . . . . ? Bi3 O17 Bi2 O3 -153.5(4) . . . . ? Bi1 O17 Bi2 O4 158.7(5) . . . . ? Bi3 O17 Bi2 O4 -71.2(4) . . . . ? Bi1 O17 Bi2 O2 -9.9(4) . . . . ? Bi3 O17 Bi2 O2 120.2(5) . . . . ? Bi1 O17 Bi2 O5 -121.6(5) . . . . ? Bi3 O17 Bi2 O5 8.6(3) . . . . ? Bi3 O17 Bi2 Bi1 130.1(7) . . . . ? C34 O3 Bi2 O17 -169.6(9) . . . . ? C34 O3 Bi2 O4 102.0(9) . . . . ? C34 O3 Bi2 O2 -98.7(9) . . . . ? C34 O3 Bi2 O5 156.9(8) . . . . ? C34 O3 Bi2 Bi1 -135.7(9) . . . . ? C48 O4 Bi2 O17 170.3(10) . . . . ? C48 O4 Bi2 O3 -105.6(10) . . . . ? C48 O4 Bi2 O2 -163.2(10) . . . . ? C48 O4 Bi2 O5 100.2(10) . . . . ? C48 O4 Bi2 Bi1 -176.3(9) . . . . ? C20 O2 Bi2 O17 172.8(13) . . . . ? Bi1 O2 Bi2 O17 9.2(4) . . . . ? C20 O2 Bi2 O3 87.4(12) . . . . ? Bi1 O2 Bi2 O3 -76.2(4) . . . . ? C20 O2 Bi2 O4 144.6(12) . . . . ? Bi1 O2 Bi2 O4 -19.1(11) . . . . ? C20 O2 Bi2 O5 -123.8(12) . . . . ? Bi1 O2 Bi2 O5 72.5(4) . . . . ? C20 O2 Bi2 Bi1 163.7(14) . . . . ? C62 O5 Bi2 O17 177.1(10) . . . . ? Bi3 O5 Bi2 O17 -8.2(3) . . . . ? C62 O5 Bi2 O3 -147.1(9) . . . . ? Bi3 O5 Bi2 O3 27.5(8) . . . . ? C62 O5 Bi2 O4 -91.6(9) . . . . ? Bi3 O5 Bi2 O4 83.1(4) . . . . ? C62 O5 Bi2 O2 113.4(9) . . . . ? Bi3 O5 Bi2 O2 -71.9(4) . . . . ? C62 O5 Bi2 Bi1 148.7(9) . . . . ? Bi3 O5 Bi2 Bi1 -36.6(3) . . . . ? O18 Bi1 Bi2 O17 -38.5(5) . . . . ? O1 Bi1 Bi2 O17 -109.0(5) . . . . ? O2 Bi1 Bi2 O17 -164.4(7) . . . . ? O19 Bi1 Bi2 O17 33.8(5) . . . . ? Bi4 Bi1 Bi2 O17 -67.2(5) . . . . ? O18 Bi1 Bi2 O3 -136.4(4) . . . . ? O17 Bi1 Bi2 O3 -97.9(5) . . . . ? O1 Bi1 Bi2 O3 153.1(4) . . . . ? O2 Bi1 Bi2 O3 97.7(5) . . . . ? O19 Bi1 Bi2 O3 -64.2(3) . . . . ? Bi4 Bi1 Bi2 O3 -165.1(3) . . . . ? O18 Bi1 Bi2 O4 -63.1(4) . . . . ? O17 Bi1 Bi2 O4 -24.5(6) . . . . ? O1 Bi1 Bi2 O4 -133.5(4) . . . . ? O2 Bi1 Bi2 O4 171.0(6) . . . . ? O19 Bi1 Bi2 O4 9.2(4) . . . . ? Bi4 Bi1 Bi2 O4 -91.8(3) . . . . ? O18 Bi1 Bi2 O2 125.9(5) . . . . ? O17 Bi1 Bi2 O2 164.4(7) . . . . ? O1 Bi1 Bi2 O2 55.4(5) . . . . ? O19 Bi1 Bi2 O2 -161.8(5) . . . . ? Bi4 Bi1 Bi2 O2 97.2(4) . . . . ? O18 Bi1 Bi2 O5 14.7(3) . . . . ? O17 Bi1 Bi2 O5 53.2(5) . . . . ? O1 Bi1 Bi2 O5 -55.8(3) . . . . ? O2 Bi1 Bi2 O5 -111.2(5) . . . . ? O19 Bi1 Bi2 O5 86.9(3) . . . . ? Bi4 Bi1 Bi2 O5 -14.0(2) . . . . ? C62 O5 Bi3 O6 -62.1(13) . . . . ? Bi2 O5 Bi3 O6 125.1(4) . . . . ? C62 O5 Bi3 O17 -179.8(13) . . . . ? Bi2 O5 Bi3 O17 7.4(3) . . . . ? C62 O5 Bi3 O18 -126.8(13) . . . . ? Bi2 O5 Bi3 O18 60.4(4) . . . . ? C62 O5 Bi3 O21 108.9(13) . . . . ? Bi2 O5 Bi3 O21 -63.9(3) . . . . ? C76 O6 Bi3 O5 66.9(14) . . . . ? Bi4 O6 Bi3 O5 -128.3(4) . . . . ? C76 O6 Bi3 O17 136.0(13) . . . . ? Bi4 O6 Bi3 O17 -59.2(4) . . . . ? C76 O6 Bi3 O18 -173.2(14) . . . . ? Bi4 O6 Bi3 O18 -8.4(3) . . . . ? C76 O6 Bi3 O21 17(3) . . . . ? Bi4 O6 Bi3 O21 -178.5(14) . . . . ? Bi2 O17 Bi3 O5 -9.6(4) . . . . ? Bi1 O17 Bi3 O5 122.0(4) . . . . ? Bi2 O17 Bi3 O6 -86.0(4) . . . . ? Bi1 O17 Bi3 O6 45.7(5) . . . . ? Bi2 O17 Bi3 O18 -138.3(5) . . . . ? Bi1 O17 Bi3 O18 -6.6(3) . . . . ? Bi2 O17 Bi3 O21 83.2(4) . . . . ? Bi1 O17 Bi3 O21 -145.1(4) . . . . ? Bi4 O18 Bi3 O5 83.7(5) . . . . ? Bi1 O18 Bi3 O5 -49.5(5) . . . . ? Bi5 O18 Bi3 O5 -162.2(3) . . . . ? Bi4 O18 Bi3 O6 10.0(4) . . . . ? Bi1 O18 Bi3 O6 -123.3(5) . . . . ? Bi5 O18 Bi3 O6 124.1(4) . . . . ? Bi4 O18 Bi3 O17 140.0(5) . . . . ? Bi1 O18 Bi3 O17 6.7(3) . . . . ? Bi5 O18 Bi3 O17 -105.9(4) . . . . ? Bi4 O18 Bi3 O21 -172.4(3) . . . . ? Bi1 O18 Bi3 O21 54.3(5) . . . . ? Bi5 O18 Bi3 O21 -58.3(4) . . . . ? Bi7 O21 Bi3 O5 123.1(4) . . . . ? Bi7 O21 Bi3 O6 173.1(15) . . . . ? Bi7 O21 Bi3 O17 49.8(3) . . . . ? Bi7 O21 Bi3 O18 4.1(4) . . . . ? Bi1 O18 Bi4 O8 -76.1(4) . . . . ? Bi3 O18 Bi4 O8 152.5(4) . . . . ? Bi5 O18 Bi4 O8 37.3(3) . . . . ? Bi1 O18 Bi4 O7 -155.7(5) . . . . ? Bi3 O18 Bi4 O7 73.0(4) . . . . ? Bi5 O18 Bi4 O7 -42.2(4) . . . . ? Bi1 O18 Bi4 O6 122.0(5) . . . . ? Bi3 O18 Bi4 O6 -9.3(3) . . . . ? Bi5 O18 Bi4 O6 -124.5(4) . . . . ? Bi1 O18 Bi4 O1 7.6(4) . . . . ? Bi3 O18 Bi4 O1 -123.8(4) . . . . ? Bi5 O18 Bi4 O1 121.1(4) . . . . ? Bi3 O18 Bi4 Bi1 -131.4(6) . . . . ? Bi5 O18 Bi4 Bi1 113.5(5) . . . . ? C104 O8 Bi4 O18 172.6(9) . . . . ? C104 O8 Bi4 O7 -107.4(9) . . . . ? C104 O8 Bi4 O6 -157.6(8) . . . . ? C104 O8 Bi4 O1 101.7(8) . . . . ? C104 O8 Bi4 Bi1 139.3(8) . . . . ? C90 O7 Bi4 O18 -174.5(10) . . . . ? C90 O7 Bi4 O8 104.9(9) . . . . ? C90 O7 Bi4 O6 -102.6(9) . . . . ? C90 O7 Bi4 O1 158.6(8) . . . . ? C90 O7 Bi4 Bi1 172.0(8) . . . . ? C76 O6 Bi4 O18 176.5(12) . . . . ? Bi3 O6 Bi4 O18 9.1(3) . . . . ? C76 O6 Bi4 O8 145.4(11) . . . . ? Bi3 O6 Bi4 O8 -22.0(8) . . . . ? C76 O6 Bi4 O7 95.5(11) . . . . ? Bi3 O6 Bi4 O7 -71.9(4) . . . . ? C76 O6 Bi4 O1 -121.9(11) . . . . ? Bi3 O6 Bi4 O1 70.7(4) . . . . ? C76 O6 Bi4 Bi1 -156.2(11) . . . . ? Bi3 O6 Bi4 Bi1 36.4(3) . . . . ? C1 O1 Bi4 O18 -179.2(10) . . . . ? Bi1 O1 Bi4 O18 -6.8(3) . . . . ? C1 O1 Bi4 O8 -98.1(9) . . . . ? Bi1 O1 Bi4 O8 74.4(4) . . . . ? C1 O1 Bi4 O7 -151.0(9) . . . . ? Bi1 O1 Bi4 O7 21.4(7) . . . . ? C1 O1 Bi4 O6 118.7(9) . . . . ? Bi1 O1 Bi4 O6 -68.8(4) . . . . ? C1 O1 Bi4 Bi1 -172.5(11) . . . . ? O17 Bi1 Bi4 O18 38.2(5) . . . . ? O1 Bi1 Bi4 O18 168.2(5) . . . . ? O2 Bi1 Bi4 O18 108.2(5) . . . . ? O19 Bi1 Bi4 O18 -40.7(5) . . . . ? Bi2 Bi1 Bi4 O18 67.0(4) . . . . ? O18 Bi1 Bi4 O8 95.3(5) . . . . ? O17 Bi1 Bi4 O8 133.5(3) . . . . ? O1 Bi1 Bi4 O8 -96.5(4) . . . . ? O2 Bi1 Bi4 O8 -156.5(3) . . . . ? O19 Bi1 Bi4 O8 54.6(3) . . . . ? Bi2 Bi1 Bi4 O8 162.3(2) . . . . ? O18 Bi1 Bi4 O7 25.0(5) . . . . ? O17 Bi1 Bi4 O7 63.2(4) . . . . ? O1 Bi1 Bi4 O7 -166.8(5) . . . . ? O2 Bi1 Bi4 O7 133.2(4) . . . . ? O19 Bi1 Bi4 O7 -15.7(3) . . . . ? Bi2 Bi1 Bi4 O7 92.0(3) . . . . ? O18 Bi1 Bi4 O6 -52.9(5) . . . . ? O17 Bi1 Bi4 O6 -14.7(3) . . . . ? O1 Bi1 Bi4 O6 115.3(4) . . . . ? O2 Bi1 Bi4 O6 55.3(3) . . . . ? O19 Bi1 Bi4 O6 -93.6(3) . . . . ? Bi2 Bi1 Bi4 O6 14.1(2) . . . . ? O18 Bi1 Bi4 O1 -168.2(5) . . . . ? O17 Bi1 Bi4 O1 -130.0(4) . . . . ? O2 Bi1 Bi4 O1 -60.0(4) . . . . ? O19 Bi1 Bi4 O1 151.1(4) . . . . ? Bi2 Bi1 Bi4 O1 -101.2(4) . . . . ? C216 O16 Bi5 O19 136.4(11) . . . . ? Bi8 O16 Bi5 O19 -61.2(5) . . . . ? C216 O16 Bi5 O9 69.2(12) . . . . ? Bi8 O16 Bi5 O9 -128.3(4) . . . . ? C216 O16 Bi5 O20 -170.3(13) . . . . ? Bi8 O16 Bi5 O20 -7.8(4) . . . . ? C216 O16 Bi5 O18 -132.1(11) . . . . ? Bi8 O16 Bi5 O18 30.4(7) . . . . ? C216 O16 Bi5 Bi6 103.4(12) . . . . ? Bi8 O16 Bi5 Bi6 -94.1(3) . . . . ? Bi6 O19 Bi5 O16 -86.2(5) . . . . ? Bi7 O19 Bi5 O16 48.1(5) . . . . ? Bi1 O19 Bi5 O16 161.0(3) . . . . ? Bi6 O19 Bi5 O9 -8.9(4) . . . . ? Bi7 O19 Bi5 O9 125.3(5) . . . . ? Bi1 O19 Bi5 O9 -121.8(4) . . . . ? Bi6 O19 Bi5 O20 -140.7(5) . . . . ? Bi7 O19 Bi5 O20 -6.4(3) . . . . ? Bi1 O19 Bi5 O20 106.4(4) . . . . ? Bi6 O19 Bi5 O18 135.4(5) . . . . ? Bi7 O19 Bi5 O18 -90.4(4) . . . . ? Bi1 O19 Bi5 O18 22.5(3) . . . . ? Bi7 O19 Bi5 Bi6 134.2(6) . . . . ? Bi1 O19 Bi5 Bi6 -112.9(5) . . . . ? C113 O9 Bi5 O16 -69.6(11) . . . . ? Bi6 O9 Bi5 O16 124.9(4) . . . . ? C113 O9 Bi5 O19 172.6(11) . . . . ? Bi6 O9 Bi5 O19 7.1(3) . . . . ? C113 O9 Bi5 O20 -136.0(10) . . . . ? Bi6 O9 Bi5 O20 58.5(4) . . . . ? C113 O9 Bi5 O18 127.5(10) . . . . ? Bi6 O9 Bi5 O18 -38.0(5) . . . . ? C113 O9 Bi5 Bi6 165.5(12) . . . . ? Bi8 O20 Bi5 O16 9.6(4) . . . . ? Bi7 O20 Bi5 O16 -122.1(5) . . . . ? Bi8 O20 Bi5 O19 138.2(6) . . . . ? Bi7 O20 Bi5 O19 6.5(3) . . . . ? Bi8 O20 Bi5 O9 85.7(5) . . . . ? Bi7 O20 Bi5 O9 -46.0(5) . . . . ? Bi8 O20 Bi5 O18 -146.8(5) . . . . ? Bi7 O20 Bi5 O18 81.4(4) . . . . ? Bi8 O20 Bi5 Bi6 119.1(4) . . . . ? Bi7 O20 Bi5 Bi6 -12.6(4) . . . . ? Bi4 O18 Bi5 O16 104.2(5) . . . . ? Bi1 O18 Bi5 O16 -133.9(5) . . . . ? Bi3 O18 Bi5 O16 -15.7(7) . . . . ? Bi4 O18 Bi5 O19 -148.2(4) . . . . ? Bi1 O18 Bi5 O19 -26.4(3) . . . . ? Bi3 O18 Bi5 O19 91.8(4) . . . . ? Bi4 O18 Bi5 O9 -103.5(4) . . . . ? Bi1 O18 Bi5 O9 18.4(5) . . . . ? Bi3 O18 Bi5 O9 136.6(4) . . . . ? Bi4 O18 Bi5 O20 140.9(4) . . . . ? Bi1 O18 Bi5 O20 -97.3(4) . . . . ? Bi3 O18 Bi5 O20 20.9(4) . . . . ? Bi4 O18 Bi5 Bi6 -127.0(3) . . . . ? Bi1 O18 Bi5 Bi6 -5.1(3) . . . . ? Bi3 O18 Bi5 Bi6 113.0(3) . . . . ? Bi5 O19 Bi6 O11 -155.0(5) . . . . ? Bi7 O19 Bi6 O11 72.2(4) . . . . ? Bi1 O19 Bi6 O11 -43.6(4) . . . . ? Bi5 O19 Bi6 O10 -73.9(5) . . . . ? Bi7 O19 Bi6 O10 153.4(5) . . . . ? Bi1 O19 Bi6 O10 37.5(4) . . . . ? Bi5 O19 Bi6 O12 122.3(5) . . . . ? Bi7 O19 Bi6 O12 -10.4(4) . . . . ? Bi1 O19 Bi6 O12 -126.3(4) . . . . ? Bi5 O19 Bi6 O9 8.4(4) . . . . ? Bi7 O19 Bi6 O9 -124.4(5) . . . . ? Bi1 O19 Bi6 O9 119.8(4) . . . . ? Bi7 O19 Bi6 Bi5 -132.7(6) . . . . ? Bi1 O19 Bi6 Bi5 111.5(6) . . . . ? C146 O11 Bi6 O19 -174.1(10) . . . . ? C146 O11 Bi6 O10 104.5(10) . . . . ? C146 O11 Bi6 O12 -104.0(10) . . . . ? C146 O11 Bi6 O9 158.5(9) . . . . ? C146 O11 Bi6 Bi5 171.8(9) . . . . ? C132 O10 Bi6 O19 175.7(10) . . . . ? C132 O10 Bi6 O11 -104.3(10) . . . . ? C132 O10 Bi6 O12 -157.9(8) . . . . ? C132 O10 Bi6 O9 104.3(9) . . . . ? C132 O10 Bi6 Bi5 142.0(9) . . . . ? C160 O12 Bi6 O19 170.6(12) . . . . ? Bi7 O12 Bi6 O19 10.1(4) . . . . ? C160 O12 Bi6 O11 88.9(11) . . . . ? Bi7 O12 Bi6 O11 -71.7(5) . . . . ? C160 O12 Bi6 O10 142.5(11) . . . . ? Bi7 O12 Bi6 O10 -18.0(9) . . . . ? C160 O12 Bi6 O9 -127.5(11) . . . . ? Bi7 O12 Bi6 O9 72.0(4) . . . . ? C160 O12 Bi6 Bi5 -161.7(11) . . . . ? Bi7 O12 Bi6 Bi5 37.8(3) . . . . ? C113 O9 Bi6 O19 -174.7(10) . . . . ? Bi5 O9 Bi6 O19 -7.6(3) . . . . ? C113 O9 Bi6 O11 -146.0(9) . . . . ? Bi5 O9 Bi6 O11 21.1(7) . . . . ? C113 O9 Bi6 O10 -92.0(10) . . . . ? Bi5 O9 Bi6 O10 75.1(4) . . . . ? C113 O9 Bi6 O12 124.4(9) . . . . ? Bi5 O9 Bi6 O12 -68.5(4) . . . . ? C113 O9 Bi6 Bi5 -167.1(11) . . . . ? O16 Bi5 Bi6 O19 106.6(5) . . . . ? O9 Bi5 Bi6 O19 166.9(6) . . . . ? O20 Bi5 Bi6 O19 36.1(5) . . . . ? O18 Bi5 Bi6 O19 -42.0(5) . . . . ? O16 Bi5 Bi6 O11 132.5(4) . . . . ? O19 Bi5 Bi6 O11 25.9(5) . . . . ? O9 Bi5 Bi6 O11 -167.2(5) . . . . ? O20 Bi5 Bi6 O11 62.0(4) . . . . ? O18 Bi5 Bi6 O11 -16.1(3) . . . . ? O16 Bi5 Bi6 O10 -155.6(4) . . . . ? O19 Bi5 Bi6 O10 97.7(5) . . . . ? O9 Bi5 Bi6 O10 -95.4(4) . . . . ? O20 Bi5 Bi6 O10 133.9(4) . . . . ? O18 Bi5 Bi6 O10 55.8(3) . . . . ? O16 Bi5 Bi6 O12 54.7(3) . . . . ? O19 Bi5 Bi6 O12 -51.9(5) . . . . ? O9 Bi5 Bi6 O12 115.0(4) . . . . ? O20 Bi5 Bi6 O12 -15.8(3) . . . . ? O18 Bi5 Bi6 O12 -93.9(3) . . . . ? O16 Bi5 Bi6 O9 -60.3(4) . . . . ? O19 Bi5 Bi6 O9 -166.9(6) . . . . ? O20 Bi5 Bi6 O9 -130.8(4) . . . . ? O18 Bi5 Bi6 O9 151.1(4) . . . . ? C246 C245 N2 Bi7 81(27) . . . . ? C174 O13 Bi7 O12 -63.0(14) . . . . ? Bi8 O13 Bi7 O12 125.3(4) . . . . ? C174 O13 Bi7 O20 179.2(15) . . . . ? Bi8 O13 Bi7 O20 7.5(3) . . . . ? C174 O13 Bi7 O19 -126.7(14) . . . . ? Bi8 O13 Bi7 O19 61.6(5) . . . . ? C174 O13 Bi7 O21 107.9(14) . . . . ? Bi8 O13 Bi7 O21 -63.8(4) . . . . ? C174 O13 Bi7 N2 25.1(14) . . . . ? Bi8 O13 Bi7 N2 -146.6(5) . . . . ? C174 O13 Bi7 Bi8 171.7(16) . . . . ? C160 O12 Bi7 O13 72.6(13) . . . . ? Bi6 O12 Bi7 O13 -129.8(5) . . . . ? C160 O12 Bi7 O20 141.6(13) . . . . ? Bi6 O12 Bi7 O20 -60.9(5) . . . . ? C160 O12 Bi7 O19 -166.8(14) . . . . ? Bi6 O12 Bi7 O19 -9.2(3) . . . . ? C160 O12 Bi7 O21 22(3) . . . . ? Bi6 O12 Bi7 O21 180(33) . . . . ? C160 O12 Bi7 N2 -7.6(13) . . . . ? Bi6 O12 Bi7 N2 149.9(5) . . . . ? C160 O12 Bi7 Bi8 108.3(13) . . . . ? Bi6 O12 Bi7 Bi8 -94.2(3) . . . . ? Bi8 O20 Bi7 O13 -9.8(4) . . . . ? Bi5 O20 Bi7 O13 121.9(5) . . . . ? Bi8 O20 Bi7 O12 -85.7(5) . . . . ? Bi5 O20 Bi7 O12 45.9(5) . . . . ? Bi8 O20 Bi7 O19 -138.0(5) . . . . ? Bi5 O20 Bi7 O19 -6.4(3) . . . . ? Bi8 O20 Bi7 O21 83.4(4) . . . . ? Bi5 O20 Bi7 O21 -145.0(5) . . . . ? Bi8 O20 Bi7 N2 35.9(9) . . . . ? Bi5 O20 Bi7 N2 167.6(6) . . . . ? Bi5 O20 Bi7 Bi8 131.6(7) . . . . ? Bi6 O19 Bi7 O13 84.1(5) . . . . ? Bi5 O19 Bi7 O13 -50.4(5) . . . . ? Bi1 O19 Bi7 O13 -160.9(4) . . . . ? Bi6 O19 Bi7 O12 11.3(4) . . . . ? Bi5 O19 Bi7 O12 -123.2(5) . . . . ? Bi1 O19 Bi7 O12 126.3(4) . . . . ? Bi6 O19 Bi7 O20 141.0(5) . . . . ? Bi5 O19 Bi7 O20 6.5(3) . . . . ? Bi1 O19 Bi7 O20 -104.0(4) . . . . ? Bi6 O19 Bi7 O21 -170.9(3) . . . . ? Bi5 O19 Bi7 O21 54.6(5) . . . . ? Bi1 O19 Bi7 O21 -55.8(5) . . . . ? Bi6 O19 Bi7 N2 -32.0(10) . . . . ? Bi5 O19 Bi7 N2 -166.5(7) . . . . ? Bi1 O19 Bi7 N2 83.0(9) . . . . ? Bi6 O19 Bi7 Bi8 120.6(4) . . . . ? Bi5 O19 Bi7 Bi8 -13.9(3) . . . . ? Bi1 O19 Bi7 Bi8 -124.4(3) . . . . ? Bi3 O21 Bi7 O13 122.1(4) . . . . ? Bi3 O21 Bi7 O12 172.3(16) . . . . ? Bi3 O21 Bi7 O20 48.9(3) . . . . ? Bi3 O21 Bi7 O19 2.3(5) . . . . ? Bi3 O21 Bi7 N2 -157.6(4) . . . . ? Bi3 O21 Bi7 Bi8 82.2(2) . . . . ? C245 N2 Bi7 O13 -50(2) . . . . ? C245 N2 Bi7 O12 35(2) . . . . ? C245 N2 Bi7 O20 -95(3) . . . . ? C245 N2 Bi7 O19 75(3) . . . . ? C245 N2 Bi7 O21 -139(3) . . . . ? C245 N2 Bi7 Bi8 -75(3) . . . . ? Bi7 O20 Bi8 O15 -152.0(5) . . . . ? Bi5 O20 Bi8 O15 77.8(5) . . . . ? Bi7 O20 Bi8 O14 -70.4(5) . . . . ? Bi5 O20 Bi8 O14 159.4(5) . . . . ? Bi7 O20 Bi8 O16 121.3(5) . . . . ? Bi5 O20 Bi8 O16 -8.9(4) . . . . ? Bi7 O20 Bi8 O13 8.7(4) . . . . ? Bi5 O20 Bi8 O13 -121.6(5) . . . . ? Bi7 O20 Bi8 C202 -157.9(5) . . . . ? Bi5 O20 Bi8 C202 71.9(6) . . . . ? Bi5 O20 Bi8 Bi7 -130.2(7) . . . . ? C202 O15 Bi8 O20 -167.6(10) . . . . ? C202 O15 Bi8 O14 102.5(10) . . . . ? C202 O15 Bi8 O16 -97.4(10) . . . . ? C202 O15 Bi8 O13 158.3(9) . . . . ? C202 O15 Bi8 Bi7 175.8(9) . . . . ? C188 O14 Bi8 O20 169.3(11) . . . . ? C188 O14 Bi8 O15 -107.9(11) . . . . ? C188 O14 Bi8 O16 -163.1(10) . . . . ? C188 O14 Bi8 O13 99.8(11) . . . . ? C188 O14 Bi8 C202 -81.8(11) . . . . ? C188 O14 Bi8 Bi7 136.6(11) . . . . ? C216 O16 Bi8 O20 171.1(12) . . . . ? Bi5 O16 Bi8 O20 8.5(4) . . . . ? C216 O16 Bi8 O15 86.8(12) . . . . ? Bi5 O16 Bi8 O15 -75.8(4) . . . . ? C216 O16 Bi8 O14 141.5(13) . . . . ? Bi5 O16 Bi8 O14 -21.0(12) . . . . ? C216 O16 Bi8 O13 -126.5(11) . . . . ? Bi5 O16 Bi8 O13 70.9(4) . . . . ? C216 O16 Bi8 C202 60.3(12) . . . . ? Bi5 O16 Bi8 C202 -102.3(5) . . . . ? C216 O16 Bi8 Bi7 -160.3(11) . . . . ? Bi5 O16 Bi8 Bi7 37.1(3) . . . . ? C174 O13 Bi8 O20 178.1(11) . . . . ? Bi7 O13 Bi8 O20 -8.3(4) . . . . ? C174 O13 Bi8 O15 -145.6(10) . . . . ? Bi7 O13 Bi8 O15 28.1(9) . . . . ? C174 O13 Bi8 O14 -89.3(10) . . . . ? Bi7 O13 Bi8 O14 84.4(4) . . . . ? C174 O13 Bi8 O16 115.5(10) . . . . ? Bi7 O13 Bi8 O16 -70.8(4) . . . . ? C174 O13 Bi8 C202 -96.7(19) . . . . ? Bi7 O13 Bi8 C202 76.9(18) . . . . ? C174 O13 Bi8 Bi7 -173.7(12) . . . . ? O15 C202 Bi8 O20 13.0(11) . . . . ? C201 C202 Bi8 O20 -92.8(12) . . . . ? C197 C202 Bi8 O20 130.9(11) . . . . ? C201 C202 Bi8 O15 -105.8(16) . . . . ? C197 C202 Bi8 O15 117.9(17) . . . . ? O15 C202 Bi8 O14 -75.0(10) . . . . ? C201 C202 Bi8 O14 179.2(12) . . . . ? C197 C202 Bi8 O14 42.8(11) . . . . ? O15 C202 Bi8 O16 80.9(10) . . . . ? C201 C202 Bi8 O16 -24.9(12) . . . . ? C197 C202 Bi8 O16 -161.2(11) . . . . ? O15 C202 Bi8 O13 -68(2) . . . . ? C201 C202 Bi8 O13 -173.5(14) . . . . ? C197 C202 Bi8 O13 50(2) . . . . ? O15 C202 Bi8 Bi7 -6.0(12) . . . . ? C201 C202 Bi8 Bi7 -111.7(12) . . . . ? C197 C202 Bi8 Bi7 111.9(11) . . . . ? O13 Bi7 Bi8 O20 166.1(6) . . . . ? O12 Bi7 Bi8 O20 106.9(5) . . . . ? O19 Bi7 Bi8 O20 38.3(5) . . . . ? O21 Bi7 Bi8 O20 -85.6(5) . . . . ? N2 Bi7 Bi8 O20 -157.0(6) . . . . ? O13 Bi7 Bi8 O15 -163.6(5) . . . . ? O12 Bi7 Bi8 O15 137.2(4) . . . . ? O20 Bi7 Bi8 O15 30.3(6) . . . . ? O19 Bi7 Bi8 O15 68.6(4) . . . . ? O21 Bi7 Bi8 O15 -55.3(4) . . . . ? N2 Bi7 Bi8 O15 -126.7(5) . . . . ? O13 Bi7 Bi8 O14 -88.1(5) . . . . ? O12 Bi7 Bi8 O14 -147.3(4) . . . . ? O20 Bi7 Bi8 O14 105.8(5) . . . . ? O19 Bi7 Bi8 O14 144.0(4) . . . . ? O21 Bi7 Bi8 O14 20.2(4) . . . . ? N2 Bi7 Bi8 O14 -51.3(5) . . . . ? O13 Bi7 Bi8 O16 112.8(5) . . . . ? O12 Bi7 Bi8 O16 53.7(3) . . . . ? O20 Bi7 Bi8 O16 -53.3(5) . . . . ? O19 Bi7 Bi8 O16 -15.0(3) . . . . ? O21 Bi7 Bi8 O16 -138.8(3) . . . . ? N2 Bi7 Bi8 O16 149.7(5) . . . . ? O12 Bi7 Bi8 O13 -59.2(5) . . . . ? O20 Bi7 Bi8 O13 -166.1(6) . . . . ? O19 Bi7 Bi8 O13 -127.8(5) . . . . ? O21 Bi7 Bi8 O13 108.3(5) . . . . ? N2 Bi7 Bi8 O13 36.9(6) . . . . ? O13 Bi7 Bi8 C202 -160.7(6) . . . . ? O12 Bi7 Bi8 C202 140.2(6) . . . . ? O20 Bi7 Bi8 C202 33.2(7) . . . . ? O19 Bi7 Bi8 C202 71.5(5) . . . . ? O21 Bi7 Bi8 C202 -52.3(5) . . . . ? N2 Bi7 Bi8 C202 -123.8(7) . . . . ? C160 C155 C156 C157 -1(3) . . . . ? C154 C155 C156 C157 -173.8(18) . . . . ? C158 C157 C156 C155 2(3) . . . . ? C161 C157 C156 C155 -175.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.941 _refine_diff_density_min -2.372 _refine_diff_density_rms 0.217