# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Phil Andrews' _publ_contact_author_email phil.andrews@sci.monash.edu.au _publ_author_name P.Andrews data_mb582a _database_code_depnum_ccdc_archive 'CCDC 882406' #TrackingRef '- Cmpd 1 updated.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C180 H298 Bi18 O104 S18, 21(H2 O)' _chemical_formula_sum 'C180 H340 Bi18 O125 S18' _chemical_formula_weight 8843.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.027 10.608 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 30.797(6) _cell_length_b 19.123(4) _cell_length_c 22.706(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.00(3) _cell_angle_gamma 90.00 _cell_volume 13080(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 48107 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 26.62 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8404 _exptl_absorpt_coefficient_mu 12.299 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'MX2 beamline, Australian Synchrotron' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 201r CCD' _diffrn_measurement_method '\f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48278 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.62 _reflns_number_total 25425 _reflns_number_gt 25248 _reflns_threshold_expression >2sigma(I) _computing_data_collection BluIce _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The oxygen atoms O(11), O(54)-O(60) and O(62)-O(66) are water molecules which are either located on the cluster core or are positioned within the crystal lattice. Therefore, the short inter D...A contact is probably due to hydrogen bonding. The hydrogen atoms H(58A) and H(68E) are not close to each other, and therefore, a short inter XH3 .. CHn does not exist. explanation of restraints: all of these commands/restraints were required to get a stable refinement because there was a lot of disorder in: Ligand S1: C3/C3' and C8/C8' and the corresponding H atoms Ligand S7: C61/61' to C70/C70' and the corresponding H atoms Ligand S9: C81/C81' to C90/C90' and the corrsponding H atoms explanation of restraints more detailed: EXYZ C70 C70' EADP C70 C70' Ligand S7 was completely modelled as disordered; as the atoms C70 and C70' share the same site the EXYZ and EADP constraints were used. OMIT -18 -10 24 OMIT 2 2 1 OMIT -18 -6 26 DFIX 1.55 0.01 C67' C69' DFIX 1.50 C67' C68' DANG 2.43 C68' C69' To stabilise the position of the disordered methyl groups of atoms C68' and C69' which are part of ligand S7. SIMU 0.02 0.02 1.7 C67' C69' This instruction restrains the Uij components of these atom pairs to be approximately equal with an appropriate esd - in this case SIMU was effective and EADP was not needed. DELU C62 O45 As no values are given for the standard deviation s1 and s2, this 'rigid bond' restraint is switched off. ISOR 0.005 C4 C7 O11 O64 O65 O66 ISOR 0.01 C14 C86 C81 C82 C83 The atoms O11, O64, O65 and O66 represent solvent water molecules of the crystal lattice for which DELU and SIMU were not appropriate restraints The C atoms C4 and C7 (ligand S1) and C14 (ligand S2) were dried to be modelled as disorder which was not successful - therefore the ISOR restraint was used to prevent the C atoms from going n.p.d.. Even though the C atoms C81, C82, C83 and C86 could be modelled as disorder, the ISOR restraint was still necessary to prevent atoms from going n.p.d.. SADI 0.01 C84 C85 C84' C85' SADI 0.01 C85 C86 C85' C86' The distances between these atom pairs where restraint to be equal with an effective standard deviation of 0.01. The atom pairs labelled with ' display part 2 of the modelled disorder and were therefore handeled equal. to part 1 of the disorder. SIMU 0.02 0.02 1.7 C81' C82' C86' C87' This instruction restrains the Uij components of these atom pairs to be approximately equal with an appropriate esd - in this case SIMU was effective and EADP was not needed. EADP C3 C3' EADP C8 C8' Ligand S1 displayed only disorder for the atoms C3/C3' (CH2 group) and C8/C8' (CH3 group) with occupancies for each group of 60/40. As those atoms are not occupying the same site, the EADP constraint (applying the same aniosotropic displacement parameters) was used. EXYZ C90 C90' EADP C90 C90' Ligand S9 was completely modelled as disordered; as the atoms C90 and C90' share the same site the EXYZ and EADP contraints were used DFIX 1.55 C87' C88' The position of the disordered methyl group of atom C88', which is part of ligand S9, was set to 1.55 which is in average represented as a typical C-C bond within the structure. DFIX 1.28 0.01 C82' O53' To stabilise the position of the disordered carbonyl group with O53' which is part of ligand S9. ; _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^)+(0.0454P)^2^+107.4436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(3) _refine_ls_number_reflns 25425 _refine_ls_number_parameters 1637 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad 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 0.946881(8) 0.577110(14) 0.573981(11) 0.014 Uani 1 1 d . A . Bi2 Bi 0.836644(9) 0.655859(14) 0.579580(12) 0.016 Uani 1 1 d . A . Bi3 Bi 0.850679(9) 0.466496(14) 0.592723(12) 0.015 Uani 1 1 d . A . Bi4 Bi 0.945655(9) 0.493276(14) 0.718736(11) 0.015 Uani 1 1 d . . . Bi5 Bi 0.838697(8) 0.573762(13) 0.725522(11) 0.015 Uani 1 1 d . A . Bi6 Bi 0.932173(9) 0.684100(14) 0.703426(12) 0.015 Uani 1 1 d . A . Bi7 Bi 0.955912(8) 0.592743(14) 0.887110(10) 0.013 Uani 1 1 d . . . Bi8 Bi 1.0000 0.72519(2) 1.0000 0.017 Uani 1 2 d S . . Bi9 Bi 1.074502(8) 0.589714(15) 0.964988(11) 0.015 Uani 1 1 d . . . Bi10 Bi 1.0000 0.455061(19) 1.0000 0.014 Uani 1 2 d S . . S1 S 0.99973(6) 0.75681(10) 0.60163(8) 0.017 Uani 1 1 d . H . S2 S 0.92489(7) 0.39647(10) 0.49785(9) 0.022 Uani 1 1 d . H . S3 S 0.75328(7) 0.54957(12) 0.47220(9) 0.026 Uani 1 1 d . H . S4 S 0.75145(6) 0.44504(10) 0.66781(9) 0.020 Uani 1 1 d . H . S5 S 0.92910(5) 0.40084(9) 0.84516(7) 0.013 Uani 1 1 d . . . S6 S 0.82986(6) 0.62808(10) 0.87189(8) 0.017 Uani 1 1 d . . . S7 S 0.94219(7) 0.78568(10) 0.84004(8) 0.023 Uani 1 1 d . . . S8 S 1.05110(6) 0.62177(10) 0.80134(8) 0.018 Uani 1 1 d . . . S9 S 1.07191(9) 0.36048(14) 0.88371(14) 0.042 Uani 1 1 d . . . O1 O 0.86577(16) 0.5634(3) 0.5344(2) 0.016 Uani 1 1 d . . . H1 H 0.8559 0.5592 0.4897 0.019 Uiso 1 1 calc R H . O2 O 0.90688(17) 0.6561(3) 0.6112(2) 0.017 Uani 1 1 d . . . O3 O 0.97715(16) 0.5914(3) 0.6747(2) 0.015 Uani 1 1 d . A . H3 H 1.0101 0.5974 0.6862 0.018 Uiso 1 1 calc R . . O4 O 0.92020(15) 0.4944(3) 0.6235(2) 0.013 Uani 1 1 d . A . O5 O 0.91101(15) 0.5829(2) 0.7350(2) 0.011 Uani 1 1 d . A . O6 O 0.87284(16) 0.4618(3) 0.7033(2) 0.016 Uani 1 1 d . A . H6 H 0.8652 0.4187 0.7240 0.019 Uiso 1 1 calc R . . O7 O 0.82995(17) 0.5624(3) 0.6306(2) 0.016 Uani 1 1 d . . . O8 O 0.85444(16) 0.6820(3) 0.6921(2) 0.015 Uani 1 1 d . . . H8 H 0.8398 0.7235 0.7066 0.018 Uiso 1 1 calc R H . O9 O 1.0257(2) 0.5147(4) 0.6008(3) 0.031 Uani 1 1 d . . . O10 O 0.8540(2) 0.7102(3) 0.4827(3) 0.030 Uani 1 1 d . . . O11 O 0.7814(5) 0.7755(7) 0.5974(6) 0.097 Uani 1 1 d U . . O12 O 0.92607(18) 0.6388(3) 0.4582(2) 0.023 Uani 1 1 d . . . O13 O 0.93275(17) 0.6692(3) 0.9550(2) 0.015 Uani 1 1 d . . . H13 H 0.9067 0.6999 0.9388 0.018 Uiso 1 1 calc R . . O14 O 1.01325(16) 0.6468(3) 0.9391(2) 0.013 Uani 1 1 d . H . O15 O 0.94954(16) 0.5316(3) 0.9654(2) 0.014 Uani 1 1 d . . . O16 O 1.02139(16) 0.5120(3) 0.9179(2) 0.016 Uani 1 1 d . H . H16 H 1.0293 0.4816 0.8859 0.019 Uiso 1 1 calc R . . O17 O 1.12887(18) 0.4793(3) 0.9793(2) 0.023 Uani 1 1 d . H . O18 O 0.99719(18) 0.6884(3) 0.5717(2) 0.020 Uani 1 1 d . . . O19 O 0.99415(18) 0.7481(3) 0.6634(2) 0.017 Uani 1 1 d . . . O20 O 1.03884(18) 0.7960(3) 0.5960(3) 0.023 Uani 1 1 d . . . O21 O 0.8951(2) 0.7996(3) 0.6521(3) 0.033 Uani 1 1 d . . . O22 O 0.87886(19) 0.4001(3) 0.5059(2) 0.023 Uani 1 1 d . . . O23 O 0.9452(2) 0.4668(3) 0.4988(3) 0.025 Uani 1 1 d . . . O24 O 0.9302(2) 0.3565(3) 0.4456(3) 0.029 Uani 1 1 d . . . O25 O 0.8824(2) 0.3403(3) 0.6278(3) 0.023 Uani 1 1 d . . . O26 O 0.7832(2) 0.4925(4) 0.4949(3) 0.035 Uani 1 1 d . . . O27 O 0.7603(2) 0.6096(3) 0.5146(3) 0.030 Uani 1 1 d . . . O28 O 0.7069(2) 0.5286(5) 0.4546(3) 0.045 Uani 1 1 d . . . O29 O 0.85974(18) 0.5381(3) 0.4140(2) 0.024 Uani 1 1 d . . . O30 O 0.78083(19) 0.4149(3) 0.6314(3) 0.022 Uani 1 1 d . . . O31 O 0.77610(19) 0.4815(3) 0.7212(2) 0.023 Uani 1 1 d . . . O32 O 0.7203(2) 0.3940(3) 0.6830(3) 0.029 Uani 1 1 d . . . O33 O 0.7599(2) 0.6362(3) 0.6827(3) 0.032 Uani 1 1 d . . . O34 O 0.93715(17) 0.4749(3) 0.8311(2) 0.016 Uani 1 1 d . H . O35 O 0.95634(16) 0.3797(3) 0.9033(2) 0.017 Uani 1 1 d . H . O36 O 0.93327(17) 0.3556(3) 0.7955(2) 0.018 Uani 1 1 d . H . O37 O 0.83770(18) 0.3354(3) 0.7380(2) 0.020 Uani 1 1 d . . . O38 O 0.86651(17) 0.5856(3) 0.8580(2) 0.021 Uani 1 1 d . A . O39 O 0.84491(18) 0.6858(3) 0.9123(3) 0.024 Uani 1 1 d . H . O40 O 0.79920(19) 0.6492(3) 0.8166(2) 0.025 Uani 1 1 d . A . O41 O 0.8306(2) 0.6288(4) 1.0310(3) 0.032 Uani 1 1 d . . . O42 O 0.9781(2) 0.7913(3) 0.8931(3) 0.028 Uani 1 1 d . . . O43 O 0.9308(2) 0.7113(3) 0.8251(3) 0.026 Uani 1 1 d . A . O44 O 0.9503(2) 0.8243(3) 0.7887(3) 0.031 Uani 1 1 d . A . O45 O 0.8587(3) 0.9210(5) 0.7655(5) 0.029 Uani 0.60 1 d PU A 1 O45' O 0.9339(5) 0.8323(9) 0.9929(7) 0.031 Uiso 0.40 1 d P A 2 O46 O 1.00464(17) 0.6009(3) 0.8006(2) 0.021 Uani 1 1 d . A . O47 O 1.08223(16) 0.5922(3) 0.8527(2) 0.020 Uani 1 1 d . H . O48 O 1.06346(18) 0.6060(3) 0.7448(2) 0.026 Uani 1 1 d . H . O49 O 1.0959(2) 0.7301(4) 0.9366(3) 0.036 Uani 1 1 d . H . O50 O 1.0537(3) 0.4223(4) 0.8449(4) 0.049 Uani 1 1 d . . . O51 O 1.0674(2) 0.3698(4) 0.9467(3) 0.038 Uani 1 1 d . . . O52 O 1.1175(3) 0.3422(6) 0.8815(5) 0.081 Uani 1 1 d . . . O53 O 1.0934(5) 0.2152(6) 0.7882(7) 0.056 Uani 0.70 1 d P B 1 O53' O 1.1014(7) 0.1943(12) 0.8006(9) 0.030 Uiso 0.30 1 d PD C 2 C1 C 0.9388(3) 0.8684(4) 0.5946(4) 0.025 Uani 1 1 d . . . C2 C 0.9038(3) 0.8562(5) 0.6321(5) 0.034 Uani 1 1 d . D . C3 C 0.8856(9) 0.9279(13) 0.6449(12) 0.051 Uani 0.60 1 d P D 1 H3A H 0.8948 0.9409 0.6879 0.062 Uiso 0.60 1 calc PR D 1 H3B H 0.8528 0.9297 0.6327 0.062 Uiso 0.60 1 calc PR D 1 C4 C 0.9079(4) 0.9746(6) 0.6045(5) 0.047 Uani 1 1 d U . . H4 H 0.8921 1.0196 0.5920 0.056 Uiso 1 1 calc R D 1 C5 C 0.9541(4) 0.9829(5) 0.6435(5) 0.048 Uani 1 1 d . D . H5A H 0.9526 0.9938 0.6857 0.057 Uiso 1 1 calc R . . H5B H 0.9708 1.0205 0.6279 0.057 Uiso 1 1 calc R . . C6 C 0.9763(3) 0.9095(5) 0.6389(4) 0.033 Uani 1 1 d . D . H6A H 0.9840 0.8863 0.6787 0.040 Uiso 1 1 calc R . . H6B H 1.0035 0.9138 0.6222 0.040 Uiso 1 1 calc R . . C7 C 0.9158(3) 0.9282(5) 0.5515(4) 0.031 Uani 1 1 d U D . C8' C 0.8742(10) 0.8932(13) 0.4999(16) 0.042 Uani 0.40 1 d P D 2 H8'1 H 0.8527 0.8709 0.5204 0.063 Uiso 0.40 1 calc PR D 2 H8'2 H 0.8862 0.8582 0.4761 0.063 Uiso 0.40 1 calc PR D 2 H8'3 H 0.8593 0.9302 0.4732 0.063 Uiso 0.40 1 calc PR D 2 C9 C 0.9458(4) 0.9602(5) 0.5124(5) 0.043 Uani 1 1 d . . . H9A H 0.9490 0.9272 0.4805 0.065 Uiso 1 1 calc R D . H9B H 0.9751 0.9701 0.5374 0.065 Uiso 1 1 calc R . . H9C H 0.9326 1.0038 0.4942 0.065 Uiso 1 1 calc R . . C10 C 0.9526(3) 0.8035(4) 0.5631(4) 0.021 Uani 1 1 d . H . H10A H 0.9584 0.8184 0.5236 0.026 Uiso 1 1 calc R . . H10B H 0.9271 0.7709 0.5550 0.026 Uiso 1 1 calc R . . C11 C 0.9386(3) 0.2839(4) 0.5804(3) 0.021 Uani 1 1 d . . . C12 C 0.9042(3) 0.2900(4) 0.6203(4) 0.023 Uani 1 1 d . H . C13 C 0.9033(3) 0.2202(4) 0.6513(4) 0.030 Uani 1 1 d . . . H13A H 0.8739 0.1974 0.6391 0.036 Uiso 1 1 calc R H . H13B H 0.9106 0.2253 0.6956 0.036 Uiso 1 1 calc R . . C14 C 0.9391(3) 0.1794(4) 0.6287(4) 0.030 Uani 1 1 d U H . H14 H 0.9518 0.1391 0.6548 0.036 Uiso 1 1 calc R . . C15 C 0.9190(4) 0.1598(5) 0.5624(5) 0.041 Uani 1 1 d . . . H15A H 0.8889 0.1397 0.5583 0.050 Uiso 1 1 calc R H . H15B H 0.9381 0.1260 0.5466 0.050 Uiso 1 1 calc R . . C16 C 0.9175(3) 0.2320(4) 0.5296(4) 0.030 Uani 1 1 d . H . H16A H 0.9349 0.2305 0.4976 0.036 Uiso 1 1 calc R . . H16B H 0.8866 0.2455 0.5116 0.036 Uiso 1 1 calc R . . C17 C 0.9728(3) 0.2377(5) 0.6233(4) 0.027 Uani 1 1 d . H . C18 C 0.9942(4) 0.2744(6) 0.6817(4) 0.039 Uani 1 1 d . . . H18A H 1.0150 0.3100 0.6733 0.059 Uiso 1 1 calc R H . H18B H 1.0102 0.2401 0.7102 0.059 Uiso 1 1 calc R . . H18C H 0.9711 0.2968 0.6991 0.059 Uiso 1 1 calc R . . C19 C 1.0115(3) 0.2102(5) 0.5947(5) 0.038 Uani 1 1 d . . . H19A H 0.9992 0.1855 0.5571 0.057 Uiso 1 1 calc R H . H19B H 1.0301 0.1780 0.6228 0.057 Uiso 1 1 calc R . . H19C H 1.0295 0.2497 0.5863 0.057 Uiso 1 1 calc R . . C20 C 0.9560(3) 0.3532(5) 0.5620(4) 0.027 Uani 1 1 d . H . H20A H 0.9863 0.3450 0.5549 0.032 Uiso 1 1 calc R . . H20B H 0.9590 0.3855 0.5967 0.032 Uiso 1 1 calc R . . C21 C 0.7823(3) 0.5340(4) 0.3629(4) 0.023 Uani 1 1 d . H . C22 C 0.8323(3) 0.5243(4) 0.3698(4) 0.022 Uani 1 1 d . . . C23 C 0.8415(3) 0.4958(6) 0.3105(4) 0.035 Uani 1 1 d . . . H23A H 0.8547 0.4484 0.3155 0.042 Uiso 1 1 calc R . . H23B H 0.8611 0.5273 0.2932 0.042 Uiso 1 1 calc R . . C24 C 0.7934(3) 0.4946(6) 0.2714(4) 0.035 Uani 1 1 d . . . H24 H 0.7920 0.4940 0.2270 0.042 Uiso 1 1 calc R . . C25 C 0.7678(4) 0.4340(6) 0.2941(5) 0.042 Uani 1 1 d . . . H25A H 0.7386 0.4265 0.2668 0.051 Uiso 1 1 calc R . . H25B H 0.7850 0.3899 0.2973 0.051 Uiso 1 1 calc R . . C26 C 0.7623(3) 0.4588(5) 0.3557(4) 0.036 Uani 1 1 d . . . H26A H 0.7783 0.4276 0.3878 0.043 Uiso 1 1 calc R . . H26B H 0.7305 0.4597 0.3580 0.043 Uiso 1 1 calc R . . C27 C 0.7714(3) 0.5600(5) 0.2939(4) 0.028 Uani 1 1 d . . . C28 C 0.7933(3) 0.6294(6) 0.2857(4) 0.037 Uani 1 1 d . . . H28A H 0.8253 0.6258 0.3015 0.056 Uiso 1 1 calc R . . H28B H 0.7809 0.6660 0.3075 0.056 Uiso 1 1 calc R . . H28C H 0.7877 0.6411 0.2428 0.056 Uiso 1 1 calc R . . C29 C 0.7214(3) 0.5669(6) 0.2692(5) 0.038 Uani 1 1 d . . . H29A H 0.7068 0.5226 0.2748 0.058 Uiso 1 1 calc R . . H29B H 0.7161 0.5783 0.2262 0.058 Uiso 1 1 calc R . . H29C H 0.7095 0.6042 0.2908 0.058 Uiso 1 1 calc R . . C30 C 0.7699(3) 0.5840(5) 0.4073(4) 0.026 Uani 1 1 d . . . H30A H 0.7453 0.6136 0.3856 0.031 Uiso 1 1 calc R H . H30B H 0.7956 0.6152 0.4214 0.031 Uiso 1 1 calc R . . C31 C 0.6948(3) 0.5644(5) 0.6427(4) 0.027 Uani 1 1 d . . . C32 C 0.7211(3) 0.6231(5) 0.6795(4) 0.026 Uani 1 1 d . H . C33 C 0.6877(3) 0.6649(6) 0.7056(4) 0.036 Uani 1 1 d . . . H33A H 0.6953 0.6641 0.7502 0.044 Uiso 1 1 calc R H . H33B H 0.6866 0.7140 0.6917 0.044 Uiso 1 1 calc R . . C34 C 0.6442(3) 0.6283(5) 0.6821(4) 0.034 Uani 1 1 d . H . H34 H 0.6208 0.6375 0.7058 0.040 Uiso 1 1 calc R . . C35 C 0.6301(4) 0.6457(7) 0.6136(4) 0.045 Uani 1 1 d . . . H35A H 0.6001 0.6275 0.5963 0.054 Uiso 1 1 calc R H . H35B H 0.6306 0.6967 0.6064 0.054 Uiso 1 1 calc R . . C36 C 0.6658(3) 0.6077(5) 0.5875(4) 0.032 Uani 1 1 d . H . H36A H 0.6846 0.6417 0.5715 0.038 Uiso 1 1 calc R . . H36B H 0.6519 0.5757 0.5547 0.038 Uiso 1 1 calc R . . C37 C 0.6587(3) 0.5495(6) 0.6810(4) 0.033 Uani 1 1 d . H . C38 C 0.6772(4) 0.5223(6) 0.7441(4) 0.041 Uani 1 1 d . . . H38A H 0.7005 0.5539 0.7647 0.061 Uiso 1 1 calc R H . H38B H 0.6896 0.4755 0.7417 0.061 Uiso 1 1 calc R . . H38C H 0.6533 0.5201 0.7667 0.061 Uiso 1 1 calc R . . C39 C 0.6224(3) 0.5016(7) 0.6495(4) 0.042 Uani 1 1 d . . . H39A H 0.6103 0.5195 0.6089 0.064 Uiso 1 1 calc R H . H39B H 0.5987 0.4995 0.6724 0.064 Uiso 1 1 calc R . . H39C H 0.6345 0.4547 0.6467 0.064 Uiso 1 1 calc R . . C40 C 0.7213(3) 0.5090(4) 0.6187(3) 0.022 Uani 1 1 d . H . H40A H 0.7428 0.5334 0.5990 0.027 Uiso 1 1 calc R . . H40B H 0.7005 0.4836 0.5866 0.027 Uiso 1 1 calc R . . C41 C 0.8509(2) 0.3290(4) 0.8473(3) 0.017 Uani 1 1 d . . . C42 C 0.8300(2) 0.3086(4) 0.7837(3) 0.017 Uani 1 1 d . H . C43 C 0.7971(3) 0.2506(4) 0.7865(4) 0.023 Uani 1 1 d . . . H43A H 0.8060 0.2065 0.7695 0.027 Uiso 1 1 calc R H . H43B H 0.7668 0.2636 0.7651 0.027 Uiso 1 1 calc R . . C44 C 0.8002(2) 0.2448(4) 0.8541(4) 0.019 Uani 1 1 d . H . H44 H 0.7735 0.2229 0.8652 0.023 Uiso 1 1 calc R . . C45 C 0.8429(3) 0.2085(4) 0.8806(4) 0.028 Uani 1 1 d . . . H45A H 0.8467 0.1658 0.8575 0.034 Uiso 1 1 calc R H . H45B H 0.8442 0.1957 0.9232 0.034 Uiso 1 1 calc R . . C46 C 0.8791(3) 0.2652(4) 0.8751(4) 0.022 Uani 1 1 d . H . H46A H 0.8975 0.2768 0.9151 0.026 Uiso 1 1 calc R . . H46B H 0.8987 0.2488 0.8484 0.026 Uiso 1 1 calc R . . C47 C 0.8084(2) 0.3219(4) 0.8759(3) 0.016 Uani 1 1 d . H . C48 C 0.7714(3) 0.3742(4) 0.8494(4) 0.021 Uani 1 1 d . . . H48A H 0.7647 0.3705 0.8054 0.032 Uiso 1 1 calc R H . H48B H 0.7813 0.4218 0.8612 0.032 Uiso 1 1 calc R . . H48C H 0.7447 0.3635 0.8647 0.032 Uiso 1 1 calc R . . C49 C 0.8182(3) 0.3300(5) 0.9445(4) 0.027 Uani 1 1 d . . . H49A H 0.8418 0.2976 0.9626 0.040 Uiso 1 1 calc R H . H49B H 0.7913 0.3197 0.9596 0.040 Uiso 1 1 calc R . . H49C H 0.8276 0.3781 0.9552 0.040 Uiso 1 1 calc R . . C50 C 0.8730(2) 0.4013(4) 0.8540(3) 0.016 Uani 1 1 d . H . H50A H 0.8720 0.4201 0.8944 0.019 Uiso 1 1 calc R . . H50B H 0.8556 0.4332 0.8237 0.019 Uiso 1 1 calc R . . C51 C 0.7692(2) 0.6022(4) 0.9455(3) 0.018 Uani 1 1 d . . . C52 C 0.7915(3) 0.6232(5) 1.0103(4) 0.028 Uani 1 1 d . H . C53 C 0.7535(3) 0.6368(6) 1.0422(4) 0.040 Uani 1 1 d . . . H53A H 0.7515 0.6870 1.0520 0.047 Uiso 1 1 calc R H . H53B H 0.7570 0.6090 1.0797 0.047 Uiso 1 1 calc R . . C54 C 0.7130(3) 0.6131(6) 0.9957(4) 0.033 Uani 1 1 d . H . H54 H 0.6873 0.5986 1.0135 0.040 Uiso 1 1 calc R . . C55 C 0.7021(3) 0.6719(5) 0.9485(4) 0.036 Uani 1 1 d . . . H55A H 0.7007 0.7180 0.9679 0.043 Uiso 1 1 calc R H . H55B H 0.6736 0.6630 0.9201 0.043 Uiso 1 1 calc R . . C56 C 0.7420(3) 0.6680(5) 0.9162(4) 0.027 Uani 1 1 d . H . H56A H 0.7603 0.7109 0.9234 0.033 Uiso 1 1 calc R . . H56B H 0.7316 0.6615 0.8723 0.033 Uiso 1 1 calc R . . C57 C 0.7315(3) 0.5537(5) 0.9616(4) 0.025 Uani 1 1 d . H . C58 C 0.7496(3) 0.4921(5) 0.9993(4) 0.033 Uani 1 1 d . . . H58A H 0.7257 0.4696 1.0149 0.049 Uiso 1 1 calc R H . H58B H 0.7729 0.5076 1.0331 0.049 Uiso 1 1 calc R . . H58C H 0.7622 0.4585 0.9748 0.049 Uiso 1 1 calc R . . C59 C 0.6982(3) 0.5286(5) 0.9060(4) 0.028 Uani 1 1 d . . . H59A H 0.6866 0.5689 0.8809 0.043 Uiso 1 1 calc R H . H59B H 0.6736 0.5043 0.9186 0.043 Uiso 1 1 calc R . . H59C H 0.7130 0.4965 0.8828 0.043 Uiso 1 1 calc R . . C60 C 0.8002(2) 0.5684(4) 0.9100(3) 0.018 Uani 1 1 d . H . H60A H 0.7826 0.5366 0.8797 0.022 Uiso 1 1 calc R . . H60B H 0.8220 0.5395 0.9378 0.022 Uiso 1 1 calc R . . C61 C 0.8852(5) 0.8937(7) 0.8741(6) 0.018 Uani 0.60 1 d P A 1 C62 C 0.8748(4) 0.9410(7) 0.8157(6) 0.022 Uani 0.60 1 d PU A 1 C63 C 0.8821(6) 1.0154(8) 0.8342(8) 0.037 Uani 0.60 1 d P A 1 H63A H 0.8552 1.0440 0.8195 0.045 Uiso 0.60 1 calc PR A 1 H63B H 0.9074 1.0359 0.8196 0.045 Uiso 0.60 1 calc PR A 1 C64 C 0.8923(6) 1.0089(8) 0.9037(7) 0.032 Uani 0.60 1 d P A 1 H64 H 0.9066 1.0512 0.9254 0.038 Uiso 0.60 1 calc PR A 1 C65 C 0.8503(6) 0.9865(8) 0.9221(8) 0.038 Uani 0.60 1 d P A 1 H65A H 0.8251 1.0170 0.9036 0.046 Uiso 0.60 1 calc PR A 1 H65B H 0.8537 0.9880 0.9664 0.046 Uiso 0.60 1 calc PR A 1 C66 C 0.8427(6) 0.9092(8) 0.8980(7) 0.029 Uani 0.60 1 d P A 1 H66A H 0.8397 0.8765 0.9307 0.035 Uiso 0.60 1 calc PR A 1 H66B H 0.8159 0.9058 0.8654 0.035 Uiso 0.60 1 calc PR A 1 C67 C 0.9211(5) 0.9418(8) 0.9150(7) 0.030 Uani 0.60 1 d P A 1 C68 C 0.9650(5) 0.9521(8) 0.8929(9) 0.039 Uani 0.60 1 d P A 1 H68A H 0.9583 0.9674 0.8508 0.058 Uiso 0.60 1 calc PR A 1 H68B H 0.9814 0.9078 0.8962 0.058 Uiso 0.60 1 calc PR A 1 H68C H 0.9832 0.9876 0.9177 0.058 Uiso 0.60 1 calc PR A 1 C69 C 0.9333(7) 0.9172(12) 0.9796(7) 0.045 Uani 0.60 1 d P A 1 H69A H 0.9061 0.9098 0.9950 0.068 Uiso 0.60 1 calc PR A 1 H69B H 0.9516 0.9528 1.0041 0.068 Uiso 0.60 1 calc PR A 1 H69C H 0.9499 0.8733 0.9817 0.068 Uiso 0.60 1 calc PR A 1 C70 C 0.8930(3) 0.8180(4) 0.8603(4) 0.029 Uani 0.60 1 d P A 1 H70A H 0.8681 0.8042 0.8273 0.034 Uiso 0.60 1 calc PR A 1 H70B H 0.8894 0.7910 0.8962 0.034 Uiso 0.60 1 calc PR A 1 C61' C 0.9069(7) 0.8924(11) 0.8943(9) 0.019 Uiso 0.40 1 d P A 2 C62' C 0.9190(7) 0.8827(12) 0.9630(10) 0.028 Uiso 0.40 1 d P A 2 C63' C 0.9084(7) 0.9506(12) 0.9897(10) 0.029 Uiso 0.40 1 d P A 2 H63C H 0.9356 0.9735 1.0126 0.034 Uiso 0.40 1 calc PR A 2 H63D H 0.8871 0.9441 1.0164 0.034 Uiso 0.40 1 calc PR A 2 C64' C 0.8867(9) 0.9948(15) 0.9303(13) 0.040 Uiso 0.40 1 d P A 2 H64' H 0.8682 1.0359 0.9369 0.048 Uiso 0.40 1 calc PR A 2 C65' C 0.9285(13) 1.012(2) 0.9054(18) 0.068 Uiso 0.40 1 d P A 2 H65C H 0.9217 1.0484 0.8740 0.082 Uiso 0.40 1 calc PR A 2 H65D H 0.9524 1.0293 0.9382 0.082 Uiso 0.40 1 calc PR A 2 C66' C 0.9428(10) 0.9484(15) 0.8799(13) 0.042 Uiso 0.40 1 d P A 2 H66C H 0.9734 0.9354 0.8999 0.051 Uiso 0.40 1 calc PR A 2 H66D H 0.9410 0.9532 0.8361 0.051 Uiso 0.40 1 calc PR A 2 C67' C 0.8621(8) 0.9358(15) 0.8925(10) 0.041 Uiso 0.40 1 d PDU A 2 C68' C 0.8271(10) 0.8940(17) 0.9145(13) 0.053 Uiso 0.40 1 d PD A 2 H68D H 0.8142 0.8597 0.8838 0.080 Uiso 0.40 1 calc PR A 2 H68E H 0.8038 0.9255 0.9222 0.080 Uiso 0.40 1 calc PR A 2 H68F H 0.8407 0.8697 0.9518 0.080 Uiso 0.40 1 calc PR A 2 C69' C 0.8396(13) 0.963(2) 0.8291(12) 0.078 Uiso 0.40 1 d PDU A 2 H69D H 0.8610 0.9900 0.8122 0.116 Uiso 0.40 1 calc PR A 2 H69E H 0.8142 0.9925 0.8324 0.116 Uiso 0.40 1 calc PR A 2 H69F H 0.8292 0.9229 0.8028 0.116 Uiso 0.40 1 calc PR A 2 C70' C 0.8930(3) 0.8180(4) 0.8603(4) 0.029 Uani 0.40 1 d P A 2 H70C H 0.8693 0.8249 0.8240 0.034 Uiso 0.40 1 calc PR A 2 H70D H 0.8823 0.7848 0.8876 0.034 Uiso 0.40 1 calc PR A 2 C71 C 1.0961(2) 0.7482(4) 0.8299(4) 0.020 Uani 1 1 d . . . C72 C 1.1115(3) 0.7576(5) 0.8972(4) 0.027 Uani 1 1 d . H . C73 C 1.1482(3) 0.8123(5) 0.9073(4) 0.036 Uani 1 1 d . . . H73A H 1.1771 0.7918 0.9274 0.043 Uiso 1 1 calc R H . H73B H 1.1410 0.8520 0.9315 0.043 Uiso 1 1 calc R . . C74 C 1.1488(3) 0.8347(5) 0.8429(4) 0.029 Uani 1 1 d . H . H74 H 1.1619 0.8820 0.8395 0.034 Uiso 1 1 calc R . . C75 C 1.1718(3) 0.7744(5) 0.8148(5) 0.040 Uani 1 1 d . . . H75A H 1.1777 0.7881 0.7751 0.048 Uiso 1 1 calc R H . H75B H 1.2001 0.7606 0.8417 0.048 Uiso 1 1 calc R . . C76 C 1.1372(3) 0.7144(5) 0.8084(5) 0.038 Uani 1 1 d . H . H76A H 1.1491 0.6741 0.8340 0.046 Uiso 1 1 calc R . . H76B H 1.1287 0.6986 0.7660 0.046 Uiso 1 1 calc R . . C77 C 1.0992(3) 0.8277(5) 0.8104(4) 0.028 Uani 1 1 d . H . C78 C 1.0676(3) 0.8743(5) 0.8348(5) 0.039 Uani 1 1 d . . . H78A H 1.0720 0.8679 0.8785 0.059 Uiso 1 1 calc R H . H78B H 1.0369 0.8620 0.8159 0.059 Uiso 1 1 calc R . . H78C H 1.0732 0.9232 0.8259 0.059 Uiso 1 1 calc R . . C79 C 1.0931(4) 0.8369(6) 0.7420(4) 0.045 Uani 1 1 d . . . H79A H 1.1141 0.8067 0.7271 0.068 Uiso 1 1 calc R H . H79B H 1.0986 0.8858 0.7329 0.068 Uiso 1 1 calc R . . H79C H 1.0627 0.8240 0.7225 0.068 Uiso 1 1 calc R . . C80 C 1.0510(2) 0.7137(4) 0.8097(3) 0.019 Uani 1 1 d . H . H80A H 1.0364 0.7344 0.7707 0.023 Uiso 1 1 calc R . . H80B H 1.0326 0.7254 0.8393 0.023 Uiso 1 1 calc R . . C81 C 1.0525(7) 0.2185(10) 0.8752(7) 0.027 Uani 0.70 1 d PU B 1 C82 C 1.0771(5) 0.1828(9) 0.8274(7) 0.035 Uani 0.70 1 d PU B 1 C83 C 1.0780(5) 0.1051(8) 0.8358(7) 0.038 Uani 0.70 1 d PU B 1 H83A H 1.1085 0.0881 0.8521 0.045 Uiso 0.70 1 calc PR B 1 H83B H 1.0658 0.0807 0.7975 0.045 Uiso 0.70 1 calc PR B 1 C84 C 1.0483(5) 0.0953(8) 0.8809(7) 0.037 Uani 0.70 1 d PD B 1 H84 H 1.0345 0.0480 0.8808 0.044 Uiso 0.70 1 calc PR B 1 C85 C 1.0759(5) 0.1199(8) 0.9431(7) 0.040 Uani 0.70 1 d PD B 1 H85A H 1.0609 0.1062 0.9759 0.047 Uiso 0.70 1 calc PR B 1 H85B H 1.1059 0.0990 0.9509 0.047 Uiso 0.70 1 calc PR B 1 C86 C 1.0787(4) 0.2010(8) 0.9389(6) 0.033 Uani 0.70 1 d PDU B 1 H86A H 1.0652 0.2237 0.9699 0.040 Uiso 0.70 1 calc PR B 1 H86B H 1.1100 0.2165 0.9443 0.040 Uiso 0.70 1 calc PR B 1 C87 C 1.0155(4) 0.1562(7) 0.8642(7) 0.030 Uani 0.70 1 d P B 1 C88 C 0.9865(5) 0.1491(7) 0.7996(8) 0.038 Uani 0.70 1 d P B 1 H88A H 0.9663 0.1892 0.7911 0.057 Uiso 0.70 1 calc PR B 1 H88B H 0.9692 0.1058 0.7967 0.057 Uiso 0.70 1 calc PR B 1 H88C H 1.0058 0.1480 0.7702 0.057 Uiso 0.70 1 calc PR B 1 C89 C 0.9839(4) 0.1669(9) 0.9085(7) 0.040 Uani 0.70 1 d P B 1 H89A H 0.9640 0.2063 0.8949 0.059 Uiso 0.70 1 calc PR B 1 H89B H 1.0015 0.1768 0.9488 0.059 Uiso 0.70 1 calc PR B 1 H89C H 0.9664 0.1244 0.9097 0.059 Uiso 0.70 1 calc PR B 1 C81' C 1.0518(12) 0.2120(18) 0.8660(12) 0.013 Uiso 0.30 1 d PU C 2 C82' C 1.0815(10) 0.1740(19) 0.8418(11) 0.027 Uiso 0.30 1 d PDU C 2 C83' C 1.0707(12) 0.101(2) 0.8575(16) 0.039 Uiso 0.30 1 d P C 2 H83C H 1.0981 0.0730 0.8711 0.047 Uiso 0.30 1 calc PR C 2 H83D H 1.0519 0.0769 0.8225 0.047 Uiso 0.30 1 calc PR C 2 C84' C 1.0458(11) 0.110(2) 0.9082(16) 0.043 Uiso 0.30 1 d PD C 2 H84' H 1.0295 0.0678 0.9188 0.051 Uiso 0.30 1 calc PR C 2 C85' C 1.0797(11) 0.1444(17) 0.9608(13) 0.035 Uiso 0.30 1 d PD C 2 H85C H 1.0670 0.1528 0.9968 0.042 Uiso 0.30 1 calc PR C 2 H85D H 1.1076 0.1172 0.9722 0.042 Uiso 0.30 1 calc PR C 2 C86' C 1.0860(11) 0.2131(15) 0.9268(14) 0.028 Uiso 0.30 1 d PDU C 2 H86C H 1.0809 0.2542 0.9509 0.034 Uiso 0.30 1 calc PR C 2 H86D H 1.1166 0.2157 0.9195 0.034 Uiso 0.30 1 calc PR C 2 C87' C 1.0153(10) 0.1765(16) 0.8802(12) 0.025 Uiso 0.30 1 d PDU C 2 C88' C 0.9917(11) 0.2048(18) 0.9281(13) 0.035 Uiso 0.30 1 d PD C 2 H88D H 0.9667 0.1744 0.9309 0.052 Uiso 0.30 1 calc PR C 2 H88E H 0.9808 0.2522 0.9171 0.052 Uiso 0.30 1 calc PR C 2 H88F H 1.0126 0.2061 0.9671 0.052 Uiso 0.30 1 calc PR C 2 C89' C 0.9801(11) 0.1673(18) 0.8212(14) 0.030 Uiso 0.30 1 d P C 2 H89D H 0.9945 0.1505 0.7892 0.045 Uiso 0.30 1 calc PR C 2 H89E H 0.9657 0.2124 0.8093 0.045 Uiso 0.30 1 calc PR C 2 H89F H 0.9577 0.1333 0.8276 0.045 Uiso 0.30 1 calc PR C 2 C90 C 1.0376(4) 0.2903(5) 0.8526(5) 0.040 Uani 0.70 1 d P B 1 H90A H 1.0076 0.2984 0.8604 0.048 Uiso 0.70 1 calc PR B 1 H90B H 1.0350 0.2909 0.8084 0.048 Uiso 0.70 1 calc PR B 1 O55 O 0.8141(3) 0.8000(4) 0.7168(3) 0.041 Uani 1 1 d . E 2 O56 O 0.7945(2) 0.7932(4) 0.4089(3) 0.043 Uani 1 1 d . F 2 O57 O 0.7635(3) 0.7890(4) 0.8027(3) 0.047 Uani 1 1 d . G 2 O58 O 1.0461(3) 0.4497(6) 0.7139(4) 0.061 Uani 1 1 d . H 2 O59 O 0.6961(3) 0.7190(7) 0.4706(4) 0.078 Uani 1 1 d . I 2 O60 O 1.1594(3) 0.4980(4) 0.8715(3) 0.044 Uani 1 1 d . J 2 O62 O 0.7425(4) 0.3583(5) 0.4979(4) 0.068 Uani 1 1 d . K 2 O63 O 0.7883(2) 0.2426(3) 0.6413(3) 0.031 Uani 1 1 d . L 2 O65 O 0.6413(7) 0.8220(12) 0.6330(10) 0.073 Uani 0.50 1 d PU M 2 O64 O 0.8945(8) 0.3296(13) 0.3091(10) 0.076 Uani 0.50 1 d PU N 2 O66 O 1.1809(7) 0.3562(12) 0.8217(9) 0.069 Uani 0.50 1 d PU O 2 C3' C 0.8776(14) 0.923(2) 0.6300(18) 0.051 Uani 0.40 1 d P D 2 H3'1 H 0.8740 0.9375 0.6706 0.062 Uiso 0.40 1 calc PR D 2 H3'2 H 0.8481 0.9190 0.6029 0.062 Uiso 0.40 1 calc PR D 2 C8 C 0.8730(7) 0.9073(9) 0.5142(11) 0.042 Uani 0.60 1 d P D 1 H8A H 0.8543 0.8870 0.5399 0.063 Uiso 0.60 1 calc PR D 1 H8B H 0.8779 0.8726 0.4845 0.063 Uiso 0.60 1 calc PR D 1 H8C H 0.8582 0.9484 0.4934 0.063 Uiso 0.60 1 calc PR D 1 C90' C 1.0376(4) 0.2903(5) 0.8526(5) 0.040 Uani 0.30 1 d P C 2 H90C H 1.0089 0.2966 0.8650 0.048 Uiso 0.30 1 calc PR C 2 H90D H 1.0316 0.2962 0.8083 0.048 Uiso 0.30 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.016 0.012 0.015 0.002 0.006 0.000 Bi2 0.016 0.013 0.020 0.002 0.005 0.001 Bi3 0.015 0.011 0.019 0.000 0.006 0.000 Bi4 0.016 0.014 0.014 0.002 0.005 0.002 Bi5 0.015 0.014 0.017 0.001 0.006 -0.001 Bi6 0.017 0.013 0.016 0.000 0.005 -0.002 Bi7 0.012 0.014 0.013 0.000 0.003 -0.002 Bi8 0.018 0.015 0.016 0.000 0.001 0.000 Bi9 0.012 0.017 0.016 0.001 0.003 -0.001 Bi10 0.014 0.012 0.016 0.000 0.002 0.000 S1 0.018 0.015 0.017 0.001 0.006 -0.001 S2 0.030 0.013 0.027 0.003 0.018 0.001 S3 0.023 0.029 0.026 0.002 0.003 -0.008 S4 0.018 0.019 0.024 -0.001 0.008 -0.004 S5 0.010 0.013 0.015 -0.001 0.002 -0.001 S6 0.013 0.019 0.021 0.000 0.007 0.003 S7 0.033 0.017 0.019 0.000 0.007 0.000 S8 0.015 0.024 0.016 0.000 0.005 -0.005 S9 0.034 0.033 0.064 -0.028 0.021 -0.001 O1 0.018 0.012 0.018 0.000 0.004 0.002 O2 0.017 0.012 0.020 -0.001 0.002 -0.001 O3 0.020 0.010 0.017 0.008 0.006 0.001 O4 0.012 0.011 0.016 0.004 0.004 0.002 O5 0.014 0.005 0.017 0.003 0.009 0.000 O6 0.012 0.020 0.018 0.004 0.008 -0.004 O7 0.019 0.010 0.020 0.003 0.006 -0.004 O8 0.014 0.010 0.024 0.002 0.010 0.002 O9 0.030 0.042 0.022 0.000 0.009 0.012 O10 0.034 0.024 0.032 0.010 0.009 0.004 O11 0.104 0.091 0.090 0.000 0.007 0.010 O12 0.021 0.026 0.022 0.004 0.008 -0.004 O13 0.021 0.013 0.013 0.000 0.006 0.005 O14 0.015 0.012 0.013 -0.001 0.004 -0.004 O15 0.014 0.015 0.015 0.002 0.004 0.000 O16 0.014 0.020 0.014 -0.004 0.007 -0.004 O17 0.021 0.021 0.027 -0.003 0.006 -0.001 O18 0.022 0.018 0.024 -0.002 0.012 -0.001 O19 0.025 0.017 0.011 0.003 0.009 0.003 O20 0.020 0.022 0.026 0.000 0.007 -0.003 O21 0.043 0.019 0.046 0.012 0.027 0.006 O22 0.026 0.019 0.028 -0.002 0.017 -0.003 O23 0.034 0.013 0.034 0.002 0.022 -0.005 O24 0.040 0.022 0.030 -0.001 0.019 -0.001 O25 0.031 0.015 0.028 0.006 0.016 0.001 O26 0.045 0.032 0.025 0.012 0.001 -0.004 O27 0.029 0.033 0.029 -0.003 0.006 0.000 O28 0.029 0.073 0.034 0.004 0.007 -0.018 O29 0.020 0.027 0.024 0.000 0.002 -0.004 O30 0.028 0.016 0.026 0.001 0.013 0.003 O31 0.026 0.021 0.021 -0.002 0.005 -0.007 O32 0.023 0.031 0.036 -0.007 0.010 -0.017 O33 0.031 0.027 0.034 0.000 -0.002 0.000 O34 0.017 0.013 0.019 -0.001 0.005 -0.006 O35 0.014 0.018 0.020 0.008 0.005 -0.003 O36 0.016 0.020 0.021 0.000 0.011 -0.001 O37 0.022 0.022 0.016 0.006 0.004 -0.004 O38 0.022 0.018 0.025 0.000 0.011 0.007 O39 0.021 0.021 0.030 -0.003 0.008 -0.001 O40 0.022 0.032 0.023 0.004 0.006 0.011 O41 0.020 0.047 0.029 -0.006 0.006 0.002 O42 0.041 0.018 0.027 0.000 0.009 -0.001 O43 0.037 0.025 0.021 0.002 0.012 0.006 O44 0.054 0.021 0.018 0.004 0.007 -0.003 O45 0.029 0.023 0.029 0.001 -0.003 0.008 O46 0.017 0.026 0.021 0.003 0.004 -0.009 O47 0.014 0.023 0.021 0.001 0.003 -0.001 O48 0.023 0.039 0.020 -0.007 0.013 -0.007 O49 0.031 0.037 0.036 0.008 -0.005 -0.007 O50 0.082 0.025 0.054 -0.018 0.049 -0.012 O51 0.032 0.030 0.051 -0.022 0.009 0.006 O52 0.034 0.094 0.120 -0.084 0.030 -0.015 O53 0.063 0.037 0.085 -0.012 0.056 0.004 C1 0.033 0.014 0.029 0.004 0.011 0.004 C2 0.042 0.019 0.049 0.002 0.027 0.007 C3 0.066 0.020 0.084 0.004 0.051 0.012 C4 0.048 0.035 0.061 0.005 0.019 0.004 C5 0.079 0.014 0.060 -0.004 0.036 0.002 C6 0.046 0.013 0.040 0.004 0.007 0.005 C7 0.030 0.019 0.043 0.016 0.010 0.002 C8' 0.028 0.015 0.073 0.006 -0.012 0.003 C9 0.044 0.023 0.062 0.026 0.009 -0.003 C10 0.023 0.017 0.027 0.015 0.012 0.004 C11 0.027 0.020 0.021 0.003 0.016 0.004 C12 0.031 0.017 0.023 0.004 0.011 0.002 C13 0.037 0.017 0.042 0.008 0.022 0.003 C14 0.052 0.011 0.031 0.005 0.018 -0.001 C15 0.070 0.015 0.044 -0.002 0.025 -0.008 C16 0.050 0.016 0.028 -0.001 0.019 -0.003 C17 0.035 0.021 0.030 0.008 0.017 0.005 C18 0.043 0.042 0.034 -0.001 0.011 0.006 C19 0.044 0.032 0.044 0.014 0.022 0.022 C20 0.020 0.033 0.030 0.006 0.011 0.006 C21 0.018 0.022 0.029 0.006 0.004 -0.004 C22 0.025 0.016 0.023 0.005 0.001 0.000 C23 0.040 0.047 0.017 0.000 0.004 -0.001 C24 0.040 0.043 0.020 -0.012 -0.002 0.001 C25 0.035 0.034 0.051 -0.003 -0.005 0.001 C26 0.036 0.026 0.040 0.006 -0.002 0.003 C27 0.026 0.033 0.023 0.010 -0.002 -0.002 C28 0.035 0.043 0.035 0.009 0.009 -0.008 C29 0.022 0.039 0.046 0.016 -0.013 -0.003 C30 0.025 0.020 0.033 0.011 0.009 0.008 C31 0.021 0.037 0.023 -0.007 0.004 0.000 C32 0.022 0.031 0.024 0.000 0.004 0.006 C33 0.032 0.045 0.031 -0.007 0.003 0.013 C34 0.032 0.034 0.034 -0.011 0.007 0.009 C35 0.037 0.070 0.030 0.011 0.013 0.020 C36 0.033 0.044 0.019 0.003 0.006 0.004 C37 0.024 0.049 0.027 0.004 0.008 0.001 C38 0.051 0.046 0.028 0.007 0.013 0.017 C39 0.025 0.070 0.038 -0.009 0.019 -0.004 C40 0.022 0.024 0.022 -0.002 0.005 0.007 C41 0.016 0.014 0.024 -0.002 0.007 -0.001 C42 0.019 0.012 0.021 -0.002 0.006 -0.002 C43 0.026 0.016 0.026 -0.004 0.005 -0.007 C44 0.018 0.011 0.030 -0.002 0.008 -0.007 C45 0.035 0.016 0.039 0.003 0.020 0.000 C46 0.019 0.017 0.029 0.001 0.005 -0.004 C47 0.015 0.014 0.021 0.003 0.007 -0.004 C48 0.017 0.018 0.029 0.001 0.005 -0.003 C49 0.023 0.031 0.027 0.002 0.009 0.001 C50 0.018 0.013 0.020 0.005 0.011 -0.002 C51 0.017 0.013 0.024 -0.004 0.003 0.002 C52 0.022 0.031 0.033 -0.015 0.012 -0.001 C53 0.034 0.055 0.032 -0.012 0.010 -0.005 C54 0.023 0.050 0.031 -0.008 0.012 0.001 C55 0.027 0.040 0.041 -0.018 0.009 0.012 C56 0.024 0.023 0.038 0.001 0.014 0.008 C57 0.022 0.028 0.026 -0.008 0.010 -0.008 C58 0.033 0.031 0.041 0.003 0.024 -0.005 C59 0.020 0.027 0.039 -0.011 0.008 -0.008 C60 0.017 0.014 0.025 0.005 0.010 -0.001 C61 0.022 0.018 0.016 0.003 0.008 0.008 C62 0.009 0.025 0.026 -0.005 -0.007 0.000 C63 0.034 0.020 0.051 0.014 -0.006 0.000 C64 0.046 0.018 0.030 -0.014 0.007 -0.004 C65 0.045 0.020 0.050 -0.020 0.011 0.000 C66 0.037 0.022 0.036 0.003 0.021 0.000 C67 0.030 0.026 0.033 -0.005 0.005 0.003 C68 0.017 0.021 0.067 -0.001 -0.019 -0.004 C69 0.050 0.059 0.025 -0.011 0.005 0.016 C70 0.040 0.014 0.029 -0.001 0.003 0.003 C70' 0.040 0.014 0.029 -0.001 0.003 0.003 C71 0.013 0.018 0.026 0.001 -0.001 0.002 C72 0.014 0.032 0.036 0.008 0.005 -0.008 C73 0.027 0.033 0.042 0.002 -0.005 -0.012 C74 0.021 0.022 0.042 0.001 0.005 -0.006 C75 0.022 0.030 0.073 -0.009 0.025 -0.011 C76 0.018 0.032 0.068 -0.002 0.013 0.000 C77 0.018 0.030 0.034 0.009 0.001 -0.004 C78 0.024 0.025 0.064 0.005 0.000 0.002 C79 0.061 0.042 0.030 0.011 0.003 -0.025 C80 0.016 0.026 0.017 0.002 0.006 -0.005 C81 0.026 0.023 0.035 -0.007 0.013 0.006 C82 0.040 0.024 0.038 -0.003 0.004 -0.003 C83 0.035 0.029 0.050 -0.003 0.009 0.013 C84 0.036 0.029 0.042 0.010 -0.001 -0.001 C85 0.036 0.024 0.050 0.010 -0.010 0.001 C86 0.017 0.048 0.035 0.014 0.008 0.008 C87 0.024 0.016 0.048 0.012 0.001 -0.003 C88 0.029 0.021 0.059 0.023 -0.002 -0.006 C89 0.014 0.060 0.049 0.022 0.015 0.008 C90 0.040 0.030 0.048 -0.021 0.005 0.005 O55 0.057 0.022 0.048 -0.002 0.021 0.018 O56 0.032 0.049 0.046 0.019 0.003 0.000 O57 0.068 0.036 0.044 0.010 0.027 0.004 O58 0.042 0.096 0.050 0.014 0.019 0.012 O59 0.054 0.136 0.048 0.018 0.019 0.049 O60 0.051 0.041 0.047 0.003 0.026 0.009 O62 0.123 0.047 0.040 -0.011 0.031 -0.046 O63 0.034 0.029 0.029 -0.006 0.000 -0.006 O65 0.072 0.070 0.074 0.000 0.005 0.004 O64 0.076 0.076 0.078 0.002 0.020 0.006 O66 0.065 0.075 0.074 0.012 0.029 -0.003 C3' 0.066 0.020 0.084 0.004 0.051 0.012 C8 0.028 0.015 0.073 0.006 -0.012 0.003 C90' 0.040 0.030 0.048 -0.021 0.005 0.005 _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 O4 2.197(5) . ? Bi1 O2 2.225(5) . ? Bi1 O3 2.299(5) . ? Bi1 O1 2.486(5) . ? Bi1 O18 2.639(6) . ? Bi1 O9 2.659(6) . ? Bi1 O23 2.707(6) . ? Bi1 O12 2.831(5) . ? Bi2 O2 2.133(5) . ? Bi2 O7 2.162(5) . ? Bi2 O1 2.316(5) . ? Bi2 O8 2.549(5) . ? Bi2 O10 2.586(6) . ? Bi2 O27 2.654(6) . ? Bi2 O11 2.928(14) . ? Bi3 O4 2.176(5) . ? Bi3 O7 2.178(5) . ? Bi3 O1 2.380(5) . ? Bi3 O6 2.464(5) . ? Bi3 O22 2.639(5) . ? Bi3 O25 2.663(6) . ? Bi3 O30 2.676(6) . ? Bi3 O26 2.754(6) . ? Bi4 O5 2.091(5) . ? Bi4 O4 2.141(5) . ? Bi4 O6 2.278(5) . ? Bi4 O3 2.422(5) . ? Bi4 O34 2.642(5) . ? Bi4 O46 3.096(5) . ? Bi4 O36 3.224(5) . ? Bi4 O58 3.226(8) . ? Bi5 O7 2.127(5) . ? Bi5 O5 2.199(4) . ? Bi5 O8 2.291(5) . ? Bi5 O6 2.482(5) . ? Bi5 O31 2.600(6) . ? Bi5 O33 2.699(6) . ? Bi5 O38 2.960(5) . ? Bi5 O40 2.981(6) . ? Bi6 O2 2.144(5) . ? Bi6 O5 2.209(5) . ? Bi6 O8 2.354(5) . ? Bi6 O3 2.421(5) . ? Bi6 O19 2.587(5) . ? Bi6 O21 2.644(6) . ? Bi6 O43 2.819(6) . ? Bi6 O46 3.214(5) . ? Bi6 O44 3.286(6) . ? Bi7 O15 2.170(5) . ? Bi7 O14 2.170(5) . ? Bi7 O13 2.341(5) . ? Bi7 O16 2.521(5) . ? Bi7 O34 2.594(5) . ? Bi7 O43 2.695(6) . ? Bi7 O38 2.698(5) . ? Bi7 O46 2.713(5) . ? Bi8 O14 2.137(5) . ? Bi8 O14 2.137(5) 2_757 ? Bi8 O13 2.367(5) . ? Bi8 O13 2.367(5) 2_757 ? Bi8 O42 2.695(6) . ? Bi8 O42 2.695(6) 2_757 ? Bi8 O45' 2.868(17) 2_757 ? Bi8 O45' 2.868(17) . ? Bi9 O14 2.152(5) . ? Bi9 O15 2.185(5) 2_757 ? Bi9 O16 2.302(5) . ? Bi9 O13 2.415(5) 2_757 ? Bi9 O47 2.610(5) . ? Bi9 O17 2.672(6) . ? Bi9 O49 2.869(7) . ? Bi9 O41 2.999(6) 2_757 ? Bi10 O15 2.160(5) 2_757 ? Bi10 O15 2.160(5) . ? Bi10 O16 2.367(5) 2_757 ? Bi10 O16 2.367(5) . ? Bi10 O35 2.735(5) . ? Bi10 O35 2.735(5) 2_757 ? Bi10 O51 3.078(6) 2_757 ? Bi10 O51 3.078(6) . ? S1 O20 1.447(6) . ? S1 O19 1.457(5) . ? S1 O18 1.468(6) . ? S1 C10 1.772(8) . ? S2 O24 1.448(6) . ? S2 O22 1.468(6) . ? S2 O23 1.482(6) . ? S2 C20 1.775(9) . ? S3 O26 1.451(7) . ? S3 O28 1.456(7) . ? S3 O27 1.485(7) . ? S3 C30 1.782(8) . ? S4 O32 1.459(6) . ? S4 O30 1.464(6) . ? S4 O31 1.466(6) . ? S4 C40 1.782(8) . ? S5 O36 1.448(5) . ? S5 O35 1.466(5) . ? S5 O34 1.483(5) . ? S5 C50 1.782(7) . ? S6 O39 1.449(6) . ? S6 O40 1.462(6) . ? S6 O38 1.477(5) . ? S6 C60 1.793(7) . ? S7 O44 1.446(6) . ? S7 O42 1.459(7) . ? S7 O43 1.488(7) . ? S7 C70 1.781(10) . ? S8 O48 1.444(5) . ? S8 O47 1.461(5) . ? S8 O46 1.482(5) . ? S8 C80 1.768(9) . ? S9 O52 1.459(9) . ? S9 O51 1.478(8) . ? S9 O50 1.511(9) . ? S9 C90 1.763(10) . ? O13 Bi9 2.415(5) 2_757 ? O15 Bi9 2.185(5) 2_757 ? O21 C2 1.223(11) . ? O25 C12 1.204(10) . ? O29 C22 1.200(10) . ? O33 C32 1.206(11) . ? O37 C42 1.223(9) . ? O41 C52 1.202(11) . ? O45 C62 1.205(16) . ? O45' C62' 1.21(3) . ? O49 C72 1.220(11) . ? O53 C82 1.272(19) . ? O53' C82' 1.281(10) . ? C1 C2 1.524(12) . ? C1 C10 1.536(11) . ? C1 C7 1.575(11) . ? C1 C6 1.576(13) . ? C2 C3' 1.51(4) . ? C2 C3 1.53(3) . ? C3 C4 1.54(3) . ? C4 C5 1.519(18) . ? C4 C3' 1.55(4) . ? C4 C7 1.555(15) . ? C5 C6 1.576(13) . ? C7 C8 1.47(2) . ? C7 C9 1.537(13) . ? C7 C8' 1.68(3) . ? C11 C20 1.520(12) . ? C11 C12 1.534(10) . ? C11 C17 1.552(12) . ? C11 C16 1.556(12) . ? C12 C13 1.512(11) . ? C13 C14 1.524(12) . ? C14 C17 1.545(12) . ? C14 C15 1.551(14) . ? C15 C16 1.565(12) . ? C17 C18 1.523(13) . ? C17 C19 1.563(12) . ? C21 C30 1.497(12) . ? C21 C22 1.525(11) . ? C21 C26 1.561(12) . ? C21 C27 1.610(11) . ? C22 C23 1.534(12) . ? C23 C24 1.561(13) . ? C24 C25 1.549(15) . ? C24 C27 1.560(14) . ? C25 C26 1.521(15) . ? C27 C28 1.516(13) . ? C27 C29 1.529(11) . ? C31 C40 1.505(11) . ? C31 C32 1.528(12) . ? C31 C37 1.575(11) . ? C31 C36 1.609(12) . ? C32 C33 1.517(12) . ? C33 C34 1.508(14) . ? C34 C35 1.562(13) . ? C34 C37 1.573(14) . ? C35 C36 1.537(13) . ? C37 C39 1.505(14) . ? C37 C38 1.520(12) . ? C41 C42 1.506(10) . ? C41 C50 1.533(10) . ? C41 C46 1.554(11) . ? C41 C47 1.584(9) . ? C42 C43 1.512(10) . ? C43 C44 1.523(11) . ? C44 C45 1.496(12) . ? C44 C47 1.558(10) . ? C45 C46 1.579(11) . ? C47 C49 1.532(11) . ? C47 C48 1.541(10) . ? C51 C60 1.516(10) . ? C51 C52 1.543(11) . ? C51 C56 1.579(11) . ? C51 C57 1.585(11) . ? C52 C53 1.520(12) . ? C53 C54 1.526(13) . ? C54 C55 1.543(15) . ? C54 C57 1.548(12) . ? C55 C56 1.560(12) . ? C57 C58 1.495(13) . ? C57 C59 1.531(11) . ? C61 C70 1.510(15) . ? C61 C66 1.547(19) . ? C61 C62 1.582(18) . ? C61 C67 1.58(2) . ? C62 C63 1.49(2) . ? C63 C64 1.55(2) . ? C64 C65 1.50(2) . ? C64 C67 1.55(2) . ? C65 C66 1.58(2) . ? C67 C69 1.51(2) . ? C67 C68 1.55(2) . ? C61' C62' 1.54(3) . ? C61' C67' 1.60(3) . ? C61' C66' 1.62(3) . ? C62' C63' 1.50(3) . ? C63' C64' 1.62(3) . ? C64' C67' 1.52(4) . ? C64' C65' 1.54(5) . ? C65' C66' 1.45(5) . ? C67' C68' 1.507(18) . ? C67' C69' 1.551(10) . ? C71 C72 1.513(11) . ? C71 C80 1.519(10) . ? C71 C76 1.586(12) . ? C71 C77 1.592(12) . ? C72 C73 1.522(11) . ? C73 C74 1.527(13) . ? C74 C75 1.558(13) . ? C74 C77 1.558(11) . ? C75 C76 1.551(13) . ? C77 C78 1.506(14) . ? C77 C79 1.535(13) . ? C81 C90 1.50(2) . ? C81 C86 1.54(2) . ? C81 C82 1.60(2) . ? C81 C87 1.63(2) . ? C82 C83 1.50(2) . ? C83 C84 1.52(2) . ? C84 C87 1.537(19) . ? C84 C85 1.56(2) . ? C85 C86 1.56(2) . ? C87 C89 1.55(2) . ? C87 C88 1.56(2) . ? C81' C82' 1.37(5) . ? C81' C87' 1.41(5) . ? C81' C86' 1.55(4) . ? C82' C83' 1.50(5) . ? C83' C84' 1.52(5) . ? C84' C85' 1.56(2) . ? C84' C87' 1.63(5) . ? C85' C86' 1.56(2) . ? C87' C88' 1.529(19) . ? C87' C89' 1.55(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Bi1 O2 89.91(19) . . ? O4 Bi1 O3 72.16(18) . . ? O2 Bi1 O3 71.53(18) . . ? O4 Bi1 O1 69.80(17) . . ? O2 Bi1 O1 67.35(17) . . ? O3 Bi1 O1 122.76(16) . . ? O4 Bi1 O18 150.92(17) . . ? O2 Bi1 O18 80.40(17) . . ? O3 Bi1 O18 78.76(17) . . ? O1 Bi1 O18 128.87(17) . . ? O4 Bi1 O9 88.87(19) . . ? O2 Bi1 O9 140.25(18) . . ? O3 Bi1 O9 70.33(18) . . ? O1 Bi1 O9 146.7(2) . . ? O18 Bi1 O9 81.7(2) . . ? O4 Bi1 O23 78.59(17) . . ? O2 Bi1 O23 146.05(18) . . ? O3 Bi1 O23 132.09(18) . . ? O1 Bi1 O23 78.71(17) . . ? O18 Bi1 O23 123.39(16) . . ? O9 Bi1 O23 72.0(2) . . ? O4 Bi1 O12 137.65(17) . . ? O2 Bi1 O12 91.93(18) . . ? O3 Bi1 O12 147.23(18) . . ? O1 Bi1 O12 72.04(16) . . ? O18 Bi1 O12 70.51(17) . . ? O9 Bi1 O12 114.80(17) . . ? O23 Bi1 O12 76.59(17) . . ? O2 Bi2 O7 91.4(2) . . ? O2 Bi2 O1 72.07(19) . . ? O7 Bi2 O1 72.29(18) . . ? O2 Bi2 O8 70.74(18) . . ? O7 Bi2 O8 69.49(17) . . ? O1 Bi2 O8 124.86(17) . . ? O2 Bi2 O10 84.9(2) . . ? O7 Bi2 O10 147.9(2) . . ? O1 Bi2 O10 76.25(19) . . ? O8 Bi2 O10 137.24(19) . . ? O2 Bi2 O27 155.13(19) . . ? O7 Bi2 O27 81.38(19) . . ? O1 Bi2 O27 83.06(18) . . ? O8 Bi2 O27 127.12(17) . . ? O10 Bi2 O27 88.7(2) . . ? O2 Bi2 O11 121.9(3) . . ? O7 Bi2 O11 116.6(3) . . ? O1 Bi2 O11 161.3(3) . . ? O8 Bi2 O11 73.6(3) . . ? O10 Bi2 O11 91.9(3) . . ? O27 Bi2 O11 82.2(3) . . ? O4 Bi3 O7 90.91(19) . . ? O4 Bi3 O1 72.22(17) . . ? O7 Bi3 O1 70.77(17) . . ? O4 Bi3 O6 68.64(17) . . ? O7 Bi3 O6 70.71(18) . . ? O1 Bi3 O6 123.43(17) . . ? O4 Bi3 O22 84.48(18) . . ? O7 Bi3 O22 150.41(18) . . ? O1 Bi3 O22 80.02(17) . . ? O6 Bi3 O22 132.81(18) . . ? O4 Bi3 O25 81.42(18) . . ? O7 Bi3 O25 139.93(18) . . ? O1 Bi3 O25 140.38(17) . . ? O6 Bi3 O25 69.87(18) . . ? O22 Bi3 O25 68.25(17) . . ? O4 Bi3 O30 142.13(17) . . ? O7 Bi3 O30 81.91(17) . . ? O1 Bi3 O30 137.18(17) . . ? O6 Bi3 O30 73.92(17) . . ? O22 Bi3 O30 118.66(17) . . ? O25 Bi3 O30 80.68(17) . . ? O4 Bi3 O26 137.90(19) . . ? O7 Bi3 O26 86.1(2) . . ? O1 Bi3 O26 67.17(18) . . ? O6 Bi3 O26 146.27(19) . . ? O22 Bi3 O26 78.2(2) . . ? O25 Bi3 O26 125.0(2) . . ? O30 Bi3 O26 78.94(19) . . ? O5 Bi4 O4 94.37(18) . . ? O5 Bi4 O6 73.81(19) . . ? O4 Bi4 O6 72.88(18) . . ? O5 Bi4 O3 72.59(17) . . ? O4 Bi4 O3 70.66(17) . . ? O6 Bi4 O3 127.39(18) . . ? O5 Bi4 O34 77.43(17) . . ? O4 Bi4 O34 152.56(17) . . ? O6 Bi4 O34 79.68(16) . . ? O3 Bi4 O34 129.11(16) . . ? O5 Bi4 O46 66.84(17) . . ? O4 Bi4 O46 130.18(16) . . ? O6 Bi4 O46 134.72(17) . . ? O3 Bi4 O46 59.85(15) . . ? O34 Bi4 O46 70.87(14) . . ? O5 Bi4 O36 116.86(15) . . ? O4 Bi4 O36 119.66(16) . . ? O6 Bi4 O36 69.14(16) . . ? O3 Bi4 O36 163.47(15) . . ? O34 Bi4 O36 47.34(14) . . ? O46 Bi4 O36 109.81(14) . . ? O5 Bi4 O58 138.2(2) . . ? O4 Bi4 O58 96.9(2) . . ? O6 Bi4 O58 147.9(2) . . ? O3 Bi4 O58 73.5(2) . . ? O34 Bi4 O58 106.68(19) . . ? O46 Bi4 O58 75.2(2) . . ? O36 Bi4 O58 91.7(2) . . ? O7 Bi5 O5 91.10(18) . . ? O7 Bi5 O8 75.36(19) . . ? O5 Bi5 O8 71.40(17) . . ? O7 Bi5 O6 71.12(18) . . ? O5 Bi5 O6 67.98(17) . . ? O8 Bi5 O6 125.76(16) . . ? O7 Bi5 O31 87.46(18) . . ? O5 Bi5 O31 141.75(18) . . ? O8 Bi5 O31 143.78(18) . . ? O6 Bi5 O31 75.47(17) . . ? O7 Bi5 O33 76.4(2) . . ? O5 Bi5 O33 144.78(18) . . ? O8 Bi5 O33 73.59(19) . . ? O6 Bi5 O33 134.09(18) . . ? O31 Bi5 O33 71.46(19) . . ? O7 Bi5 O38 170.59(17) . . ? O5 Bi5 O38 79.73(15) . . ? O8 Bi5 O38 103.36(17) . . ? O6 Bi5 O38 103.11(15) . . ? O31 Bi5 O38 98.40(16) . . ? O33 Bi5 O38 112.37(17) . . ? O7 Bi5 O40 140.21(18) . . ? O5 Bi5 O40 116.42(17) . . ? O8 Bi5 O40 86.40(17) . . ? O6 Bi5 O40 144.04(16) . . ? O31 Bi5 O40 87.05(18) . . ? O33 Bi5 O40 64.49(17) . . ? O38 Bi5 O40 48.05(14) . . ? O2 Bi6 O5 91.50(19) . . ? O2 Bi6 O8 74.60(19) . . ? O5 Bi6 O8 70.05(17) . . ? O2 Bi6 O3 70.50(18) . . ? O5 Bi6 O3 70.71(16) . . ? O8 Bi6 O3 125.72(18) . . ? O2 Bi6 O19 85.39(18) . . ? O5 Bi6 O19 144.88(16) . . ? O8 Bi6 O19 141.02(17) . . ? O3 Bi6 O19 75.32(16) . . ? O2 Bi6 O21 75.0(2) . . ? O5 Bi6 O21 138.25(19) . . ? O8 Bi6 O21 68.30(19) . . ? O3 Bi6 O21 135.35(17) . . ? O19 Bi6 O21 74.43(18) . . ? O2 Bi6 O43 157.86(19) . . ? O5 Bi6 O43 77.20(17) . . ? O8 Bi6 O43 83.60(18) . . ? O3 Bi6 O43 121.65(16) . . ? O19 Bi6 O43 114.79(17) . . ? O21 Bi6 O43 100.68(19) . . ? O2 Bi6 O46 127.32(17) . . ? O5 Bi6 O46 63.47(15) . . ? O8 Bi6 O46 127.71(15) . . ? O3 Bi6 O46 57.88(15) . . ? O19 Bi6 O46 91.03(14) . . ? O21 Bi6 O46 152.96(19) . . ? O43 Bi6 O46 64.41(16) . . ? O2 Bi6 O44 139.58(17) . . ? O5 Bi6 O44 123.35(15) . . ? O8 Bi6 O44 97.04(18) . . ? O3 Bi6 O44 136.01(18) . . ? O19 Bi6 O44 76.89(16) . . ? O21 Bi6 O44 65.34(19) . . ? O43 Bi6 O44 46.21(16) . . ? O46 Bi6 O44 89.47(15) . . ? O15 Bi7 O14 90.76(19) . . ? O15 Bi7 O13 72.88(18) . . ? O14 Bi7 O13 70.72(18) . . ? O15 Bi7 O16 69.25(17) . . ? O14 Bi7 O16 68.12(18) . . ? O13 Bi7 O16 122.40(17) . . ? O15 Bi7 O34 83.35(17) . . ? O14 Bi7 O34 138.87(17) . . ? O13 Bi7 O34 142.98(17) . . ? O16 Bi7 O34 71.78(16) . . ? O15 Bi7 O43 144.72(18) . . ? O14 Bi7 O43 89.78(19) . . ? O13 Bi7 O43 74.07(17) . . ? O16 Bi7 O43 141.81(17) . . ? O34 Bi7 O43 117.65(16) . . ? O15 Bi7 O38 84.96(17) . . ? O14 Bi7 O38 146.19(17) . . ? O13 Bi7 O38 75.99(17) . . ? O16 Bi7 O38 138.90(17) . . ? O34 Bi7 O38 73.97(17) . . ? O43 Bi7 O38 75.39(19) . . ? O15 Bi7 O46 141.41(18) . . ? O14 Bi7 O46 81.72(16) . . ? O13 Bi7 O46 136.96(18) . . ? O16 Bi7 O46 72.86(16) . . ? O34 Bi7 O46 78.19(16) . . ? O43 Bi7 O46 73.42(17) . . ? O38 Bi7 O46 121.02(15) . . ? O14 Bi8 O14 90.8(3) . 2_757 ? O14 Bi8 O13 70.77(18) . . ? O14 Bi8 O13 72.20(18) 2_757 . ? O14 Bi8 O13 72.20(18) . 2_757 ? O14 Bi8 O13 70.77(17) 2_757 2_757 ? O13 Bi8 O13 126.2(2) . 2_757 ? O14 Bi8 O42 77.98(18) . . ? O14 Bi8 O42 150.06(19) 2_757 . ? O13 Bi8 O42 77.89(18) . . ? O13 Bi8 O42 129.35(18) 2_757 . ? O14 Bi8 O42 150.06(19) . 2_757 ? O14 Bi8 O42 77.98(18) 2_757 2_757 ? O13 Bi8 O42 129.35(18) . 2_757 ? O13 Bi8 O42 77.89(18) 2_757 2_757 ? O42 Bi8 O42 124.1(3) . 2_757 ? O14 Bi8 O45' 108.0(4) . 2_757 ? O14 Bi8 O45' 133.9(3) 2_757 2_757 ? O13 Bi8 O45' 153.4(3) . 2_757 ? O13 Bi8 O45' 75.6(4) 2_757 2_757 ? O42 Bi8 O45' 76.0(3) . 2_757 ? O42 Bi8 O45' 64.7(3) 2_757 2_757 ? O14 Bi8 O45' 133.9(3) . . ? O14 Bi8 O45' 108.0(4) 2_757 . ? O13 Bi8 O45' 75.6(4) . . ? O13 Bi8 O45' 153.4(3) 2_757 . ? O42 Bi8 O45' 64.7(3) . . ? O42 Bi8 O45' 76.0(3) 2_757 . ? O45' Bi8 O45' 88.9(7) 2_757 . ? O14 Bi9 O15 92.65(19) . 2_757 ? O14 Bi9 O16 72.71(19) . . ? O15 Bi9 O16 72.08(18) 2_757 . ? O14 Bi9 O13 70.97(18) . 2_757 ? O15 Bi9 O13 71.17(18) 2_757 2_757 ? O16 Bi9 O13 126.01(18) . 2_757 ? O14 Bi9 O47 88.63(17) . . ? O15 Bi9 O47 146.11(18) 2_757 . ? O16 Bi9 O47 76.04(17) . . ? O13 Bi9 O47 139.90(18) 2_757 . ? O14 Bi9 O17 157.67(18) . . ? O15 Bi9 O17 78.94(18) 2_757 . ? O16 Bi9 O17 85.00(18) . . ? O13 Bi9 O17 124.02(17) 2_757 . ? O47 Bi9 O17 87.21(17) . . ? O14 Bi9 O49 72.16(19) . . ? O15 Bi9 O49 140.1(2) 2_757 . ? O16 Bi9 O49 132.38(18) . . ? O13 Bi9 O49 69.00(19) 2_757 . ? O47 Bi9 O49 72.0(2) . . ? O17 Bi9 O49 126.81(19) . . ? O15 Bi10 O15 94.7(3) 2_757 . ? O15 Bi10 O16 72.47(18) 2_757 2_757 ? O15 Bi10 O16 71.24(18) . 2_757 ? O15 Bi10 O16 71.24(18) 2_757 . ? O15 Bi10 O16 72.47(18) . . ? O16 Bi10 O16 125.3(3) 2_757 . ? O15 Bi10 O35 147.74(16) 2_757 . ? O15 Bi10 O35 82.42(17) . . ? O16 Bi10 O35 134.72(16) 2_757 . ? O16 Bi10 O35 77.34(16) . . ? O15 Bi10 O35 82.42(17) 2_757 2_757 ? O15 Bi10 O35 147.74(16) . 2_757 ? O16 Bi10 O35 77.34(16) 2_757 2_757 ? O16 Bi10 O35 134.72(16) . 2_757 ? O35 Bi10 O35 116.4(2) . 2_757 ? O15 Bi10 O51 135.13(19) 2_757 2_757 ? O15 Bi10 O51 90.54(18) . 2_757 ? O16 Bi10 O51 67.3(2) 2_757 2_757 ? O16 Bi10 O51 150.91(18) . 2_757 ? O35 Bi10 O51 77.12(18) . 2_757 ? O35 Bi10 O51 70.39(17) 2_757 2_757 ? O15 Bi10 O51 90.54(18) 2_757 . ? O15 Bi10 O51 135.13(19) . . ? O16 Bi10 O51 150.91(18) 2_757 . ? O16 Bi10 O51 67.3(2) . . ? O35 Bi10 O51 70.39(17) . . ? O35 Bi10 O51 77.12(18) 2_757 . ? O51 Bi10 O51 116.0(3) 2_757 . ? O20 S1 O19 114.3(3) . . ? O20 S1 O18 112.7(3) . . ? O19 S1 O18 109.8(3) . . ? O20 S1 C10 107.8(4) . . ? O19 S1 C10 106.5(3) . . ? O18 S1 C10 105.1(4) . . ? O24 S2 O22 113.8(4) . . ? O24 S2 O23 111.8(3) . . ? O22 S2 O23 111.8(3) . . ? O24 S2 C20 107.0(4) . . ? O22 S2 C20 106.9(4) . . ? O23 S2 C20 104.9(4) . . ? O26 S3 O28 113.8(5) . . ? O26 S3 O27 110.8(4) . . ? O28 S3 O27 113.2(4) . . ? O26 S3 C30 107.5(4) . . ? O28 S3 C30 107.9(4) . . ? O27 S3 C30 102.8(4) . . ? O32 S4 O30 112.6(4) . . ? O32 S4 O31 112.1(3) . . ? O30 S4 O31 112.3(3) . . ? O32 S4 C40 108.9(4) . . ? O30 S4 C40 102.7(3) . . ? O31 S4 C40 107.7(4) . . ? O36 S5 O35 114.2(3) . . ? O36 S5 O34 110.9(3) . . ? O35 S5 O34 111.5(3) . . ? O36 S5 C50 109.6(3) . . ? O35 S5 C50 106.7(3) . . ? O34 S5 C50 103.3(3) . . ? O39 S6 O40 113.4(4) . . ? O39 S6 O38 113.3(3) . . ? O40 S6 O38 110.8(3) . . ? O39 S6 C60 107.9(3) . . ? O40 S6 C60 106.7(4) . . ? O38 S6 C60 104.0(3) . . ? O44 S7 O42 113.6(4) . . ? O44 S7 O43 112.1(3) . . ? O42 S7 O43 111.1(4) . . ? O44 S7 C70 109.3(4) . . ? O42 S7 C70 107.4(4) . . ? O43 S7 C70 102.7(4) . . ? O48 S8 O47 112.2(3) . . ? O48 S8 O46 111.5(3) . . ? O47 S8 O46 112.1(3) . . ? O48 S8 C80 108.1(4) . . ? O47 S8 C80 108.3(4) . . ? O46 S8 C80 104.2(4) . . ? O52 S9 O51 110.3(6) . . ? O52 S9 O50 114.3(7) . . ? O51 S9 O50 111.8(4) . . ? O52 S9 C90 107.8(5) . . ? O51 S9 C90 108.1(5) . . ? O50 S9 C90 104.1(5) . . ? Bi2 O1 Bi3 102.10(18) . . ? Bi2 O1 Bi1 102.25(19) . . ? Bi3 O1 Bi1 100.28(18) . . ? Bi2 O2 Bi6 117.8(2) . . ? Bi2 O2 Bi1 118.2(2) . . ? Bi6 O2 Bi1 115.0(2) . . ? Bi1 O3 Bi6 102.64(18) . . ? Bi1 O3 Bi4 101.8(2) . . ? Bi6 O3 Bi4 98.93(17) . . ? Bi4 O4 Bi3 116.8(2) . . ? Bi4 O4 Bi1 115.3(2) . . ? Bi3 O4 Bi1 117.4(2) . . ? Bi4 O5 Bi5 117.5(2) . . ? Bi4 O5 Bi6 117.73(19) . . ? Bi5 O5 Bi6 113.5(2) . . ? Bi4 O6 Bi3 101.65(17) . . ? Bi4 O6 Bi5 100.7(2) . . ? Bi3 O6 Bi5 97.84(18) . . ? Bi5 O7 Bi2 116.9(2) . . ? Bi5 O7 Bi3 120.0(2) . . ? Bi2 O7 Bi3 114.6(2) . . ? Bi5 O8 Bi6 105.03(19) . . ? Bi5 O8 Bi2 97.96(18) . . ? Bi6 O8 Bi2 96.58(17) . . ? Bi7 O13 Bi8 101.99(19) . . ? Bi7 O13 Bi9 101.00(19) . 2_757 ? Bi8 O13 Bi9 99.75(18) . 2_757 ? Bi8 O14 Bi9 116.9(2) . . ? Bi8 O14 Bi7 116.3(2) . . ? Bi9 O14 Bi7 118.4(2) . . ? Bi10 O15 Bi7 118.9(2) . . ? Bi10 O15 Bi9 114.1(2) . 2_757 ? Bi7 O15 Bi9 114.9(2) . 2_757 ? Bi9 O16 Bi10 102.63(18) . . ? Bi9 O16 Bi7 100.6(2) . . ? Bi10 O16 Bi7 99.36(18) . . ? S1 O18 Bi1 133.2(3) . . ? S1 O19 Bi6 129.5(3) . . ? C2 O21 Bi6 142.6(7) . . ? S2 O22 Bi3 126.3(3) . . ? S2 O23 Bi1 132.0(3) . . ? C12 O25 Bi3 149.5(5) . . ? S3 O26 Bi3 137.6(4) . . ? S3 O27 Bi2 127.7(3) . . ? S4 O30 Bi3 132.3(3) . . ? S4 O31 Bi5 127.4(3) . . ? C32 O33 Bi5 137.2(6) . . ? S5 O34 Bi7 138.9(3) . . ? S5 O34 Bi4 112.9(3) . . ? Bi7 O34 Bi4 107.52(18) . . ? S5 O35 Bi10 132.2(3) . . ? S5 O36 Bi4 88.4(2) . . ? S6 O38 Bi7 134.9(3) . . ? S6 O38 Bi5 100.8(3) . . ? Bi7 O38 Bi5 108.54(16) . . ? S6 O40 Bi5 100.2(3) . . ? S7 O42 Bi8 135.6(4) . . ? S7 O43 Bi7 131.1(3) . . ? S7 O43 Bi6 110.5(3) . . ? Bi7 O43 Bi6 107.2(2) . . ? S7 O44 Bi6 91.2(3) . . ? C62' O45' Bi8 141.3(15) . . ? S8 O46 Bi7 133.3(3) . . ? S8 O46 Bi4 129.1(3) . . ? Bi7 O46 Bi4 93.02(14) . . ? S8 O46 Bi6 113.9(3) . . ? Bi7 O46 Bi6 96.66(16) . . ? Bi4 O46 Bi6 71.33(11) . . ? S8 O47 Bi9 127.5(3) . . ? C72 O49 Bi9 135.4(7) . . ? S9 O51 Bi10 130.7(4) . . ? C2 C1 C10 115.7(7) . . ? C2 C1 C7 100.4(7) . . ? C10 C1 C7 115.4(7) . . ? C2 C1 C6 103.2(8) . . ? C10 C1 C6 117.6(7) . . ? C7 C1 C6 102.1(7) . . ? O21 C2 C3' 127.3(17) . . ? O21 C2 C1 125.2(8) . . ? C3' C2 C1 106.7(17) . . ? O21 C2 C3 127.2(12) . . ? C1 C2 C3 107.4(12) . . ? C2 C3 C4 100.3(15) . . ? C5 C4 C3 101.2(13) . . ? C5 C4 C3' 114.4(19) . . ? C5 C4 C7 103.5(9) . . ? C3 C4 C7 106.9(12) . . ? C3' C4 C7 97.5(15) . . ? C4 C5 C6 103.6(9) . . ? C5 C6 C1 102.5(8) . . ? C8 C7 C9 110.6(13) . . ? C8 C7 C4 109.6(11) . . ? C9 C7 C4 115.4(9) . . ? C8 C7 C1 113.3(10) . . ? C9 C7 C1 113.7(8) . . ? C4 C7 C1 93.2(7) . . ? C9 C7 C8' 102.7(15) . . ? C4 C7 C8' 123.1(14) . . ? C1 C7 C8' 108.8(11) . . ? C1 C10 S1 117.0(6) . . ? C20 C11 C12 114.9(7) . . ? C20 C11 C17 115.8(7) . . ? C12 C11 C17 97.7(6) . . ? C20 C11 C16 118.0(7) . . ? C12 C11 C16 104.7(7) . . ? C17 C11 C16 103.1(7) . . ? O25 C12 C13 125.0(7) . . ? O25 C12 C11 128.1(7) . . ? C13 C12 C11 106.9(7) . . ? C12 C13 C14 102.1(7) . . ? C13 C14 C17 101.6(7) . . ? C13 C14 C15 106.2(8) . . ? C17 C14 C15 103.6(7) . . ? C14 C15 C16 102.4(7) . . ? C11 C16 C15 104.1(7) . . ? C18 C17 C14 116.1(7) . . ? C18 C17 C11 113.5(7) . . ? C14 C17 C11 94.7(7) . . ? C18 C17 C19 106.6(8) . . ? C14 C17 C19 111.8(8) . . ? C11 C17 C19 114.0(7) . . ? C11 C20 S2 118.0(6) . . ? C30 C21 C22 113.7(7) . . ? C30 C21 C26 120.5(7) . . ? C22 C21 C26 105.5(7) . . ? C30 C21 C27 115.3(7) . . ? C22 C21 C27 98.0(6) . . ? C26 C21 C27 100.7(7) . . ? O29 C22 C21 125.4(8) . . ? O29 C22 C23 125.9(8) . . ? C21 C22 C23 108.7(7) . . ? C22 C23 C24 100.2(7) . . ? C25 C24 C27 101.8(8) . . ? C25 C24 C23 108.1(8) . . ? C27 C24 C23 103.1(7) . . ? C26 C25 C24 103.7(8) . . ? C25 C26 C21 105.4(8) . . ? C28 C27 C29 108.6(8) . . ? C28 C27 C24 115.3(8) . . ? C29 C27 C24 114.9(8) . . ? C28 C27 C21 112.4(7) . . ? C29 C27 C21 112.0(7) . . ? C24 C27 C21 93.1(7) . . ? C21 C30 S3 118.6(6) . . ? C40 C31 C32 116.7(7) . . ? C40 C31 C37 124.9(8) . . ? C32 C31 C37 100.7(7) . . ? C40 C31 C36 109.6(6) . . ? C32 C31 C36 101.1(7) . . ? C37 C31 C36 100.4(6) . . ? O33 C32 C33 127.5(9) . . ? O33 C32 C31 126.2(8) . . ? C33 C32 C31 106.0(7) . . ? C34 C33 C32 104.0(8) . . ? C33 C34 C35 107.3(9) . . ? C33 C34 C37 102.5(7) . . ? C35 C34 C37 102.1(8) . . ? C36 C35 C34 102.1(7) . . ? C35 C36 C31 105.7(7) . . ? C39 C37 C38 109.6(9) . . ? C39 C37 C34 114.0(8) . . ? C38 C37 C34 111.3(8) . . ? C39 C37 C31 112.8(7) . . ? C38 C37 C31 114.4(8) . . ? C34 C37 C31 94.1(7) . . ? C31 C40 S4 120.4(6) . . ? C42 C41 C50 114.9(6) . . ? C42 C41 C46 106.1(6) . . ? C50 C41 C46 118.0(6) . . ? C42 C41 C47 98.4(6) . . ? C50 C41 C47 115.1(6) . . ? C46 C41 C47 101.9(6) . . ? O37 C42 C41 125.8(7) . . ? O37 C42 C43 126.3(7) . . ? C41 C42 C43 107.9(6) . . ? C42 C43 C44 101.2(6) . . ? C45 C44 C43 107.7(7) . . ? C45 C44 C47 103.9(6) . . ? C43 C44 C47 102.9(6) . . ? C44 C45 C46 103.1(6) . . ? C41 C46 C45 103.0(6) . . ? C49 C47 C48 107.7(6) . . ? C49 C47 C44 113.8(6) . . ? C48 C47 C44 115.6(6) . . ? C49 C47 C41 113.8(6) . . ? C48 C47 C41 113.0(6) . . ? C44 C47 C41 92.6(5) . . ? C41 C50 S5 113.9(5) . . ? C60 C51 C52 114.4(6) . . ? C60 C51 C56 116.8(6) . . ? C52 C51 C56 106.7(6) . . ? C60 C51 C57 116.4(6) . . ? C52 C51 C57 97.8(6) . . ? C56 C51 C57 102.4(6) . . ? O41 C52 C53 127.3(8) . . ? O41 C52 C51 127.3(7) . . ? C53 C52 C51 105.3(7) . . ? C52 C53 C54 102.7(7) . . ? C53 C54 C55 107.1(9) . . ? C53 C54 C57 103.3(7) . . ? C55 C54 C57 103.7(7) . . ? C54 C55 C56 102.2(7) . . ? C55 C56 C51 103.9(7) . . ? C58 C57 C59 109.4(8) . . ? C58 C57 C54 115.0(7) . . ? C59 C57 C54 112.9(7) . . ? C58 C57 C51 113.0(7) . . ? C59 C57 C51 113.0(7) . . ? C54 C57 C51 92.8(6) . . ? C51 C60 S6 115.2(5) . . ? C70 C61 C66 116.1(11) . . ? C70 C61 C62 112.8(10) . . ? C66 C61 C62 98.4(10) . . ? C70 C61 C67 123.7(11) . . ? C66 C61 C67 102.8(11) . . ? C62 C61 C67 98.9(10) . . ? O45 C62 C63 125.3(13) . . ? O45 C62 C61 125.6(13) . . ? C63 C62 C61 108.6(11) . . ? C62 C63 C64 101.4(12) . . ? C65 C64 C63 107.6(14) . . ? C65 C64 C67 102.5(13) . . ? C63 C64 C67 102.9(12) . . ? C64 C65 C66 104.1(12) . . ? C61 C66 C65 103.2(13) . . ? C69 C67 C68 107.3(14) . . ? C69 C67 C64 115.7(13) . . ? C68 C67 C64 110.5(13) . . ? C69 C67 C61 113.0(14) . . ? C68 C67 C61 115.7(12) . . ? C64 C67 C61 94.4(11) . . ? C61 C70 S7 124.5(8) . . ? C62' C61' C67' 96.6(16) . . ? C62' C61' C66' 104.7(18) . . ? C67' C61' C66' 105.8(18) . . ? O45' C62' C63' 124(2) . . ? O45' C62' C61' 130(2) . . ? C63' C62' C61' 106.1(18) . . ? C62' C63' C64' 101.8(18) . . ? C67' C64' C65' 108(2) . . ? C67' C64' C63' 99(2) . . ? C65' C64' C63' 101(2) . . ? C66' C65' C64' 108(3) . . ? C65' C66' C61' 101(2) . . ? C68' C67' C64' 121(2) . . ? C68' C67' C69' 106(2) . . ? C64' C67' C69' 110(3) . . ? C68' C67' C61' 113(2) . . ? C64' C67' C61' 92.6(18) . . ? C69' C67' C61' 114(2) . . ? C72 C71 C80 115.6(7) . . ? C72 C71 C76 104.9(7) . . ? C80 C71 C76 117.9(7) . . ? C72 C71 C77 98.2(6) . . ? C80 C71 C77 115.7(6) . . ? C76 C71 C77 101.9(7) . . ? O49 C72 C71 126.9(8) . . ? O49 C72 C73 125.4(8) . . ? C71 C72 C73 107.5(7) . . ? C72 C73 C74 101.8(7) . . ? C73 C74 C75 106.3(8) . . ? C73 C74 C77 103.0(7) . . ? C75 C74 C77 103.2(7) . . ? C76 C75 C74 102.9(7) . . ? C75 C76 C71 104.3(7) . . ? C78 C77 C79 110.6(9) . . ? C78 C77 C74 114.9(8) . . ? C79 C77 C74 111.7(8) . . ? C78 C77 C71 112.5(7) . . ? C79 C77 C71 112.9(8) . . ? C74 C77 C71 93.4(6) . . ? C71 C80 S8 116.3(6) . . ? C90 C81 C86 125.6(12) . . ? C90 C81 C82 108.2(13) . . ? C86 C81 C82 108.4(14) . . ? C90 C81 C87 117.4(14) . . ? C86 C81 C87 101.5(14) . . ? C82 C81 C87 89.9(11) . . ? O53 C82 C83 125.0(15) . . ? O53 C82 C81 125.4(15) . . ? C83 C82 C81 109.6(14) . . ? C82 C83 C84 102.2(12) . . ? C83 C84 C87 101.3(11) . . ? C83 C84 C85 106.5(12) . . ? C87 C84 C85 101.5(13) . . ? C86 C85 C84 105.8(11) . . ? C81 C86 C85 104.3(13) . . ? C84 C87 C89 114.1(12) . . ? C84 C87 C88 112.7(13) . . ? C89 C87 C88 108.0(12) . . ? C84 C87 C81 96.5(11) . . ? C89 C87 C81 108.4(12) . . ? C88 C87 C81 117.0(12) . . ? C82' C81' C87' 118(3) . . ? C82' C81' C86' 89(3) . . ? C87' C81' C86' 103(2) . . ? O53' C82' C81' 126(3) . . ? O53' C82' C83' 128(3) . . ? C81' C82' C83' 102(3) . . ? C82' C83' C84' 104(3) . . ? C83' C84' C85' 105(3) . . ? C83' C84' C87' 98(3) . . ? C85' C84' C87' 102(3) . . ? C86' C85' C84' 96(2) . . ? C81' C86' C85' 107(3) . . ? C81' C87' C88' 121(3) . . ? C81' C87' C89' 108(2) . . ? C88' C87' C89' 108(2) . . ? C81' C87' C84' 93(2) . . ? C88' C87' C84' 109(3) . . ? C89' C87' C84' 119(3) . . ? C81 C90 S9 116.3(10) . . ? C2 C3' C4 101(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.741 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.194 # Attachment '- Cmpd 2 updated.CIF' data_rp_2ab _database_code_depnum_ccdc_archive 'CCDC 882407' #TrackingRef '- Cmpd 2 updated.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi6 H16 N6 O26 S6, H2 O' _chemical_formula_sum 'Bi6 H18 N6 O27 S6' _chemical_formula_weight 1980.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.7996(2) _cell_length_b 14.7996(2) _cell_length_c 11.1737(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2119.47(7) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2831 _cell_measurement_theta_min 2.4133 _cell_measurement_theta_max 31.5810 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.0958 _exptl_crystal_size_mid 0.0939 _exptl_crystal_size_min 0.0857 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2610 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 0 0.0378 0.0000 1.0000 0.0000 -0.0246 0.0240 -0.0434 0 -1 0 0.0479 0.0000 -1.0000 -0.0000 0.0246 -0.0240 0.0434 0 0 -1 0.0479 0.0000 0.0000 -1.0000 0.0405 -0.0292 -0.0391 0 0 1 0.0479 0.0000 0.0000 1.0000 -0.0405 0.0292 0.0391 -2 1 0 0.0439 -2.0000 1.0000 0.0000 -0.0601 -0.0743 -0.0069 2 -1 0 0.0499 2.0000 -1.0000 -0.0000 0.0601 0.0743 0.0069 _exptl_absorpt_coefficient_mu 37.830 _exptl_absorpt_correction_T_min 0.055 _exptl_absorpt_correction_T_max 0.134 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_detector_area_resol_mean 10.3389 _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5418 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 31.65 _reflns_number_total 1455 _reflns_number_gt 1346 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. explanation of restraints: commands/restraints were required to get a stable refinement because there was disorder in: O atoms O4/O5 and O6/O7 explanation of restraints more detailed: DFIX 0.88 N1 H1N N1 H2N DANG 1.3 H1N H2N To stabilise the distance and position of the hydrogen atoms of the amino group which is part of the ligand. Hydrogen atoms were refined and not calculated. DFIX 2.88 0.001 O8 O5 As O atom O5 is part of a disorder the distance to the existing water molecule in the crystal lattice was restrained using the DFIX command. ISOR 0.001 O4 O5 O6 O7 Even though these O atoms were modelled as disorder, the ISOR restraint was still necessary to stabilise the refinement. EQIV $1 1-X+Y, 2-X, Z EQIV $2 5/3-X, 4/3-Y, 1/3-Z EQIV $3 4/3-Y, 2/3+X-Y, Z-1/3 EQIV $4 5/3-Y, 1/3+X-Y, 1/3+Z EQIV $5 Y, 1-X+Y, 1-Z HTAB N1 O1_$5 HTAB N1 O2_$4 HTAB O5 O8 These commands defined the intra- and intermolecular hydrogen bonds present in the structure. ; _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^)+(0.0129P)^2^+37.1168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1455 _refine_ls_number_parameters 89 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.138 _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 0.842364(16) 0.877435(16) 0.135067(19) 0.00974(7) Uani 1 1 d . . . S1 S 0.93313(11) 0.74640(12) 0.34257(12) 0.0122(3) Uani 1 1 d . . . O1 O 1.0362(3) 0.8407(3) 0.3410(4) 0.0171(9) Uani 1 1 d . . . O2 O 0.9338(4) 0.6639(4) 0.2725(4) 0.0209(10) Uani 1 1 d . . . O3 O 0.8497(4) 0.7671(4) 0.3091(4) 0.0260(11) Uani 1 1 d . . . O4 O 1.0000 1.0000 0.1645(11) 0.0088(12) Uani 0.50 3 d SPU . 1 O5 O 1.0000 1.0000 0.24222(9) 0.0078(12) Uani 0.50 3 d SPDU . 2 H5 H 1.0000 1.0000 0.3317 0.009 Uiso 0.50 3 calc SPR . 2 O6 O 0.9518(6) 0.8138(7) 0.0703(7) 0.0078(14) Uani 0.50 1 d PU . 2 H6 H 0.9347 0.7429 0.0986 0.009 Uiso 0.50 1 calc PR . 2 O7 O 0.9682(6) 0.8659(6) 0.0649(6) 0.0054(14) Uani 0.50 1 d PU . 1 O8 O 1.0000 1.0000 0.5000 0.045(4) Uani 1 6 d SD . . N1 N 0.9003(4) 0.6988(4) 0.4778(4) 0.0160(10) Uani 1 1 d D . . H1N H 0.950(5) 0.691(7) 0.506(6) 0.04(2) Uiso 1 1 d D . . H2N H 0.895(6) 0.736(6) 0.535(5) 0.04(3) Uiso 1 1 d 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 0.00547(10) 0.00663(11) 0.01660(11) 0.00223(7) 0.00148(7) 0.00264(8) S1 0.0089(6) 0.0154(7) 0.0092(6) 0.0014(5) 0.0000(5) 0.0037(5) O1 0.013(2) 0.014(2) 0.018(2) 0.0037(16) 0.0002(16) 0.0014(18) O2 0.021(2) 0.017(2) 0.017(2) -0.0018(18) 0.0033(18) 0.004(2) O3 0.018(2) 0.047(3) 0.021(2) 0.016(2) 0.0046(18) 0.022(2) O4 0.0086(11) 0.0086(11) 0.0092(16) 0.000 0.000 0.0043(6) O5 0.0077(11) 0.0077(11) 0.0081(16) 0.000 0.000 0.0039(6) O6 0.0076(17) 0.0080(17) 0.0073(17) 0.0003(10) 0.0003(9) 0.0035(11) O7 0.0050(16) 0.0056(16) 0.0059(16) -0.0003(9) 0.0003(9) 0.0030(11) O8 0.053(6) 0.053(6) 0.029(7) 0.000 0.000 0.026(3) N1 0.015(3) 0.022(3) 0.010(2) 0.005(2) -0.0006(19) 0.008(2) _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 O7 2.105(7) . ? Bi1 O4 2.147(2) . ? Bi1 O7 2.152(7) 3_675 ? Bi1 O7 2.258(7) 11_565 ? Bi1 O6 2.323(7) 11_565 ? Bi1 O6 2.357(8) . ? Bi1 O5 2.4361(5) . ? Bi1 O6 2.502(8) 3_675 ? Bi1 O3 2.576(4) . ? Bi1 O2 2.794(5) 13_665 ? Bi1 O1 2.821(4) 3_675 ? Bi1 N1 3.012(5) 8_654 ? S1 O2 1.454(5) . ? S1 O3 1.462(5) . ? S1 O1 1.465(4) . ? S1 N1 1.634(5) . ? O4 Bi1 2.147(2) 3_675 ? O4 Bi1 2.147(2) 2_765 ? O5 Bi1 2.4361(5) 3_675 ? O5 Bi1 2.4361(5) 2_765 ? O6 Bi1 2.323(7) 12_655 ? O6 Bi1 2.502(8) 2_765 ? O7 Bi1 2.152(7) 2_765 ? O7 Bi1 2.258(7) 12_655 ? 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 Bi1 O4 59.6(3) . . ? O7 Bi1 O7 93.9(4) . 3_675 ? O4 Bi1 O7 58.9(3) . 3_675 ? O7 Bi1 O7 63.8(3) . 11_565 ? O4 Bi1 O7 90.5(4) . 11_565 ? O7 Bi1 O7 63.1(3) 3_675 11_565 ? O7 Bi1 O6 75.5(3) . 11_565 ? O4 Bi1 O6 107.5(4) . 11_565 ? O7 Bi1 O6 72.4(3) 3_675 11_565 ? O7 Bi1 O6 17.1(2) 11_565 11_565 ? O7 Bi1 O6 16.4(2) . . ? O4 Bi1 O6 73.2(2) . . ? O7 Bi1 O6 109.8(3) 3_675 . ? O7 Bi1 O6 70.0(3) 11_565 . ? O6 Bi1 O6 77.6(2) 11_565 . ? O7 Bi1 O5 71.7(2) . . ? O4 Bi1 O5 20.6(3) . . ? O7 Bi1 O5 71.0(2) 3_675 . ? O7 Bi1 O5 111.1(2) 11_565 . ? O6 Bi1 O5 128.2(2) 11_565 . ? O6 Bi1 O5 81.67(19) . . ? O7 Bi1 O6 108.2(3) . 3_675 ? O4 Bi1 O6 70.3(2) . 3_675 ? O7 Bi1 O6 14.6(2) 3_675 3_675 ? O7 Bi1 O6 69.3(3) 11_565 3_675 ? O6 Bi1 O6 74.7(2) 11_565 3_675 ? O6 Bi1 O6 123.9(4) . 3_675 ? O5 Bi1 O6 78.79(18) . 3_675 ? O7 Bi1 O3 84.9(2) . . ? O4 Bi1 O3 92.7(3) . . ? O7 Bi1 O3 146.4(2) 3_675 . ? O7 Bi1 O3 141.1(2) 11_565 . ? O6 Bi1 O3 138.3(2) 11_565 . ? O6 Bi1 O3 74.0(2) . . ? O5 Bi1 O3 76.85(12) . . ? O6 Bi1 O3 146.9(2) 3_675 . ? O7 Bi1 O2 81.3(2) . 13_665 ? O4 Bi1 O2 139.73(14) . 13_665 ? O7 Bi1 O2 139.9(2) 3_675 13_665 ? O7 Bi1 O2 79.6(2) 11_565 13_665 ? O6 Bi1 O2 67.8(2) 11_565 13_665 ? O6 Bi1 O2 66.7(2) . 13_665 ? O5 Bi1 O2 141.10(10) . 13_665 ? O6 Bi1 O2 137.6(2) 3_675 13_665 ? O3 Bi1 O2 73.18(16) . 13_665 ? O7 Bi1 O1 136.5(2) . 3_675 ? O4 Bi1 O1 82.6(3) . 3_675 ? O7 Bi1 O1 82.7(2) 3_675 3_675 ? O7 Bi1 O1 143.1(2) 11_565 3_675 ? O6 Bi1 O1 141.5(2) 11_565 3_675 ? O6 Bi1 O1 139.8(2) . 3_675 ? O5 Bi1 O1 66.11(10) . 3_675 ? O6 Bi1 O1 74.2(2) 3_675 3_675 ? O3 Bi1 O1 75.67(14) . 3_675 ? O2 Bi1 O1 127.19(13) 13_665 3_675 ? O7 Bi1 N1 159.1(2) . 8_654 ? O4 Bi1 N1 133.39(12) . 8_654 ? O7 Bi1 N1 84.2(2) 3_675 8_654 ? O7 Bi1 N1 97.3(2) 11_565 8_654 ? O6 Bi1 N1 84.2(2) 11_565 8_654 ? O6 Bi1 N1 151.9(2) . 8_654 ? O5 Bi1 N1 126.37(10) . 8_654 ? O6 Bi1 N1 69.9(2) 3_675 8_654 ? O3 Bi1 N1 108.11(14) . 8_654 ? O2 Bi1 N1 86.77(14) 13_665 8_654 ? O1 Bi1 N1 64.06(13) 3_675 8_654 ? O2 S1 O3 113.5(3) . . ? O2 S1 O1 110.6(3) . . ? O3 S1 O1 112.5(3) . . ? O2 S1 N1 105.2(3) . . ? O3 S1 N1 103.1(3) . . ? O1 S1 N1 111.4(3) . . ? S1 O3 Bi1 129.4(3) . . ? Bi1 O4 Bi1 117.70(17) . 3_675 ? Bi1 O4 Bi1 117.70(17) . 2_765 ? Bi1 O4 Bi1 117.70(17) 3_675 2_765 ? Bi1 O5 Bi1 97.91(3) . 3_675 ? Bi1 O5 Bi1 97.91(3) . 2_765 ? Bi1 O5 Bi1 97.91(3) 3_675 2_765 ? Bi1 O6 Bi1 104.0(3) 12_655 . ? Bi1 O6 Bi1 99.7(3) 12_655 2_765 ? Bi1 O6 Bi1 98.2(3) . 2_765 ? Bi1 O7 Bi1 119.3(3) . 2_765 ? Bi1 O7 Bi1 115.4(3) . 12_655 ? Bi1 O7 Bi1 113.5(3) 2_765 12_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N O1 0.87(2) 2.10(3) 2.951(7) 165(7) 11_566 N1 H1N O2 0.87(2) 2.12(5) 2.915(7) 151(8) 5_655 O5 H5 O8 1.00 1.88 2.8803(10) 180.0 . _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.300 _refine_diff_density_min -2.529 _refine_diff_density_rms 0.287 # Attachment '- Cmpd 3 updated.cif' data_mb529 _database_code_depnum_ccdc_archive 'CCDC 882408' #TrackingRef '- Cmpd 3 updated.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C224 H274 Bi38 O131 S24' _chemical_formula_weight 13773.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 22.5150(12) _cell_length_b 24.2440(4) _cell_length_c 31.4000(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.452(2) _cell_angle_gamma 90.00 _cell_volume 17134.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 99637 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 26.40 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12408 _exptl_absorpt_coefficient_mu 19.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'MX1 beamline, Australian Synchrotron' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r CCD' _diffrn_measurement_method '\f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122277 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.44 _reflns_number_total 33883 _reflns_number_gt 29917 _reflns_threshold_expression >2sigma(I) _computing_data_collection BlueIce _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The sulfate oxygen atom O(60) is located on the disordered ligand S11, in which only the mesityl moiety is disordered a trial modelling of the sulphate group, and therefore, the oxygen atom O(60) as disordered was not successful. The oxygen atom O(28) is a coordinated water molecule located in the vicinity of the disordered ligand S10. It shows elongated thermal ellipsoids suggesting disorder. However, the disorder could not be modelled. A void was located centred at 010 and contains presumably a xylene molecule, but this could not be modelled. Hydrogen atoms H(12A) and H(12C) are not located on C(137) and are from two different diseordered components. Hydrogen atom H(123) is not located on C(133) adn hydrogen atoms H(99A) and H(99D) are not positioned on O(59). Oxygen atoms O(26), O(27) and O(29) are probably water molecules and involved in hydrogen bonding which accounts for their short interaction with teh oxygen atoms O(60), O(64') and O(64). explanation of restraints: all of these commands/restraints were required to get a stable refinement because there was a lot of disorder in: Ligand S9: C81/C81' to C89/C89' and the corresponding H atoms, S9/S9', O54/O54' to O56/O56' Ligand S10: C91/91' to C99/C99' and the corresponding H atoms, S10/S10', O57/O57' to O59/O59' Ligand S11: C101/C111 to C109/C119 and the corrsponding H atoms, S11/S11' Ligand S12: C121/C131 to C129/C139 and the corrsponding H atoms, S12/S12', O63/O63' and O64/O64' Bi atoms: Bi8/Bi20 explanation of restraints more detailed: FLAT C81 > C89 DFIX 1.55 0.01 C82 C87 C84 C88 C86 C89 DANG 2.53 0.01 C81 C87 C83 C87 C83 C88 C85 C88 C85 C89 C81 C89 To stabilise the refinement of the mesiyl moiety of the disordered ligand S9 (part 1) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C81' > C89' DFIX 1.55 0.01 C82' C87' C84' C88' C86' C89' DANG 2.53 0.01 C81' C87' C83' C87' C83' C88' C85' C88' C85' C89' C81' C89' To stabilise the refinement of the mesiyl moiety of the disordered ligand S9' (part 2) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C91 > C99 DFIX 1.55 0.01 C92 C97 C94 C98 C96 C99 DANG 2.53 0.01 C91 C97 C93 C97 C93 C98 C95 C98 C95 C99 C91 C99 To stabilise the refinement of the mesiyl moiety of the disordered ligand S10 (part 1) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C91' > C99' DFIX 1.55 0.01 C92' C97' C94' C98' C96' C99' DANG 2.53 0.01 C91' C97' C93' C97' C93' C98' C95' C98' C95' C99' C91' C99' To stabilise the refinement of the mesiyl moiety of the disordered ligand S10' (part 2) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C101 > C109 All atoms of the arene moiety of the disordered ligand S11 (part 1) were restrained to be coplanar by a FLAT restraint. FLAT C111 > C119 DFIX 1.55 0.01 C106 C109 To stabilise the refinement of the mesiyl moiety of the disordered ligand S11' (part 2) the distances of these C atoms were restraint using the DFIX command. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C121 > C129 DFIX 1.55 0.01 C122 C127 C124 C128 C126 C129 DANG 2.53 0.01 C121 C127 C123 C127 C123 C128 C125 C128 C125 C129 C121 C129 To stabilise the refinement of the mesiyl moiety of the disordered ligand S12 (part 1) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. FLAT C131 > C139 DFIX 1.55 0.01 C132 C137 C134 C138 C136 C139 DANG 2.53 0.01 C131 C137 C133 C137 C133 C138 C135 C138 C135 C139 C131 C139 To stabilise the refinement of the mesiyl moiety of the disordered ligand S12' (part 2) the distances and angles of these C atoms were restraint using the DFIX and DANG commands. Additionally, all atoms of the arene moiety were restrained to be coplanar by a FLAT restraint. SIMU 0.01 0.01 1.7 C91' > C99' SIMU 0.01 0.01 1.7 C91 > C99 SIMU 0.01 0.01 1.7 C81 > C89 SIMU 0.01 0.01 1.7 C81' > C89' SIMU 0.01 0.01 1.7 C111 > C119 SIMU 0.01 0.01 1.7 C131 > C139 The SIMU instruction restrains the Uij components of these C atoms of the disorderd ligands S9/S9', S10/S10', S11' and S12' to be approximately equal with an appropriate esd. ; _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^)+(0.0685P)^2^+288.1185P] 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 33883 _refine_ls_number_parameters 1922 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.60077(3) 0.46982(2) -0.035577(16) 0.062 Uani 1 1 d . . . Bi2 Bi 0.55131(2) 0.587664(18) 0.025200(12) 0.039 Uani 1 1 d . . . Bi3 Bi 0.53020(2) 0.45079(2) 0.070424(16) 0.049 Uani 1 1 d . . . Bi4 Bi 0.693722(19) 0.513431(18) 0.062701(14) 0.040 Uani 1 1 d . A . Bi5 Bi 0.679312(17) 0.389303(17) 0.123053(12) 0.033 Uani 1 1 d . . . Bi6 Bi 0.749648(17) 0.395790(17) 0.011487(12) 0.034 Uani 1 1 d . . . Bi7 Bi 0.758733(18) 0.536738(18) -0.049668(12) 0.036 Uani 1 1 d . . . Bi8 Bi 0.63614(3) 0.60871(3) -0.07964(2) 0.026 Uani 0.50 1 d P A . Bi9 Bi 0.704906(17) 0.663971(16) 0.015971(12) 0.034 Uani 1 1 d . . . Bi10 Bi 0.569382(18) 0.741761(16) -0.035008(12) 0.033 Uani 1 1 d . . . Bi11 Bi 0.41998(2) 0.679824(18) -0.015219(13) 0.047 Uani 1 1 d . . . Bi12 Bi 0.492978(18) 0.733406(16) 0.076116(12) 0.033 Uani 1 1 d . A . Bi13 Bi 0.335592(18) 0.667773(16) 0.081009(12) 0.034 Uani 1 1 d . A . Bi14 Bi 0.330947(18) 0.532507(17) 0.143761(12) 0.033 Uani 1 1 d . . . Bi15 Bi 0.489113(19) 0.576290(17) 0.136811(11) 0.035 Uani 1 1 d . A . Bi16 Bi 0.461963(18) 0.442824(17) 0.184759(12) 0.035 Uani 1 1 d . A . Bi17 Bi 0.528464(18) 0.316871(16) 0.130447(11) 0.032 Uani 1 1 d . . . Bi18 Bi 0.619408(19) 0.515216(17) 0.180274(11) 0.035 Uani 1 1 d . . . Bi19 Bi 0.623990(19) 0.657135(16) 0.123032(12) 0.035 Uani 1 1 d . . . Bi20 Bi 0.60863(5) 0.62131(4) -0.08705(3) 0.042 Uani 0.50 1 d P . . S1 S 0.86504(14) 0.48774(15) 0.02915(10) 0.049 Uani 1 1 d . . . S2 S 0.75454(17) 0.5757(2) 0.17990(12) 0.072 Uani 1 1 d . . . S3 S 0.60906(13) 0.36417(12) 0.21726(8) 0.040 Uani 1 1 d . . . S4 S 0.40260(13) 0.24672(13) 0.14170(9) 0.043 Uani 1 1 d . . . S5 S 0.31671(14) 0.41991(12) 0.20557(9) 0.042 Uani 1 1 d . . . S6 S 0.41969(17) 0.74975(14) 0.17749(10) 0.054 Uani 1 1 d . . . S7 S 0.65775(13) 0.77781(12) 0.07069(9) 0.040 Uani 1 1 d . . . S8 S 0.79377(13) 0.39860(13) -0.10891(9) 0.040 Uani 1 1 d . . . S9 S 0.7605(4) 0.2651(4) 0.0640(3) 0.054 Uani 0.50 1 d P A 1 S9' S 0.7481(4) 0.2598(4) 0.0698(3) 0.056 Uani 0.50 1 d P B 2 S10 S 0.5224(4) 0.5355(3) 0.2622(2) 0.047 Uani 0.50 1 d P C 1 S10' S 0.5154(6) 0.5495(4) 0.2610(3) 0.072 Uani 0.50 1 d P D 2 S11 S 0.463(13) 0.838(9) 0.002(7) 0.051 Uani 0.50 1 d P E 1 S11' S 0.463(13) 0.839(9) 0.002(7) 0.051 Uani 0.50 1 d P E 2 S12 S 0.8152(4) 0.7091(4) -0.0469(2) 0.033 Uani 0.50 1 d P F 1 S12' S 0.8176(9) 0.7054(8) -0.0496(7) 0.109 Uani 0.50 1 d P F 2 O1 O 0.5000 0.5000 0.0000 0.065 Uani 1 2 d S . . O2 O 0.6078(3) 0.5112(3) 0.0365(2) 0.031 Uani 1 1 d . . . O3 O 0.5686(3) 0.5616(3) -0.04799(19) 0.029 Uani 1 1 d . . . O4 O 0.4905(3) 0.5470(3) 0.0745(2) 0.028 Uani 1 1 d . . . O5 O 0.6504(3) 0.4735(3) 0.1254(2) 0.036 Uani 1 1 d . A . O6 O 0.6953(3) 0.4234(3) 0.0625(2) 0.032 Uani 1 1 d . A . O7 O 0.7205(3) 0.4778(3) -0.0051(2) 0.041 Uani 1 1 d . A . O8 O 0.6783(3) 0.5191(3) -0.0860(2) 0.039 Uani 1 1 d . . . O9 O 0.6999(4) 0.5878(4) -0.0180(4) 0.077 Uani 1 1 d . A . O10 O 0.6230(3) 0.6710(3) -0.0254(2) 0.033 Uani 1 1 d . A . O11 O 0.6495(3) 0.6246(3) 0.0621(2) 0.035 Uani 1 1 d . . . O12 O 0.5350(3) 0.6597(3) 0.0973(2) 0.034 Uani 1 1 d . A . O13 O 0.5118(3) 0.7079(3) 0.0121(2) 0.031 Uani 1 1 d . A . O14 O 0.4197(3) 0.6825(3) 0.0560(2) 0.033 Uani 1 1 d . A . O15 O 0.3302(3) 0.6329(3) 0.0183(2) 0.034 Uani 1 1 d . . . O16 O 0.3705(3) 0.5897(3) 0.1017(2) 0.038 Uani 1 1 d . . . O17 O 0.4182(3) 0.5017(3) 0.1445(2) 0.033 Uani 1 1 d . . . O18 O 0.5308(3) 0.4949(3) 0.1591(2) 0.035 Uani 1 1 d . A . O19 O 0.4757(3) 0.3936(3) 0.1294(2) 0.032 Uani 1 1 d . . . O20 O 0.5923(3) 0.3674(3) 0.0981(2) 0.032 Uani 1 1 d . . . O21 O 0.5915(3) 0.5774(3) 0.1356(2) 0.038 Uani 1 1 d . A . O100 O 0.5147(6) 0.6870(4) -0.0699(3) 0.082 Uani 1 1 d . . . O22 O 0.4541(4) 0.6000(3) -0.0114(2) 0.037 Uani 1 1 d . . . O23 O 0.7855(4) 0.4349(4) 0.1411(3) 0.053 Uani 1 1 d . . . O24 O 0.7841(4) 0.6129(5) 0.0590(4) 0.074 Uani 1 1 d . . . O25 O 0.3068(5) 0.7578(4) 0.0354(3) 0.060 Uani 1 1 d . . . O26 O 0.3857(4) 0.5993(4) 0.1967(3) 0.049 Uani 1 1 d . . . O27 O 0.5903(6) 0.2388(4) 0.0926(3) 0.071 Uani 1 1 d . . . O28 O 0.5627(7) 0.6737(6) 0.1930(3) 0.104 Uani 1 1 d . . . O29 O 0.7465(5) 0.6127(4) -0.1050(3) 0.064 Uani 1 1 d . A . O30 O 0.8544(4) 0.4571(5) -0.0099(3) 0.059 Uani 1 1 d . . . O31 O 0.8220(3) 0.4705(4) 0.0615(3) 0.046 Uani 1 1 d . . . O32 O 0.8613(5) 0.5476(4) 0.0216(4) 0.067 Uani 1 1 d . . . O33 O 0.7481(5) 0.5182(5) 0.1934(4) 0.085 Uani 1 1 d . . . O34 O 0.6984(5) 0.6033(5) 0.1835(4) 0.086 Uani 1 1 d . . . O35 O 0.7768(8) 0.5768(10) 0.1386(4) 0.148 Uani 1 1 d . . . O36 O 0.5456(4) 0.3703(4) 0.2077(3) 0.048 Uani 1 1 d . A . O37 O 0.6338(4) 0.3166(3) 0.1955(3) 0.045 Uani 1 1 d . . . O38 O 0.6407(4) 0.4148(4) 0.2056(3) 0.051 Uani 1 1 d . . . O39 O 0.4312(4) 0.2862(4) 0.1712(3) 0.053 Uani 1 1 d . . . O40 O 0.3663(4) 0.2749(4) 0.1091(3) 0.050 Uani 1 1 d . . . O41 O 0.4456(4) 0.2116(4) 0.1217(3) 0.050 Uani 1 1 d . . . O42 O 0.3578(4) 0.3946(4) 0.1770(3) 0.048 Uani 1 1 d . . . O43 O 0.3430(4) 0.4709(3) 0.2226(2) 0.047 Uani 1 1 d . . . O44 O 0.2593(4) 0.4298(4) 0.1845(3) 0.050 Uani 1 1 d . . . O45 O 0.4022(4) 0.7336(4) 0.1341(3) 0.054 Uani 1 1 d . . . O46 O 0.4848(5) 0.7577(5) 0.1798(4) 0.085 Uani 1 1 d . . . O47 O 0.3980(7) 0.7104(5) 0.2082(3) 0.095 Uani 1 1 d . . . O48 O 0.6029(4) 0.7608(3) 0.0907(3) 0.044 Uani 1 1 d . A . O49 O 0.6505(4) 0.7752(3) 0.0247(2) 0.045 Uani 1 1 d . . . O50 O 0.7072(4) 0.7449(4) 0.0865(3) 0.046 Uani 1 1 d . . . O51 O 0.7959(4) 0.4586(4) -0.1056(3) 0.047 Uani 1 1 d . . . O52 O 0.7780(4) 0.3735(4) -0.0680(3) 0.049 Uani 1 1 d . . . O53 O 0.7530(4) 0.3798(4) -0.1424(3) 0.045 Uani 1 1 d . . . O54 O 0.7451(10) 0.3209(8) 0.0773(6) 0.057 Uani 0.50 1 d P A 1 O55 O 0.7803(10) 0.2657(10) 0.0203(7) 0.069 Uani 0.50 1 d P A 1 O56 O 0.7113(8) 0.2271(8) 0.0695(7) 0.053 Uani 0.50 1 d P A 1 O54' O 0.7251(10) 0.3171(9) 0.0686(6) 0.053 Uani 0.50 1 d P B 2 O55' O 0.7849(12) 0.2489(12) 0.0338(6) 0.088 Uani 0.50 1 d P B 2 O56' O 0.6969(13) 0.2198(11) 0.0768(10) 0.089 Uani 0.50 1 d P B 2 O57 O 0.5479(10) 0.4858(13) 0.2535(8) 0.058 Uani 0.50 1 d P C 1 O58 O 0.5632(10) 0.5766(9) 0.2469(7) 0.068 Uani 0.50 1 d P C 1 O59 O 0.4618(10) 0.5407(9) 0.2420(5) 0.064 Uani 0.50 1 d P C 1 O58' O 0.5418(10) 0.5859(8) 0.2289(6) 0.059 Uani 0.50 1 d P D 2 O57' O 0.5328(17) 0.4855(13) 0.2523(10) 0.100 Uani 0.50 1 d P D 2 O59' O 0.4546(10) 0.5534(14) 0.2639(8) 0.095 Uani 0.50 1 d P D 2 O60 O 0.4712(7) 0.8357(6) -0.0431(3) 0.105 Uani 1 1 d . . . O61 O 0.5190(5) 0.8278(4) 0.0258(4) 0.064 Uani 1 1 d . . . O62 O 0.4176(4) 0.8003(4) 0.0158(3) 0.057 Uani 1 1 d . . . O63 O 0.7688(13) 0.7399(13) -0.0379(10) 0.095 Uani 0.50 1 d P F 1 O64 O 0.8212(11) 0.6976(12) -0.0945(8) 0.077 Uani 0.50 1 d P F 1 O64' O 0.7960(9) 0.7072(8) -0.0918(6) 0.053 Uani 0.50 1 d P F 2 O63' O 0.7796(12) 0.7480(10) -0.0240(7) 0.065 Uani 0.50 1 d P F 2 O65 O 0.8137(4) 0.6530(4) -0.0269(3) 0.054 Uani 1 1 d . . . C1 C 0.9366(5) 0.4721(5) 0.0504(4) 0.047 Uani 1 1 d . . . C2 C 0.9763(6) 0.4371(6) 0.0290(4) 0.054 Uani 1 1 d . . . C3 C 1.0298(6) 0.4221(6) 0.0503(5) 0.059 Uani 1 1 d . . . H3 H 1.0572 0.3985 0.0366 0.071 Uiso 1 1 calc R . . C4 C 1.0429(6) 0.4414(8) 0.0912(6) 0.075 Uani 1 1 d . . . C5 C 1.0059(6) 0.4799(7) 0.1094(5) 0.069 Uani 1 1 d . . . H5 H 1.0177 0.4966 0.1356 0.082 Uiso 1 1 calc R . . C6 C 0.9526(6) 0.4945(6) 0.0905(5) 0.056 Uani 1 1 d . . . C7 C 0.9664(7) 0.4152(7) -0.0159(5) 0.069 Uani 1 1 d . . . H7A H 1.0003 0.3922 -0.0237 0.103 Uiso 1 1 calc R . . H7B H 0.9625 0.4461 -0.0359 0.103 Uiso 1 1 calc R . . H7C H 0.9300 0.3930 -0.0172 0.103 Uiso 1 1 calc R . . C8 C 1.1003(7) 0.4215(10) 0.1134(7) 0.102 Uani 1 1 d . . . H8A H 1.1033 0.4374 0.1421 0.153 Uiso 1 1 calc R . . H8B H 1.1344 0.4333 0.0969 0.153 Uiso 1 1 calc R . . H8C H 1.0998 0.3812 0.1154 0.153 Uiso 1 1 calc R . . C9 C 0.9138(7) 0.5385(8) 0.1125(5) 0.075 Uani 1 1 d . . . H9A H 0.8787 0.5465 0.0945 0.112 Uiso 1 1 calc R . . H9B H 0.9370 0.5724 0.1168 0.112 Uiso 1 1 calc R . . H9C H 0.9014 0.5245 0.1402 0.112 Uiso 1 1 calc R . . C11 C 0.8059(5) 0.6094(6) 0.2155(4) 0.049 Uani 1 1 d . . . C12 C 0.8439(8) 0.5780(7) 0.2402(6) 0.074 Uani 1 1 d . . . C13 C 0.8846(7) 0.6056(8) 0.2660(6) 0.082 Uani 1 1 d . . . H13 H 0.9112 0.5849 0.2836 0.099 Uiso 1 1 calc R . . C14 C 0.8878(6) 0.6625(7) 0.2671(5) 0.067 Uani 1 1 d . . . C15 C 0.8507(7) 0.6925(7) 0.2420(5) 0.068 Uani 1 1 d . . . H15 H 0.8527 0.7316 0.2429 0.081 Uiso 1 1 calc R . . C16 C 0.8095(8) 0.6670(7) 0.2146(5) 0.069 Uani 1 1 d . . . C17 C 0.8467(13) 0.5154(9) 0.2392(10) 0.149 Uani 1 1 d . . . H17A H 0.8785 0.5026 0.2587 0.224 Uiso 1 1 calc R . . H17B H 0.8547 0.5030 0.2102 0.224 Uiso 1 1 calc R . . H17C H 0.8086 0.5002 0.2481 0.224 Uiso 1 1 calc R . . C18 C 0.9332(8) 0.6921(8) 0.2952(7) 0.102 Uani 1 1 d . . . H18A H 0.9292 0.7321 0.2912 0.153 Uiso 1 1 calc R . . H18B H 0.9733 0.6806 0.2875 0.153 Uiso 1 1 calc R . . H18C H 0.9267 0.6829 0.3251 0.153 Uiso 1 1 calc R . . C19 C 0.7687(13) 0.7048(10) 0.1893(11) 0.162 Uani 1 1 d . . . H19A H 0.7814 0.7431 0.1935 0.242 Uiso 1 1 calc R . . H19B H 0.7279 0.7005 0.1990 0.242 Uiso 1 1 calc R . . H19C H 0.7702 0.6954 0.1590 0.242 Uiso 1 1 calc R . . C21 C 0.6183(5) 0.3561(5) 0.2734(3) 0.041 Uani 1 1 d . A . C22 C 0.5702(6) 0.3439(7) 0.2997(4) 0.058 Uani 1 1 d . . . C23 C 0.5821(8) 0.3369(9) 0.3435(5) 0.086 Uani 1 1 d . A . H23 H 0.5502 0.3301 0.3620 0.103 Uiso 1 1 calc R . . C24 C 0.6404(8) 0.3399(11) 0.3603(5) 0.101 Uani 1 1 d . . . C25 C 0.6857(7) 0.3521(9) 0.3336(4) 0.081 Uani 1 1 d . A . H25 H 0.7248 0.3558 0.3454 0.097 Uiso 1 1 calc R . . C26 C 0.6766(6) 0.3594(7) 0.2899(4) 0.059 Uani 1 1 d . . . C27 C 0.5060(7) 0.3375(9) 0.2846(5) 0.081 Uani 1 1 d . A . H27A H 0.5033 0.3421 0.2536 0.121 Uiso 1 1 calc R . . H27B H 0.4816 0.3655 0.2982 0.121 Uiso 1 1 calc R . . H27C H 0.4917 0.3007 0.2922 0.121 Uiso 1 1 calc R . . C28 C 0.6539(11) 0.3297(15) 0.4066(5) 0.166 Uani 1 1 d . A . H28A H 0.6168 0.3232 0.4215 0.249 Uiso 1 1 calc R . . H28B H 0.6742 0.3619 0.4190 0.249 Uiso 1 1 calc R . . H28C H 0.6797 0.2973 0.4097 0.249 Uiso 1 1 calc R . . C29 C 0.7312(6) 0.3700(8) 0.2623(5) 0.071 Uani 1 1 d . A . H29A H 0.7671 0.3715 0.2805 0.106 Uiso 1 1 calc R . . H29B H 0.7262 0.4052 0.2472 0.106 Uiso 1 1 calc R . . H29C H 0.7349 0.3401 0.2415 0.106 Uiso 1 1 calc R . . C31 C 0.3536(5) 0.2047(5) 0.1710(4) 0.043 Uani 1 1 d . A . C32 C 0.3119(6) 0.1736(5) 0.1483(4) 0.044 Uani 1 1 d . . . C33 C 0.2720(6) 0.1413(5) 0.1712(4) 0.053 Uani 1 1 d . A . H33 H 0.2429 0.1206 0.1556 0.063 Uiso 1 1 calc R . . C34 C 0.2726(6) 0.1378(5) 0.2145(4) 0.049 Uani 1 1 d . . . C35 C 0.3166(6) 0.1678(5) 0.2360(4) 0.051 Uani 1 1 d . A . H35 H 0.3187 0.1650 0.2661 0.061 Uiso 1 1 calc R . . C36 C 0.3578(5) 0.2018(5) 0.2164(4) 0.046 Uani 1 1 d . . . C37 C 0.3061(7) 0.1732(6) 0.1000(4) 0.058 Uani 1 1 d . A . H37A H 0.2733 0.1489 0.0912 0.087 Uiso 1 1 calc R . . H37B H 0.3431 0.1597 0.0880 0.087 Uiso 1 1 calc R . . H37C H 0.2981 0.2107 0.0897 0.087 Uiso 1 1 calc R . . C38 C 0.2272(7) 0.1048(7) 0.2382(5) 0.072 Uani 1 1 d . A . H38A H 0.2352 0.1080 0.2690 0.108 Uiso 1 1 calc R . . H38B H 0.2294 0.0660 0.2297 0.108 Uiso 1 1 calc R . . H38C H 0.1873 0.1191 0.2314 0.108 Uiso 1 1 calc R . . C39 C 0.4019(6) 0.2321(6) 0.2437(4) 0.057 Uani 1 1 d . A . H39A H 0.4280 0.2538 0.2257 0.086 Uiso 1 1 calc R . . H39B H 0.4258 0.2056 0.2604 0.086 Uiso 1 1 calc R . . H39C H 0.3811 0.2567 0.2630 0.086 Uiso 1 1 calc R . . C41 C 0.3058(5) 0.3730(5) 0.2483(3) 0.039 Uani 1 1 d . . . C42 C 0.2724(6) 0.3246(5) 0.2381(4) 0.049 Uani 1 1 d . A . C43 C 0.2605(6) 0.2898(6) 0.2727(4) 0.055 Uani 1 1 d . . . H43 H 0.2376 0.2575 0.2676 0.066 Uiso 1 1 calc R A . C44 C 0.2807(7) 0.3007(7) 0.3138(5) 0.065 Uani 1 1 d . A . C45 C 0.3151(8) 0.3457(7) 0.3210(4) 0.069 Uani 1 1 d . . . H45 H 0.3313 0.3514 0.3489 0.082 Uiso 1 1 calc R A . C46 C 0.3281(7) 0.3846(6) 0.2893(4) 0.056 Uani 1 1 d . A . C47 C 0.2510(6) 0.3087(5) 0.1954(4) 0.051 Uani 1 1 d . . . H47A H 0.2624 0.3371 0.1748 0.076 Uiso 1 1 calc R A . H47B H 0.2077 0.3052 0.1952 0.076 Uiso 1 1 calc R . . H47C H 0.2687 0.2734 0.1875 0.076 Uiso 1 1 calc R . . C48 C 0.2653(11) 0.2596(8) 0.3487(5) 0.098 Uani 1 1 d . . . H48A H 0.2407 0.2300 0.3365 0.147 Uiso 1 1 calc R A . H48B H 0.2434 0.2786 0.3710 0.147 Uiso 1 1 calc R . . H48C H 0.3020 0.2439 0.3611 0.147 Uiso 1 1 calc R . . C49 C 0.3650(9) 0.4318(7) 0.3013(5) 0.080 Uani 1 1 d . . . H49A H 0.3749 0.4301 0.3318 0.120 Uiso 1 1 calc R A . H49B H 0.3433 0.4660 0.2949 0.120 Uiso 1 1 calc R . . H49C H 0.4017 0.4310 0.2851 0.120 Uiso 1 1 calc R . . C51 C 0.3890(6) 0.8152(5) 0.1903(4) 0.050 Uani 1 1 d . . . C52 C 0.3692(9) 0.8521(6) 0.1570(5) 0.071 Uani 1 1 d . A . C53 C 0.3442(9) 0.9014(7) 0.1693(5) 0.076 Uani 1 1 d . . . H53 H 0.3306 0.9261 0.1476 0.091 Uiso 1 1 calc R A . C54 C 0.3377(6) 0.9167(6) 0.2111(5) 0.058 Uani 1 1 d . A . C55 C 0.3602(6) 0.8816(5) 0.2425(4) 0.049 Uani 1 1 d . . . H55 H 0.3585 0.8925 0.2715 0.059 Uiso 1 1 calc R A . C56 C 0.3853(6) 0.8305(5) 0.2325(4) 0.047 Uani 1 1 d . A . C57 C 0.3764(15) 0.8405(9) 0.1100(5) 0.154 Uani 1 1 d . . . H57A H 0.3949 0.8043 0.1065 0.231 Uiso 1 1 calc R A . H57B H 0.4015 0.8690 0.0977 0.231 Uiso 1 1 calc R . . H57C H 0.3373 0.8408 0.0956 0.231 Uiso 1 1 calc R . . C58 C 0.3099(7) 0.9725(6) 0.2218(5) 0.065 Uani 1 1 d . . . H58A H 0.3090 0.9770 0.2528 0.098 Uiso 1 1 calc R A . H58B H 0.2692 0.9741 0.2099 0.098 Uiso 1 1 calc R . . H58C H 0.3335 1.0022 0.2095 0.098 Uiso 1 1 calc R . . C59 C 0.4075(7) 0.7944(7) 0.2693(4) 0.067 Uani 1 1 d . . . H59A H 0.4003 0.8132 0.2964 0.101 Uiso 1 1 calc R A . H59B H 0.4502 0.7878 0.2667 0.101 Uiso 1 1 calc R . . H59C H 0.3863 0.7591 0.2686 0.101 Uiso 1 1 calc R . . C61 C 0.6721(5) 0.8471(5) 0.0858(4) 0.046 Uani 1 1 d . A . C62 C 0.7003(9) 0.8836(6) 0.0581(5) 0.073 Uani 1 1 d . . . C63 C 0.7108(10) 0.9367(7) 0.0729(7) 0.100 Uani 1 1 d . A . H63 H 0.7316 0.9616 0.0553 0.120 Uiso 1 1 calc R . . C64 C 0.6921(11) 0.9549(7) 0.1124(7) 0.097 Uani 1 1 d . . . C65 C 0.6664(7) 0.9181(6) 0.1393(6) 0.071 Uani 1 1 d . A . H65 H 0.6557 0.9300 0.1668 0.085 Uiso 1 1 calc R . . C66 C 0.6555(6) 0.8639(6) 0.1276(4) 0.054 Uani 1 1 d . . . C67 C 0.7224(11) 0.8661(11) 0.0162(6) 0.120 Uani 1 1 d . A . H67A H 0.7392 0.8980 0.0015 0.180 Uiso 1 1 calc R . . H67B H 0.6894 0.8509 -0.0011 0.180 Uiso 1 1 calc R . . H67C H 0.7531 0.8379 0.0203 0.180 Uiso 1 1 calc R . . C68 C 0.7041(17) 1.0156(9) 0.1249(12) 0.202 Uani 1 1 d . A . H68A H 0.7235 1.0345 0.1014 0.303 Uiso 1 1 calc R . . H68B H 0.7301 1.0168 0.1504 0.303 Uiso 1 1 calc R . . H68C H 0.6664 1.0340 0.1307 0.303 Uiso 1 1 calc R . . C69 C 0.6296(7) 0.8269(7) 0.1609(4) 0.063 Uani 1 1 d . A . H69A H 0.6253 0.7895 0.1495 0.095 Uiso 1 1 calc R . . H69B H 0.5906 0.8410 0.1688 0.095 Uiso 1 1 calc R . . H69C H 0.6561 0.8262 0.1862 0.095 Uiso 1 1 calc R . . C71 C 0.8661(6) 0.3746(5) -0.1214(4) 0.044 Uani 1 1 d . A . C72 C 0.8917(6) 0.3999(6) -0.1574(5) 0.056 Uani 1 1 d . . . C73 C 0.9480(6) 0.3805(7) -0.1688(5) 0.063 Uani 1 1 d . A . H73 H 0.9663 0.3967 -0.1927 0.076 Uiso 1 1 calc R . . C74 C 0.9770(6) 0.3402(6) -0.1476(4) 0.054 Uani 1 1 d . . . C75 C 0.9501(6) 0.3146(6) -0.1131(5) 0.060 Uani 1 1 d . A . H75 H 0.9702 0.2857 -0.0984 0.073 Uiso 1 1 calc R . . C76 C 0.8925(6) 0.3315(6) -0.0999(4) 0.051 Uani 1 1 d . . . C77 C 0.8625(7) 0.4441(6) -0.1836(5) 0.064 Uani 1 1 d . A . H77A H 0.8889 0.4553 -0.2064 0.096 Uiso 1 1 calc R . . H77B H 0.8542 0.4760 -0.1655 0.096 Uiso 1 1 calc R . . H77C H 0.8251 0.4300 -0.1961 0.096 Uiso 1 1 calc R . . C78 C 1.0377(7) 0.3209(9) -0.1615(6) 0.087 Uani 1 1 d . A . H78A H 1.0519 0.2914 -0.1426 0.131 Uiso 1 1 calc R . . H78B H 1.0656 0.3519 -0.1601 0.131 Uiso 1 1 calc R . . H78C H 1.0346 0.3071 -0.1908 0.131 Uiso 1 1 calc R . . C79 C 0.8684(7) 0.2996(7) -0.0616(5) 0.074 Uani 1 1 d . A . H79A H 0.8965 0.2705 -0.0532 0.111 Uiso 1 1 calc R . . H79B H 0.8300 0.2829 -0.0696 0.111 Uiso 1 1 calc R . . H79C H 0.8632 0.3250 -0.0377 0.111 Uiso 1 1 calc R . . C81 C 0.8210(11) 0.2451(12) 0.0988(9) 0.126 Uiso 0.50 1 d PGDU A 1 C82 C 0.8719(12) 0.2775(10) 0.0992(9) 0.115 Uiso 0.50 1 d PGDU A 1 C83 C 0.9212(11) 0.2620(11) 0.1239(9) 0.129 Uiso 0.50 1 d PGDU A 1 H83 H 0.9561 0.2842 0.1242 0.154 Uiso 0.50 1 calc PR A 1 C84 C 0.9196(11) 0.2141(12) 0.1482(9) 0.146 Uiso 0.50 1 d PGDU A 1 C85 C 0.8687(13) 0.1817(10) 0.1478(9) 0.155 Uiso 0.50 1 d PGDU A 1 H85 H 0.8676 0.1490 0.1644 0.186 Uiso 0.50 1 calc PR A 1 C86 C 0.8194(12) 0.1972(11) 0.1231(10) 0.151 Uiso 0.50 1 d PGDU A 1 C87 C 0.8736(19) 0.3315(14) 0.0736(13) 0.102 Uiso 0.50 1 d PDU A 1 H87A H 0.9133 0.3480 0.0765 0.153 Uiso 0.50 1 calc PR A 1 H87B H 0.8440 0.3572 0.0844 0.153 Uiso 0.50 1 calc PR A 1 H87C H 0.8647 0.3238 0.0435 0.153 Uiso 0.50 1 calc PR A 1 C88 C 0.9744(15) 0.1970(18) 0.1753(14) 0.150 Uiso 0.50 1 d PDU A 1 H88A H 1.0069 0.2230 0.1706 0.225 Uiso 0.50 1 calc PR A 1 H88B H 0.9869 0.1598 0.1670 0.225 Uiso 0.50 1 calc PR A 1 H88C H 0.9645 0.1971 0.2055 0.225 Uiso 0.50 1 calc PR A 1 C89 C 0.7618(15) 0.1630(17) 0.1248(16) 0.160 Uiso 0.50 1 d PDU A 1 H89A H 0.7317 0.1790 0.1053 0.239 Uiso 0.50 1 calc PR A 1 H89B H 0.7471 0.1633 0.1539 0.239 Uiso 0.50 1 calc PR A 1 H89C H 0.7699 0.1249 0.1162 0.239 Uiso 0.50 1 calc PR A 1 C81' C 0.7994(11) 0.2615(11) 0.1177(7) 0.100 Uiso 0.50 1 d PGDU B 2 C82' C 0.8500(11) 0.2944(10) 0.1184(7) 0.101 Uiso 0.50 1 d PGDU B 2 C83' C 0.8820(10) 0.3024(10) 0.1564(8) 0.122 Uiso 0.50 1 d PGDU B 2 H83' H 0.9165 0.3249 0.1568 0.146 Uiso 0.50 1 calc PR B 2 C84' C 0.8633(12) 0.2776(12) 0.1936(7) 0.142 Uiso 0.50 1 d PGDU B 2 C85' C 0.8127(12) 0.2447(12) 0.1929(7) 0.140 Uiso 0.50 1 d PGDU B 2 H85' H 0.8000 0.2277 0.2184 0.168 Uiso 0.50 1 calc PR B 2 C86' C 0.7808(10) 0.2366(11) 0.1550(8) 0.126 Uiso 0.50 1 d PGDU B 2 C87' C 0.8699(18) 0.3239(17) 0.0778(9) 0.099 Uiso 0.50 1 d PDU B 2 H87D H 0.8409 0.3168 0.0546 0.149 Uiso 0.50 1 calc PR B 2 H87E H 0.9089 0.3100 0.0698 0.149 Uiso 0.50 1 calc PR B 2 H87F H 0.8724 0.3637 0.0831 0.149 Uiso 0.50 1 calc PR B 2 C88' C 0.9001(17) 0.2845(19) 0.2352(9) 0.155 Uiso 0.50 1 d PDU B 2 H88D H 0.9350 0.3074 0.2298 0.232 Uiso 0.50 1 calc PR B 2 H88E H 0.9131 0.2483 0.2456 0.232 Uiso 0.50 1 calc PR B 2 H88F H 0.8758 0.3024 0.2566 0.232 Uiso 0.50 1 calc PR B 2 C89' C 0.7258(15) 0.1990(17) 0.1543(12) 0.137 Uiso 0.50 1 d PDU B 2 H89D H 0.7063 0.2004 0.1260 0.206 Uiso 0.50 1 calc PR B 2 H89E H 0.6980 0.2115 0.1758 0.206 Uiso 0.50 1 calc PR B 2 H89F H 0.7380 0.1610 0.1606 0.206 Uiso 0.50 1 calc PR B 2 C91 C 0.5204(9) 0.5414(10) 0.3168(6) 0.081 Uiso 0.50 1 d PGDU C 1 C92 C 0.5695(8) 0.5225(10) 0.3403(7) 0.096 Uiso 0.50 1 d PGDU C 1 C93 C 0.5675(9) 0.5194(11) 0.3844(7) 0.115 Uiso 0.50 1 d PGDU C 1 H93 H 0.6010 0.5066 0.4005 0.138 Uiso 0.50 1 calc PR C 1 C94 C 0.5163(10) 0.5352(11) 0.4051(6) 0.128 Uiso 0.50 1 d PGDU C 1 C95 C 0.4672(9) 0.5541(11) 0.3817(7) 0.122 Uiso 0.50 1 d PGDU C 1 H95 H 0.4323 0.5648 0.3958 0.146 Uiso 0.50 1 calc PR C 1 C96 C 0.4693(8) 0.5571(10) 0.3375(6) 0.099 Uiso 0.50 1 d PGDU C 1 C97 C 0.6278(10) 0.5084(16) 0.3180(9) 0.105 Uiso 0.50 1 d PDU C 1 H97A H 0.6215 0.5107 0.2870 0.157 Uiso 0.50 1 calc PR C 1 H97B H 0.6403 0.4710 0.3258 0.157 Uiso 0.50 1 calc PR C 1 H97C H 0.6588 0.5347 0.3269 0.157 Uiso 0.50 1 calc PR C 1 C98 C 0.5151(16) 0.534(2) 0.4540(6) 0.146 Uiso 0.50 1 d PDU C 1 H98A H 0.4760 0.5458 0.4634 0.218 Uiso 0.50 1 calc PR C 1 H98B H 0.5457 0.5585 0.4658 0.218 Uiso 0.50 1 calc PR C 1 H98C H 0.5227 0.4961 0.4640 0.218 Uiso 0.50 1 calc PR C 1 C99 C 0.4160(11) 0.5810(15) 0.3120(9) 0.096 Uiso 0.50 1 d PDU C 1 H99A H 0.4234 0.5781 0.2815 0.144 Uiso 0.50 1 calc PR C 1 H99B H 0.4106 0.6198 0.3197 0.144 Uiso 0.50 1 calc PR C 1 H99C H 0.3800 0.5602 0.3187 0.144 Uiso 0.50 1 calc PR C 1 C91' C 0.5551(11) 0.5702(11) 0.3096(8) 0.117 Uiso 0.50 1 d PGDU D 2 C92' C 0.5529(11) 0.6245(10) 0.3237(8) 0.130 Uiso 0.50 1 d PGDU D 2 C93' C 0.5884(12) 0.6413(9) 0.3582(8) 0.129 Uiso 0.50 1 d PGDU D 2 H93' H 0.5869 0.6784 0.3678 0.155 Uiso 0.50 1 calc PR D 2 C94' C 0.6262(12) 0.6038(11) 0.3785(8) 0.130 Uiso 0.50 1 d PGDU D 2 C95' C 0.6284(11) 0.5495(10) 0.3645(8) 0.128 Uiso 0.50 1 d PGDU D 2 H95' H 0.6542 0.5238 0.3784 0.153 Uiso 0.50 1 calc PR D 2 C96' C 0.5929(12) 0.5327(9) 0.3300(8) 0.126 Uiso 0.50 1 d PGDU D 2 C97' C 0.5145(18) 0.6670(14) 0.2992(12) 0.140 Uiso 0.50 1 d PDU D 2 H97D H 0.4920 0.6485 0.2763 0.210 Uiso 0.50 1 calc PR D 2 H97E H 0.5402 0.6952 0.2871 0.210 Uiso 0.50 1 calc PR D 2 H97F H 0.4869 0.6845 0.3188 0.210 Uiso 0.50 1 calc PR D 2 C98' C 0.6673(17) 0.6226(16) 0.4156(11) 0.138 Uiso 0.50 1 d PDU D 2 H98D H 0.6907 0.5911 0.4262 0.208 Uiso 0.50 1 calc PR D 2 H98E H 0.6434 0.6373 0.4386 0.208 Uiso 0.50 1 calc PR D 2 H98F H 0.6941 0.6514 0.4056 0.208 Uiso 0.50 1 calc PR D 2 C99' C 0.5967(19) 0.4729(11) 0.3139(13) 0.141 Uiso 0.50 1 d PDU D 2 H99D H 0.5648 0.4662 0.2927 0.212 Uiso 0.50 1 calc PR D 2 H99E H 0.5925 0.4474 0.3378 0.212 Uiso 0.50 1 calc PR D 2 H99F H 0.6353 0.4670 0.3008 0.212 Uiso 0.50 1 calc PR D 2 C101 C 0.4498(10) 0.9091(9) 0.0090(7) 0.050 Uiso 0.50 1 d PD E 1 C102 C 0.3908(9) 0.9264(9) 0.0000(6) 0.053 Uiso 0.50 1 d PD E 1 C103 C 0.3762(11) 0.9802(10) 0.0083(7) 0.060 Uiso 0.50 1 d PD E 1 H103 H 0.3368 0.9922 0.0022 0.072 Uiso 0.50 1 calc PR E 1 C104 C 0.4163(11) 1.0176(11) 0.0252(8) 0.057 Uiso 0.50 1 d PD E 1 C105 C 0.4749(15) 0.9998(15) 0.0346(12) 0.105 Uiso 0.50 1 d PD E 1 H105 H 0.5034 1.0246 0.0467 0.126 Uiso 0.50 1 calc PR E 1 C106 C 0.4898(12) 0.9458(13) 0.0261(11) 0.087 Uiso 0.50 1 d PD E 1 C107 C 0.3422(14) 0.8870(14) -0.0168(13) 0.117 Uiso 0.50 1 d PD E 1 H10A H 0.3063 0.9081 -0.0242 0.176 Uiso 0.50 1 calc PR E 1 H10B H 0.3332 0.8599 0.0053 0.176 Uiso 0.50 1 calc PR E 1 H10C H 0.3561 0.8679 -0.0421 0.176 Uiso 0.50 1 calc PR E 1 C108 C 0.3994(16) 1.0770(14) 0.0351(12) 0.095 Uiso 0.50 1 d PD E 1 H10D H 0.4332 1.0957 0.0491 0.143 Uiso 0.50 1 calc PR E 1 H10E H 0.3654 1.0773 0.0540 0.143 Uiso 0.50 1 calc PR E 1 H10F H 0.3887 1.0962 0.0085 0.143 Uiso 0.50 1 calc PR E 1 C109 C 0.5562(13) 0.9315(18) 0.0338(15) 0.140 Uiso 0.50 1 d PD E 1 H10G H 0.5629 0.8927 0.0267 0.210 Uiso 0.50 1 calc PR E 1 H10H H 0.5672 0.9379 0.0638 0.210 Uiso 0.50 1 calc PR E 1 H10I H 0.5806 0.9549 0.0157 0.210 Uiso 0.50 1 calc PR E 1 C111 C 0.4342(11) 0.9017(10) 0.0233(8) 0.076 Uiso 0.50 1 d PDU E 2 C112 C 0.3779(11) 0.9207(10) 0.0083(7) 0.073 Uiso 0.50 1 d PDU E 2 C113 C 0.3535(12) 0.9653(11) 0.0282(8) 0.089 Uiso 0.50 1 d PDU E 2 H113 H 0.3156 0.9781 0.0186 0.106 Uiso 0.50 1 calc PR E 2 C114 C 0.3814(14) 0.9921(14) 0.0616(11) 0.099 Uiso 0.50 1 d PDU E 2 C115 C 0.4373(15) 0.9728(15) 0.0766(11) 0.098 Uiso 0.50 1 d PDU E 2 H115 H 0.4571 0.9899 0.1002 0.118 Uiso 0.50 1 calc PR E 2 C116 C 0.4627(12) 0.9286(14) 0.0561(10) 0.089 Uiso 0.50 1 d PDU E 2 C117 C 0.3450(11) 0.8946(11) -0.0300(9) 0.065 Uiso 0.50 1 d PDU E 2 H11A H 0.3096 0.9166 -0.0373 0.098 Uiso 0.50 1 calc PR E 2 H11B H 0.3330 0.8570 -0.0228 0.098 Uiso 0.50 1 calc PR E 2 H11C H 0.3712 0.8937 -0.0544 0.098 Uiso 0.50 1 calc PR E 2 C118 C 0.3531(17) 1.0406(15) 0.0845(13) 0.109 Uiso 0.50 1 d PDU E 2 H11D H 0.3786 1.0516 0.1088 0.163 Uiso 0.50 1 calc PR E 2 H11E H 0.3140 1.0297 0.0946 0.163 Uiso 0.50 1 calc PR E 2 H11F H 0.3486 1.0717 0.0647 0.163 Uiso 0.50 1 calc PR E 2 C119 C 0.5235(13) 0.9100(15) 0.0752(11) 0.089 Uiso 0.50 1 d PDU E 2 H11G H 0.5334 0.8734 0.0641 0.134 Uiso 0.50 1 calc PR E 2 H11H H 0.5213 0.9083 0.1063 0.134 Uiso 0.50 1 calc PR E 2 H11I H 0.5542 0.9365 0.0672 0.134 Uiso 0.50 1 calc PR E 2 C121 C 0.8885(9) 0.7322(7) -0.0418(5) 0.035 Uiso 0.50 1 d PD F 1 C122 C 0.9208(9) 0.7265(7) -0.0056(6) 0.040 Uiso 0.50 1 d PD F 1 C123 C 0.9808(10) 0.7472(8) -0.0014(9) 0.061 Uiso 0.50 1 d PD F 1 H123 H 1.0030 0.7435 0.0246 0.073 Uiso 0.50 1 calc PR F 1 C124 C 1.0047(10) 0.7722(12) -0.0360(10) 0.064 Uiso 0.50 1 d PD F 1 C125 C 0.9730(16) 0.7758(19) -0.0740(15) 0.122 Uiso 0.50 1 d PD F 1 H125 H 0.9914 0.7906 -0.0984 0.146 Uiso 0.50 1 calc PR F 1 C126 C 0.9165(16) 0.7589(15) -0.0768(8) 0.084 Uiso 0.50 1 d PD F 1 C127 C 0.8996(9) 0.6916(9) 0.0324(6) 0.046 Uiso 0.50 1 d PD F 1 H12A H 0.9295 0.6931 0.0556 0.069 Uiso 0.50 1 calc PR F 1 H12B H 0.8940 0.6532 0.0233 0.069 Uiso 0.50 1 calc PR F 1 H12C H 0.8619 0.7064 0.0423 0.069 Uiso 0.50 1 calc PR F 1 C128 C 1.0683(11) 0.7970(17) -0.0327(12) 0.128 Uiso 0.50 1 d PD F 1 H12D H 1.0784 0.8134 -0.0601 0.191 Uiso 0.50 1 calc PR F 1 H12E H 1.0968 0.7677 -0.0254 0.191 Uiso 0.50 1 calc PR F 1 H12F H 1.0697 0.8254 -0.0105 0.191 Uiso 0.50 1 calc PR F 1 C129 C 0.8791(17) 0.763(2) -0.1188(7) 0.168 Uiso 0.50 1 d PD F 1 H12G H 0.8662 0.7260 -0.1276 0.253 Uiso 0.50 1 calc PR F 1 H12H H 0.9032 0.7794 -0.1410 0.253 Uiso 0.50 1 calc PR F 1 H12I H 0.8441 0.7861 -0.1142 0.253 Uiso 0.50 1 calc PR F 1 C131 C 0.8753(12) 0.7515(13) -0.0321(11) 0.159 Uiso 0.50 1 d PGDU F 2 C132 C 0.9073(14) 0.7402(13) 0.0054(10) 0.164 Uiso 0.50 1 d PGDU F 2 C133 C 0.9633(14) 0.7632(14) 0.0122(9) 0.163 Uiso 0.50 1 d PGDU F 2 H133 H 0.9852 0.7555 0.0377 0.196 Uiso 0.50 1 calc PR F 2 C134 C 0.9873(13) 0.7974(14) -0.0185(11) 0.164 Uiso 0.50 1 d PGDU F 2 C135 C 0.9552(14) 0.8087(13) -0.0559(10) 0.163 Uiso 0.50 1 d PGDU F 2 H135 H 0.9716 0.8321 -0.0768 0.196 Uiso 0.50 1 calc PR F 2 C136 C 0.8992(14) 0.7857(14) -0.0627(9) 0.157 Uiso 0.50 1 d PGDU F 2 C137 C 0.879(2) 0.707(2) 0.0409(13) 0.170 Uiso 0.50 1 d PDU F 2 H13A H 0.8392 0.6939 0.0312 0.255 Uiso 0.50 1 calc PR F 2 H13B H 0.8745 0.7298 0.0662 0.255 Uiso 0.50 1 calc PR F 2 H13C H 0.9036 0.6747 0.0480 0.255 Uiso 0.50 1 calc PR F 2 C138 C 1.0494(15) 0.823(2) -0.0110(15) 0.169 Uiso 0.50 1 d PDU F 2 H13D H 1.0655 0.8109 0.0169 0.253 Uiso 0.50 1 calc PR F 2 H13E H 1.0465 0.8630 -0.0116 0.253 Uiso 0.50 1 calc PR F 2 H13F H 1.0758 0.8103 -0.0334 0.253 Uiso 0.50 1 calc PR F 2 C139 C 0.8627(19) 0.800(2) -0.1032(12) 0.156 Uiso 0.50 1 d PDU F 2 H13G H 0.8244 0.7811 -0.1028 0.234 Uiso 0.50 1 calc PR F 2 H13H H 0.8844 0.7888 -0.1283 0.234 Uiso 0.50 1 calc PR F 2 H13I H 0.8560 0.8402 -0.1043 0.234 Uiso 0.50 1 calc PR F 2 C151 C 0.5041(6) 0.9837(6) 0.2008(6) 0.198 Uani 0.50 1 d PG . . C152 C 0.5357(7) 1.0034(7) 0.1666(6) 0.068 Uani 0.50 1 d PG G . H152 H 0.5678 0.9826 0.1559 0.081 Uiso 0.50 1 calc PR . . C153 C 0.5203(8) 1.0536(8) 0.1479(5) 0.103 Uani 0.50 1 d PG G . C154 C 0.4733(9) 1.0840(7) 0.1635(7) 0.077 Uani 0.50 1 d PG G . H154 H 0.4628 1.1183 0.1507 0.092 Uiso 0.50 1 calc PR . . C155 C 0.4417(9) 1.0644(7) 0.1977(8) 0.116 Uani 0.50 1 d PG G . H155 H 0.4096 1.0852 0.2084 0.139 Uiso 0.50 1 calc PR . . C156 C 0.4571(8) 1.0142(7) 0.2164(6) 0.073 Uani 0.50 1 d PG G . H156 H 0.4354 1.0008 0.2398 0.087 Uiso 0.50 1 calc PR . . C157 C 0.5120(9) 0.9278(7) 0.2173(10) 0.169 Uani 0.50 1 d PG G 1 H15A H 0.4777 0.9051 0.2087 0.254 Uiso 0.50 1 calc PR G 1 H15B H 0.5154 0.9289 0.2485 0.254 Uiso 0.50 1 calc PR G 1 H15C H 0.5482 0.9117 0.2058 0.254 Uiso 0.50 1 calc PR G 1 C158 C 0.5605(12) 1.0777(12) 0.1161(8) 0.191 Uani 0.50 1 d PG G 2 H15D H 0.5997 1.0840 0.1295 0.287 Uiso 0.50 1 calc PR G 2 H15E H 0.5440 1.1129 0.1059 0.287 Uiso 0.50 1 calc PR G 2 H15F H 0.5642 1.0522 0.0921 0.287 Uiso 0.50 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.107 0.036 0.040 -0.002 -0.029 -0.002 Bi2 0.048 0.040 0.028 0.006 0.010 0.010 Bi3 0.041 0.058 0.049 -0.029 0.003 0.000 Bi4 0.037 0.039 0.045 -0.004 -0.004 -0.001 Bi5 0.036 0.039 0.024 0.004 -0.003 0.002 Bi6 0.035 0.038 0.029 0.004 0.002 0.006 Bi7 0.037 0.041 0.031 0.004 0.004 -0.002 Bi8 0.026 0.030 0.022 0.005 0.000 0.004 Bi9 0.036 0.033 0.032 0.001 0.000 -0.003 Bi10 0.040 0.030 0.028 0.001 0.001 -0.001 Bi11 0.078 0.034 0.028 -0.004 -0.014 0.018 Bi12 0.044 0.031 0.025 -0.003 0.002 0.002 Bi13 0.041 0.034 0.028 -0.002 0.004 0.007 Bi14 0.040 0.037 0.024 0.002 0.008 0.004 Bi15 0.053 0.035 0.019 -0.002 0.002 0.005 Bi16 0.042 0.041 0.023 0.008 0.005 0.004 Bi17 0.040 0.035 0.021 0.004 0.000 0.000 Bi18 0.047 0.036 0.021 0.000 -0.006 -0.001 Bi19 0.046 0.033 0.026 -0.002 -0.007 -0.002 Bi20 0.058 0.039 0.028 0.001 0.013 -0.011 S1 0.045 0.060 0.043 0.008 0.003 -0.008 S2 0.056 0.116 0.043 -0.004 -0.012 -0.019 S3 0.052 0.042 0.025 0.003 -0.005 0.003 S4 0.046 0.044 0.038 0.013 0.009 0.002 S5 0.050 0.044 0.032 0.008 0.013 0.001 S6 0.077 0.049 0.037 -0.008 0.004 0.012 S7 0.049 0.033 0.037 -0.003 -0.008 -0.003 S8 0.039 0.048 0.034 0.001 0.008 0.006 S9 0.054 0.036 0.072 -0.003 -0.024 0.002 S9' 0.064 0.054 0.048 0.000 -0.002 0.029 S10 0.068 0.053 0.020 0.000 0.007 0.004 S10' 0.099 0.086 0.029 0.000 -0.011 -0.026 S11 0.080 0.035 0.041 -0.001 0.011 0.006 S11' 0.080 0.035 0.041 -0.001 0.011 0.006 S12 0.035 0.037 0.028 0.012 0.002 -0.016 S12' 0.119 0.085 0.127 0.014 0.052 0.012 O1 0.133 0.031 0.031 -0.003 0.027 -0.006 O2 0.026 0.039 0.028 -0.001 -0.002 -0.004 O3 0.033 0.036 0.018 0.007 0.008 -0.001 O4 0.041 0.025 0.019 -0.006 0.005 0.005 O5 0.042 0.035 0.029 -0.002 -0.001 0.001 O6 0.039 0.030 0.028 0.003 0.003 0.003 O7 0.047 0.039 0.037 0.013 0.009 0.012 O8 0.048 0.038 0.030 -0.005 -0.003 0.006 O9 0.045 0.056 0.133 -0.052 0.022 -0.008 O10 0.035 0.033 0.032 0.000 -0.005 0.001 O11 0.042 0.033 0.029 -0.004 0.005 -0.001 O12 0.038 0.035 0.029 -0.002 0.000 -0.002 O13 0.043 0.023 0.027 -0.003 0.006 -0.001 O14 0.041 0.041 0.017 -0.004 0.004 0.000 O15 0.033 0.046 0.024 -0.002 0.006 -0.002 O16 0.041 0.039 0.033 0.007 0.011 0.009 O17 0.038 0.035 0.026 0.006 0.004 0.001 O18 0.045 0.042 0.018 0.006 0.002 0.001 O19 0.035 0.033 0.027 0.005 -0.001 0.001 O20 0.034 0.040 0.023 0.007 0.001 -0.002 O21 0.047 0.036 0.030 0.002 -0.009 -0.004 O100 0.138 0.068 0.037 0.024 -0.052 -0.064 O22 0.052 0.035 0.025 0.000 -0.011 0.006 O23 0.057 0.059 0.042 0.002 -0.006 -0.005 O24 0.054 0.087 0.081 0.043 0.003 0.009 O25 0.079 0.049 0.051 0.012 0.002 0.016 O26 0.060 0.048 0.041 -0.010 0.016 0.001 O27 0.115 0.040 0.058 -0.007 0.022 0.005 O28 0.139 0.138 0.034 -0.001 0.013 0.077 O29 0.079 0.069 0.043 0.019 -0.009 -0.005 O30 0.048 0.091 0.039 0.003 0.005 -0.009 O31 0.036 0.060 0.044 0.011 0.002 -0.001 O32 0.063 0.056 0.082 0.026 0.000 -0.010 O33 0.069 0.057 0.130 -0.043 -0.022 -0.006 O34 0.071 0.064 0.122 0.027 -0.030 -0.005 O35 0.125 0.267 0.051 -0.010 0.002 -0.085 O36 0.060 0.048 0.035 0.001 -0.007 0.015 O37 0.052 0.046 0.037 -0.001 -0.003 0.002 O38 0.069 0.043 0.040 0.009 0.002 0.004 O39 0.063 0.051 0.045 0.008 0.011 -0.015 O40 0.055 0.049 0.045 0.015 0.003 0.008 O41 0.049 0.054 0.049 0.012 0.014 0.007 O42 0.055 0.054 0.036 -0.003 0.015 0.000 O43 0.064 0.045 0.031 0.005 0.009 -0.002 O44 0.056 0.051 0.044 0.016 0.004 0.004 O45 0.071 0.052 0.041 -0.016 0.011 -0.001 O46 0.068 0.091 0.095 -0.035 -0.022 0.030 O47 0.184 0.053 0.051 0.005 0.049 0.011 O48 0.049 0.037 0.045 -0.002 -0.006 -0.002 O49 0.059 0.040 0.037 -0.003 -0.006 0.000 O50 0.048 0.046 0.044 0.003 -0.009 -0.001 O51 0.048 0.051 0.042 -0.002 0.014 0.005 O52 0.052 0.062 0.034 -0.001 0.011 0.006 O53 0.047 0.049 0.038 0.000 0.004 0.004 O54 0.096 0.038 0.039 0.002 0.019 0.019 O55 0.055 0.094 0.057 -0.031 -0.016 0.011 O56 0.049 0.036 0.073 0.014 -0.006 -0.035 O54' 0.079 0.044 0.037 0.007 -0.006 0.024 O55' 0.103 0.123 0.036 -0.024 -0.027 0.074 O56' 0.091 0.056 0.121 0.034 0.032 -0.013 O57 0.063 0.074 0.037 0.007 -0.003 0.019 O58 0.080 0.056 0.068 0.016 0.002 -0.002 O59 0.086 0.100 0.007 -0.006 -0.003 0.026 O58' 0.089 0.050 0.039 -0.007 0.021 -0.004 O57' 0.206 0.057 0.037 -0.006 -0.021 -0.066 O59' 0.062 0.164 0.059 0.052 -0.010 -0.029 O60 0.150 0.122 0.044 -0.015 0.039 -0.061 O61 0.065 0.042 0.086 -0.001 -0.001 0.009 O62 0.064 0.050 0.060 0.008 0.018 0.005 O63 0.079 0.083 0.125 0.039 0.056 0.049 O64 0.078 0.098 0.055 0.012 0.021 -0.026 O64' 0.065 0.050 0.044 0.012 -0.002 -0.025 O63' 0.076 0.050 0.070 0.005 0.024 -0.008 O65 0.060 0.052 0.051 0.012 0.006 -0.006 C1 0.032 0.051 0.058 0.015 0.005 -0.006 C2 0.052 0.056 0.055 0.006 0.011 -0.005 C3 0.050 0.063 0.065 0.010 0.018 0.001 C4 0.042 0.097 0.086 0.020 0.013 0.009 C5 0.046 0.098 0.061 -0.025 -0.004 -0.009 C6 0.036 0.074 0.058 -0.003 0.000 -0.010 C7 0.074 0.067 0.066 -0.012 0.023 -0.001 C8 0.044 0.145 0.116 -0.008 -0.007 0.012 C9 0.060 0.096 0.068 -0.035 0.005 -0.006 C11 0.042 0.065 0.041 -0.010 -0.010 0.000 C12 0.075 0.069 0.076 -0.015 -0.034 0.005 C13 0.064 0.092 0.089 -0.031 -0.041 0.018 C14 0.049 0.070 0.082 -0.041 -0.016 0.004 C15 0.070 0.056 0.077 -0.016 -0.001 -0.009 C16 0.079 0.057 0.071 0.006 -0.025 -0.006 C17 0.175 0.075 0.193 -0.021 -0.092 0.018 C18 0.084 0.079 0.140 -0.031 -0.058 -0.001 C19 0.161 0.073 0.246 0.040 -0.098 -0.006 C21 0.050 0.046 0.027 0.010 -0.008 -0.002 C22 0.056 0.084 0.034 0.008 -0.014 -0.002 C23 0.063 0.156 0.038 0.016 -0.001 0.000 C24 0.074 0.204 0.025 0.018 -0.015 -0.008 C25 0.050 0.155 0.036 0.010 -0.020 -0.009 C26 0.058 0.079 0.041 0.011 -0.004 -0.015 C27 0.053 0.146 0.043 0.020 0.011 -0.007 C28 0.124 0.343 0.029 0.032 -0.016 0.029 C29 0.048 0.106 0.057 0.014 0.000 -0.010 C31 0.047 0.042 0.040 0.005 0.009 0.004 C32 0.064 0.031 0.039 0.004 0.017 -0.002 C33 0.057 0.045 0.057 -0.003 0.013 -0.013 C34 0.054 0.049 0.045 0.008 0.017 0.000 C35 0.063 0.055 0.035 0.013 0.019 -0.002 C36 0.047 0.048 0.044 0.012 0.008 0.004 C37 0.089 0.047 0.039 -0.008 0.010 -0.011 C38 0.074 0.080 0.063 0.012 0.035 -0.010 C39 0.062 0.070 0.040 0.010 0.000 -0.002 C41 0.047 0.039 0.033 0.014 0.011 0.006 C42 0.048 0.051 0.048 0.011 0.019 0.004 C43 0.064 0.051 0.050 0.019 0.013 0.003 C44 0.072 0.070 0.053 0.015 0.011 -0.010 C45 0.095 0.078 0.032 0.016 0.001 -0.015 C46 0.065 0.059 0.043 0.000 0.007 -0.005 C47 0.063 0.041 0.048 0.006 0.007 0.004 C48 0.159 0.085 0.049 0.026 -0.001 -0.027 C49 0.118 0.071 0.051 0.018 0.004 -0.036 C51 0.072 0.038 0.041 -0.008 0.014 0.009 C52 0.114 0.052 0.048 -0.009 0.010 0.023 C53 0.128 0.055 0.044 -0.003 0.016 0.016 C54 0.064 0.053 0.057 -0.020 0.023 -0.009 C55 0.061 0.048 0.038 -0.015 0.011 -0.006 C56 0.054 0.050 0.036 -0.006 0.005 0.001 C57 0.327 0.099 0.037 0.015 0.029 0.113 C58 0.084 0.053 0.062 -0.013 0.032 0.002 C59 0.085 0.080 0.037 -0.008 -0.006 0.021 C61 0.047 0.042 0.049 0.004 -0.013 -0.003 C62 0.112 0.043 0.062 0.006 -0.016 -0.027 C63 0.139 0.055 0.105 0.024 -0.036 -0.044 C64 0.139 0.051 0.099 -0.016 -0.044 -0.020 C65 0.081 0.051 0.079 -0.021 -0.021 0.001 C66 0.053 0.051 0.057 -0.019 -0.020 0.008 C67 0.145 0.156 0.059 0.012 0.024 -0.078 C68 0.282 0.052 0.266 -0.030 -0.115 -0.039 C69 0.065 0.078 0.047 -0.017 -0.003 -0.014 C71 0.052 0.045 0.034 0.001 0.003 0.004 C72 0.051 0.061 0.058 0.006 0.020 0.005 C73 0.048 0.093 0.050 -0.016 0.018 0.001 C74 0.046 0.068 0.049 -0.008 0.007 0.008 C75 0.051 0.068 0.063 -0.008 0.003 0.019 C76 0.053 0.055 0.047 0.000 0.006 0.010 C77 0.063 0.069 0.060 0.026 0.016 0.000 C78 0.056 0.120 0.087 -0.018 0.018 0.019 C79 0.067 0.085 0.071 0.029 0.013 0.019 C151 0.082 0.352 0.162 -0.115 0.054 -0.147 C152 0.053 0.077 0.073 -0.011 0.005 0.022 C153 0.137 0.067 0.100 0.015 -0.065 -0.015 C154 0.099 0.050 0.081 0.000 -0.002 0.025 C155 0.093 0.120 0.136 -0.062 0.042 -0.062 C156 0.080 0.033 0.107 -0.008 0.037 -0.005 C157 0.017 0.039 0.453 0.076 0.048 -0.002 C158 0.143 0.258 0.175 0.186 0.066 0.067 _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 2.369(7) . ? Bi1 O4 2.399(7) 3_665 ? Bi1 O2 2.477(7) . ? Bi1 O22 2.579(8) 3_665 ? Bi1 O16 2.624(7) 3_665 ? Bi1 O1 2.6569(7) . ? Bi1 O8 2.668(8) . ? Bi1 Bi2 3.6266(7) . ? Bi1 Bi3 3.6651(8) 3_665 ? Bi2 O2 2.272(7) . ? Bi2 O4 2.313(7) . ? Bi2 O3 2.424(6) . ? Bi2 O22 2.464(7) . ? Bi2 O1 2.5360(5) . ? Bi2 O11 2.627(7) . ? Bi3 O22 2.260(7) 3_665 ? Bi3 O3 2.336(7) 3_665 ? Bi3 O4 2.503(6) . ? Bi3 O2 2.535(7) . ? Bi3 O1 2.5883(6) . ? Bi3 O20 2.595(7) . ? Bi3 O19 2.641(7) . ? Bi4 O2 2.083(6) . ? Bi4 O6 2.182(7) . ? Bi4 O7 2.389(8) . ? Bi4 O5 2.422(7) . ? Bi5 O6 2.114(7) . ? Bi5 O5 2.144(7) . ? Bi5 O20 2.157(7) . ? Bi5 O54 2.67(2) . ? Bi5 O54' 2.67(2) . ? Bi5 O23 2.681(9) . ? Bi6 O15 2.122(7) 3_665 ? Bi6 O6 2.146(7) . ? Bi6 O7 2.153(7) . ? Bi6 O52 2.647(8) . ? Bi6 O54' 2.69(2) . ? Bi6 O54 2.76(2) . ? Bi7 O9 2.083(9) . ? Bi7 O8 2.158(8) . ? Bi7 O7 2.192(7) . ? Bi7 O29 2.542(9) . ? Bi7 O51 2.729(8) . ? Bi8 O3 2.164(6) . ? Bi8 O10 2.300(7) . ? Bi8 O8 2.382(8) . ? Bi8 O9 2.434(13) . ? Bi8 O29 2.631(11) . ? Bi9 O9 2.135(9) . ? Bi9 O11 2.157(7) . ? Bi9 O10 2.235(7) . ? Bi9 O24 2.534(10) . ? Bi10 O100 2.100(8) . ? Bi10 O10 2.116(7) . ? Bi10 O13 2.154(7) . ? Bi10 O49 2.709(8) . ? Bi11 O22 2.086(7) . ? Bi11 O14 2.236(6) . ? Bi11 O13 2.320(7) . ? Bi11 O15 2.568(7) . ? Bi12 O12 2.120(7) . ? Bi12 O14 2.143(7) . ? Bi12 O13 2.155(6) . ? Bi12 O48 2.593(8) . ? Bi13 O14 2.099(7) . ? Bi13 O16 2.143(7) . ? Bi13 O15 2.144(7) . ? Bi13 O25 2.681(9) . ? Bi13 O45 2.730(9) . ? Bi14 O17 2.101(7) . ? Bi14 O16 2.127(7) . ? Bi14 O8 2.210(7) 3_665 ? Bi14 O26 2.608(9) . ? Bi15 O4 2.082(6) . ? Bi15 O18 2.286(7) . ? Bi15 O21 2.307(8) . ? Bi15 O17 2.429(7) . ? Bi15 O12 2.600(7) . ? Bi16 O17 2.131(7) . ? Bi16 O19 2.137(7) . ? Bi16 O18 2.170(7) . ? Bi16 O42 2.627(9) . ? Bi16 O36 2.662(8) . ? Bi17 O100 2.115(8) 3_665 ? Bi17 O20 2.161(7) . ? Bi17 O19 2.206(7) . ? Bi17 O27 2.649(10) . ? Bi17 O39 2.671(8) . ? Bi18 O5 2.131(7) . ? Bi18 O21 2.143(7) . ? Bi18 O18 2.145(7) . ? Bi18 O38 2.601(8) . ? Bi19 O21 2.108(7) . ? Bi19 O12 2.143(7) . ? Bi19 O11 2.161(7) . ? Bi19 O28 2.655(11) . ? Bi19 O48 2.748(8) . ? Bi20 O3 2.114(6) . ? Bi20 O10 2.295(7) . ? Bi20 O19 2.319(7) 3_665 ? Bi20 O40 2.674(9) 3_665 ? Bi20 O100 2.711(15) . ? S1 O30 1.447(10) . ? S1 O32 1.471(10) . ? S1 O31 1.483(8) . ? S1 C1 1.770(12) . ? S2 O35 1.402(14) . ? S2 O34 1.437(13) . ? S2 O33 1.467(13) . ? S2 C11 1.785(12) . ? S3 O37 1.459(9) . ? S3 O36 1.461(9) . ? S3 O38 1.471(9) . ? S3 C21 1.782(10) . ? S4 O41 1.446(9) . ? S4 O40 1.463(9) . ? S4 O39 1.469(10) . ? S4 C31 1.776(12) . ? S5 O42 1.443(8) . ? S5 O44 1.458(9) . ? S5 O43 1.465(9) . ? S5 C41 1.781(10) . ? S6 O47 1.449(11) . ? S6 O45 1.462(9) . ? S6 O46 1.478(12) . ? S6 C51 1.781(12) . ? S7 O50 1.447(9) . ? S7 O49 1.449(8) . ? S7 O48 1.459(9) . ? S7 C61 1.774(13) . ? S8 O53 1.451(9) . ? S8 O51 1.459(9) . ? S8 O52 1.474(8) . ? S8 C71 1.782(12) . ? S9 O55 1.45(2) . ? S9 O56 1.454(16) . ? S9 O54 1.46(2) . ? S9 C81 1.79(2) . ? S9' O55' 1.44(3) . ? S9' O54' 1.48(2) . ? S9' O56' 1.53(2) . ? S9' C81' 1.88(2) . ? S10 O57 1.37(3) . ? S10 O58 1.45(2) . ? S10 O59 1.49(2) . ? S10 C91 1.725(19) . ? S10' O59' 1.38(3) . ? S10' O58' 1.47(2) . ? S10' O57' 1.63(4) . ? S10' C91' 1.82(2) . ? S11 O60 1.4(2) . ? S11 O62 1.5(3) . ? S11 O61 1.5(3) . ? S11 C101 1.8(2) . ? S11' O60 1.4(2) . ? S11' O62 1.5(3) . ? S11' O61 1.5(3) . ? S11' C111 1.8(2) . ? S12 O63 1.32(3) . ? S12 O65 1.500(12) . ? S12 O64 1.53(3) . ? S12 C121 1.75(2) . ? S12' O64' 1.40(3) . ? S12' O65 1.46(2) . ? S12' O63' 1.58(3) . ? S12' C131 1.79(4) . ? O1 Bi2 2.5360(5) 3_665 ? O1 Bi3 2.5883(6) 3_665 ? O1 Bi1 2.6569(7) 3_665 ? O3 Bi3 2.336(7) 3_665 ? O4 Bi1 2.399(7) 3_665 ? O8 Bi14 2.210(7) 3_665 ? O15 Bi6 2.122(7) 3_665 ? O16 Bi1 2.624(7) 3_665 ? O19 Bi20 2.319(7) 3_665 ? O100 Bi17 2.115(8) 3_665 ? O22 Bi3 2.260(7) 3_665 ? O22 Bi1 2.579(8) 3_665 ? O40 Bi20 2.674(9) 3_665 ? C1 C6 1.408(19) . ? C1 C2 1.416(18) . ? C2 C3 1.41(2) . ? C2 C7 1.52(2) . ? C3 C4 1.39(2) . ? C4 C5 1.38(2) . ? C4 C8 1.53(2) . ? C5 C6 1.37(2) . ? C6 C9 1.55(2) . ? C11 C12 1.37(2) . ? C11 C16 1.40(2) . ? C12 C13 1.38(2) . ? C12 C17 1.52(3) . ? C13 C14 1.38(2) . ? C14 C15 1.35(2) . ? C14 C18 1.517(19) . ? C15 C16 1.39(2) . ? C16 C19 1.51(3) . ? C21 C26 1.401(17) . ? C21 C22 1.408(18) . ? C22 C23 1.406(18) . ? C22 C27 1.517(19) . ? C23 C24 1.40(2) . ? C24 C25 1.37(2) . ? C24 C28 1.50(2) . ? C25 C26 1.395(18) . ? C26 C29 1.543(19) . ? C31 C32 1.387(18) . ? C31 C36 1.428(17) . ? C32 C33 1.406(16) . ? C32 C37 1.517(17) . ? C33 C34 1.363(18) . ? C34 C35 1.389(19) . ? C34 C38 1.510(17) . ? C35 C36 1.395(16) . ? C36 C39 1.489(19) . ? C41 C46 1.400(18) . ? C41 C42 1.424(18) . ? C42 C43 1.406(16) . ? C42 C47 1.467(19) . ? C43 C44 1.38(2) . ? C44 C45 1.36(2) . ? C44 C48 1.53(2) . ? C45 C46 1.405(19) . ? C46 C49 1.46(2) . ? C51 C56 1.380(16) . ? C51 C52 1.44(2) . ? C52 C53 1.38(2) . ? C52 C57 1.51(2) . ? C53 C54 1.376(19) . ? C54 C55 1.39(2) . ? C54 C58 1.532(19) . ? C55 C56 1.400(17) . ? C56 C59 1.525(19) . ? C61 C62 1.403(19) . ? C61 C66 1.432(18) . ? C62 C63 1.39(2) . ? C62 C67 1.48(3) . ? C63 C64 1.39(3) . ? C64 C65 1.37(3) . ? C64 C68 1.54(2) . ? C65 C66 1.383(19) . ? C66 C69 1.51(2) . ? C71 C76 1.371(17) . ? C71 C72 1.421(17) . ? C72 C73 1.406(18) . ? C72 C77 1.495(19) . ? C73 C74 1.34(2) . ? C74 C75 1.40(2) . ? C74 C78 1.518(19) . ? C75 C76 1.430(18) . ? C76 C79 1.541(19) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C82 C87 1.538(6) . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C84 C88 1.538(6) . ? C85 C86 1.3900 . ? C86 C89 1.541(6) . ? C81' C82' 1.3900 . ? C81' C86' 1.3900 . ? C82' C83' 1.3900 . ? C82' C87' 1.540(6) . ? C83' C84' 1.3900 . ? C84' C85' 1.3900 . ? C84' C88' 1.537(6) . ? C85' C86' 1.3900 . ? C86' C89' 1.538(6) . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C92 C97 1.542(6) . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C94 C98 1.537(6) . ? C95 C96 1.3900 . ? C96 C99 1.538(6) . ? C91' C92' 1.3900 . ? C91' C96' 1.3900 . ? C92' C93' 1.3900 . ? C92' C97' 1.538(6) . ? C93' C94' 1.3900 . ? C94' C95' 1.3900 . ? C94' C98' 1.538(6) . ? C95' C96' 1.3900 . ? C96' C99' 1.539(6) . ? C101 C106 1.37(3) . ? C101 C102 1.42(2) . ? C102 C103 1.37(3) . ? C102 C107 1.53(3) . ? C103 C104 1.37(3) . ? C104 C105 1.41(4) . ? C104 C108 1.53(4) . ? C105 C106 1.38(4) . ? C106 C109 1.548(10) . ? C111 C116 1.36(3) . ? C111 C112 1.42(2) . ? C112 C113 1.37(3) . ? C112 C117 1.53(3) . ? C113 C114 1.37(3) . ? C114 C115 1.41(4) . ? C114 C118 1.52(4) . ? C115 C116 1.38(4) . ? C116 C119 1.547(13) . ? C121 C122 1.34(2) . ? C121 C126 1.44(4) . ? C122 C123 1.44(3) . ? C122 C127 1.549(10) . ? C123 C124 1.37(3) . ? C124 C125 1.38(4) . ? C124 C128 1.553(10) . ? C125 C126 1.34(4) . ? C126 C129 1.549(10) . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C132 C137 1.539(6) . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C134 C138 1.540(6) . ? C135 C136 1.3900 . ? C136 C139 1.538(6) . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C151 C157 1.4616 . ? C152 C153 1.3900 . ? C153 C154 1.3900 . ? C153 C158 1.4823 . ? C154 C155 1.3900 . ? C155 C156 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Bi1 O4 79.7(2) . 3_665 ? O3 Bi1 O2 77.4(2) . . ? O4 Bi1 O2 124.7(2) 3_665 . ? O3 Bi1 O22 124.1(2) . 3_665 ? O4 Bi1 O22 76.3(2) 3_665 3_665 ? O2 Bi1 O22 76.3(2) . 3_665 ? O3 Bi1 O16 117.8(2) . 3_665 ? O4 Bi1 O16 74.2(2) 3_665 3_665 ? O2 Bi1 O16 159.2(2) . 3_665 ? O22 Bi1 O16 102.9(2) 3_665 3_665 ? O3 Bi1 O1 63.25(15) . . ? O4 Bi1 O1 62.08(14) 3_665 . ? O2 Bi1 O1 62.61(15) . . ? O22 Bi1 O1 60.91(17) 3_665 . ? O16 Bi1 O1 135.59(17) 3_665 . ? O3 Bi1 O8 71.6(2) . . ? O4 Bi1 O8 109.8(2) 3_665 . ? O2 Bi1 O8 109.5(2) . . ? O22 Bi1 O8 164.3(2) 3_665 . ? O16 Bi1 O8 66.4(2) 3_665 . ? O1 Bi1 O8 134.81(16) . . ? O3 Bi1 Bi2 41.42(15) . . ? O4 Bi1 Bi2 97.58(15) 3_665 . ? O2 Bi1 Bi2 38.16(16) . . ? O22 Bi1 Bi2 93.32(16) 3_665 . ? O16 Bi1 Bi2 159.26(16) 3_665 . ? O1 Bi1 Bi2 44.353(11) . . ? O8 Bi1 Bi2 100.01(16) . . ? O3 Bi1 Bi3 38.50(16) . 3_665 ? O4 Bi1 Bi3 42.71(15) 3_665 3_665 ? O2 Bi1 Bi3 95.32(16) . 3_665 ? O22 Bi1 Bi3 96.99(17) 3_665 3_665 ? O16 Bi1 Bi3 105.37(16) 3_665 3_665 ? O1 Bi1 Bi3 44.911(12) . 3_665 ? O8 Bi1 Bi3 96.99(16) . 3_665 ? Bi2 Bi1 Bi3 59.201(13) . 3_665 ? O2 Bi2 O4 83.5(2) . . ? O2 Bi2 O3 80.4(2) . . ? O4 Bi2 O3 129.5(2) . . ? O2 Bi2 O22 131.2(2) . . ? O4 Bi2 O22 80.2(2) . . ? O3 Bi2 O22 75.6(2) . . ? O2 Bi2 O1 67.26(17) . . ? O4 Bi2 O1 65.11(15) . . ? O3 Bi2 O1 64.45(16) . . ? O22 Bi2 O1 64.13(17) . . ? O2 Bi2 O11 75.4(2) . . ? O4 Bi2 O11 110.9(2) . . ? O3 Bi2 O11 110.7(2) . . ? O22 Bi2 O11 153.1(2) . . ? O1 Bi2 O11 142.67(16) . . ? O2 Bi2 Bi3 100.97(17) . 3_665 ? O4 Bi2 Bi3 98.62(16) . 3_665 ? O3 Bi2 Bi3 39.91(16) . 3_665 ? O22 Bi2 Bi3 38.27(17) . 3_665 ? O1 Bi2 Bi3 45.935(12) . 3_665 ? O11 Bi2 Bi3 149.44(15) . 3_665 ? O2 Bi2 Bi1 42.34(17) . . ? O4 Bi2 Bi1 102.22(15) . . ? O3 Bi2 Bi1 40.27(16) . . ? O22 Bi2 Bi1 97.52(17) . . ? O1 Bi2 Bi1 47.087(13) . . ? O11 Bi2 Bi1 103.58(15) . . ? Bi3 Bi2 Bi1 60.933(13) 3_665 . ? O2 Bi2 Bi3 43.45(17) . . ? O4 Bi2 Bi3 42.81(16) . . ? O3 Bi2 Bi3 99.07(16) . . ? O22 Bi2 Bi3 99.71(18) . . ? O1 Bi2 Bi3 45.235(10) . . ? O11 Bi2 Bi3 104.81(16) . . ? Bi3 Bi2 Bi3 91.169(16) 3_665 . ? Bi1 Bi2 Bi3 62.138(13) . . ? O22 Bi3 O3 81.4(3) 3_665 3_665 ? O22 Bi3 O4 127.8(2) 3_665 . ? O3 Bi3 O4 78.3(2) 3_665 . ? O22 Bi3 O2 81.1(3) 3_665 . ? O3 Bi3 O2 127.5(2) 3_665 . ? O4 Bi3 O2 74.6(2) . . ? O22 Bi3 O1 66.00(18) 3_665 . ? O3 Bi3 O1 64.79(15) 3_665 . ? O4 Bi3 O1 61.81(14) . . ? O2 Bi3 O1 62.86(15) . . ? O22 Bi3 O20 75.9(2) 3_665 . ? O3 Bi3 O20 120.1(2) 3_665 . ? O4 Bi3 O20 154.0(2) . . ? O2 Bi3 O20 102.7(2) . . ? O1 Bi3 O20 140.64(15) . . ? O22 Bi3 O19 112.0(3) 3_665 . ? O3 Bi3 O19 71.8(2) 3_665 . ? O4 Bi3 O19 106.3(2) . . ? O2 Bi3 O19 159.3(2) . . ? O1 Bi3 O19 136.44(15) . . ? O20 Bi3 O19 67.1(2) . . ? O22 Bi3 Bi2 42.47(19) 3_665 3_665 ? O3 Bi3 Bi2 41.76(15) 3_665 3_665 ? O4 Bi3 Bi2 96.24(15) . 3_665 ? O2 Bi3 Bi2 98.12(15) . 3_665 ? O1 Bi3 Bi2 44.751(10) . 3_665 ? O20 Bi3 Bi2 109.68(16) . 3_665 ? O19 Bi3 Bi2 102.29(15) . 3_665 ? O22 Bi3 Bi20 90.5(2) 3_665 3_665 ? O3 Bi3 Bi20 33.34(15) 3_665 3_665 ? O4 Bi3 Bi20 97.54(16) . 3_665 ? O2 Bi3 Bi20 160.68(15) . 3_665 ? O1 Bi3 Bi20 97.83(2) . 3_665 ? O20 Bi3 Bi20 92.02(15) . 3_665 ? O19 Bi3 Bi20 39.59(15) . 3_665 ? Bi2 Bi3 Bi20 64.714(17) 3_665 3_665 ? O22 Bi3 Bi2 98.70(19) 3_665 . ? O3 Bi3 Bi2 97.60(16) 3_665 . ? O4 Bi3 Bi2 38.90(15) . . ? O2 Bi3 Bi2 38.06(16) . . ? O1 Bi3 Bi2 44.079(11) . . ? O20 Bi3 Bi2 139.92(15) . . ? O19 Bi3 Bi2 144.97(15) . . ? Bi2 Bi3 Bi2 88.831(16) 3_665 . ? Bi20 Bi3 Bi2 127.99(2) 3_665 . ? O22 Bi3 Bi1 100.51(18) 3_665 3_665 ? O3 Bi3 Bi1 39.16(17) 3_665 3_665 ? O4 Bi3 Bi1 40.53(16) . 3_665 ? O2 Bi3 Bi1 97.43(16) . 3_665 ? O1 Bi3 Bi1 46.445(13) . 3_665 ? O20 Bi3 Bi1 158.68(15) . 3_665 ? O19 Bi3 Bi1 95.78(15) . 3_665 ? Bi2 Bi3 Bi1 59.866(13) 3_665 3_665 ? Bi20 Bi3 Bi1 66.84(2) 3_665 3_665 ? Bi2 Bi3 Bi1 61.153(15) . 3_665 ? O2 Bi4 O6 89.3(3) . . ? O2 Bi4 O7 83.7(3) . . ? O6 Bi4 O7 68.3(2) . . ? O2 Bi4 O5 85.5(3) . . ? O6 Bi4 O5 67.0(2) . . ? O7 Bi4 O5 134.1(3) . . ? O2 Bi4 Bi6 97.89(19) . . ? O6 Bi4 Bi6 35.19(18) . . ? O7 Bi4 Bi6 36.79(17) . . ? O5 Bi4 Bi6 101.73(17) . . ? O2 Bi4 Bi5 95.24(19) . . ? O6 Bi4 Bi5 33.08(18) . . ? O7 Bi4 Bi5 101.31(18) . . ? O5 Bi4 Bi5 35.76(17) . . ? Bi6 Bi4 Bi5 66.346(12) . . ? O6 Bi5 O5 73.6(3) . . ? O6 Bi5 O20 86.8(3) . . ? O5 Bi5 O20 88.4(3) . . ? O6 Bi5 O54 69.5(5) . . ? O5 Bi5 O54 141.6(5) . . ? O20 Bi5 O54 99.4(5) . . ? O6 Bi5 O54' 66.6(5) . . ? O5 Bi5 O54' 140.2(5) . . ? O20 Bi5 O54' 88.2(5) . . ? O54 Bi5 O54' 11.4(6) . . ? O6 Bi5 O23 81.8(3) . . ? O5 Bi5 O23 82.6(3) . . ? O20 Bi5 O23 167.1(3) . . ? O54 Bi5 O23 82.3(5) . . ? O54' Bi5 O23 92.8(5) . . ? O6 Bi5 Bi4 34.28(19) . . ? O5 Bi5 Bi4 41.31(19) . . ? O20 Bi5 Bi4 96.23(18) . . ? O54 Bi5 Bi4 100.3(4) . . ? O54' Bi5 Bi4 99.8(4) . . ? O23 Bi5 Bi4 70.90(19) . . ? O15 Bi6 O6 86.5(3) 3_665 . ? O15 Bi6 O7 86.9(3) 3_665 . ? O6 Bi6 O7 73.5(3) . . ? O15 Bi6 O52 74.9(3) 3_665 . ? O6 Bi6 O52 157.3(3) . . ? O7 Bi6 O52 92.3(3) . . ? O15 Bi6 O54' 82.8(5) 3_665 . ? O6 Bi6 O54' 66.0(5) . . ? O7 Bi6 O54' 138.7(5) . . ? O52 Bi6 O54' 122.9(5) . . ? O15 Bi6 O54 93.8(5) 3_665 . ? O6 Bi6 O54 67.3(5) . . ? O7 Bi6 O54 140.6(5) . . ? O52 Bi6 O54 125.9(5) . . ? O54' Bi6 O54 11.1(6) . . ? O15 Bi6 Bi4 99.1(2) 3_665 . ? O6 Bi6 Bi4 35.86(18) . . ? O7 Bi6 Bi4 41.6(2) . . ? O52 Bi6 Bi4 133.9(2) . . ? O54' Bi6 Bi4 100.9(4) . . ? O54 Bi6 Bi4 99.8(4) . . ? O9 Bi7 O8 80.5(4) . . ? O9 Bi7 O7 79.5(4) . . ? O8 Bi7 O7 82.5(3) . . ? O9 Bi7 O29 80.6(5) . . ? O8 Bi7 O29 73.0(3) . . ? O7 Bi7 O29 150.6(3) . . ? O9 Bi7 O51 158.2(3) . . ? O8 Bi7 O51 77.8(3) . . ? O7 Bi7 O51 95.1(3) . . ? O29 Bi7 O51 95.3(3) . . ? O9 Bi7 Bi8 45.7(4) . . ? O8 Bi7 Bi8 44.5(2) . . ? O7 Bi7 Bi8 100.5(2) . . ? O29 Bi7 Bi8 50.4(2) . . ? O51 Bi7 Bi8 116.15(19) . . ? Bi20 Bi8 O3 76.4(2) . . ? Bi20 Bi8 O10 80.56(19) . . ? O3 Bi8 O10 84.4(3) . . ? Bi20 Bi8 O8 134.3(2) . . ? O3 Bi8 O8 81.0(3) . . ? O10 Bi8 O8 136.0(2) . . ? Bi20 Bi8 O9 145.7(2) . . ? O3 Bi8 O9 86.1(3) . . ? O10 Bi8 O9 68.5(3) . . ? O8 Bi8 O9 69.4(3) . . ? Bi20 Bi8 O29 134.0(2) . . ? O3 Bi8 O29 147.0(3) . . ? O10 Bi8 O29 109.9(3) . . ? O8 Bi8 O29 68.1(3) . . ? O9 Bi8 O29 72.9(3) . . ? Bi20 Bi8 Bi7 173.67(11) . . ? O3 Bi8 Bi7 100.26(18) . . ? O10 Bi8 Bi7 104.61(17) . . ? O8 Bi8 Bi7 39.42(18) . . ? O9 Bi8 Bi7 37.8(2) . . ? O29 Bi8 Bi7 48.1(2) . . ? Bi20 Bi8 Bi9 117.21(10) . . ? O3 Bi8 Bi9 96.07(18) . . ? O10 Bi8 Bi9 36.81(17) . . ? O8 Bi8 Bi9 104.18(18) . . ? O9 Bi8 Bi9 35.1(2) . . ? O29 Bi8 Bi9 81.3(2) . . ? Bi7 Bi8 Bi9 68.225(17) . . ? O9 Bi9 O11 85.9(4) . . ? O9 Bi9 O10 75.1(4) . . ? O11 Bi9 O10 86.6(3) . . ? O9 Bi9 O24 82.6(5) . . ? O11 Bi9 O24 80.7(3) . . ? O10 Bi9 O24 155.0(3) . . ? O9 Bi9 Bi8 41.0(4) . . ? O11 Bi9 Bi8 98.70(19) . . ? O10 Bi9 Bi8 38.05(18) . . ? O24 Bi9 Bi8 123.0(3) . . ? O100 Bi10 O10 83.4(4) . . ? O100 Bi10 O13 76.3(3) . . ? O10 Bi10 O13 86.8(3) . . ? O100 Bi10 O49 157.9(3) . . ? O10 Bi10 O49 76.8(3) . . ? O13 Bi10 O49 92.6(3) . . ? O100 Bi10 Bi20 51.3(4) . . ? O10 Bi10 Bi20 39.94(19) . . ? O13 Bi10 Bi20 99.63(17) . . ? O49 Bi10 Bi20 113.76(18) . . ? O22 Bi11 O14 88.9(3) . . ? O22 Bi11 O13 85.8(3) . . ? O14 Bi11 O13 69.3(2) . . ? O22 Bi11 O15 81.8(3) . . ? O14 Bi11 O15 65.3(2) . . ? O13 Bi11 O15 133.0(2) . . ? O22 Bi11 Bi12 97.58(19) . . ? O14 Bi11 Bi12 35.66(18) . . ? O13 Bi11 Bi12 36.55(16) . . ? O15 Bi11 Bi12 100.73(15) . . ? O22 Bi11 Bi13 94.4(2) . . ? O14 Bi11 Bi13 32.17(18) . . ? O13 Bi11 Bi13 101.33(16) . . ? O15 Bi11 Bi13 35.66(15) . . ? Bi12 Bi11 Bi13 66.031(12) . . ? O12 Bi12 O14 86.7(3) . . ? O12 Bi12 O13 87.4(3) . . ? O14 Bi12 O13 74.2(2) . . ? O12 Bi12 O48 75.2(3) . . ? O14 Bi12 O48 157.6(3) . . ? O13 Bi12 O48 91.7(3) . . ? O12 Bi12 Bi11 98.07(19) . . ? O14 Bi12 Bi11 37.47(17) . . ? O13 Bi12 Bi11 39.88(19) . . ? O48 Bi12 Bi11 131.53(18) . . ? O14 Bi13 O16 86.4(3) . . ? O14 Bi13 O15 75.8(3) . . ? O16 Bi13 O15 86.7(3) . . ? O14 Bi13 O25 82.5(3) . . ? O16 Bi13 O25 164.2(3) . . ? O15 Bi13 O25 79.8(3) . . ? O14 Bi13 O45 69.0(3) . . ? O16 Bi13 O45 98.0(3) . . ? O15 Bi13 O45 144.0(3) . . ? O25 Bi13 O45 88.4(3) . . ? O14 Bi13 Bi11 34.56(18) . . ? O16 Bi13 Bi11 97.35(18) . . ? O15 Bi13 Bi11 44.28(19) . . ? O25 Bi13 Bi11 67.3(2) . . ? O45 Bi13 Bi11 99.82(19) . . ? O17 Bi14 O16 80.4(3) . . ? O17 Bi14 O8 82.9(3) . 3_665 ? O16 Bi14 O8 83.8(3) . 3_665 ? O17 Bi14 O26 77.7(3) . . ? O16 Bi14 O26 77.9(3) . . ? O8 Bi14 O26 155.2(3) 3_665 . ? O4 Bi15 O18 88.7(2) . . ? O4 Bi15 O21 87.1(3) . . ? O18 Bi15 O21 67.2(3) . . ? O4 Bi15 O17 82.3(2) . . ? O18 Bi15 O17 66.0(3) . . ? O21 Bi15 O17 132.1(3) . . ? O4 Bi15 O12 78.6(2) . . ? O18 Bi15 O12 130.7(2) . . ? O21 Bi15 O12 64.8(2) . . ? O17 Bi15 O12 153.8(2) . . ? O4 Bi15 Bi18 100.87(18) . . ? O18 Bi15 Bi18 35.84(19) . . ? O21 Bi15 Bi18 35.93(18) . . ? O17 Bi15 Bi18 101.02(16) . . ? O12 Bi15 Bi18 100.06(16) . . ? O4 Bi15 Bi16 95.32(18) . . ? O18 Bi15 Bi16 34.46(19) . . ? O21 Bi15 Bi16 101.32(18) . . ? O17 Bi15 Bi16 34.53(16) . . ? O12 Bi15 Bi16 164.83(16) . . ? Bi18 Bi15 Bi16 67.197(12) . . ? O4 Bi15 Bi19 92.27(19) . . ? O18 Bi15 Bi19 99.41(19) . . ? O21 Bi15 Bi19 32.52(19) . . ? O17 Bi15 Bi19 164.36(17) . . ? O12 Bi15 Bi19 35.31(16) . . ? Bi18 Bi15 Bi19 65.491(12) . . ? Bi16 Bi15 Bi19 132.673(15) . . ? O17 Bi16 O19 88.1(3) . . ? O17 Bi16 O18 73.4(3) . . ? O19 Bi16 O18 84.5(3) . . ? O17 Bi16 O42 81.1(3) . . ? O19 Bi16 O42 79.8(3) . . ? O18 Bi16 O42 150.3(3) . . ? O17 Bi16 O36 156.4(3) . . ? O19 Bi16 O36 74.6(3) . . ? O18 Bi16 O36 88.8(3) . . ? O42 Bi16 O36 110.8(3) . . ? O17 Bi16 Bi15 40.26(19) . . ? O19 Bi16 Bi15 97.56(18) . . ? O18 Bi16 Bi15 36.6(2) . . ? O42 Bi16 Bi15 121.2(2) . . ? O36 Bi16 Bi15 125.2(2) . . ? O100 Bi17 O20 84.2(3) 3_665 . ? O100 Bi17 O19 77.8(4) 3_665 . ? O20 Bi17 O19 83.1(3) . . ? O100 Bi17 O27 78.5(5) 3_665 . ? O20 Bi17 O27 80.3(3) . . ? O19 Bi17 O27 152.2(3) . . ? O100 Bi17 O39 93.1(4) 3_665 . ? O20 Bi17 O39 161.1(3) . . ? O19 Bi17 O39 78.1(3) . . ? O27 Bi17 O39 117.6(3) . . ? O100 Bi17 Bi20 47.1(4) 3_665 3_665 ? O20 Bi17 Bi20 99.06(18) . 3_665 ? O19 Bi17 Bi20 37.01(18) . 3_665 ? O27 Bi17 Bi20 125.0(3) . 3_665 ? O39 Bi17 Bi20 66.3(2) . 3_665 ? O5 Bi18 O21 84.3(3) . . ? O5 Bi18 O18 87.8(3) . . ? O21 Bi18 O18 72.7(3) . . ? O5 Bi18 O38 75.0(3) . . ? O21 Bi18 O38 155.1(3) . . ? O18 Bi18 O38 92.5(3) . . ? O5 Bi18 Bi15 99.9(2) . . ? O21 Bi18 Bi15 39.2(2) . . ? O18 Bi18 Bi15 38.6(2) . . ? O38 Bi18 Bi15 131.0(2) . . ? O21 Bi19 O12 76.8(3) . . ? O21 Bi19 O11 86.1(3) . . ? O12 Bi19 O11 86.8(3) . . ? O21 Bi19 O28 78.1(4) . . ? O12 Bi19 O28 78.8(4) . . ? O11 Bi19 O28 160.7(4) . . ? O21 Bi19 O48 148.3(3) . . ? O12 Bi19 O48 71.5(3) . . ? O11 Bi19 O48 93.1(3) . . ? O28 Bi19 O48 94.5(3) . . ? O21 Bi19 Bi15 36.0(2) . . ? O12 Bi19 Bi15 44.53(19) . . ? O11 Bi19 Bi15 98.61(19) . . ? O28 Bi19 Bi15 62.1(4) . . ? O48 Bi19 Bi15 113.50(17) . . ? Bi8 Bi20 O3 84.2(2) . . ? Bi8 Bi20 O10 81.3(2) . . ? O3 Bi20 O10 85.6(3) . . ? Bi8 Bi20 O19 143.2(2) . 3_665 ? O3 Bi20 O19 82.6(2) . 3_665 ? O10 Bi20 O19 131.4(3) . 3_665 ? Bi8 Bi20 O40 107.2(2) . 3_665 ? O3 Bi20 O40 153.0(3) . 3_665 ? O10 Bi20 O40 72.4(3) . 3_665 ? O19 Bi20 O40 100.0(3) 3_665 3_665 ? Bi8 Bi20 O100 148.1(2) . . ? O3 Bi20 O100 86.6(3) . . ? O10 Bi20 O100 67.6(2) . . ? O19 Bi20 O100 64.8(2) 3_665 . ? O40 Bi20 O100 70.7(3) 3_665 . ? Bi8 Bi20 Bi10 115.45(10) . . ? O3 Bi20 Bi10 100.70(19) . . ? O10 Bi20 Bi10 36.29(17) . . ? O19 Bi20 Bi10 100.74(18) 3_665 . ? O40 Bi20 Bi10 52.28(19) 3_665 . ? O100 Bi20 Bi10 37.22(17) . . ? Bi8 Bi20 Bi3 118.92(10) . 3_665 ? O3 Bi20 Bi3 37.40(18) . 3_665 ? O10 Bi20 Bi3 103.60(18) . 3_665 ? O19 Bi20 Bi3 46.54(17) 3_665 3_665 ? O40 Bi20 Bi3 132.73(19) 3_665 3_665 ? O100 Bi20 Bi3 64.89(18) . 3_665 ? Bi10 Bi20 Bi3 96.14(3) . 3_665 ? Bi8 Bi20 Bi17 176.89(10) . 3_665 ? O3 Bi20 Bi17 97.38(19) . 3_665 ? O10 Bi20 Bi17 101.46(18) . 3_665 ? O19 Bi20 Bi17 34.93(17) 3_665 3_665 ? O40 Bi20 Bi17 72.55(19) 3_665 3_665 ? O100 Bi20 Bi17 34.89(17) . 3_665 ? Bi10 Bi20 Bi17 66.97(2) . 3_665 ? Bi3 Bi20 Bi17 61.97(2) 3_665 3_665 ? O30 S1 O32 111.2(7) . . ? O30 S1 O31 109.8(5) . . ? O32 S1 O31 110.6(6) . . ? O30 S1 C1 109.9(6) . . ? O32 S1 C1 108.6(6) . . ? O31 S1 C1 106.6(5) . . ? O35 S2 O34 113.5(11) . . ? O35 S2 O33 109.0(11) . . ? O34 S2 O33 109.0(7) . . ? O35 S2 C11 109.2(8) . . ? O34 S2 C11 107.2(7) . . ? O33 S2 C11 108.8(7) . . ? O37 S3 O36 111.6(5) . . ? O37 S3 O38 110.5(5) . . ? O36 S3 O38 110.0(5) . . ? O37 S3 C21 109.8(5) . . ? O36 S3 C21 107.7(5) . . ? O38 S3 C21 107.1(5) . . ? O41 S4 O40 109.8(5) . . ? O41 S4 O39 111.8(6) . . ? O40 S4 O39 111.4(6) . . ? O41 S4 C31 108.7(5) . . ? O40 S4 C31 106.7(6) . . ? O39 S4 C31 108.3(5) . . ? O42 S5 O44 111.3(5) . . ? O42 S5 O43 109.1(5) . . ? O44 S5 O43 111.8(5) . . ? O42 S5 C41 107.4(5) . . ? O44 S5 C41 108.1(5) . . ? O43 S5 C41 109.0(5) . . ? O47 S6 O45 110.9(7) . . ? O47 S6 O46 113.7(9) . . ? O45 S6 O46 108.9(6) . . ? O47 S6 C51 107.3(6) . . ? O45 S6 C51 110.6(6) . . ? O46 S6 C51 105.3(7) . . ? O50 S7 O49 112.6(5) . . ? O50 S7 O48 110.5(5) . . ? O49 S7 O48 109.9(5) . . ? O50 S7 C61 107.3(5) . . ? O49 S7 C61 108.8(5) . . ? O48 S7 C61 107.6(6) . . ? O53 S8 O51 112.5(5) . . ? O53 S8 O52 109.9(5) . . ? O51 S8 O52 111.0(5) . . ? O53 S8 C71 107.6(5) . . ? O51 S8 C71 108.3(5) . . ? O52 S8 C71 107.3(5) . . ? O55 S9 O56 111.8(14) . . ? O55 S9 O54 110.0(14) . . ? O56 S9 O54 111.4(14) . . ? O55 S9 C81 109.5(14) . . ? O56 S9 C81 109.0(13) . . ? O54 S9 C81 105.0(14) . . ? O55' S9' O54' 111.1(15) . . ? O55' S9' O56' 116.5(19) . . ? O54' S9' O56' 109.5(15) . . ? O55' S9' C81' 106.1(13) . . ? O54' S9' C81' 102.0(12) . . ? O56' S9' C81' 110.5(15) . . ? O57 S10 O58 105.6(16) . . ? O57 S10 O59 111.9(14) . . ? O58 S10 O59 112.5(13) . . ? O57 S10 C91 107.0(14) . . ? O58 S10 C91 107.8(13) . . ? O59 S10 C91 111.6(10) . . ? O59' S10' O58' 115.0(15) . . ? O59' S10' O57' 109(2) . . ? O58' S10' O57' 110.7(16) . . ? O59' S10' C91' 113.2(16) . . ? O58' S10' C91' 102.2(14) . . ? O57' S10' C91' 106.8(15) . . ? O60 S11 O62 111(10) . . ? O60 S11 O61 111(10) . . ? O62 S11 O61 110(10) . . ? O60 S11 C101 101(10) . . ? O62 S11 C101 117(10) . . ? O61 S11 C101 105(10) . . ? O60 S11' O62 111(10) . . ? O60 S11' O61 111(10) . . ? O62 S11' O61 110(10) . . ? O60 S11' C111 117(10) . . ? O62 S11' C111 100(10) . . ? O61 S11' C111 107(10) . . ? O63 S12 O65 113.5(15) . . ? O63 S12 O64 113.7(18) . . ? O65 S12 O64 104.3(12) . . ? O63 S12 C121 123.3(17) . . ? O65 S12 C121 106.4(8) . . ? O64 S12 C121 92.4(11) . . ? O64' S12' O65 117.6(17) . . ? O64' S12' O63' 106.5(19) . . ? O65 S12' O63' 106.2(15) . . ? O64' S12' C131 120.4(18) . . ? O65 S12' C131 116.4(18) . . ? O63' S12' C131 80.4(16) . . ? Bi2 O1 Bi2 180.00(2) 3_665 . ? Bi2 O1 Bi3 89.314(14) 3_665 . ? Bi2 O1 Bi3 90.686(14) . . ? Bi2 O1 Bi3 90.686(14) 3_665 3_665 ? Bi2 O1 Bi3 89.314(14) . 3_665 ? Bi3 O1 Bi3 180.00(3) . 3_665 ? Bi2 O1 Bi1 88.560(14) 3_665 3_665 ? Bi2 O1 Bi1 91.440(14) . 3_665 ? Bi3 O1 Bi1 88.645(14) . 3_665 ? Bi3 O1 Bi1 91.356(14) 3_665 3_665 ? Bi2 O1 Bi1 91.440(14) 3_665 . ? Bi2 O1 Bi1 88.560(14) . . ? Bi3 O1 Bi1 91.355(14) . . ? Bi3 O1 Bi1 88.644(14) 3_665 . ? Bi1 O1 Bi1 180.000(19) 3_665 . ? Bi4 O2 Bi2 123.4(3) . . ? Bi4 O2 Bi1 114.1(3) . . ? Bi2 O2 Bi1 99.5(2) . . ? Bi4 O2 Bi3 119.5(3) . . ? Bi2 O2 Bi3 98.5(2) . . ? Bi1 O2 Bi3 97.0(2) . . ? Bi20 O3 Bi8 19.44(6) . . ? Bi20 O3 Bi3 109.3(3) . 3_665 ? Bi8 O3 Bi3 127.2(3) . 3_665 ? Bi20 O3 Bi1 127.3(3) . . ? Bi8 O3 Bi1 110.9(3) . . ? Bi3 O3 Bi1 102.3(3) 3_665 . ? Bi20 O3 Bi2 116.9(3) . . ? Bi8 O3 Bi2 115.4(3) . . ? Bi3 O3 Bi2 98.3(2) 3_665 . ? Bi1 O3 Bi2 98.3(2) . . ? Bi15 O4 Bi2 120.5(3) . . ? Bi15 O4 Bi1 120.3(3) . 3_665 ? Bi2 O4 Bi1 104.2(2) . 3_665 ? Bi15 O4 Bi3 112.3(3) . . ? Bi2 O4 Bi3 98.3(2) . . ? Bi1 O4 Bi3 96.8(2) 3_665 . ? Bi18 O5 Bi5 125.9(3) . . ? Bi18 O5 Bi4 127.9(3) . . ? Bi5 O5 Bi4 102.9(3) . . ? Bi5 O6 Bi6 131.5(3) . . ? Bi5 O6 Bi4 112.6(3) . . ? Bi6 O6 Bi4 108.9(3) . . ? Bi6 O7 Bi7 129.3(4) . . ? Bi6 O7 Bi4 101.6(3) . . ? Bi7 O7 Bi4 116.4(3) . . ? Bi7 O8 Bi14 127.4(4) . 3_665 ? Bi7 O8 Bi8 96.1(3) . . ? Bi14 O8 Bi8 123.7(3) 3_665 . ? Bi7 O8 Bi1 109.2(3) . . ? Bi14 O8 Bi1 100.6(3) 3_665 . ? Bi8 O8 Bi1 95.2(3) . . ? Bi7 O9 Bi9 136.6(5) . . ? Bi7 O9 Bi8 96.5(5) . . ? Bi9 O9 Bi8 103.8(5) . . ? Bi10 O10 Bi9 127.1(3) . . ? Bi10 O10 Bi20 103.8(3) . . ? Bi9 O10 Bi20 123.2(3) . . ? Bi10 O10 Bi8 120.7(3) . . ? Bi9 O10 Bi8 105.1(3) . . ? Bi20 O10 Bi8 18.13(6) . . ? Bi9 O11 Bi19 127.2(3) . . ? Bi9 O11 Bi2 110.5(3) . . ? Bi19 O11 Bi2 106.0(3) . . ? Bi12 O12 Bi19 123.3(3) . . ? Bi12 O12 Bi15 128.8(3) . . ? Bi19 O12 Bi15 100.2(3) . . ? Bi10 O13 Bi12 131.8(3) . . ? Bi10 O13 Bi11 113.8(3) . . ? Bi12 O13 Bi11 103.6(3) . . ? Bi13 O14 Bi12 133.1(3) . . ? Bi13 O14 Bi11 113.3(3) . . ? Bi12 O14 Bi11 106.9(3) . . ? Bi6 O15 Bi13 124.2(3) 3_665 . ? Bi6 O15 Bi11 129.2(3) 3_665 . ? Bi13 O15 Bi11 100.1(3) . . ? Bi14 O16 Bi13 127.4(3) . . ? Bi14 O16 Bi1 104.3(3) . 3_665 ? Bi13 O16 Bi1 110.0(3) . 3_665 ? Bi14 O17 Bi16 131.6(3) . . ? Bi14 O17 Bi15 110.5(3) . . ? Bi16 O17 Bi15 105.2(3) . . ? Bi18 O18 Bi16 133.3(3) . . ? Bi18 O18 Bi15 105.6(3) . . ? Bi16 O18 Bi15 109.0(3) . . ? Bi16 O19 Bi17 123.2(3) . . ? Bi16 O19 Bi20 114.8(3) . 3_665 ? Bi17 O19 Bi20 108.1(3) . 3_665 ? Bi16 O19 Bi3 110.9(3) . . ? Bi17 O19 Bi3 101.2(3) . . ? Bi20 O19 Bi3 93.9(2) 3_665 . ? Bi5 O20 Bi17 125.3(3) . . ? Bi5 O20 Bi3 114.0(3) . . ? Bi17 O20 Bi3 103.9(3) . . ? Bi19 O21 Bi18 132.1(4) . . ? Bi19 O21 Bi15 111.4(3) . . ? Bi18 O21 Bi15 104.9(3) . . ? Bi10 O100 Bi17 138.3(4) . 3_665 ? Bi10 O100 Bi20 91.5(4) . . ? Bi17 O100 Bi20 98.0(5) 3_665 . ? Bi11 O22 Bi3 121.5(3) . 3_665 ? Bi11 O22 Bi2 117.4(3) . . ? Bi3 O22 Bi2 99.3(3) 3_665 . ? Bi11 O22 Bi1 117.4(3) . 3_665 ? Bi3 O22 Bi1 101.5(3) 3_665 3_665 ? Bi2 O22 Bi1 95.0(2) . 3_665 ? Bi7 O29 Bi8 81.5(3) . . ? S3 O36 Bi16 143.5(5) . . ? S3 O38 Bi18 140.4(6) . . ? S4 O39 Bi17 103.3(4) . . ? S4 O40 Bi20 120.2(5) . 3_665 ? S5 O42 Bi16 109.7(5) . . ? S6 O45 Bi13 148.9(6) . . ? S7 O48 Bi12 144.2(5) . . ? S7 O48 Bi19 106.1(4) . . ? Bi12 O48 Bi19 89.2(2) . . ? S7 O49 Bi10 139.4(5) . . ? S8 O51 Bi7 136.8(5) . . ? S8 O52 Bi6 143.8(5) . . ? S9 O54 Bi5 150.4(14) . . ? S9 O54 Bi6 112.4(11) . . ? Bi5 O54 Bi6 91.5(6) . . ? S9' O54' Bi5 137.6(11) . . ? S9' O54' Bi6 127.2(12) . . ? Bi5 O54' Bi6 92.9(6) . . ? S11' O60 S11 0(10) . . ? S11' O61 S11 0(10) . . ? S11' O62 S11 0(10) . . ? S12' O65 S12 5.1(10) . . ? C6 C1 C2 120.4(12) . . ? C6 C1 S1 117.7(10) . . ? C2 C1 S1 121.9(11) . . ? C3 C2 C1 118.0(13) . . ? C3 C2 C7 117.0(13) . . ? C1 C2 C7 124.9(13) . . ? C4 C3 C2 120.6(14) . . ? C5 C4 C3 119.4(15) . . ? C5 C4 C8 122.4(18) . . ? C3 C4 C8 118.1(16) . . ? C6 C5 C4 121.7(15) . . ? C5 C6 C1 119.2(13) . . ? C5 C6 C9 118.7(13) . . ? C1 C6 C9 121.9(12) . . ? C12 C11 C16 121.9(13) . . ? C12 C11 S2 119.0(11) . . ? C16 C11 S2 118.9(10) . . ? C11 C12 C13 117.3(16) . . ? C11 C12 C17 124.7(15) . . ? C13 C12 C17 117.9(17) . . ? C14 C13 C12 122.0(16) . . ? C15 C14 C13 119.6(13) . . ? C15 C14 C18 119.0(15) . . ? C13 C14 C18 121.4(15) . . ? C14 C15 C16 121.0(15) . . ? C15 C16 C11 118.0(14) . . ? C15 C16 C19 116.2(17) . . ? C11 C16 C19 125.5(16) . . ? C26 C21 C22 121.6(10) . . ? C26 C21 S3 116.3(9) . . ? C22 C21 S3 122.0(9) . . ? C23 C22 C21 117.9(12) . . ? C23 C22 C27 116.7(13) . . ? C21 C22 C27 125.4(11) . . ? C24 C23 C22 121.0(15) . . ? C25 C24 C23 119.1(13) . . ? C25 C24 C28 119.5(17) . . ? C23 C24 C28 121.4(17) . . ? C24 C25 C26 122.4(13) . . ? C25 C26 C21 118.0(12) . . ? C25 C26 C29 118.4(13) . . ? C21 C26 C29 123.7(12) . . ? C32 C31 C36 121.0(11) . . ? C32 C31 S4 117.7(9) . . ? C36 C31 S4 121.3(10) . . ? C31 C32 C33 118.2(11) . . ? C31 C32 C37 124.0(11) . . ? C33 C32 C37 117.8(12) . . ? C34 C33 C32 123.7(13) . . ? C33 C34 C35 116.2(11) . . ? C33 C34 C38 122.3(13) . . ? C35 C34 C38 121.5(12) . . ? C34 C35 C36 124.8(12) . . ? C35 C36 C31 116.1(12) . . ? C35 C36 C39 118.6(11) . . ? C31 C36 C39 125.3(11) . . ? C46 C41 C42 123.1(11) . . ? C46 C41 S5 120.8(10) . . ? C42 C41 S5 116.1(9) . . ? C43 C42 C41 115.6(12) . . ? C43 C42 C47 119.0(13) . . ? C41 C42 C47 125.5(11) . . ? C44 C43 C42 122.8(14) . . ? C45 C44 C43 118.8(13) . . ? C45 C44 C48 123.1(15) . . ? C43 C44 C48 118.1(15) . . ? C44 C45 C46 123.5(14) . . ? C41 C46 C45 116.1(13) . . ? C41 C46 C49 125.7(12) . . ? C45 C46 C49 118.2(13) . . ? C56 C51 C52 120.3(12) . . ? C56 C51 S6 119.3(10) . . ? C52 C51 S6 120.4(9) . . ? C53 C52 C51 117.2(13) . . ? C53 C52 C57 119.0(15) . . ? C51 C52 C57 123.7(13) . . ? C54 C53 C52 123.6(16) . . ? C53 C54 C55 117.7(13) . . ? C53 C54 C58 120.1(15) . . ? C55 C54 C58 122.0(12) . . ? C54 C55 C56 121.7(11) . . ? C51 C56 C55 119.2(12) . . ? C51 C56 C59 123.3(12) . . ? C55 C56 C59 117.6(11) . . ? C62 C61 C66 121.5(13) . . ? C62 C61 S7 120.8(11) . . ? C66 C61 S7 117.6(10) . . ? C63 C62 C61 117.0(17) . . ? C63 C62 C67 120.3(17) . . ? C61 C62 C67 122.6(15) . . ? C62 C63 C64 122.6(18) . . ? C65 C64 C63 119.0(15) . . ? C65 C64 C68 123(2) . . ? C63 C64 C68 118(2) . . ? C64 C65 C66 122.2(17) . . ? C65 C66 C61 117.5(15) . . ? C65 C66 C69 116.8(14) . . ? C61 C66 C69 125.6(12) . . ? C76 C71 C72 122.7(12) . . ? C76 C71 S8 121.9(10) . . ? C72 C71 S8 115.2(9) . . ? C73 C72 C71 116.5(13) . . ? C73 C72 C77 119.1(13) . . ? C71 C72 C77 124.4(12) . . ? C74 C73 C72 123.1(14) . . ? C73 C74 C75 119.4(12) . . ? C73 C74 C78 120.7(14) . . ? C75 C74 C78 119.8(14) . . ? C74 C75 C76 120.8(13) . . ? C71 C76 C75 117.4(13) . . ? C71 C76 C79 127.5(12) . . ? C75 C76 C79 115.0(12) . . ? C82 C81 C86 120.0 . . ? C82 C81 S9 117.8(14) . . ? C86 C81 S9 122.1(14) . . ? C81 C82 C83 120.0 . . ? C81 C82 C87 120.5(6) . . ? C83 C82 C87 119.4(6) . . ? C84 C83 C82 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 C88 120.2(6) . . ? C83 C84 C88 119.8(6) . . ? C84 C85 C86 120.0 . . ? C85 C86 C81 120.0 . . ? C85 C86 C89 119.7(6) . . ? C81 C86 C89 120.2(6) . . ? C82' C81' C86' 120.0 . . ? C82' C81' S9' 120.9(12) . . ? C86' C81' S9' 118.3(12) . . ? C83' C82' C81' 120.0 . . ? C83' C82' C87' 119.4(6) . . ? C81' C82' C87' 120.6(6) . . ? C82' C83' C84' 120.0 . . ? C83' C84' C85' 120.0 . . ? C83' C84' C88' 119.9(6) . . ? C85' C84' C88' 120.0(6) . . ? C84' C85' C86' 120.0 . . ? C85' C86' C81' 120.0 . . ? C85' C86' C89' 119.6(6) . . ? C81' C86' C89' 120.4(6) . . ? C92 C91 C96 120.0 . . ? C92 C91 S10 117.4(10) . . ? C96 C91 S10 122.0(10) . . ? C93 C92 C91 120.0 . . ? C93 C92 C97 119.4(6) . . ? C91 C92 C97 120.5(6) . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 C98 120.2(6) . . ? C93 C94 C98 119.8(6) . . ? C96 C95 C94 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 C99 119.6(6) . . ? C91 C96 C99 120.3(6) . . ? C92' C91' C96' 120.0 . . ? C92' C91' S10' 120.5(13) . . ? C96' C91' S10' 119.2(13) . . ? C91' C92' C93' 120.0 . . ? C91' C92' C97' 120.0(6) . . ? C93' C92' C97' 119.8(6) . . ? C92' C93' C94' 120.0 . . ? C95' C94' C93' 120.0 . . ? C95' C94' C98' 119.7(6) . . ? C93' C94' C98' 120.2(6) . . ? C94' C95' C96' 120.0 . . ? C95' C96' C91' 120.0 . . ? C95' C96' C99' 119.7(6) . . ? C91' C96' C99' 120.2(6) . . ? C106 C101 C102 119.5(19) . . ? C106 C101 S11 125(9) . . ? C102 C101 S11 116(9) . . ? C103 C102 C101 118.1(18) . . ? C103 C102 C107 119.1(19) . . ? C101 C102 C107 122.8(18) . . ? C102 C103 C104 123(2) . . ? C103 C104 C105 119(3) . . ? C103 C104 C108 122(2) . . ? C105 C104 C108 119(3) . . ? C106 C105 C104 119(3) . . ? C101 C106 C105 122(2) . . ? C101 C106 C109 123(3) . . ? C105 C106 C109 115(3) . . ? C116 C111 C112 119.7(19) . . ? C116 C111 S11' 121(9) . . ? C112 C111 S11' 119(9) . . ? C113 C112 C111 118.0(18) . . ? C113 C112 C117 119.4(19) . . ? C111 C112 C117 122.6(18) . . ? C112 C113 C114 123(2) . . ? C113 C114 C115 119(3) . . ? C113 C114 C118 122(2) . . ? C115 C114 C118 119(3) . . ? C116 C115 C114 119(3) . . ? C111 C116 C115 122(2) . . ? C111 C116 C119 123(3) . . ? C115 C116 C119 115(3) . . ? C122 C121 C126 117.1(19) . . ? C122 C121 S12 122.6(13) . . ? C126 C121 S12 120.4(14) . . ? C121 C122 C123 121.9(16) . . ? C121 C122 C127 122.5(17) . . ? C123 C122 C127 115.2(17) . . ? C124 C123 C122 118(2) . . ? C123 C124 C125 121(2) . . ? C123 C124 C128 120(2) . . ? C125 C124 C128 119(3) . . ? C126 C125 C124 121(4) . . ? C125 C126 C121 122(2) . . ? C125 C126 C129 122(3) . . ? C121 C126 C129 116(2) . . ? C132 C131 C136 120.0 . . ? C132 C131 S12' 119.7(18) . . ? C136 C131 S12' 116.8(18) . . ? C133 C132 C131 120.0 . . ? C133 C132 C137 119.8(6) . . ? C131 C132 C137 119.9(6) . . ? C132 C133 C134 120.0 . . ? C135 C134 C133 120.0 . . ? C135 C134 C138 120.1(6) . . ? C133 C134 C138 119.9(6) . . ? C136 C135 C134 120.0 . . ? C135 C136 C131 120.0 . . ? C135 C136 C139 119.9(6) . . ? C131 C136 C139 120.0(6) . . ? C152 C151 C156 120.0 . . ? C152 C151 C157 122.1 . . ? C156 C151 C157 117.2 . . ? C151 C152 C153 120.0 . . ? C154 C153 C152 120.0 . . ? C154 C153 C158 120.6 . . ? C152 C153 C158 118.7 . . ? C155 C154 C153 120.0 . . ? C154 C155 C156 120.0 . . ? C155 C156 C151 120.0 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 6.346 _refine_diff_density_min -5.552 _refine_diff_density_rms 0.253