# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 885528' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Bi2 Fe3 O12' _chemical_formula_sum 'C36 H24 Bi2 Fe3 O12' _chemical_formula_weight 1234.06 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.446(7) _cell_length_b 13.148(8) _cell_length_c 13.638(8) _cell_angle_alpha 104.612(11) _cell_angle_beta 110.110(10) _cell_angle_gamma 106.666(10) _cell_volume 1700.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160.0 _exptl_absorpt_coefficient_mu 11.633 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 2.56 _exptl_absorpt_correction_T_max 24.62 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6202 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6202 _reflns_number_gt 4464 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+0.3044P] 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 6202 _refine_ls_number_parameters 478 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _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 1.09668(5) 0.38215(5) 0.52099(5) 0.0446(2) Uani 1 1 d . . . Bi2 Bi 0.55808(5) 0.46065(4) 0.15730(4) 0.0412(2) Uani 1 1 d . . . Fe1 Fe 0.8953(3) 0.26053(19) 0.0505(2) 0.0507(6) Uani 1 1 d . . . Fe2 Fe 0.5625(2) 0.23778(18) 0.48286(18) 0.0443(5) Uani 1 1 d . . . Fe3 Fe 0.17623(18) 0.11627(16) -0.25622(15) 0.0325(4) Uani 1 1 d . . . O1 O 1.1259(12) 0.3140(10) 0.3481(10) 0.061(3) Uani 1 1 d . . . O2 O 0.9279(10) 0.2801(8) 0.3476(8) 0.043(2) Uani 1 1 d . . . O3 O 0.8027(10) 0.4984(9) 0.2099(8) 0.049(3) Uani 1 1 d . . . O4 O 0.6294(10) 0.3684(8) 0.0484(8) 0.047(2) Uani 1 1 d . . . O5 O 0.9321(10) 0.2893(8) 0.5639(8) 0.045(2) Uani 1 1 d . . . O6 O 0.9151(11) 0.4476(9) 0.5450(9) 0.051(3) Uani 1 1 d . . . O7 O 0.6041(11) 0.3617(10) 0.2613(9) 0.055(3) Uani 1 1 d . . . O8 O 0.4462(13) 0.4030(10) 0.2930(11) 0.071(3) Uani 1 1 d . . . O9 O 0.3700(11) 0.2925(9) 0.0519(8) 0.052(3) Uani 1 1 d . . . O10 O 0.3533(11) 0.4070(8) -0.0394(9) 0.052(3) Uani 1 1 d . . . O11 O 1.1150(10) 0.2117(8) 0.5122(8) 0.046(2) Uani 1 1 d . . . O12 O 1.2997(11) 0.3505(8) 0.6527(8) 0.046(2) Uani 1 1 d . . . C1 C 0.9293(19) 0.1962(14) 0.1739(14) 0.056(4) Uani 1 1 d . . . C2 C 0.991(2) 0.1633(15) 0.1037(16) 0.067(5) Uani 1 1 d . . . H2 H 1.0880 0.1797 0.1282 0.080 Uiso 1 1 calc R . . C3 C 0.883(2) 0.0983(17) -0.0088(17) 0.073(6) Uani 1 1 d . . . H3 H 0.8909 0.0615 -0.0768 0.087 Uiso 1 1 calc R . . C4 C 0.765(2) 0.0935(15) -0.0019(16) 0.069(5) Uani 1 1 d . . . H4 H 0.6758 0.0562 -0.0682 0.083 Uiso 1 1 calc R . . C5 C 0.785(2) 0.1521(14) 0.1009(14) 0.058(5) Uani 1 1 d . . . H5 H 0.7153 0.1607 0.1238 0.069 Uiso 1 1 calc R . . C6 C 0.8535(16) 0.4009(12) 0.0656(12) 0.045(4) Uani 1 1 d . . . C7 C 0.9929(19) 0.4327(15) 0.1212(16) 0.063(5) Uani 1 1 d . . . H7 H 1.0502 0.4783 0.2026 0.076 Uiso 1 1 calc R . . C8 C 1.038(2) 0.3903(16) 0.0476(18) 0.064(5) Uani 1 1 d . . . H8 H 1.1328 0.4006 0.0667 0.077 Uiso 1 1 calc R . . C9 C 0.928(2) 0.3282(19) -0.0591(18) 0.073(6) Uani 1 1 d . . . H9 H 0.9313 0.2880 -0.1286 0.088 Uiso 1 1 calc R . . C10 C 0.8139(18) 0.3387(14) -0.0505(14) 0.056(4) Uani 1 1 d . . . H10 H 0.7214 0.3048 -0.1127 0.067 Uiso 1 1 calc R . . C11 C 0.9990(16) 0.2691(13) 0.2970(14) 0.046(4) Uani 1 1 d . . . C12 C 0.7554(16) 0.4239(12) 0.1120(13) 0.046(4) Uani 1 1 d . . . C13 C 0.7570(15) 0.3325(13) 0.5948(11) 0.045(4) Uani 1 1 d . . . C14 C 0.6833(18) 0.3995(15) 0.6053(14) 0.062(5) Uani 1 1 d . . . H14 H 0.6981 0.4721 0.5944 0.074 Uiso 1 1 calc R . . C15 C 0.5851(18) 0.3437(15) 0.6353(14) 0.064(5) Uani 1 1 d . . . H15 H 0.5165 0.3694 0.6465 0.077 Uiso 1 1 calc R . . C16 C 0.5956(19) 0.2443(16) 0.6393(15) 0.063(5) Uani 1 1 d . . . H16 H 0.5367 0.1880 0.6560 0.076 Uiso 1 1 calc R . . C17 C 0.7065(17) 0.2359(14) 0.6202(14) 0.054(4) Uani 1 1 d . . . H17 H 0.7408 0.1759 0.6232 0.064 Uiso 1 1 calc R . . C18 C 0.4814(15) 0.2438(13) 0.3280(14) 0.050(4) Uani 1 1 d . . . C19 C 0.3762(16) 0.2044(15) 0.3577(16) 0.064(5) Uani 1 1 d . . . H19 H 0.3139 0.2403 0.3654 0.077 Uiso 1 1 calc R . . C20 C 0.378(2) 0.1011(18) 0.3755(19) 0.085(6) Uani 1 1 d . . . H20 H 0.3168 0.0528 0.3970 0.103 Uiso 1 1 calc R . . C21 C 0.486(2) 0.0821(15) 0.3535(16) 0.069(6) Uani 1 1 d . . . H21 H 0.5119 0.0182 0.3583 0.083 Uiso 1 1 calc R . . C22 C 0.5457(19) 0.1674(14) 0.3270(15) 0.060(4) Uani 1 1 d . . . H22 H 0.6227 0.1750 0.3089 0.072 Uiso 1 1 calc R . . C23 C 0.8704(13) 0.3587(11) 0.5634(10) 0.034(3) Uani 1 1 d U . . C24 C 0.5127(15) 0.3437(13) 0.2951(12) 0.045(4) Uani 1 1 d . . . C25 C 0.3063(14) 0.3131(12) -0.0320(11) 0.037(3) Uani 1 1 d . . . C26 C 0.1778(13) 0.2189(11) -0.1178(11) 0.036(3) Uani 1 1 d . . . C27 C 0.1217(14) 0.1047(13) -0.1318(12) 0.046(4) Uani 1 1 d . . . H27 H 0.1614 0.0740 -0.0766 0.055 Uiso 1 1 calc R . . C28 C 0.0116(13) 0.0398(11) -0.2320(12) 0.041(3) Uani 1 1 d . . . H28 H -0.0421 -0.0434 -0.2602 0.050 Uiso 1 1 calc R . . C29 C -0.0136(13) 0.1122(12) -0.2897(11) 0.037(3) Uani 1 1 d . . . H29 H -0.0881 0.0883 -0.3649 0.045 Uiso 1 1 calc R . . C30 C 0.0886(13) 0.2269(12) -0.2185(12) 0.042(3) Uani 1 1 d . . . H30 H 0.0971 0.2964 -0.2348 0.051 Uiso 1 1 calc R . . C31 C 0.3671(13) 0.1878(12) -0.2446(12) 0.038(3) Uani 1 1 d . . . H31 H 0.4379 0.2646 -0.1914 0.046 Uiso 1 1 calc R . . C32 C 0.2590(13) 0.1602(11) -0.3551(11) 0.032(3) Uani 1 1 d . . . C33 C 0.1791(15) 0.0413(11) -0.4055(11) 0.038(3) Uani 1 1 d . . . H33 H 0.1004 -0.0015 -0.4805 0.045 Uiso 1 1 calc R . . C34 C 0.2370(16) -0.0057(12) -0.3281(12) 0.045(4) Uani 1 1 d . . . H34 H 0.2002 -0.0872 -0.3396 0.054 Uiso 1 1 calc R . . C35 C 0.3501(15) 0.0844(12) -0.2271(14) 0.047(4) Uani 1 1 d . . . H35 H 0.4059 0.0758 -0.1595 0.057 Uiso 1 1 calc R . . C36 C 1.2248(13) 0.2476(12) 0.6004(11) 0.035(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0342(3) 0.0366(3) 0.0588(4) 0.0260(3) 0.0113(3) 0.0144(3) Bi2 0.0421(3) 0.0369(3) 0.0324(3) 0.0088(2) 0.0064(2) 0.0170(3) Fe1 0.0782(17) 0.0450(13) 0.0561(13) 0.0294(11) 0.0451(13) 0.0343(12) Fe2 0.0430(12) 0.0423(12) 0.0522(12) 0.0219(10) 0.0238(10) 0.0177(10) Fe3 0.0309(10) 0.0306(10) 0.0339(10) 0.0130(8) 0.0107(8) 0.0143(8) O1 0.068(8) 0.076(8) 0.078(8) 0.053(7) 0.044(7) 0.047(7) O2 0.046(6) 0.040(6) 0.052(6) 0.019(5) 0.031(5) 0.019(5) O3 0.045(6) 0.048(6) 0.047(6) 0.014(5) 0.016(5) 0.019(5) O4 0.045(6) 0.033(5) 0.043(6) 0.000(4) 0.012(5) 0.012(5) O5 0.044(6) 0.044(6) 0.048(6) 0.025(5) 0.018(5) 0.014(5) O6 0.049(6) 0.046(6) 0.060(7) 0.023(5) 0.023(5) 0.021(5) O7 0.045(6) 0.080(8) 0.058(7) 0.054(6) 0.017(5) 0.034(6) O8 0.071(8) 0.054(7) 0.099(10) 0.030(7) 0.042(7) 0.037(7) O9 0.062(7) 0.045(6) 0.035(5) 0.026(5) 0.003(5) 0.020(5) O10 0.057(7) 0.035(6) 0.050(6) 0.022(5) 0.006(5) 0.015(5) O11 0.046(6) 0.032(5) 0.039(5) 0.011(4) -0.001(5) 0.013(5) O12 0.061(7) 0.032(6) 0.035(5) 0.014(4) 0.014(5) 0.013(5) C1 0.084(13) 0.051(10) 0.062(10) 0.044(9) 0.039(10) 0.040(9) C2 0.125(17) 0.061(11) 0.080(13) 0.053(10) 0.077(13) 0.066(12) C3 0.14(2) 0.070(13) 0.077(13) 0.053(11) 0.076(15) 0.074(14) C4 0.091(15) 0.048(11) 0.056(11) 0.020(9) 0.028(11) 0.017(10) C5 0.104(15) 0.057(10) 0.059(10) 0.040(9) 0.053(11) 0.057(11) C6 0.061(10) 0.032(8) 0.048(8) 0.023(7) 0.026(8) 0.020(7) C7 0.069(12) 0.056(11) 0.067(11) 0.036(9) 0.023(10) 0.028(9) C8 0.081(13) 0.072(12) 0.103(15) 0.060(12) 0.071(13) 0.055(11) C9 0.113(17) 0.104(16) 0.085(14) 0.078(13) 0.080(14) 0.073(14) C10 0.073(11) 0.064(11) 0.049(9) 0.035(8) 0.032(9) 0.036(9) C11 0.046(9) 0.048(9) 0.064(10) 0.036(8) 0.035(8) 0.024(8) C12 0.055(10) 0.027(8) 0.054(9) 0.022(7) 0.016(8) 0.021(7) C13 0.045(8) 0.060(10) 0.032(7) 0.029(7) 0.005(7) 0.032(8) C14 0.063(11) 0.045(10) 0.062(11) -0.001(8) 0.025(9) 0.025(9) C15 0.065(11) 0.063(11) 0.061(10) 0.006(9) 0.048(10) 0.013(9) C16 0.067(12) 0.063(12) 0.064(11) 0.024(9) 0.033(10) 0.028(10) C17 0.059(10) 0.055(10) 0.064(10) 0.040(9) 0.032(9) 0.025(8) C18 0.039(8) 0.039(9) 0.052(9) 0.005(7) 0.018(7) 0.003(7) C19 0.036(9) 0.059(12) 0.081(13) 0.014(10) 0.025(9) 0.012(8) C20 0.056(12) 0.074(15) 0.089(15) 0.018(12) 0.027(11) -0.004(10) C21 0.070(12) 0.035(9) 0.078(13) 0.016(9) 0.006(10) 0.027(9) C22 0.078(12) 0.041(9) 0.064(11) 0.019(8) 0.038(10) 0.023(9) C23 0.041(6) 0.040(6) 0.024(5) 0.023(5) 0.004(5) 0.024(5) C24 0.034(8) 0.055(10) 0.043(8) 0.028(7) 0.005(7) 0.021(7) C25 0.037(8) 0.036(8) 0.037(7) 0.017(6) 0.016(6) 0.014(6) C26 0.035(7) 0.036(8) 0.029(7) 0.011(6) 0.008(6) 0.013(6) C27 0.036(8) 0.049(9) 0.043(8) 0.029(7) 0.012(7) 0.000(7) C28 0.030(7) 0.027(7) 0.055(9) 0.010(7) 0.013(7) 0.007(6) C29 0.032(7) 0.048(8) 0.035(7) 0.015(6) 0.017(6) 0.019(6) C30 0.028(7) 0.035(8) 0.047(8) 0.008(6) 0.006(6) 0.012(6) C31 0.024(7) 0.035(8) 0.046(8) 0.015(6) 0.011(6) 0.007(6) C32 0.036(7) 0.034(7) 0.035(7) 0.014(6) 0.020(6) 0.020(6) C33 0.052(8) 0.024(7) 0.036(7) 0.006(6) 0.019(7) 0.019(6) C34 0.068(10) 0.034(8) 0.056(9) 0.023(7) 0.037(8) 0.035(8) C35 0.045(9) 0.044(9) 0.070(10) 0.028(8) 0.033(8) 0.027(7) C36 0.030(7) 0.040(8) 0.039(7) 0.011(6) 0.022(6) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O2 2.213(10) . ? Bi1 O5 2.276(10) . ? Bi1 O11 2.287(9) . ? Bi1 O1 2.475(11) . ? Bi1 O6 2.552(10) . ? Bi1 O12 2.619(10) . ? Bi1 O6 2.636(11) 2_766 ? Bi1 C11 2.683(16) . ? Bi1 C23 2.792(14) . ? Bi2 O7 2.189(9) . ? Bi2 O4 2.199(9) . ? Bi2 O9 2.264(10) . ? Bi2 O3 2.499(10) . ? Bi2 O10 2.638(10) . ? Bi2 O12 2.658(9) 2_766 ? Bi2 C12 2.675(16) . ? Bi2 O8 2.724(13) . ? Bi2 C24 2.800(15) . ? Bi2 C25 2.808(13) . ? Fe1 C7 2.002(18) . ? Fe1 C9 2.008(16) . ? Fe1 C6 2.015(14) . ? Fe1 C8 2.017(18) . ? Fe1 C2 2.022(17) . ? Fe1 C3 2.025(17) . ? Fe1 C5 2.036(17) . ? Fe1 C4 2.037(18) . ? Fe1 C1 2.038(15) . ? Fe1 C10 2.050(16) . ? Fe2 C13 1.988(15) . ? Fe2 C16 2.008(18) . ? Fe2 C22 2.008(17) . ? Fe2 C18 2.026(17) . ? Fe2 C17 2.037(16) . ? Fe2 C14 2.038(16) . ? Fe2 C21 2.038(17) . ? Fe2 C20 2.050(19) . ? Fe2 C19 2.058(18) . ? Fe2 C15 2.072(15) . ? Fe3 C32 2.002(13) . ? Fe3 C26 2.015(13) . ? Fe3 C27 2.024(14) . ? Fe3 C33 2.042(13) . ? Fe3 C29 2.042(13) . ? Fe3 C28 2.044(14) . ? Fe3 C31 2.047(13) . ? Fe3 C30 2.049(13) . ? Fe3 C35 2.077(14) . ? Fe3 C34 2.082(13) . ? O1 C11 1.244(18) . ? O2 C11 1.250(16) . ? O3 C12 1.255(18) . ? O4 C12 1.258(18) . ? O5 C23 1.304(15) . ? O6 C23 1.258(16) . ? O6 Bi1 2.636(11) 2_766 ? O7 C24 1.268(18) . ? O8 C24 1.234(16) . ? O9 C25 1.268(16) . ? O10 C25 1.243(16) . ? O11 C36 1.258(16) . ? O12 C36 1.226(16) . ? O12 Bi2 2.658(9) 2_766 ? C1 C2 1.43(2) . ? C1 C5 1.44(2) . ? C1 C11 1.48(2) . ? C2 C3 1.43(3) . ? C3 C4 1.36(3) . ? C4 C5 1.32(2) . ? C6 C7 1.39(2) . ? C6 C10 1.42(2) . ? C6 C12 1.53(2) . ? C7 C8 1.35(2) . ? C8 C9 1.38(3) . ? C9 C10 1.40(2) . ? C13 C14 1.40(2) . ? C13 C17 1.42(2) . ? C13 C23 1.48(2) . ? C14 C15 1.40(2) . ? C15 C16 1.36(2) . ? C16 C17 1.41(2) . ? C18 C19 1.40(2) . ? C18 C22 1.40(2) . ? C18 C24 1.48(2) . ? C19 C20 1.44(3) . ? C20 C21 1.44(3) . ? C21 C22 1.34(3) . ? C25 C26 1.452(18) . ? C26 C27 1.385(19) . ? C26 C30 1.453(18) . ? C27 C28 1.340(19) . ? C28 C29 1.41(2) . ? C29 C30 1.433(19) . ? C31 C35 1.41(2) . ? C31 C32 1.455(18) . ? C32 C33 1.399(18) . ? C32 C36 1.513(18) 1_454 ? C33 C34 1.420(19) . ? C34 C35 1.43(2) . ? C36 C32 1.513(18) 1_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Bi1 O5 80.7(4) . . ? O2 Bi1 O11 85.0(3) . . ? O5 Bi1 O11 75.4(4) . . ? O2 Bi1 O1 55.0(4) . . ? O5 Bi1 O1 128.1(4) . . ? O11 Bi1 O1 75.1(4) . . ? O2 Bi1 O6 80.7(3) . . ? O5 Bi1 O6 54.2(3) . . ? O11 Bi1 O6 129.2(4) . . ? O1 Bi1 O6 129.2(4) . . ? O2 Bi1 O12 134.6(3) . . ? O5 Bi1 O12 98.9(3) . . ? O11 Bi1 O12 52.0(3) . . ? O1 Bi1 O12 95.4(3) . . ? O6 Bi1 O12 135.3(3) . . ? O2 Bi1 O6 81.2(3) . 2_766 ? O5 Bi1 O6 120.1(3) . 2_766 ? O11 Bi1 O6 156.8(3) . 2_766 ? O1 Bi1 O6 81.7(3) . 2_766 ? O6 Bi1 O6 66.7(4) . 2_766 ? O12 Bi1 O6 132.6(3) . 2_766 ? O2 Bi1 C11 27.5(4) . . ? O5 Bi1 C11 104.6(4) . . ? O11 Bi1 C11 78.4(4) . . ? O1 Bi1 C11 27.5(4) . . ? O6 Bi1 C11 105.6(4) . . ? O12 Bi1 C11 116.4(4) . . ? O6 Bi1 C11 80.8(4) 2_766 . ? O2 Bi1 C23 79.1(3) . . ? O5 Bi1 C23 27.5(3) . . ? O11 Bi1 C23 102.6(4) . . ? O1 Bi1 C23 134.1(4) . . ? O6 Bi1 C23 26.7(3) . . ? O12 Bi1 C23 119.7(3) . . ? O6 Bi1 C23 93.0(3) 2_766 . ? C11 Bi1 C23 106.6(4) . . ? O7 Bi2 O4 87.5(4) . . ? O7 Bi2 O9 80.0(4) . . ? O4 Bi2 O9 80.0(4) . . ? O7 Bi2 O3 75.4(4) . . ? O4 Bi2 O3 55.5(3) . . ? O9 Bi2 O3 129.3(4) . . ? O7 Bi2 O10 132.3(4) . . ? O4 Bi2 O10 82.6(4) . . ? O9 Bi2 O10 52.4(3) . . ? O3 Bi2 O10 130.8(3) . . ? O7 Bi2 O12 87.7(4) . 2_766 ? O4 Bi2 O12 129.5(3) . 2_766 ? O9 Bi2 O12 147.6(4) . 2_766 ? O3 Bi2 O12 74.7(3) . 2_766 ? O10 Bi2 O12 133.1(3) . 2_766 ? O7 Bi2 C12 81.8(4) . . ? O4 Bi2 C12 27.8(4) . . ? O9 Bi2 C12 105.7(4) . . ? O3 Bi2 C12 27.8(4) . . ? O10 Bi2 C12 106.6(4) . . ? O12 Bi2 C12 102.0(4) 2_766 . ? O7 Bi2 O8 51.1(4) . . ? O4 Bi2 O8 132.3(4) . . ? O9 Bi2 O8 71.2(4) . . ? O3 Bi2 O8 120.0(4) . . ? O10 Bi2 O8 106.8(4) . . ? O12 Bi2 O8 77.7(3) 2_766 . ? C12 Bi2 O8 132.9(4) . . ? O7 Bi2 C24 25.9(4) . . ? O4 Bi2 C24 108.6(4) . . ? O9 Bi2 C24 70.0(4) . . ? O3 Bi2 C24 99.9(4) . . ? O10 Bi2 C24 118.7(4) . . ? O12 Bi2 C24 85.9(4) 2_766 . ? C12 Bi2 C24 107.5(4) . . ? O8 Bi2 C24 25.8(4) . . ? O7 Bi2 C25 106.2(4) . . ? O4 Bi2 C25 80.5(4) . . ? O9 Bi2 C25 26.3(4) . . ? O3 Bi2 C25 136.0(4) . . ? O10 Bi2 C25 26.1(3) . . ? O12 Bi2 C25 148.2(4) 2_766 . ? C12 Bi2 C25 108.2(4) . . ? O8 Bi2 C25 88.8(4) . . ? C24 Bi2 C25 94.5(4) . . ? C7 Fe1 C9 67.3(8) . . ? C7 Fe1 C6 40.4(6) . . ? C9 Fe1 C6 69.0(7) . . ? C7 Fe1 C8 39.4(7) . . ? C9 Fe1 C8 40.2(8) . . ? C6 Fe1 C8 67.8(6) . . ? C7 Fe1 C2 119.9(8) . . ? C9 Fe1 C2 121.5(7) . . ? C6 Fe1 C2 155.9(7) . . ? C8 Fe1 C2 105.2(7) . . ? C7 Fe1 C3 154.3(9) . . ? C9 Fe1 C3 105.2(8) . . ? C6 Fe1 C3 162.3(8) . . ? C8 Fe1 C3 119.1(8) . . ? C2 Fe1 C3 41.4(7) . . ? C7 Fe1 C5 129.4(7) . . ? C9 Fe1 C5 155.5(9) . . ? C6 Fe1 C5 110.9(6) . . ? C8 Fe1 C5 164.0(8) . . ? C2 Fe1 C5 69.1(7) . . ? C3 Fe1 C5 67.2(7) . . ? C7 Fe1 C4 165.2(8) . . ? C9 Fe1 C4 122.0(9) . . ? C6 Fe1 C4 128.7(8) . . ? C8 Fe1 C4 155.1(8) . . ? C2 Fe1 C4 66.9(8) . . ? C3 Fe1 C4 39.3(8) . . ? C5 Fe1 C4 37.8(7) . . ? C7 Fe1 C1 109.6(7) . . ? C9 Fe1 C1 159.8(8) . . ? C6 Fe1 C1 122.6(6) . . ? C8 Fe1 C1 124.7(8) . . ? C2 Fe1 C1 41.1(6) . . ? C3 Fe1 C1 68.5(7) . . ? C5 Fe1 C1 41.4(7) . . ? C4 Fe1 C1 65.9(7) . . ? C7 Fe1 C10 66.9(7) . . ? C9 Fe1 C10 40.2(7) . . ? C6 Fe1 C10 40.9(6) . . ? C8 Fe1 C10 66.9(7) . . ? C2 Fe1 C10 159.4(6) . . ? C3 Fe1 C10 124.2(7) . . ? C5 Fe1 C10 123.4(7) . . ? C4 Fe1 C10 111.7(8) . . ? C1 Fe1 C10 158.9(7) . . ? C13 Fe2 C16 68.2(7) . . ? C13 Fe2 C22 110.7(7) . . ? C16 Fe2 C22 153.8(7) . . ? C13 Fe2 C18 122.6(6) . . ? C16 Fe2 C18 162.3(7) . . ? C22 Fe2 C18 40.7(6) . . ? C13 Fe2 C17 41.2(6) . . ? C16 Fe2 C17 40.8(7) . . ? C22 Fe2 C17 120.7(7) . . ? C18 Fe2 C17 156.5(6) . . ? C13 Fe2 C14 40.6(6) . . ? C16 Fe2 C14 67.1(8) . . ? C22 Fe2 C14 130.3(8) . . ? C18 Fe2 C14 110.9(7) . . ? C17 Fe2 C14 68.4(7) . . ? C13 Fe2 C21 126.8(7) . . ? C16 Fe2 C21 119.5(8) . . ? C22 Fe2 C21 38.6(7) . . ? C18 Fe2 C21 67.2(7) . . ? C17 Fe2 C21 107.1(7) . . ? C14 Fe2 C21 165.0(8) . . ? C13 Fe2 C20 162.8(8) . . ? C16 Fe2 C20 105.4(9) . . ? C22 Fe2 C20 67.5(8) . . ? C18 Fe2 C20 68.1(8) . . ? C17 Fe2 C20 123.7(9) . . ? C14 Fe2 C20 153.3(8) . . ? C21 Fe2 C20 41.2(8) . . ? C13 Fe2 C19 155.6(7) . . ? C16 Fe2 C19 124.3(7) . . ? C22 Fe2 C19 68.0(7) . . ? C18 Fe2 C19 40.2(7) . . ? C17 Fe2 C19 161.3(7) . . ? C14 Fe2 C19 120.4(7) . . ? C21 Fe2 C19 68.5(7) . . ? C20 Fe2 C19 41.1(8) . . ? C13 Fe2 C15 67.4(7) . . ? C16 Fe2 C15 38.9(7) . . ? C22 Fe2 C15 166.9(7) . . ? C18 Fe2 C15 128.3(8) . . ? C17 Fe2 C15 67.2(8) . . ? C14 Fe2 C15 39.9(7) . . ? C21 Fe2 C15 153.1(8) . . ? C20 Fe2 C15 118.4(8) . . ? C19 Fe2 C15 108.0(7) . . ? C32 Fe3 C26 129.1(5) . . ? C32 Fe3 C27 168.1(5) . . ? C26 Fe3 C27 40.1(6) . . ? C32 Fe3 C33 40.5(5) . . ? C26 Fe3 C33 168.1(6) . . ? C27 Fe3 C33 151.0(6) . . ? C32 Fe3 C29 117.8(5) . . ? C26 Fe3 C29 69.2(5) . . ? C27 Fe3 C29 66.3(6) . . ? C33 Fe3 C29 109.0(6) . . ? C32 Fe3 C28 151.5(6) . . ? C26 Fe3 C28 67.8(5) . . ? C27 Fe3 C28 38.5(5) . . ? C33 Fe3 C28 119.0(6) . . ? C29 Fe3 C28 40.4(5) . . ? C32 Fe3 C31 42.1(5) . . ? C26 Fe3 C31 106.4(5) . . ? C27 Fe3 C31 129.1(6) . . ? C33 Fe3 C31 69.2(6) . . ? C29 Fe3 C31 151.6(6) . . ? C28 Fe3 C31 165.7(6) . . ? C32 Fe3 C30 107.7(6) . . ? C26 Fe3 C30 41.9(5) . . ? C27 Fe3 C30 67.5(6) . . ? C33 Fe3 C30 129.2(6) . . ? C29 Fe3 C30 41.0(5) . . ? C28 Fe3 C30 68.3(6) . . ? C31 Fe3 C30 116.8(6) . . ? C32 Fe3 C35 69.1(6) . . ? C26 Fe3 C35 115.1(6) . . ? C27 Fe3 C35 109.1(6) . . ? C33 Fe3 C35 69.1(6) . . ? C29 Fe3 C35 167.9(6) . . ? C28 Fe3 C35 129.2(6) . . ? C31 Fe3 C35 40.0(5) . . ? C30 Fe3 C35 149.3(6) . . ? C32 Fe3 C34 67.2(5) . . ? C26 Fe3 C34 149.4(6) . . ? C27 Fe3 C34 119.6(6) . . ? C33 Fe3 C34 40.3(5) . . ? C29 Fe3 C34 131.0(6) . . ? C28 Fe3 C34 110.9(6) . . ? C31 Fe3 C34 67.0(6) . . ? C30 Fe3 C34 168.4(6) . . ? C35 Fe3 C34 40.3(6) . . ? C11 O1 Bi1 85.6(9) . . ? C11 O2 Bi1 97.7(9) . . ? C12 O3 Bi2 83.9(9) . . ? C12 O4 Bi2 97.7(9) . . ? C23 O5 Bi1 98.9(8) . . ? C23 O6 Bi1 87.3(8) . . ? C23 O6 Bi1 156.5(9) . 2_766 ? Bi1 O6 Bi1 113.3(4) . 2_766 ? C24 O7 Bi2 105.0(8) . . ? C24 O8 Bi2 80.5(9) . . ? C25 O9 Bi2 101.5(9) . . ? C25 O10 Bi2 84.6(8) . . ? C36 O11 Bi1 100.0(8) . . ? C36 O12 Bi1 85.1(8) . . ? C36 O12 Bi2 151.7(9) . 2_766 ? Bi1 O12 Bi2 106.8(3) . 2_766 ? C2 C1 C5 106.9(16) . . ? C2 C1 C11 127.3(17) . . ? C5 C1 C11 125.6(14) . . ? C2 C1 Fe1 68.8(9) . . ? C5 C1 Fe1 69.3(9) . . ? C11 C1 Fe1 123.6(11) . . ? C1 C2 C3 106.3(18) . . ? C1 C2 Fe1 70.0(9) . . ? C3 C2 Fe1 69.4(10) . . ? C4 C3 C2 106.4(16) . . ? C4 C3 Fe1 70.8(10) . . ? C2 C3 Fe1 69.2(10) . . ? C5 C4 C3 113.6(19) . . ? C5 C4 Fe1 71.1(11) . . ? C3 C4 Fe1 69.9(11) . . ? C4 C5 C1 106.7(17) . . ? C4 C5 Fe1 71.1(11) . . ? C1 C5 Fe1 69.4(10) . . ? C7 C6 C10 105.5(15) . . ? C7 C6 C12 130.2(14) . . ? C10 C6 C12 124.3(14) . . ? C7 C6 Fe1 69.3(9) . . ? C10 C6 Fe1 70.8(9) . . ? C12 C6 Fe1 124.2(10) . . ? C8 C7 C6 110.4(17) . . ? C8 C7 Fe1 70.9(11) . . ? C6 C7 Fe1 70.3(9) . . ? C7 C8 C9 108.5(17) . . ? C7 C8 Fe1 69.7(10) . . ? C9 C8 Fe1 69.5(11) . . ? C8 C9 C10 107.4(16) . . ? C8 C9 Fe1 70.2(10) . . ? C10 C9 Fe1 71.5(9) . . ? C9 C10 C6 107.9(17) . . ? C9 C10 Fe1 68.3(9) . . ? C6 C10 Fe1 68.2(8) . . ? O1 C11 O2 121.7(15) . . ? O1 C11 C1 119.6(14) . . ? O2 C11 C1 118.7(14) . . ? O1 C11 Bi1 66.9(9) . . ? O2 C11 Bi1 54.8(8) . . ? C1 C11 Bi1 172.4(11) . . ? O3 C12 O4 122.6(15) . . ? O3 C12 C6 119.4(14) . . ? O4 C12 C6 118.0(13) . . ? O3 C12 Bi2 68.3(8) . . ? O4 C12 Bi2 54.6(7) . . ? C6 C12 Bi2 170.2(10) . . ? C14 C13 C17 109.0(15) . . ? C14 C13 C23 125.6(15) . . ? C17 C13 C23 125.3(13) . . ? C14 C13 Fe2 71.7(9) . . ? C17 C13 Fe2 71.3(9) . . ? C23 C13 Fe2 123.7(9) . . ? C13 C14 C15 107.2(17) . . ? C13 C14 Fe2 67.8(9) . . ? C15 C14 Fe2 71.4(10) . . ? C16 C15 C14 108.2(16) . . ? C16 C15 Fe2 68.0(10) . . ? C14 C15 Fe2 68.8(9) . . ? C15 C16 C17 110.4(17) . . ? C15 C16 Fe2 73.1(11) . . ? C17 C16 Fe2 70.7(10) . . ? C16 C17 C13 104.9(15) . . ? C16 C17 Fe2 68.5(10) . . ? C13 C17 Fe2 67.5(8) . . ? C19 C18 C22 108.2(16) . . ? C19 C18 C24 125.7(16) . . ? C22 C18 C24 125.9(15) . . ? C19 C18 Fe2 71.1(11) . . ? C22 C18 Fe2 68.9(10) . . ? C24 C18 Fe2 128.9(11) . . ? C18 C19 C20 106.6(16) . . ? C18 C19 Fe2 68.7(10) . . ? C20 C19 Fe2 69.1(11) . . ? C21 C20 C19 106.4(17) . . ? C21 C20 Fe2 69.0(10) . . ? C19 C20 Fe2 69.7(10) . . ? C22 C21 C20 108.6(16) . . ? C22 C21 Fe2 69.5(10) . . ? C20 C21 Fe2 69.9(10) . . ? C21 C22 C18 110.2(17) . . ? C21 C22 Fe2 71.9(11) . . ? C18 C22 Fe2 70.3(10) . . ? O6 C23 O5 119.6(13) . . ? O6 C23 C13 123.4(12) . . ? O5 C23 C13 116.8(12) . . ? O6 C23 Bi1 65.9(8) . . ? O5 C23 Bi1 53.7(7) . . ? C13 C23 Bi1 170.1(9) . . ? O8 C24 O7 120.7(14) . . ? O8 C24 C18 121.5(15) . . ? O7 C24 C18 117.6(13) . . ? O8 C24 Bi2 73.7(9) . . ? O7 C24 Bi2 49.0(7) . . ? C18 C24 Bi2 156.5(11) . . ? O10 C25 O9 121.5(13) . . ? O10 C25 C26 123.4(13) . . ? O9 C25 C26 115.1(12) . . ? O10 C25 Bi2 69.3(8) . . ? O9 C25 Bi2 52.2(7) . . ? C26 C25 Bi2 167.3(10) . . ? C27 C26 C25 130.6(12) . . ? C27 C26 C30 105.7(12) . . ? C25 C26 C30 123.3(12) . . ? C27 C26 Fe3 70.3(8) . . ? C25 C26 Fe3 118.2(10) . . ? C30 C26 Fe3 70.3(7) . . ? C28 C27 C26 112.5(13) . . ? C28 C27 Fe3 71.6(9) . . ? C26 C27 Fe3 69.6(8) . . ? C27 C28 C29 107.9(12) . . ? C27 C28 Fe3 69.9(8) . . ? C29 C28 Fe3 69.8(8) . . ? C28 C29 C30 107.9(12) . . ? C28 C29 Fe3 69.9(8) . . ? C30 C29 Fe3 69.8(7) . . ? C29 C30 C26 105.9(12) . . ? C29 C30 Fe3 69.2(7) . . ? C26 C30 Fe3 67.8(7) . . ? C35 C31 C32 107.7(12) . . ? C35 C31 Fe3 71.2(8) . . ? C32 C31 Fe3 67.3(7) . . ? C33 C32 C31 108.9(12) . . ? C33 C32 C36 125.2(12) . 1_454 ? C31 C32 C36 125.2(12) . 1_454 ? C33 C32 Fe3 71.3(8) . . ? C31 C32 Fe3 70.6(7) . . ? C36 C32 Fe3 116.7(8) 1_454 . ? C32 C33 C34 106.6(12) . . ? C32 C33 Fe3 68.2(7) . . ? C34 C33 Fe3 71.3(8) . . ? C33 C34 C35 110.1(12) . . ? C33 C34 Fe3 68.4(7) . . ? C35 C34 Fe3 69.7(7) . . ? C31 C35 C34 106.6(13) . . ? C31 C35 Fe3 68.9(8) . . ? C34 C35 Fe3 70.1(8) . . ? O12 C36 O11 121.8(13) . . ? O12 C36 C32 120.1(12) . 1_656 ? O11 C36 C32 118.0(12) . 1_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 4.851 _refine_diff_density_min -2.928 _refine_diff_density_rms 0.344 data_2 _database_code_depnum_ccdc_archive 'CCDC 885529' #TrackingRef '- Final cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H27 Bi Fe3 O6' _chemical_formula_sum 'C33 H27 Bi Fe3 O6' _chemical_formula_weight 896.08 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' Fe Fe 0.3463 0.8444 '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 Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 14.261(5) _cell_length_b 14.261(5) _cell_length_c 12.252(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 2157.9(14) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2728 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.82 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1302 _exptl_absorpt_coefficient_mu 7.627 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2081 _exptl_absorpt_correction_T_max 0.3107 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11513 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.49 _reflns_number_total 5261 _reflns_number_gt 4576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non hydrogen atoms were refined anisotropically. Carbon atoms C9 and C23 were having large anisotropic diplacement parameteres and hence refined isotropically. The thermal parameters of C18 C19 C20 C21 C22 were refined anisotropically but constrained to share common parameters (EADP). ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(6) _refine_ls_number_reflns 5261 _refine_ls_number_parameters 364 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.881 _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 0.21964(3) 0.60634(3) 0.52672(3) 0.01790(9) Uani 1 1 d . . . Fe1 Fe 0.30216(12) 0.36742(12) 0.23011(11) 0.0225(3) Uani 1 1 d . . . Fe2 Fe 0.03227(12) 0.21920(12) 0.75612(12) 0.0222(4) Uani 1 1 d . . . Fe3 Fe -0.16908(12) 0.36989(12) 0.32938(11) 0.0222(3) Uani 1 1 d . . . O1 O 0.3478(5) 0.6053(5) 0.3943(5) 0.0215(15) Uani 1 1 d . . . O2 O 0.2468(5) 0.4669(5) 0.4982(5) 0.0220(15) Uani 1 1 d . . . O3 O 0.2234(5) 0.5238(5) 0.7215(5) 0.0204(15) Uani 1 1 d . . . O4 O 0.0786(5) 0.4708(5) 0.6184(5) 0.0235(16) Uani 1 1 d . . . O5 O 0.0502(5) 0.6198(5) 0.4746(5) 0.0263(16) Uani 1 1 d . . . O6 O 0.1185(5) 0.5348(5) 0.3817(5) 0.0180(14) Uani 1 1 d . . . C1 C 0.3182(8) 0.5090(7) 0.4228(7) 0.019(2) Uani 1 1 d . . . C2 C 0.3615(8) 0.4458(8) 0.3736(7) 0.020(2) Uani 1 1 d . . . C3 C 0.3229(8) 0.3336(8) 0.3859(8) 0.025(2) Uani 1 1 d . . . H3 H 0.2666 0.2837 0.4363 0.030 Uiso 1 1 calc R . . C4 C 0.3864(8) 0.3091(8) 0.3132(8) 0.023(2) Uani 1 1 d . . . H4 H 0.3784 0.2373 0.3029 0.027 Uiso 1 1 calc R . . C5 C 0.4576(8) 0.4011(8) 0.2568(8) 0.025(2) Uani 1 1 d . . . H5 H 0.5085 0.4056 0.2005 0.030 Uiso 1 1 calc R . . C6 C 0.4428(7) 0.4867(8) 0.2915(8) 0.024(2) Uani 1 1 d . . . H6 H 0.4829 0.5617 0.2654 0.029 Uiso 1 1 calc R . . C7 C 0.2087(9) 0.2567(10) 0.1137(9) 0.035(3) Uani 1 1 d . . . H7 H 0.2050 0.1874 0.0986 0.042 Uiso 1 1 calc R . . C8 C 0.1444(9) 0.2750(10) 0.1896(9) 0.040(3) Uani 1 1 d . . . H8 H 0.0872 0.2202 0.2359 0.048 Uiso 1 1 calc R . . C9 C 0.1811(9) 0.3931(9) 0.1879(9) 0.035(3) Uani 1 1 d U . . H9 H 0.1517 0.4307 0.2306 0.042 Uiso 1 1 calc R . . C10 C 0.2583(9) 0.4363(10) 0.1073(8) 0.034(3) Uani 1 1 d . . . H10 H 0.2983 0.5130 0.0871 0.041 Uiso 1 1 calc R . . C11 C 0.2795(11) 0.3564(11) 0.0661(9) 0.041(3) Uani 1 1 d . . . H11 H 0.3349 0.3689 0.0117 0.049 Uiso 1 1 calc R . . C12 C 0.1261(8) 0.4604(8) 0.7035(7) 0.017(2) Uani 1 1 d . . . C13 C 0.0574(8) 0.3689(8) 0.7787(7) 0.018(2) Uani 1 1 d . . . C14 C -0.0550(8) 0.2971(8) 0.7704(7) 0.022(2) Uani 1 1 d . . . H14 H -0.1044 0.2992 0.7161 0.026 Uiso 1 1 calc R . . C15 C -0.0813(8) 0.2200(8) 0.8532(8) 0.023(2) Uani 1 1 d . . . H15 H -0.1535 0.1579 0.8667 0.028 Uiso 1 1 calc R . . C16 C 0.0106(8) 0.2464(8) 0.9139(8) 0.023(2) Uani 1 1 d . . . H16 H 0.0136 0.2052 0.9765 0.028 Uiso 1 1 calc R . . C17 C 0.0997(8) 0.3390(8) 0.8697(8) 0.026(2) Uani 1 1 d . . . H17 H 0.1746 0.3758 0.8962 0.031 Uiso 1 1 calc R . . C18 C -0.0010(12) 0.1435(11) 0.6088(13) 0.0595(18) Uani 1 1 d . . . H18 H -0.0509 0.1441 0.5540 0.071 Uiso 1 1 calc R . . C19 C 0.1080(12) 0.2182(12) 0.6163(13) 0.0595(18) Uani 1 1 d . . . H19 H 0.1484 0.2802 0.5675 0.071 Uiso 1 1 calc R . . C20 C 0.1516(12) 0.1906(11) 0.7069(12) 0.0595(18) Uani 1 1 d . . . H20 H 0.2271 0.2275 0.7315 0.071 Uiso 1 1 calc R . . C21 C 0.0623(11) 0.0938(11) 0.7511(13) 0.0595(18) Uani 1 1 d . . . H21 H 0.0657 0.0537 0.8146 0.071 Uiso 1 1 calc R . . C22 C -0.0282(13) 0.0659(12) 0.6896(12) 0.0595(18) Uani 1 1 d . . . H22 H -0.1004 0.0037 0.7026 0.071 Uiso 1 1 calc R . . C23 C 0.0468(8) 0.5626(7) 0.3961(7) 0.019(2) Uani 1 1 d U . . C24 C -0.0414(8) 0.5222(8) 0.3153(7) 0.022(2) Uani 1 1 d . . . C25 C -0.0509(8) 0.4622(9) 0.2188(9) 0.025(2) Uani 1 1 d . . . H25 H 0.0039 0.4470 0.1887 0.030 Uiso 1 1 calc R . . C26 C -0.1585(8) 0.4270(8) 0.1738(8) 0.025(2) Uani 1 1 d . . . H26 H -0.1894 0.3827 0.1083 0.030 Uiso 1 1 calc R . . C27 C -0.2109(8) 0.4657(8) 0.2425(8) 0.027(2) Uani 1 1 d . . . H27 H -0.2846 0.4530 0.2328 0.033 Uiso 1 1 calc R . . C28 C -0.1395(9) 0.5247(8) 0.3294(8) 0.028(2) Uani 1 1 d . . . H28 H -0.1553 0.5601 0.3893 0.034 Uiso 1 1 calc R . . C29 C -0.1490(10) 0.2406(8) 0.3643(9) 0.037(3) Uani 1 1 d . . . H29 H -0.0948 0.2258 0.3322 0.044 Uiso 1 1 calc R . . C30 C -0.1360(10) 0.3019(8) 0.4589(9) 0.035(3) Uani 1 1 d . . . H30 H -0.0700 0.3378 0.5032 0.042 Uiso 1 1 calc R . . C31 C -0.2309(9) 0.3064(8) 0.4788(8) 0.033(3) Uani 1 1 d . . . H31 H -0.2423 0.3445 0.5393 0.040 Uiso 1 1 calc R . . C32 C -0.3078(10) 0.2452(9) 0.3956(9) 0.037(3) Uani 1 1 d . . . H32 H -0.3812 0.2339 0.3884 0.045 Uiso 1 1 calc R . . C33 C -0.2562(9) 0.2036(8) 0.3235(9) 0.029(3) Uani 1 1 d . . . H33 H -0.2884 0.1593 0.2582 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0203(2) 0.0177(2) 0.01533(16) -0.00035(18) -0.00018(18) 0.0092(2) Fe1 0.0311(9) 0.0273(9) 0.0145(8) -0.0007(6) -0.0034(6) 0.0187(8) Fe2 0.0206(8) 0.0202(8) 0.0243(9) 0.0020(7) 0.0030(7) 0.0090(7) Fe3 0.0256(8) 0.0200(8) 0.0180(8) 0.0013(6) -0.0016(6) 0.0091(7) O1 0.024(4) 0.015(4) 0.019(4) 0.000(3) 0.005(3) 0.006(3) O2 0.026(4) 0.023(4) 0.022(4) 0.007(3) 0.008(3) 0.016(3) O3 0.019(4) 0.018(4) 0.015(4) -0.003(3) -0.006(3) 0.003(3) O4 0.020(4) 0.026(4) 0.021(4) 0.003(3) -0.001(3) 0.009(3) O5 0.025(4) 0.027(4) 0.023(4) -0.001(3) 0.000(3) 0.010(3) O6 0.018(4) 0.015(3) 0.018(4) 0.000(3) -0.002(3) 0.007(3) C1 0.022(5) 0.015(5) 0.017(5) -0.001(4) -0.004(4) 0.008(4) C2 0.024(5) 0.034(6) 0.006(5) 0.000(4) -0.006(4) 0.016(5) C3 0.026(6) 0.027(6) 0.020(5) 0.001(4) -0.010(4) 0.011(5) C4 0.032(6) 0.023(6) 0.019(5) -0.004(4) -0.007(5) 0.018(5) C5 0.023(6) 0.033(6) 0.021(5) 0.000(5) -0.003(4) 0.016(5) C6 0.009(5) 0.020(6) 0.034(6) -0.010(5) 0.001(4) 0.000(4) C7 0.039(7) 0.037(7) 0.035(7) -0.017(6) -0.017(6) 0.023(6) C8 0.028(7) 0.048(8) 0.032(7) 0.001(6) -0.011(5) 0.010(6) C9 0.042(5) 0.051(5) 0.032(4) 0.001(4) 0.000(4) 0.038(4) C10 0.053(8) 0.042(7) 0.021(6) 0.008(5) -0.006(5) 0.034(6) C11 0.067(9) 0.074(10) 0.020(6) 0.001(6) -0.007(6) 0.064(9) C12 0.027(6) 0.017(5) 0.007(5) -0.004(4) -0.005(4) 0.010(5) C13 0.029(6) 0.018(5) 0.006(5) 0.002(4) 0.000(4) 0.012(5) C14 0.024(6) 0.025(6) 0.012(5) 0.001(4) 0.006(4) 0.009(5) C15 0.017(5) 0.017(5) 0.026(6) -0.006(4) 0.007(4) 0.002(4) C16 0.027(6) 0.022(6) 0.015(5) -0.004(4) -0.004(4) 0.008(5) C17 0.019(6) 0.022(6) 0.030(6) 0.010(5) 0.008(5) 0.007(5) C18 0.065(5) 0.050(4) 0.073(5) -0.016(3) 0.007(4) 0.036(4) C19 0.065(5) 0.050(4) 0.073(5) -0.016(3) 0.007(4) 0.036(4) C20 0.065(5) 0.050(4) 0.073(5) -0.016(3) 0.007(4) 0.036(4) C21 0.065(5) 0.050(4) 0.073(5) -0.016(3) 0.007(4) 0.036(4) C22 0.065(5) 0.050(4) 0.073(5) -0.016(3) 0.007(4) 0.036(4) C23 0.023(4) 0.015(4) 0.011(4) 0.004(3) 0.002(3) 0.004(3) C24 0.022(6) 0.028(6) 0.008(5) -0.004(4) -0.007(4) 0.007(5) C25 0.012(5) 0.032(7) 0.025(6) 0.008(5) 0.005(4) 0.005(5) C26 0.020(6) 0.021(6) 0.020(6) 0.013(4) 0.002(4) 0.000(5) C27 0.021(6) 0.022(6) 0.036(6) 0.011(5) 0.004(5) 0.008(5) C28 0.034(6) 0.034(6) 0.023(6) -0.003(5) -0.010(5) 0.021(5) C29 0.050(8) 0.023(6) 0.039(7) 0.008(5) 0.001(6) 0.019(6) C30 0.044(7) 0.022(6) 0.042(7) 0.009(5) -0.002(6) 0.019(6) C31 0.047(7) 0.025(6) 0.014(5) 0.004(4) -0.002(5) 0.007(6) C32 0.045(7) 0.032(7) 0.033(7) 0.004(5) -0.004(6) 0.019(6) C33 0.035(7) 0.016(6) 0.022(6) 0.009(4) -0.006(5) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O6 2.192(6) . ? Bi1 O2 2.236(6) . ? Bi1 O4 2.271(7) . ? Bi1 O1 2.449(6) . ? Bi1 O5 2.597(7) . ? Bi1 O3 2.674(6) . ? Bi1 O3 2.703(6) 3_564 ? Bi1 C1 2.734(9) . ? Bi1 C23 2.737(10) . ? Bi1 C12 2.833(9) . ? Fe1 C9 2.004(11) . ? Fe1 C6 2.018(9) . ? Fe1 C8 2.019(11) . ? Fe1 C3 2.026(9) . ? Fe1 C2 2.028(9) . ? Fe1 C11 2.029(11) . ? Fe1 C4 2.042(9) . ? Fe1 C5 2.046(10) . ? Fe1 C7 2.049(11) . ? Fe1 C10 2.058(10) . ? Fe2 C13 1.999(10) . ? Fe2 C15 2.015(9) . ? Fe2 C16 2.026(10) . ? Fe2 C19 2.029(14) . ? Fe2 C20 2.029(13) . ? Fe2 C17 2.034(11) . ? Fe2 C18 2.034(14) . ? Fe2 C21 2.038(13) . ? Fe2 C14 2.048(10) . ? Fe2 C22 2.074(13) . ? Fe3 C24 2.027(10) . ? Fe3 C28 2.029(10) . ? Fe3 C30 2.034(11) . ? Fe3 C31 2.038(10) . ? Fe3 C27 2.042(10) . ? Fe3 C29 2.047(11) . ? Fe3 C25 2.047(10) . ? Fe3 C26 2.048(9) . ? Fe3 C32 2.053(12) . ? Fe3 C33 2.056(10) . ? O1 C1 1.268(10) . ? O2 C1 1.280(11) . ? O3 C12 1.239(11) . ? O3 Bi1 2.703(6) 2_665 ? O4 C12 1.292(11) . ? O5 C23 1.246(11) . ? O6 C23 1.281(11) . ? C1 C2 1.454(13) . ? C2 C3 1.415(13) . ? C2 C6 1.422(13) . ? C3 C4 1.433(13) . ? C3 H3 0.9800 . ? C4 C5 1.378(14) . ? C4 H4 0.9800 . ? C5 C6 1.404(13) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C11 1.395(17) . ? C7 C8 1.418(16) . ? C7 H7 0.9800 . ? C8 C9 1.495(16) . ? C8 H8 0.9800 . ? C9 C10 1.374(15) . ? C9 H9 0.9800 . ? C10 C11 1.410(15) . ? C10 H10 0.9800 . ? C11 H11 0.9800 . ? C12 C13 1.494(13) . ? C13 C14 1.410(13) . ? C13 C17 1.431(13) . ? C14 C15 1.403(13) . ? C14 H14 0.9800 . ? C15 C16 1.385(14) . ? C15 H15 0.9800 . ? C16 C17 1.405(13) . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C18 C19 1.380(18) . ? C18 C22 1.39(2) . ? C18 H18 0.9800 . ? C19 C20 1.42(2) . ? C19 H19 0.9800 . ? C20 C21 1.437(19) . ? C20 H20 0.9800 . ? C21 C22 1.37(2) . ? C21 H21 0.9800 . ? C22 H22 0.9800 . ? C23 C24 1.472(13) . ? C24 C25 1.427(14) . ? C24 C28 1.427(14) . ? C25 C26 1.463(14) . ? C25 H25 0.9800 . ? C26 C27 1.409(14) . ? C26 H26 0.9800 . ? C27 C28 1.421(13) . ? C27 H27 0.9800 . ? C28 H28 0.9800 . ? C29 C30 1.407(15) . ? C29 C33 1.435(15) . ? C29 H29 0.9800 . ? C30 C31 1.407(15) . ? C30 H30 0.9800 . ? C31 C32 1.431(15) . ? C31 H31 0.9800 . ? C32 C33 1.452(15) . ? C32 H32 0.9800 . ? C33 H33 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Bi1 O2 80.0(2) . . ? O6 Bi1 O4 84.7(2) . . ? O2 Bi1 O4 78.1(2) . . ? O6 Bi1 O1 77.3(2) . . ? O2 Bi1 O1 55.2(2) . . ? O4 Bi1 O1 131.9(2) . . ? O6 Bi1 O5 54.2(2) . . ? O2 Bi1 O5 127.5(2) . . ? O4 Bi1 O5 74.0(2) . . ? O1 Bi1 O5 124.2(2) . . ? O6 Bi1 O3 132.2(2) . . ? O2 Bi1 O3 72.4(2) . . ? O4 Bi1 O3 52.2(2) . . ? O1 Bi1 O3 114.2(2) . . ? O5 Bi1 O3 118.4(2) . . ? O6 Bi1 O3 78.2(2) . 3_564 ? O2 Bi1 O3 121.0(2) . 3_564 ? O4 Bi1 O3 150.9(2) . 3_564 ? O1 Bi1 O3 66.8(2) . 3_564 ? O5 Bi1 O3 76.91(19) . 3_564 ? O3 Bi1 O3 149.62(19) . 3_564 ? O6 Bi1 C1 76.8(3) . . ? O2 Bi1 C1 27.6(2) . . ? O4 Bi1 C1 105.0(3) . . ? O1 Bi1 C1 27.6(2) . . ? O5 Bi1 C1 131.0(2) . . ? O3 Bi1 C1 93.7(2) . . ? O3 Bi1 C1 93.9(2) 3_564 . ? O6 Bi1 C23 27.4(2) . . ? O2 Bi1 C23 104.1(3) . . ? O4 Bi1 C23 77.4(3) . . ? O1 Bi1 C23 101.6(3) . . ? O5 Bi1 C23 26.8(2) . . ? O3 Bi1 C23 129.5(2) . . ? O3 Bi1 C23 76.6(2) 3_564 . ? C1 Bi1 C23 104.2(3) . . ? O6 Bi1 C12 108.6(2) . . ? O2 Bi1 C12 72.1(2) . . ? O4 Bi1 C12 26.5(3) . . ? O1 Bi1 C12 125.5(2) . . ? O5 Bi1 C12 97.4(2) . . ? O3 Bi1 C12 25.8(2) . . ? O3 Bi1 C12 166.6(2) 3_564 . ? C1 Bi1 C12 99.0(3) . . ? C23 Bi1 C12 103.9(3) . . ? C9 Fe1 C6 121.7(4) . . ? C9 Fe1 C8 43.6(5) . . ? C6 Fe1 C8 162.8(5) . . ? C9 Fe1 C3 121.9(4) . . ? C6 Fe1 C3 69.4(4) . . ? C8 Fe1 C3 108.9(4) . . ? C9 Fe1 C2 106.5(4) . . ? C6 Fe1 C2 41.2(4) . . ? C8 Fe1 C2 126.5(4) . . ? C3 Fe1 C2 40.9(4) . . ? C9 Fe1 C11 68.9(5) . . ? C6 Fe1 C11 119.1(5) . . ? C8 Fe1 C11 67.9(5) . . ? C3 Fe1 C11 162.0(4) . . ? C2 Fe1 C11 155.2(5) . . ? C9 Fe1 C4 159.9(4) . . ? C6 Fe1 C4 67.6(4) . . ? C8 Fe1 C4 123.1(4) . . ? C3 Fe1 C4 41.3(4) . . ? C2 Fe1 C4 67.9(4) . . ? C11 Fe1 C4 124.4(4) . . ? C9 Fe1 C5 158.4(4) . . ? C6 Fe1 C5 40.4(4) . . ? C8 Fe1 C5 156.2(5) . . ? C3 Fe1 C5 68.6(4) . . ? C2 Fe1 C5 68.1(4) . . ? C11 Fe1 C5 106.8(5) . . ? C4 Fe1 C5 39.4(4) . . ? C9 Fe1 C7 70.9(5) . . ? C6 Fe1 C7 154.0(5) . . ? C8 Fe1 C7 40.8(5) . . ? C3 Fe1 C7 126.0(5) . . ? C2 Fe1 C7 163.7(5) . . ? C11 Fe1 C7 40.0(5) . . ? C4 Fe1 C7 108.7(4) . . ? C5 Fe1 C7 120.2(4) . . ? C9 Fe1 C10 39.5(4) . . ? C6 Fe1 C10 106.3(5) . . ? C8 Fe1 C10 68.1(5) . . ? C3 Fe1 C10 156.6(4) . . ? C2 Fe1 C10 120.9(4) . . ? C11 Fe1 C10 40.4(4) . . ? C4 Fe1 C10 160.0(4) . . ? C5 Fe1 C10 123.8(4) . . ? C7 Fe1 C10 67.9(5) . . ? C13 Fe2 C15 68.2(4) . . ? C13 Fe2 C16 68.1(4) . . ? C15 Fe2 C16 40.1(4) . . ? C13 Fe2 C19 108.2(5) . . ? C15 Fe2 C19 158.6(5) . . ? C16 Fe2 C19 160.0(5) . . ? C13 Fe2 C20 122.3(5) . . ? C15 Fe2 C20 159.1(5) . . ? C16 Fe2 C20 123.1(5) . . ? C19 Fe2 C20 41.0(5) . . ? C13 Fe2 C17 41.5(4) . . ? C15 Fe2 C17 68.6(4) . . ? C16 Fe2 C17 40.5(4) . . ? C19 Fe2 C17 123.6(5) . . ? C20 Fe2 C17 106.3(5) . . ? C13 Fe2 C18 124.0(5) . . ? C15 Fe2 C18 123.5(5) . . ? C16 Fe2 C18 158.6(5) . . ? C19 Fe2 C18 39.7(5) . . ? C20 Fe2 C18 68.0(6) . . ? C17 Fe2 C18 160.0(5) . . ? C13 Fe2 C21 159.6(5) . . ? C15 Fe2 C21 123.0(5) . . ? C16 Fe2 C21 108.4(5) . . ? C19 Fe2 C21 67.8(6) . . ? C20 Fe2 C21 41.4(5) . . ? C17 Fe2 C21 122.6(5) . . ? C18 Fe2 C21 66.6(6) . . ? C13 Fe2 C14 40.8(4) . . ? C15 Fe2 C14 40.4(4) . . ? C16 Fe2 C14 67.8(4) . . ? C19 Fe2 C14 123.0(5) . . ? C20 Fe2 C14 158.7(5) . . ? C17 Fe2 C14 69.3(4) . . ? C18 Fe2 C14 108.6(5) . . ? C21 Fe2 C14 158.4(5) . . ? C13 Fe2 C22 159.7(5) . . ? C15 Fe2 C22 109.0(5) . . ? C16 Fe2 C22 123.6(5) . . ? C19 Fe2 C22 66.6(6) . . ? C20 Fe2 C22 67.7(6) . . ? C17 Fe2 C22 157.9(5) . . ? C18 Fe2 C22 39.5(6) . . ? C21 Fe2 C22 38.9(5) . . ? C14 Fe2 C22 124.1(5) . . ? C24 Fe3 C28 41.2(4) . . ? C24 Fe3 C30 106.2(4) . . ? C28 Fe3 C30 123.2(4) . . ? C24 Fe3 C31 120.7(4) . . ? C28 Fe3 C31 107.0(4) . . ? C30 Fe3 C31 40.4(4) . . ? C24 Fe3 C27 69.2(4) . . ? C28 Fe3 C27 40.9(4) . . ? C30 Fe3 C27 160.1(4) . . ? C31 Fe3 C27 124.0(5) . . ? C24 Fe3 C29 121.9(4) . . ? C28 Fe3 C29 158.9(4) . . ? C30 Fe3 C29 40.3(4) . . ? C31 Fe3 C29 68.6(5) . . ? C27 Fe3 C29 158.5(4) . . ? C24 Fe3 C25 41.0(4) . . ? C28 Fe3 C25 69.2(4) . . ? C30 Fe3 C25 120.7(4) . . ? C31 Fe3 C25 156.2(4) . . ? C27 Fe3 C25 69.3(4) . . ? C29 Fe3 C25 106.0(5) . . ? C24 Fe3 C26 69.3(4) . . ? C28 Fe3 C26 68.5(4) . . ? C30 Fe3 C26 157.9(4) . . ? C31 Fe3 C26 160.5(4) . . ? C27 Fe3 C26 40.3(4) . . ? C29 Fe3 C26 122.5(5) . . ? C25 Fe3 C26 41.9(4) . . ? C24 Fe3 C32 157.2(4) . . ? C28 Fe3 C32 121.9(4) . . ? C30 Fe3 C32 68.4(5) . . ? C31 Fe3 C32 41.0(4) . . ? C27 Fe3 C32 107.9(4) . . ? C29 Fe3 C32 69.2(5) . . ? C25 Fe3 C32 161.0(4) . . ? C26 Fe3 C32 124.0(4) . . ? C24 Fe3 C33 159.1(5) . . ? C28 Fe3 C33 158.7(4) . . ? C30 Fe3 C33 68.2(4) . . ? C31 Fe3 C33 69.0(4) . . ? C27 Fe3 C33 122.9(4) . . ? C29 Fe3 C33 40.9(4) . . ? C25 Fe3 C33 123.1(4) . . ? C26 Fe3 C33 107.9(4) . . ? C32 Fe3 C33 41.4(4) . . ? C1 O1 Bi1 88.8(5) . . ? C1 O2 Bi1 98.4(5) . . ? C12 O3 Bi1 84.3(5) . . ? C12 O3 Bi1 150.4(6) . 2_665 ? Bi1 O3 Bi1 124.3(2) . 2_665 ? C12 O4 Bi1 101.8(6) . . ? C23 O5 Bi1 82.8(6) . . ? C23 O6 Bi1 100.7(5) . . ? O1 C1 O2 117.6(8) . . ? O1 C1 C2 122.9(9) . . ? O2 C1 C2 119.5(8) . . ? O1 C1 Bi1 63.6(5) . . ? O2 C1 Bi1 54.0(4) . . ? C2 C1 Bi1 173.4(7) . . ? C3 C2 C6 108.4(9) . . ? C3 C2 C1 127.7(9) . . ? C6 C2 C1 123.4(9) . . ? C3 C2 Fe1 69.5(5) . . ? C6 C2 Fe1 69.0(5) . . ? C1 C2 Fe1 120.8(6) . . ? C2 C3 C4 105.9(9) . . ? C2 C3 Fe1 69.6(5) . . ? C4 C3 Fe1 70.0(5) . . ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? Fe1 C3 H3 127.0 . . ? C5 C4 C3 109.5(9) . . ? C5 C4 Fe1 70.4(6) . . ? C3 C4 Fe1 68.8(5) . . ? C5 C4 H4 125.2 . . ? C3 C4 H4 125.2 . . ? Fe1 C4 H4 125.2 . . ? C4 C5 C6 108.5(9) . . ? C4 C5 Fe1 70.2(6) . . ? C6 C5 Fe1 68.7(6) . . ? C4 C5 H5 125.7 . . ? C6 C5 H5 125.7 . . ? Fe1 C5 H5 125.7 . . ? C5 C6 C2 107.6(9) . . ? C5 C6 Fe1 70.9(6) . . ? C2 C6 Fe1 69.8(5) . . ? C5 C6 H6 126.2 . . ? C2 C6 H6 126.2 . . ? Fe1 C6 H6 126.2 . . ? C11 C7 C8 107.0(11) . . ? C11 C7 Fe1 69.2(7) . . ? C8 C7 Fe1 68.5(6) . . ? C11 C7 H7 126.5 . . ? C8 C7 H7 126.5 . . ? Fe1 C7 H7 126.5 . . ? C7 C8 C9 107.7(10) . . ? C7 C8 Fe1 70.7(6) . . ? C9 C8 Fe1 67.7(6) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? Fe1 C8 H8 126.1 . . ? C10 C9 C8 105.4(10) . . ? C10 C9 Fe1 72.4(6) . . ? C8 C9 Fe1 68.7(6) . . ? C10 C9 H9 127.2 . . ? C8 C9 H9 127.2 . . ? Fe1 C9 H9 127.2 . . ? C9 C10 C11 110.1(11) . . ? C9 C10 Fe1 68.1(6) . . ? C11 C10 Fe1 68.7(6) . . ? C9 C10 H10 124.8 . . ? C11 C10 H10 124.8 . . ? Fe1 C10 H10 124.8 . . ? C7 C11 C10 109.6(11) . . ? C7 C11 Fe1 70.8(7) . . ? C10 C11 Fe1 70.9(6) . . ? C7 C11 H11 125.2 . . ? C10 C11 H11 125.2 . . ? Fe1 C11 H11 125.2 . . ? O3 C12 O4 121.3(8) . . ? O3 C12 C13 122.3(8) . . ? O4 C12 C13 116.4(8) . . ? O3 C12 Bi1 69.9(5) . . ? O4 C12 Bi1 51.7(4) . . ? C13 C12 Bi1 167.2(6) . . ? C14 C13 C17 109.6(8) . . ? C14 C13 C12 127.0(8) . . ? C17 C13 C12 123.4(9) . . ? C14 C13 Fe2 71.5(6) . . ? C17 C13 Fe2 70.5(6) . . ? C12 C13 Fe2 122.5(7) . . ? C15 C14 C13 106.2(9) . . ? C15 C14 Fe2 68.5(6) . . ? C13 C14 Fe2 67.8(6) . . ? C15 C14 H14 126.9 . . ? C13 C14 H14 126.9 . . ? Fe2 C14 H14 126.9 . . ? C16 C15 C14 109.2(9) . . ? C16 C15 Fe2 70.4(6) . . ? C14 C15 Fe2 71.1(6) . . ? C16 C15 H15 125.4 . . ? C14 C15 H15 125.4 . . ? Fe2 C15 H15 125.4 . . ? C15 C16 C17 109.7(9) . . ? C15 C16 Fe2 69.5(6) . . ? C17 C16 Fe2 70.1(6) . . ? C15 C16 H16 125.1 . . ? C17 C16 H16 125.1 . . ? Fe2 C16 H16 125.1 . . ? C16 C17 C13 105.3(9) . . ? C16 C17 Fe2 69.4(6) . . ? C13 C17 Fe2 67.9(6) . . ? C16 C17 H17 127.4 . . ? C13 C17 H17 127.4 . . ? Fe2 C17 H17 127.4 . . ? C19 C18 C22 109.0(15) . . ? C19 C18 Fe2 69.9(9) . . ? C22 C18 Fe2 71.8(9) . . ? C19 C18 H18 125.5 . . ? C22 C18 H18 125.5 . . ? Fe2 C18 H18 125.5 . . ? C18 C19 C20 108.6(15) . . ? C18 C19 Fe2 70.4(9) . . ? C20 C19 Fe2 69.5(8) . . ? C18 C19 H19 125.7 . . ? C20 C19 H19 125.7 . . ? Fe2 C19 H19 125.7 . . ? C19 C20 C21 105.1(14) . . ? C19 C20 Fe2 69.5(8) . . ? C21 C20 Fe2 69.6(8) . . ? C19 C20 H20 127.4 . . ? C21 C20 H20 127.4 . . ? Fe2 C20 H20 127.4 . . ? C22 C21 C20 108.9(15) . . ? C22 C21 Fe2 72.0(8) . . ? C20 C21 Fe2 69.0(8) . . ? C22 C21 H21 125.5 . . ? C20 C21 H21 125.5 . . ? Fe2 C21 H21 125.5 . . ? C21 C22 C18 108.3(15) . . ? C21 C22 Fe2 69.1(8) . . ? C18 C22 Fe2 68.7(8) . . ? C21 C22 H22 125.8 . . ? C18 C22 H22 125.8 . . ? Fe2 C22 H22 125.8 . . ? O5 C23 O6 122.2(9) . . ? O5 C23 C24 121.4(9) . . ? O6 C23 C24 116.4(9) . . ? O5 C23 Bi1 70.3(5) . . ? O6 C23 Bi1 51.9(4) . . ? C24 C23 Bi1 167.9(7) . . ? C25 C24 C28 108.3(8) . . ? C25 C24 C23 126.7(10) . . ? C28 C24 C23 124.4(9) . . ? C25 C24 Fe3 70.3(6) . . ? C28 C24 Fe3 69.5(6) . . ? C23 C24 Fe3 119.7(7) . . ? C24 C25 C26 106.6(9) . . ? C24 C25 Fe3 68.7(6) . . ? C26 C25 Fe3 69.1(5) . . ? C24 C25 H25 126.7 . . ? C26 C25 H25 126.7 . . ? Fe3 C25 H25 126.7 . . ? C27 C26 C25 108.2(9) . . ? C27 C26 Fe3 69.6(6) . . ? C25 C26 Fe3 69.0(6) . . ? C27 C26 H26 125.9 . . ? C25 C26 H26 125.9 . . ? Fe3 C26 H26 125.9 . . ? C26 C27 C28 108.4(9) . . ? C26 C27 Fe3 70.1(6) . . ? C28 C27 Fe3 69.1(6) . . ? C26 C27 H27 125.8 . . ? C28 C27 H27 125.8 . . ? Fe3 C27 H27 125.8 . . ? C27 C28 C24 108.5(9) . . ? C27 C28 Fe3 70.0(6) . . ? C24 C28 Fe3 69.3(6) . . ? C27 C28 H28 125.8 . . ? C24 C28 H28 125.8 . . ? Fe3 C28 H28 125.8 . . ? C30 C29 C33 107.5(11) . . ? C30 C29 Fe3 69.3(6) . . ? C33 C29 Fe3 69.9(6) . . ? C30 C29 H29 126.2 . . ? C33 C29 H29 126.2 . . ? Fe3 C29 H29 126.2 . . ? C29 C30 C31 109.9(10) . . ? C29 C30 Fe3 70.3(6) . . ? C31 C30 Fe3 69.9(6) . . ? C29 C30 H30 125.1 . . ? C31 C30 H30 125.1 . . ? Fe3 C30 H30 125.1 . . ? C30 C31 C32 108.0(10) . . ? C30 C31 Fe3 69.6(6) . . ? C32 C31 Fe3 70.1(6) . . ? C30 C31 H31 126.0 . . ? C32 C31 H31 126.0 . . ? Fe3 C31 H31 126.0 . . ? C31 C32 C33 107.0(10) . . ? C31 C32 Fe3 69.0(6) . . ? C33 C32 Fe3 69.4(6) . . ? C31 C32 H32 126.5 . . ? C33 C32 H32 126.5 . . ? Fe3 C32 H32 126.5 . . ? C29 C33 C32 107.6(10) . . ? C29 C33 Fe3 69.2(6) . . ? C32 C33 Fe3 69.2(6) . . ? C29 C33 H33 126.2 . . ? C32 C33 H33 126.2 . . ? Fe3 C33 H33 126.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.646 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.160 data_3 _database_code_depnum_ccdc_archive 'CCDC 885530' #TrackingRef '- Final cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H82 Bi2 Fe8 O20' _chemical_formula_weight 2324.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.651(5) _cell_length_b 14.309(5) _cell_length_c 28.339(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 92.384(5) _cell_angle_gamma 90.000(5) _cell_volume 3910(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6708 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 5.997 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3846 _exptl_absorpt_correction_T_max 0.6966 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20482 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7247 _reflns_number_gt 6206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In case of the H atoms bound to oxygen atoms of the water molecule (H100 H101 H102 H103) the O-H bond length are restrained (DFIX). ; _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^)+(0.0358P)^2^+0.9319P] 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 7247 _refine_ls_number_parameters 549 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.313963(17) 0.420379(12) 0.514749(6) 0.01357(7) Uani 1 1 d . . . Fe1 Fe -0.05510(7) 0.15709(5) 0.44079(2) 0.01629(15) Uani 1 1 d . . . Fe2 Fe 0.46508(7) 0.37346(5) 0.32766(2) 0.01469(15) Uani 1 1 d . . . Fe3 Fe 0.52146(7) 0.12293(5) 0.62001(2) 0.01699(16) Uani 1 1 d . . . Fe4 Fe 0.06292(7) 0.35572(5) 0.73071(2) 0.01611(16) Uani 1 1 d . . . O1 O 0.1799(3) 0.2876(2) 0.52751(11) 0.0160(7) Uani 1 1 d . . . O2 O 0.0677(3) 0.3848(2) 0.47931(12) 0.0203(8) Uani 1 1 d . . . O3 O 0.3569(3) 0.3322(2) 0.44884(10) 0.0169(7) Uani 1 1 d . . . O4 O 0.5177(3) 0.4415(2) 0.45645(11) 0.0175(7) Uani 1 1 d . . . O5 O 0.4998(3) 0.3285(2) 0.54138(10) 0.0165(7) Uani 1 1 d . . . O6 O 0.3651(3) 0.3640(2) 0.59993(11) 0.0180(7) Uani 1 1 d . . . O7 O 0.1060(3) 0.2364(2) 0.61489(11) 0.0208(7) Uani 1 1 d . . . H7 H 0.1293 0.2486 0.5873 0.031 Uiso 1 1 calc R . . O8 O -0.0323(3) 0.3604(2) 0.60204(11) 0.0213(8) Uani 1 1 d . . . O9 O 0.2531(4) 0.5628(2) 0.45745(13) 0.0236(8) Uani 1 1 d D . . O10 O 0.1300(4) 0.5044(3) 0.56760(13) 0.0209(8) Uani 1 1 d D . . C1 C 0.0708(5) 0.3085(3) 0.50106(16) 0.0169(10) Uani 1 1 d . . . C2 C -0.0427(5) 0.2410(3) 0.49819(15) 0.0158(10) Uani 1 1 d . . . C3 C -0.0374(5) 0.1452(3) 0.51230(16) 0.0157(10) Uani 1 1 d . . . H3 H 0.0405 0.1143 0.5307 0.019 Uiso 1 1 calc R . . C4 C -0.1616(5) 0.1012(4) 0.49536(17) 0.0199(11) Uani 1 1 d . . . H4 H -0.1858 0.0338 0.4993 0.024 Uiso 1 1 calc R . . C5 C -0.2439(5) 0.1687(3) 0.47119(17) 0.0208(11) Uani 1 1 d . . . H5 H -0.3362 0.1570 0.4549 0.025 Uiso 1 1 calc R . . C6 C -0.1718(5) 0.2551(3) 0.47213(15) 0.0165(10) Uani 1 1 d . . . H6 H -0.2054 0.3151 0.4576 0.020 Uiso 1 1 calc R . . C7 C -0.0120(6) 0.0545(4) 0.39319(18) 0.0287(13) Uani 1 1 d . . . H7A H -0.0382 -0.0130 0.3952 0.034 Uiso 1 1 calc R . . C8 C -0.0914(6) 0.1270(4) 0.37096(17) 0.0274(12) Uani 1 1 d . . . H8 H -0.1847 0.1194 0.3547 0.033 Uiso 1 1 calc R . . C9 C -0.0178(5) 0.2114(4) 0.37657(16) 0.0239(12) Uani 1 1 d . . . H9 H -0.0494 0.2740 0.3646 0.029 Uiso 1 1 calc R . . C10 C 0.1094(5) 0.1926(4) 0.40158(17) 0.0278(12) Uani 1 1 d . . . H10 H 0.1830 0.2393 0.4105 0.033 Uiso 1 1 calc R . . C11 C 0.1130(5) 0.0966(4) 0.41200(17) 0.0256(12) Uani 1 1 d . . . H11 H 0.1896 0.0634 0.4299 0.031 Uiso 1 1 calc R . . C12 C 0.4673(5) 0.3715(3) 0.43488(16) 0.0159(10) Uani 1 1 d . . . C13 C 0.5322(5) 0.3333(3) 0.39284(16) 0.0167(10) Uani 1 1 d . . . C14 C 0.4844(5) 0.2547(3) 0.36614(16) 0.0176(10) Uani 1 1 d . . . H14 H 0.4073 0.2118 0.3744 0.021 Uiso 1 1 calc R . . C15 C 0.5670(5) 0.2475(3) 0.32543(16) 0.0199(11) Uani 1 1 d . . . H15 H 0.5561 0.1995 0.2999 0.024 Uiso 1 1 calc R . . C16 C 0.6643(5) 0.3225(3) 0.32689(16) 0.0191(11) Uani 1 1 d . . . H16 H 0.7332 0.3364 0.3024 0.023 Uiso 1 1 calc R . . C17 C 0.6445(5) 0.3754(3) 0.36867(15) 0.0154(10) Uani 1 1 d . . . H17 H 0.6978 0.4323 0.3790 0.018 Uiso 1 1 calc R . . C18 C 0.2996(5) 0.4560(4) 0.33860(19) 0.0303(13) Uani 1 1 d . . . H18 H 0.2566 0.4673 0.3696 0.036 Uiso 1 1 calc R . . C19 C 0.2626(5) 0.3840(4) 0.30584(19) 0.0271(12) Uani 1 1 d . . . H19 H 0.1894 0.3355 0.3097 0.032 Uiso 1 1 calc R . . C20 C 0.3473(5) 0.3941(4) 0.26652(17) 0.0244(12) Uani 1 1 d . . . H20 H 0.3458 0.3529 0.2380 0.029 Uiso 1 1 calc R . . C21 C 0.4375(5) 0.4707(3) 0.27527(17) 0.0220(11) Uani 1 1 d . . . H21 H 0.5102 0.4934 0.2539 0.026 Uiso 1 1 calc R . . C22 C 0.4076(6) 0.5089(4) 0.31956(18) 0.0268(12) Uani 1 1 d . . . H22 H 0.4549 0.5639 0.3349 0.032 Uiso 1 1 calc R . . C23 C 0.4676(5) 0.3220(3) 0.58522(15) 0.0148(10) Uani 1 1 d . . . C24 C 0.5566(5) 0.2618(3) 0.61614(16) 0.0156(10) Uani 1 1 d . . . C25 C 0.6762(5) 0.2106(3) 0.60227(17) 0.0190(11) Uani 1 1 d . . . H25 H 0.7205 0.2139 0.5710 0.023 Uiso 1 1 calc R . . C26 C 0.7215(5) 0.1548(4) 0.64209(18) 0.0259(12) Uani 1 1 d . . . H26 H 0.8017 0.1105 0.6431 0.031 Uiso 1 1 calc R . . C27 C 0.6303(5) 0.1707(4) 0.67931(18) 0.0267(12) Uani 1 1 d . . . H27 H 0.6354 0.1391 0.7108 0.032 Uiso 1 1 calc R . . C28 C 0.5285(5) 0.2362(3) 0.66386(16) 0.0181(10) Uani 1 1 d . . . H28 H 0.4506 0.2601 0.6827 0.022 Uiso 1 1 calc R . . C29 C 0.3613(6) 0.0933(4) 0.5736(2) 0.0286(13) Uani 1 1 d . . . H29 H 0.3112 0.1395 0.5526 0.034 Uiso 1 1 calc R . . C30 C 0.4805(6) 0.0421(4) 0.56202(19) 0.0318(13) Uani 1 1 d . . . H30 H 0.5289 0.0448 0.5315 0.038 Uiso 1 1 calc R . . C31 C 0.5188(5) -0.0143(4) 0.6022(2) 0.0321(13) Uani 1 1 d . . . H31 H 0.5996 -0.0581 0.6048 0.039 Uiso 1 1 calc R . . C32 C 0.4231(5) 0.0020(4) 0.6372(2) 0.0294(13) Uani 1 1 d . . . H32 H 0.4246 -0.0276 0.6692 0.035 Uiso 1 1 calc R . . C33 C 0.3255(5) 0.0688(3) 0.6198(2) 0.0261(12) Uani 1 1 d . . . H33 H 0.2460 0.0945 0.6373 0.031 Uiso 1 1 calc R . . C34 C 0.0140(5) 0.2984(3) 0.62814(16) 0.0155(10) Uani 1 1 d . . . C35 C -0.0293(5) 0.2846(3) 0.67646(16) 0.0163(10) Uani 1 1 d . . . C36 C 0.0260(5) 0.2209(3) 0.71107(16) 0.0168(10) Uani 1 1 d . . . H36 H 0.0976 0.1718 0.7060 0.020 Uiso 1 1 calc R . . C37 C -0.0392(5) 0.2389(3) 0.75341(16) 0.0191(11) Uani 1 1 d . . . H37 H -0.0198 0.2058 0.7841 0.023 Uiso 1 1 calc R . . C38 C -0.1344(5) 0.3146(3) 0.74604(17) 0.0212(11) Uani 1 1 d . . . H38 H -0.1938 0.3430 0.7703 0.025 Uiso 1 1 calc R . . C39 C -0.1285(5) 0.3425(4) 0.69813(17) 0.0221(11) Uani 1 1 d . . . H39 H -0.1838 0.3937 0.6824 0.027 Uiso 1 1 calc R . . C40 C 0.2321(5) 0.4226(3) 0.70570(19) 0.0245(12) Uani 1 1 d . . . H40 H 0.2711 0.4132 0.6739 0.029 Uiso 1 1 calc R . . C41 C 0.2707(5) 0.3734(4) 0.74670(18) 0.0224(11) Uani 1 1 d . . . H41 H 0.3415 0.3224 0.7492 0.027 Uiso 1 1 calc R . . C42 C 0.1904(5) 0.4068(4) 0.78411(18) 0.0263(12) Uani 1 1 d . . . H42 H 0.1955 0.3841 0.8175 0.032 Uiso 1 1 calc R . . C43 C 0.1033(6) 0.4791(4) 0.7658(2) 0.0315(13) Uani 1 1 d . . . H43 H 0.0356 0.5161 0.7839 0.038 Uiso 1 1 calc R . . C44 C 0.1270(6) 0.4881(4) 0.7168(2) 0.0308(13) Uani 1 1 d . . . H44 H 0.0802 0.5333 0.6944 0.037 Uiso 1 1 calc R . . H102 H 0.080(5) 0.543(3) 0.5535(19) 0.042(19) Uiso 1 1 d D . . H101 H 0.313(4) 0.603(2) 0.4571(16) 0.010(13) Uiso 1 1 d D . . H100 H 0.191(4) 0.587(3) 0.4414(17) 0.030(17) Uiso 1 1 d D . . H103 H 0.080(5) 0.464(3) 0.579(2) 0.05(2) 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 0.01176(11) 0.01471(10) 0.01419(10) 0.00104(7) -0.00001(7) -0.00098(7) Fe1 0.0145(4) 0.0197(4) 0.0146(3) -0.0006(3) 0.0008(3) -0.0025(3) Fe2 0.0138(4) 0.0138(3) 0.0163(3) -0.0007(3) -0.0003(3) 0.0007(3) Fe3 0.0163(4) 0.0133(4) 0.0211(4) 0.0007(3) -0.0024(3) -0.0020(3) Fe4 0.0155(4) 0.0158(4) 0.0171(3) 0.0005(3) 0.0021(3) -0.0007(3) O1 0.0119(17) 0.0183(17) 0.0174(16) 0.0003(14) -0.0023(13) 0.0015(13) O2 0.0138(18) 0.0184(18) 0.0285(19) -0.0043(15) -0.0005(15) -0.0010(14) O3 0.0143(18) 0.0215(18) 0.0151(16) -0.0007(14) 0.0027(14) -0.0031(14) O4 0.0157(18) 0.0196(18) 0.0171(16) 0.0003(14) -0.0012(14) -0.0028(14) O5 0.0154(17) 0.0215(18) 0.0123(15) 0.0018(14) -0.0028(13) 0.0017(14) O6 0.0177(18) 0.0184(18) 0.0178(17) -0.0017(14) 0.0003(14) -0.0012(14) O7 0.0242(19) 0.0222(19) 0.0162(17) 0.0043(15) 0.0048(15) 0.0013(15) O8 0.0189(19) 0.025(2) 0.0192(17) 0.0088(15) -0.0025(15) 0.0004(15) O9 0.017(2) 0.018(2) 0.035(2) 0.0123(17) -0.0071(17) -0.0039(16) O10 0.0168(19) 0.020(2) 0.0263(19) 0.0061(16) 0.0001(16) 0.0024(16) C1 0.017(3) 0.020(3) 0.015(2) -0.006(2) 0.004(2) 0.000(2) C2 0.013(2) 0.022(3) 0.012(2) -0.002(2) 0.0014(19) -0.001(2) C3 0.016(3) 0.017(2) 0.015(2) 0.0014(19) 0.0030(19) 0.001(2) C4 0.018(3) 0.025(3) 0.017(2) 0.000(2) 0.004(2) -0.008(2) C5 0.015(3) 0.025(3) 0.022(3) -0.006(2) -0.003(2) -0.006(2) C6 0.011(2) 0.022(3) 0.016(2) -0.001(2) 0.0018(19) 0.003(2) C7 0.039(3) 0.027(3) 0.022(3) -0.005(2) 0.013(2) -0.004(3) C8 0.026(3) 0.039(3) 0.018(3) -0.007(2) 0.008(2) -0.007(3) C9 0.027(3) 0.031(3) 0.014(2) 0.005(2) 0.006(2) -0.002(2) C10 0.027(3) 0.039(3) 0.018(3) -0.008(2) 0.008(2) -0.008(3) C11 0.020(3) 0.044(3) 0.014(2) -0.001(2) 0.006(2) 0.008(2) C12 0.015(3) 0.015(2) 0.017(2) 0.004(2) -0.005(2) 0.004(2) C13 0.016(3) 0.016(2) 0.017(2) 0.004(2) -0.004(2) 0.001(2) C14 0.012(2) 0.015(2) 0.026(3) 0.008(2) -0.002(2) 0.0042(19) C15 0.021(3) 0.019(3) 0.019(2) -0.002(2) -0.005(2) 0.004(2) C16 0.016(3) 0.022(3) 0.019(2) 0.007(2) -0.003(2) 0.003(2) C17 0.010(2) 0.021(3) 0.015(2) 0.002(2) -0.0026(19) 0.000(2) C18 0.022(3) 0.043(3) 0.027(3) 0.003(3) 0.001(2) 0.019(3) C19 0.014(3) 0.026(3) 0.040(3) 0.004(3) -0.008(2) 0.000(2) C20 0.030(3) 0.024(3) 0.018(3) -0.001(2) -0.011(2) 0.005(2) C21 0.021(3) 0.022(3) 0.022(3) 0.007(2) -0.005(2) 0.002(2) C22 0.037(3) 0.017(3) 0.026(3) 0.000(2) -0.009(2) 0.001(2) C23 0.017(3) 0.013(2) 0.013(2) -0.0028(19) 0.0010(19) -0.008(2) C24 0.016(3) 0.010(2) 0.020(2) -0.0040(19) -0.001(2) -0.0047(19) C25 0.016(3) 0.018(3) 0.022(2) 0.006(2) -0.001(2) -0.005(2) C26 0.022(3) 0.024(3) 0.031(3) 0.002(2) -0.010(2) -0.005(2) C27 0.032(3) 0.023(3) 0.025(3) 0.006(2) -0.008(2) -0.011(2) C28 0.022(3) 0.016(2) 0.016(2) -0.006(2) -0.003(2) -0.008(2) C29 0.025(3) 0.026(3) 0.033(3) -0.007(2) -0.016(3) -0.007(2) C30 0.041(4) 0.023(3) 0.031(3) -0.011(2) 0.001(3) -0.014(3) C31 0.020(3) 0.018(3) 0.058(4) 0.000(3) -0.001(3) 0.000(2) C32 0.028(3) 0.017(3) 0.043(3) 0.009(2) 0.001(3) -0.007(2) C33 0.016(3) 0.018(3) 0.044(3) -0.009(2) 0.002(2) -0.005(2) C34 0.011(2) 0.014(2) 0.021(2) -0.001(2) -0.0007(19) -0.0053(19) C35 0.016(3) 0.014(2) 0.019(2) 0.004(2) -0.001(2) -0.0021(19) C36 0.015(2) 0.015(2) 0.020(2) 0.001(2) -0.002(2) -0.0048(19) C37 0.016(3) 0.021(3) 0.019(2) 0.005(2) -0.004(2) -0.006(2) C38 0.016(3) 0.025(3) 0.023(3) -0.003(2) 0.008(2) -0.003(2) C39 0.016(3) 0.025(3) 0.026(3) 0.006(2) 0.002(2) -0.002(2) C40 0.018(3) 0.023(3) 0.033(3) -0.004(2) 0.003(2) -0.012(2) C41 0.013(3) 0.025(3) 0.030(3) -0.004(2) 0.000(2) -0.008(2) C42 0.026(3) 0.033(3) 0.020(3) -0.005(2) 0.002(2) -0.014(2) C43 0.027(3) 0.026(3) 0.042(3) -0.013(3) 0.009(3) -0.010(2) C44 0.039(3) 0.015(3) 0.038(3) 0.006(2) -0.007(3) -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 O3 2.306(3) . ? Bi1 O5 2.324(3) . ? Bi1 O1 2.335(3) . ? Bi1 O6 2.574(3) . ? Bi1 O2 2.592(3) . ? Bi1 O4 2.638(3) . ? Bi1 O9 2.656(3) . ? Bi1 O10 2.658(4) . ? Bi1 O4 2.665(3) 3_666 ? Bi1 C23 2.815(5) . ? Bi1 C12 2.843(5) . ? Bi1 C1 2.854(5) . ? Fe1 C2 2.021(4) . ? Fe1 C9 2.025(5) . ? Fe1 C6 2.027(5) . ? Fe1 C3 2.034(4) . ? Fe1 C11 2.038(5) . ? Fe1 C10 2.040(5) . ? Fe1 C8 2.041(5) . ? Fe1 C7 2.048(5) . ? Fe1 C5 2.054(5) . ? Fe1 C4 2.054(5) . ? Fe2 C13 2.015(4) . ? Fe2 C18 2.021(5) . ? Fe2 C14 2.024(5) . ? Fe2 C22 2.026(5) . ? Fe2 C19 2.031(5) . ? Fe2 C21 2.044(5) . ? Fe2 C17 2.045(4) . ? Fe2 C20 2.054(5) . ? Fe2 C15 2.056(5) . ? Fe2 C16 2.057(5) . ? Fe3 C24 2.020(5) . ? Fe3 C31 2.028(5) . ? Fe3 C25 2.029(5) . ? Fe3 C29 2.032(5) . ? Fe3 C30 2.035(5) . ? Fe3 C28 2.041(5) . ? Fe3 C32 2.043(5) . ? Fe3 C33 2.043(5) . ? Fe3 C26 2.056(5) . ? Fe3 C27 2.061(5) . ? Fe4 C35 2.020(5) . ? Fe4 C36 2.036(5) . ? Fe4 C44 2.037(5) . ? Fe4 C39 2.039(5) . ? Fe4 C42 2.045(5) . ? Fe4 C40 2.045(5) . ? Fe4 C41 2.053(5) . ? Fe4 C43 2.056(5) . ? Fe4 C37 2.057(5) . ? Fe4 C38 2.057(5) . ? O1 C1 1.302(5) . ? O2 C1 1.253(6) . ? O3 C12 1.281(6) . ? O4 C12 1.260(5) . ? O4 Bi1 2.665(3) 3_666 ? O5 C23 1.296(5) . ? O6 C23 1.244(5) . ? O7 C34 1.321(5) . ? O7 H7 0.8400 . ? O8 C34 1.227(5) . ? O9 H101 0.813(19) . ? O9 H100 0.82(2) . ? O10 H102 0.83(2) . ? O10 H103 0.83(2) . ? C1 C2 1.461(6) . ? C2 C3 1.429(6) . ? C2 C6 1.436(6) . ? C3 C4 1.420(6) . ? C3 H3 1.0000 . ? C4 C5 1.410(7) . ? C4 H4 1.0000 . ? C5 C6 1.418(6) . ? C5 H5 1.0000 . ? C6 H6 1.0000 . ? C7 C8 1.421(8) . ? C7 C11 1.431(8) . ? C7 H7A 1.0000 . ? C8 C9 1.408(7) . ? C8 H8 1.0000 . ? C9 C10 1.418(7) . ? C9 H9 1.0000 . ? C10 C11 1.405(7) . ? C10 H10 1.0000 . ? C11 H11 1.0000 . ? C12 C13 1.474(6) . ? C13 C14 1.422(6) . ? C13 C17 1.438(6) . ? C14 C15 1.433(7) . ? C14 H14 1.0000 . ? C15 C16 1.426(7) . ? C15 H15 1.0000 . ? C16 C17 1.425(6) . ? C16 H16 1.0000 . ? C17 H17 1.0000 . ? C18 C22 1.413(8) . ? C18 C19 1.423(8) . ? C18 H18 1.0000 . ? C19 C20 1.416(8) . ? C19 H19 1.0000 . ? C20 C21 1.415(7) . ? C20 H20 1.0000 . ? C21 C22 1.410(7) . ? C21 H21 1.0000 . ? C22 H22 1.0000 . ? C23 C24 1.478(6) . ? C24 C25 1.436(6) . ? C24 C28 1.438(6) . ? C25 C26 1.435(7) . ? C25 H25 1.0000 . ? C26 C27 1.420(7) . ? C26 H26 1.0000 . ? C27 C28 1.414(7) . ? C27 H27 1.0000 . ? C28 H28 1.0000 . ? C29 C33 1.413(8) . ? C29 C30 1.414(8) . ? C29 H29 1.0000 . ? C30 C31 1.433(8) . ? C30 H30 1.0000 . ? C31 C32 1.404(8) . ? C31 H31 1.0000 . ? C32 C33 1.416(7) . ? C32 H32 1.0000 . ? C33 H33 1.0000 . ? C34 C35 1.462(6) . ? C35 C39 1.424(7) . ? C35 C36 1.426(6) . ? C36 C37 1.402(6) . ? C36 H36 1.0000 . ? C37 C38 1.429(7) . ? C37 H37 1.0000 . ? C38 C39 1.419(7) . ? C38 H38 1.0000 . ? C39 H39 1.0000 . ? C40 C41 1.396(7) . ? C40 C44 1.426(7) . ? C40 H40 1.0000 . ? C41 C42 1.422(7) . ? C41 H41 1.0000 . ? C42 C43 1.418(8) . ? C42 H42 1.0000 . ? C43 C44 1.423(7) . ? C43 H43 1.0000 . ? C44 H44 1.0000 . ? 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 O5 77.95(11) . . ? O3 Bi1 O1 78.46(11) . . ? O5 Bi1 O1 85.09(11) . . ? O3 Bi1 O6 123.67(11) . . ? O5 Bi1 O6 53.32(10) . . ? O1 Bi1 O6 71.66(10) . . ? O3 Bi1 O2 76.80(11) . . ? O5 Bi1 O2 134.22(11) . . ? O1 Bi1 O2 52.78(10) . . ? O6 Bi1 O2 116.02(10) . . ? O3 Bi1 O4 52.51(10) . . ? O5 Bi1 O4 71.53(11) . . ? O1 Bi1 O4 128.51(10) . . ? O6 Bi1 O4 120.32(10) . . ? O2 Bi1 O4 118.37(10) . . ? O3 Bi1 O9 88.12(12) . . ? O5 Bi1 O9 141.32(11) . . ? O1 Bi1 O9 127.51(11) . . ? O6 Bi1 O9 147.45(11) . . ? O2 Bi1 O9 74.80(11) . . ? O4 Bi1 O9 71.39(11) . . ? O3 Bi1 O10 148.32(11) . . ? O5 Bi1 O10 126.69(11) . . ? O1 Bi1 O10 83.88(11) . . ? O6 Bi1 O10 73.73(11) . . ? O2 Bi1 O10 71.58(11) . . ? O4 Bi1 O10 146.51(10) . . ? O9 Bi1 O10 82.02(12) . . ? O3 Bi1 O4 121.72(10) . 3_666 ? O5 Bi1 O4 82.39(11) . 3_666 ? O1 Bi1 O4 152.95(10) . 3_666 ? O6 Bi1 O4 81.64(10) . 3_666 ? O2 Bi1 O4 143.32(10) . 3_666 ? O4 Bi1 O4 69.26(11) . 3_666 ? O9 Bi1 O4 74.63(10) . 3_666 ? O10 Bi1 O4 84.55(11) . 3_666 ? O3 Bi1 C23 101.19(12) . . ? O5 Bi1 C23 27.14(12) . . ? O1 Bi1 C23 76.23(12) . . ? O6 Bi1 C23 26.21(11) . . ? O2 Bi1 C23 128.61(12) . . ? O4 Bi1 C23 96.75(12) . . ? O9 Bi1 C23 156.09(12) . . ? O10 Bi1 C23 99.85(12) . . ? O4 Bi1 C23 81.79(11) 3_666 . ? O3 Bi1 C12 26.26(12) . . ? O5 Bi1 C12 72.50(12) . . ? O1 Bi1 C12 103.50(12) . . ? O6 Bi1 C12 125.72(11) . . ? O2 Bi1 C12 98.19(12) . . ? O4 Bi1 C12 26.25(11) . . ? O9 Bi1 C12 79.13(12) . . ? O10 Bi1 C12 160.42(12) . . ? O4 Bi1 C12 95.47(12) 3_666 . ? C23 Bi1 C12 99.53(13) . . ? O3 Bi1 C1 75.98(12) . . ? O5 Bi1 C1 110.24(13) . . ? O1 Bi1 C1 26.74(12) . . ? O6 Bi1 C1 94.36(12) . . ? O2 Bi1 C1 26.04(12) . . ? O4 Bi1 C1 127.54(11) . . ? O9 Bi1 C1 100.80(13) . . ? O10 Bi1 C1 76.43(12) . . ? O4 Bi1 C1 160.92(11) 3_666 . ? C23 Bi1 C1 102.81(13) . . ? C12 Bi1 C1 101.90(13) . . ? C2 Fe1 C9 119.2(2) . . ? C2 Fe1 C6 41.55(17) . . ? C9 Fe1 C6 104.5(2) . . ? C2 Fe1 C3 41.25(18) . . ? C9 Fe1 C3 156.5(2) . . ? C6 Fe1 C3 69.30(18) . . ? C2 Fe1 C11 123.6(2) . . ? C9 Fe1 C11 68.2(2) . . ? C6 Fe1 C11 159.2(2) . . ? C3 Fe1 C11 109.15(19) . . ? C2 Fe1 C10 105.6(2) . . ? C9 Fe1 C10 40.8(2) . . ? C6 Fe1 C10 121.7(2) . . ? C3 Fe1 C10 121.9(2) . . ? C11 Fe1 C10 40.3(2) . . ? C2 Fe1 C8 155.2(2) . . ? C9 Fe1 C8 40.5(2) . . ? C6 Fe1 C8 119.7(2) . . ? C3 Fe1 C8 162.2(2) . . ? C11 Fe1 C8 68.3(2) . . ? C10 Fe1 C8 68.3(2) . . ? C2 Fe1 C7 161.6(2) . . ? C9 Fe1 C7 68.6(2) . . ? C6 Fe1 C7 156.4(2) . . ? C3 Fe1 C7 125.8(2) . . ? C11 Fe1 C7 41.0(2) . . ? C10 Fe1 C7 68.6(2) . . ? C8 Fe1 C7 40.7(2) . . ? C2 Fe1 C5 68.78(18) . . ? C9 Fe1 C5 122.7(2) . . ? C6 Fe1 C5 40.65(18) . . ? C3 Fe1 C5 68.16(19) . . ? C11 Fe1 C5 159.5(2) . . ? C10 Fe1 C5 158.8(2) . . ? C8 Fe1 C5 107.7(2) . . ? C7 Fe1 C5 122.8(2) . . ? C2 Fe1 C4 68.90(19) . . ? C9 Fe1 C4 159.9(2) . . ? C6 Fe1 C4 68.58(19) . . ? C3 Fe1 C4 40.63(18) . . ? C11 Fe1 C4 124.6(2) . . ? C10 Fe1 C4 158.8(2) . . ? C8 Fe1 C4 125.2(2) . . ? C7 Fe1 C4 109.8(2) . . ? C5 Fe1 C4 40.13(19) . . ? C13 Fe2 C18 104.6(2) . . ? C13 Fe2 C14 41.23(18) . . ? C18 Fe2 C14 117.7(2) . . ? C13 Fe2 C22 116.9(2) . . ? C18 Fe2 C22 40.9(2) . . ? C14 Fe2 C22 152.0(2) . . ? C13 Fe2 C19 124.7(2) . . ? C18 Fe2 C19 41.1(2) . . ? C14 Fe2 C19 107.0(2) . . ? C22 Fe2 C19 68.8(2) . . ? C13 Fe2 C21 152.49(19) . . ? C18 Fe2 C21 68.5(2) . . ? C14 Fe2 C21 165.8(2) . . ? C22 Fe2 C21 40.53(19) . . ? C19 Fe2 C21 68.5(2) . . ? C13 Fe2 C17 41.48(18) . . ? C18 Fe2 C17 124.1(2) . . ? C14 Fe2 C17 69.43(19) . . ? C22 Fe2 C17 105.8(2) . . ? C19 Fe2 C17 162.5(2) . . ? C21 Fe2 C17 119.00(19) . . ? C13 Fe2 C20 163.7(2) . . ? C18 Fe2 C20 68.4(2) . . ? C14 Fe2 C20 127.6(2) . . ? C22 Fe2 C20 68.1(2) . . ? C19 Fe2 C20 40.6(2) . . ? C21 Fe2 C20 40.4(2) . . ? C17 Fe2 C20 154.6(2) . . ? C13 Fe2 C15 69.04(19) . . ? C18 Fe2 C15 154.1(2) . . ? C14 Fe2 C15 41.12(19) . . ? C22 Fe2 C15 164.6(2) . . ? C19 Fe2 C15 120.8(2) . . ? C21 Fe2 C15 128.5(2) . . ? C17 Fe2 C15 68.58(19) . . ? C20 Fe2 C15 110.4(2) . . ? C13 Fe2 C16 69.13(19) . . ? C18 Fe2 C16 162.5(2) . . ? C14 Fe2 C16 69.08(19) . . ? C22 Fe2 C16 126.1(2) . . ? C19 Fe2 C16 155.6(2) . . ? C21 Fe2 C16 109.1(2) . . ? C17 Fe2 C16 40.65(18) . . ? C20 Fe2 C16 121.8(2) . . ? C15 Fe2 C16 40.57(18) . . ? C24 Fe3 C31 160.0(2) . . ? C24 Fe3 C25 41.55(18) . . ? C31 Fe3 C25 122.6(2) . . ? C24 Fe3 C29 107.2(2) . . ? C31 Fe3 C29 68.6(2) . . ? C25 Fe3 C29 121.1(2) . . ? C24 Fe3 C30 122.9(2) . . ? C31 Fe3 C30 41.3(2) . . ? C25 Fe3 C30 105.7(2) . . ? C29 Fe3 C30 40.7(2) . . ? C24 Fe3 C28 41.47(18) . . ? C31 Fe3 C28 156.9(2) . . ? C25 Fe3 C28 69.77(19) . . ? C29 Fe3 C28 124.4(2) . . ? C30 Fe3 C28 160.6(2) . . ? C24 Fe3 C32 158.0(2) . . ? C31 Fe3 C32 40.3(2) . . ? C25 Fe3 C32 159.5(2) . . ? C29 Fe3 C32 68.3(2) . . ? C30 Fe3 C32 68.6(2) . . ? C28 Fe3 C32 122.1(2) . . ? C24 Fe3 C33 122.01(19) . . ? C31 Fe3 C33 68.3(2) . . ? C25 Fe3 C33 157.5(2) . . ? C29 Fe3 C33 40.6(2) . . ? C30 Fe3 C33 68.5(2) . . ? C28 Fe3 C33 108.0(2) . . ? C32 Fe3 C33 40.6(2) . . ? C24 Fe3 C26 68.9(2) . . ? C31 Fe3 C26 107.0(2) . . ? C25 Fe3 C26 41.13(19) . . ? C29 Fe3 C26 157.3(2) . . ? C30 Fe3 C26 121.3(2) . . ? C28 Fe3 C26 68.4(2) . . ? C32 Fe3 C26 123.7(2) . . ? C33 Fe3 C26 160.4(2) . . ? C24 Fe3 C27 68.72(19) . . ? C31 Fe3 C27 121.6(2) . . ? C25 Fe3 C27 69.0(2) . . ? C29 Fe3 C27 160.9(2) . . ? C30 Fe3 C27 157.2(2) . . ? C28 Fe3 C27 40.33(19) . . ? C32 Fe3 C27 108.2(2) . . ? C33 Fe3 C27 124.6(2) . . ? C26 Fe3 C27 40.3(2) . . ? C35 Fe4 C36 41.18(17) . . ? C35 Fe4 C44 116.7(2) . . ? C36 Fe4 C44 151.6(2) . . ? C35 Fe4 C39 41.07(19) . . ? C36 Fe4 C39 69.08(19) . . ? C44 Fe4 C39 106.0(2) . . ? C35 Fe4 C42 167.4(2) . . ? C36 Fe4 C42 129.4(2) . . ? C44 Fe4 C42 68.5(2) . . ? C39 Fe4 C42 150.9(2) . . ? C35 Fe4 C40 107.8(2) . . ? C36 Fe4 C40 118.8(2) . . ? C44 Fe4 C40 40.9(2) . . ? C39 Fe4 C40 127.4(2) . . ? C42 Fe4 C40 68.0(2) . . ? C35 Fe4 C41 128.7(2) . . ? C36 Fe4 C41 109.6(2) . . ? C44 Fe4 C41 68.1(2) . . ? C39 Fe4 C41 165.8(2) . . ? C42 Fe4 C41 40.6(2) . . ? C40 Fe4 C41 39.8(2) . . ? C35 Fe4 C43 150.4(2) . . ? C36 Fe4 C43 166.9(2) . . ? C44 Fe4 C43 40.7(2) . . ? C39 Fe4 C43 116.7(2) . . ? C42 Fe4 C43 40.5(2) . . ? C40 Fe4 C43 68.1(2) . . ? C41 Fe4 C43 67.9(2) . . ? C35 Fe4 C37 68.08(18) . . ? C36 Fe4 C37 40.06(18) . . ? C44 Fe4 C37 165.9(2) . . ? C39 Fe4 C37 68.23(19) . . ? C42 Fe4 C37 109.9(2) . . ? C40 Fe4 C37 152.7(2) . . ? C41 Fe4 C37 120.5(2) . . ? C43 Fe4 C37 129.1(2) . . ? C35 Fe4 C38 68.51(19) . . ? C36 Fe4 C38 68.48(19) . . ? C44 Fe4 C38 126.8(2) . . ? C39 Fe4 C38 40.52(19) . . ? C42 Fe4 C38 118.7(2) . . ? C40 Fe4 C38 165.2(2) . . ? C41 Fe4 C38 153.3(2) . . ? C43 Fe4 C38 107.6(2) . . ? C37 Fe4 C38 40.66(19) . . ? C1 O1 Bi1 99.4(3) . . ? C1 O2 Bi1 88.7(3) . . ? C12 O3 Bi1 101.0(3) . . ? C12 O4 Bi1 86.0(3) . . ? C12 O4 Bi1 162.9(3) . 3_666 ? Bi1 O4 Bi1 110.73(11) . 3_666 ? C23 O5 Bi1 98.0(3) . . ? C23 O6 Bi1 87.8(3) . . ? C34 O7 H7 109.5 . . ? Bi1 O9 H101 114(3) . . ? Bi1 O9 H100 144(4) . . ? H101 O9 H100 101(5) . . ? Bi1 O10 H102 115(4) . . ? Bi1 O10 H103 108(5) . . ? H102 O10 H103 109(6) . . ? O2 C1 O1 119.0(4) . . ? O2 C1 C2 123.1(4) . . ? O1 C1 C2 117.8(4) . . ? O2 C1 Bi1 65.2(2) . . ? O1 C1 Bi1 53.8(2) . . ? C2 C1 Bi1 171.6(3) . . ? C3 C2 C6 107.4(4) . . ? C3 C2 C1 127.0(4) . . ? C6 C2 C1 124.6(4) . . ? C3 C2 Fe1 69.8(3) . . ? C6 C2 Fe1 69.4(3) . . ? C1 C2 Fe1 117.2(3) . . ? C4 C3 C2 108.1(4) . . ? C4 C3 Fe1 70.5(3) . . ? C2 C3 Fe1 68.9(3) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.0 . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Fe1 69.9(3) . . ? C3 C4 Fe1 68.9(3) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Fe1 C4 H4 125.9 . . ? C4 C5 C6 108.8(4) . . ? C4 C5 Fe1 69.9(3) . . ? C6 C5 Fe1 68.6(3) . . ? C4 C5 H5 125.6 . . ? C6 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C5 C6 C2 107.5(4) . . ? C5 C6 Fe1 70.7(3) . . ? C2 C6 Fe1 69.0(3) . . ? C5 C6 H6 126.2 . . ? C2 C6 H6 126.2 . . ? Fe1 C6 H6 126.2 . . ? C8 C7 C11 106.8(5) . . ? C8 C7 Fe1 69.4(3) . . ? C11 C7 Fe1 69.1(3) . . ? C8 C7 H7A 126.6 . . ? C11 C7 H7A 126.6 . . ? Fe1 C7 H7A 126.6 . . ? C9 C8 C7 108.4(5) . . ? C9 C8 Fe1 69.1(3) . . ? C7 C8 Fe1 69.9(3) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe1 C8 H8 125.8 . . ? C8 C9 C10 108.4(5) . . ? C8 C9 Fe1 70.4(3) . . ? C10 C9 Fe1 70.1(3) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe1 C9 H9 125.8 . . ? C11 C10 C9 107.7(5) . . ? C11 C10 Fe1 69.8(3) . . ? C9 C10 Fe1 69.0(3) . . ? C11 C10 H10 126.2 . . ? C9 C10 H10 126.2 . . ? Fe1 C10 H10 126.2 . . ? C10 C11 C7 108.7(5) . . ? C10 C11 Fe1 69.9(3) . . ? C7 C11 Fe1 69.8(3) . . ? C10 C11 H11 125.6 . . ? C7 C11 H11 125.6 . . ? Fe1 C11 H11 125.6 . . ? O4 C12 O3 120.5(4) . . ? O4 C12 C13 121.2(4) . . ? O3 C12 C13 118.3(4) . . ? O4 C12 Bi1 67.8(2) . . ? O3 C12 Bi1 52.8(2) . . ? C13 C12 Bi1 171.0(3) . . ? C14 C13 C17 108.2(4) . . ? C14 C13 C12 125.7(4) . . ? C17 C13 C12 125.7(4) . . ? C14 C13 Fe2 69.7(3) . . ? C17 C13 Fe2 70.4(3) . . ? C12 C13 Fe2 120.2(3) . . ? C13 C14 C15 107.8(4) . . ? C13 C14 Fe2 69.1(3) . . ? C15 C14 Fe2 70.6(3) . . ? C13 C14 H14 126.1 . . ? C15 C14 H14 126.1 . . ? Fe2 C14 H14 126.1 . . ? C16 C15 C14 108.1(4) . . ? C16 C15 Fe2 69.8(3) . . ? C14 C15 Fe2 68.2(3) . . ? C16 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Fe2 C15 H15 126.0 . . ? C17 C16 C15 108.3(4) . . ? C17 C16 Fe2 69.2(3) . . ? C15 C16 Fe2 69.7(3) . . ? C17 C16 H16 125.9 . . ? C15 C16 H16 125.9 . . ? Fe2 C16 H16 125.9 . . ? C16 C17 C13 107.6(4) . . ? C16 C17 Fe2 70.1(3) . . ? C13 C17 Fe2 68.1(2) . . ? C16 C17 H17 126.2 . . ? C13 C17 H17 126.2 . . ? Fe2 C17 H17 126.2 . . ? C22 C18 C19 107.9(5) . . ? C22 C18 Fe2 69.7(3) . . ? C19 C18 Fe2 69.8(3) . . ? C22 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? Fe2 C18 H18 126.1 . . ? C20 C19 C18 107.6(5) . . ? C20 C19 Fe2 70.6(3) . . ? C18 C19 Fe2 69.1(3) . . ? C20 C19 H19 126.2 . . ? C18 C19 H19 126.2 . . ? Fe2 C19 H19 126.2 . . ? C21 C20 C19 108.2(5) . . ? C21 C20 Fe2 69.4(3) . . ? C19 C20 Fe2 68.8(3) . . ? C21 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? Fe2 C20 H20 125.9 . . ? C22 C21 C20 108.0(5) . . ? C22 C21 Fe2 69.1(3) . . ? C20 C21 Fe2 70.2(3) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Fe2 C21 H21 126.0 . . ? C21 C22 C18 108.3(5) . . ? C21 C22 Fe2 70.4(3) . . ? C18 C22 Fe2 69.4(3) . . ? C21 C22 H22 125.9 . . ? C18 C22 H22 125.9 . . ? Fe2 C22 H22 125.9 . . ? O6 C23 O5 120.8(4) . . ? O6 C23 C24 122.2(4) . . ? O5 C23 C24 117.0(4) . . ? O6 C23 Bi1 66.0(2) . . ? O5 C23 Bi1 54.8(2) . . ? C24 C23 Bi1 171.1(3) . . ? C25 C24 C28 108.2(4) . . ? C25 C24 C23 126.1(4) . . ? C28 C24 C23 125.3(4) . . ? C25 C24 Fe3 69.6(3) . . ? C28 C24 Fe3 70.1(3) . . ? C23 C24 Fe3 120.7(3) . . ? C26 C25 C24 106.9(4) . . ? C26 C25 Fe3 70.4(3) . . ? C24 C25 Fe3 68.9(3) . . ? C26 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? Fe3 C25 H25 126.5 . . ? C27 C26 C25 108.5(5) . . ? C27 C26 Fe3 70.0(3) . . ? C25 C26 Fe3 68.4(3) . . ? C27 C26 H26 125.7 . . ? C25 C26 H26 125.7 . . ? Fe3 C26 H26 125.7 . . ? C28 C27 C26 108.7(4) . . ? C28 C27 Fe3 69.1(3) . . ? C26 C27 Fe3 69.6(3) . . ? C28 C27 H27 125.7 . . ? C26 C27 H27 125.7 . . ? Fe3 C27 H27 125.7 . . ? C27 C28 C24 107.7(4) . . ? C27 C28 Fe3 70.6(3) . . ? C24 C28 Fe3 68.5(3) . . ? C27 C28 H28 126.1 . . ? C24 C28 H28 126.1 . . ? Fe3 C28 H28 126.1 . . ? C33 C29 C30 108.6(5) . . ? C33 C29 Fe3 70.1(3) . . ? C30 C29 Fe3 69.8(3) . . ? C33 C29 H29 125.7 . . ? C30 C29 H29 125.7 . . ? Fe3 C29 H29 125.7 . . ? C29 C30 C31 107.0(5) . . ? C29 C30 Fe3 69.5(3) . . ? C31 C30 Fe3 69.1(3) . . ? C29 C30 H30 126.5 . . ? C31 C30 H30 126.5 . . ? Fe3 C30 H30 126.5 . . ? C32 C31 C30 108.2(5) . . ? C32 C31 Fe3 70.4(3) . . ? C30 C31 Fe3 69.6(3) . . ? C32 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? Fe3 C31 H31 125.9 . . ? C31 C32 C33 108.3(5) . . ? C31 C32 Fe3 69.3(3) . . ? C33 C32 Fe3 69.7(3) . . ? C31 C32 H32 125.8 . . ? C33 C32 H32 125.8 . . ? Fe3 C32 H32 125.8 . . ? C29 C33 C32 107.8(5) . . ? C29 C33 Fe3 69.3(3) . . ? C32 C33 Fe3 69.7(3) . . ? C29 C33 H33 126.1 . . ? C32 C33 H33 126.1 . . ? Fe3 C33 H33 126.1 . . ? O8 C34 O7 123.1(4) . . ? O8 C34 C35 123.5(4) . . ? O7 C34 C35 113.4(4) . . ? C39 C35 C36 108.3(4) . . ? C39 C35 C34 123.3(4) . . ? C36 C35 C34 128.1(4) . . ? C39 C35 Fe4 70.2(3) . . ? C36 C35 Fe4 70.0(3) . . ? C34 C35 Fe4 120.7(3) . . ? C37 C36 C35 107.6(4) . . ? C37 C36 Fe4 70.8(3) . . ? C35 C36 Fe4 68.8(3) . . ? C37 C36 H36 126.2 . . ? C35 C36 H36 126.2 . . ? Fe4 C36 H36 126.2 . . ? C36 C37 C38 108.9(4) . . ? C36 C37 Fe4 69.2(3) . . ? C38 C37 Fe4 69.7(3) . . ? C36 C37 H37 125.6 . . ? C38 C37 H37 125.6 . . ? Fe4 C37 H37 125.6 . . ? C39 C38 C37 107.6(4) . . ? C39 C38 Fe4 69.1(3) . . ? C37 C38 Fe4 69.7(3) . . ? C39 C38 H38 126.2 . . ? C37 C38 H38 126.2 . . ? Fe4 C38 H38 126.2 . . ? C38 C39 C35 107.7(4) . . ? C38 C39 Fe4 70.4(3) . . ? C35 C39 Fe4 68.7(3) . . ? C38 C39 H39 126.2 . . ? C35 C39 H39 126.2 . . ? Fe4 C39 H39 126.2 . . ? C41 C40 C44 108.4(5) . . ? C41 C40 Fe4 70.4(3) . . ? C44 C40 Fe4 69.2(3) . . ? C41 C40 H40 125.8 . . ? C44 C40 H40 125.8 . . ? Fe4 C40 H40 125.8 . . ? C40 C41 C42 108.4(5) . . ? C40 C41 Fe4 69.8(3) . . ? C42 C41 Fe4 69.4(3) . . ? C40 C41 H41 125.8 . . ? C42 C41 H41 125.8 . . ? Fe4 C41 H41 125.8 . . ? C43 C42 C41 107.8(5) . . ? C43 C42 Fe4 70.2(3) . . ? C41 C42 Fe4 70.0(3) . . ? C43 C42 H42 126.1 . . ? C41 C42 H42 126.1 . . ? Fe4 C42 H42 126.1 . . ? C42 C43 C44 107.8(5) . . ? C42 C43 Fe4 69.4(3) . . ? C44 C43 Fe4 68.9(3) . . ? C42 C43 H43 126.1 . . ? C44 C43 H43 126.1 . . ? Fe4 C43 H43 126.1 . . ? C43 C44 C40 107.5(5) . . ? C43 C44 Fe4 70.4(3) . . ? C40 C44 Fe4 69.9(3) . . ? C43 C44 H44 126.3 . . ? C40 C44 H44 126.3 . . ? Fe4 C44 H44 126.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.837 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.144