# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1813 data_tom _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H63 Fe3 O6 Sb' _chemical_formula_weight 989.25 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.015(3) _cell_length_b 10.748(2) _cell_length_c 29.927(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.12(3) _cell_angle_gamma 90.00 _cell_volume 4703.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 190(1) _cell_measurement_reflns_used 1276 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.04 _exptl_crystal_description plate _exptl_crystal_colour green-black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.517 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4289 _exptl_absorpt_correction_T_max 0.8721 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(1) _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 'STOE IPDS' _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 28787 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.04 _reflns_number_total 9125 _reflns_number_gt 6609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS-XP' _computing_publication_material 'SHELXL-97' _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^)+(0.0599P)^2^+9.1994P] 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 9125 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb Sb 0.19309(2) 0.66294(3) 0.388503(10) 0.02799(10) Uani 1 1 d . . . Fe1 Fe 0.20662(5) 0.84644(7) 0.45057(2) 0.03284(17) Uani 1 1 d . . . Fe2 Fe 0.02238(4) 0.64769(6) 0.33863(2) 0.02863(16) Uani 1 1 d . . . Fe3 Fe 0.31414(5) 0.69009(7) 0.33559(2) 0.03148(17) Uani 1 1 d . . . C1 C 0.2207(4) 0.9482(5) 0.40670(19) 0.0422(12) Uani 1 1 d . . . O1 O 0.2299(3) 1.0188(4) 0.37949(14) 0.0599(12) Uani 1 1 d . . . C2 C 0.0891(4) 0.8751(5) 0.43834(18) 0.0401(12) Uani 1 1 d . . . O2 O 0.0136(3) 0.9045(4) 0.43389(14) 0.0543(11) Uani 1 1 d . . . C3 C 0.0266(4) 0.8088(5) 0.33240(17) 0.0392(12) Uani 1 1 d . . . O3 O 0.0278(3) 0.9164(4) 0.32740(14) 0.0536(10) Uani 1 1 d . . . C4 C 0.0610(3) 0.6215(5) 0.28862(16) 0.0349(11) Uani 1 1 d . . . O4 O 0.0798(3) 0.6031(4) 0.25345(12) 0.0460(9) Uani 1 1 d . . . C5 C 0.2382(4) 0.8006(5) 0.30569(17) 0.0388(12) Uani 1 1 d . . . O5 O 0.1909(3) 0.8741(4) 0.28421(14) 0.0549(11) Uani 1 1 d . . . C6 C 0.3741(4) 0.7999(6) 0.3734(2) 0.0430(13) Uani 1 1 d . . . O6 O 0.4198(3) 0.8747(4) 0.39614(16) 0.0619(12) Uani 1 1 d . . . C7 C 0.2176(4) 0.8681(5) 0.52166(17) 0.0374(12) Uani 1 1 d . . . H7 H 0.1699 0.9014 0.5342 0.045 Uiso 1 1 calc R . . C8 C 0.2288(3) 0.7399(5) 0.51282(16) 0.0321(11) Uani 1 1 d . . . C9 C 0.3073(3) 0.7313(6) 0.49334(16) 0.0389(12) Uani 1 1 d . . . H9 H 0.3319 0.6570 0.4839 0.047 Uiso 1 1 calc R . . C10 C 0.3418(4) 0.8527(6) 0.49063(18) 0.0460(14) Uani 1 1 d . . . H10 H 0.3930 0.8738 0.4785 0.055 Uiso 1 1 calc R . . C11 C 0.2868(4) 0.9389(6) 0.50928(18) 0.0479(15) Uani 1 1 d . A . C12 C 0.3043(7) 1.0756(7) 0.5202(2) 0.076(2) Uani 1 1 d . . . C13A C 0.348(3) 1.090(4) 0.5720(9) 0.077(13) Uani 0.50 1 d P A -1 H13A H 0.4039 1.0409 0.5800 0.116 Uiso 0.50 1 calc PR A -1 H13B H 0.3044 1.0612 0.5898 0.116 Uiso 0.50 1 calc PR A -1 H13C H 0.3620 1.1781 0.5790 0.116 Uiso 0.50 1 calc PR A -1 C14A C 0.2348(19) 1.149(3) 0.5060(13) 0.084(8) Uani 0.50 1 d P A -1 H14A H 0.1795 1.1095 0.5117 0.125 Uiso 0.50 1 calc PR A -1 H14B H 0.2269 1.1636 0.4730 0.125 Uiso 0.50 1 calc PR A -1 H14C H 0.2455 1.2279 0.5225 0.125 Uiso 0.50 1 calc PR A -1 C15A C 0.3959(17) 1.110(2) 0.4976(9) 0.081(8) Uani 0.50 1 d P A -1 H15A H 0.3821 1.0875 0.4650 0.122 Uiso 0.50 1 calc PR A -1 H15B H 0.4494 1.0630 0.5139 0.122 Uiso 0.50 1 calc PR A -1 H15C H 0.4089 1.1993 0.5009 0.122 Uiso 0.50 1 calc PR A -1 C13B C 0.352(3) 1.078(4) 0.5704(12) 0.102(15) Uani 0.50 1 d P A -2 H13D H 0.4111 1.0367 0.5748 0.153 Uiso 0.50 1 calc PR A -2 H13E H 0.3138 1.0353 0.5883 0.153 Uiso 0.50 1 calc PR A -2 H13F H 0.3608 1.1649 0.5808 0.153 Uiso 0.50 1 calc PR A -2 C14B C 0.198(2) 1.150(3) 0.5157(15) 0.087(9) Uani 0.50 1 d P A -2 H14D H 0.1669 1.1140 0.5382 0.130 Uiso 0.50 1 calc PR A -2 H14E H 0.1601 1.1377 0.4847 0.130 Uiso 0.50 1 calc PR A -2 H14F H 0.2077 1.2390 0.5217 0.130 Uiso 0.50 1 calc PR A -2 C15B C 0.3452(19) 1.147(2) 0.4887(10) 0.098(9) Uani 0.50 1 d P A -2 H15D H 0.4011 1.1057 0.4849 0.146 Uiso 0.50 1 calc PR A -2 H15E H 0.3601 1.2309 0.5012 0.146 Uiso 0.50 1 calc PR A -2 H15F H 0.3018 1.1532 0.4589 0.146 Uiso 0.50 1 calc PR A -2 C16 C 0.1780(4) 0.6357(5) 0.52979(17) 0.0367(12) Uani 1 1 d . . . C17 C 0.1980(5) 0.5086(5) 0.5108(2) 0.0515(15) Uani 1 1 d . . . H17A H 0.1835 0.5116 0.4772 0.077 Uiso 1 1 calc R . . H17B H 0.1605 0.4447 0.5210 0.077 Uiso 1 1 calc R . . H17C H 0.2629 0.4883 0.5221 0.077 Uiso 1 1 calc R . . C18 C 0.0745(4) 0.6602(6) 0.51787(18) 0.0452(13) Uani 1 1 d . . . H18A H 0.0618 0.7386 0.5319 0.068 Uiso 1 1 calc R . . H18B H 0.0430 0.5919 0.5296 0.068 Uiso 1 1 calc R . . H18C H 0.0527 0.6656 0.4845 0.068 Uiso 1 1 calc R . . C19 C 0.2113(4) 0.6330(6) 0.58278(18) 0.0501(15) Uani 1 1 d . . . H19A H 0.2767 0.6127 0.5910 0.075 Uiso 1 1 calc R . . H19B H 0.1770 0.5698 0.5955 0.075 Uiso 1 1 calc R . . H19C H 0.2014 0.7147 0.5953 0.075 Uiso 1 1 calc R . . C20 C -0.0853(3) 0.5175(5) 0.32049(17) 0.0351(11) Uani 1 1 d . . . H20 H -0.1073 0.4862 0.2903 0.042 Uiso 1 1 calc R . . C21 C -0.1194(3) 0.6248(5) 0.33822(17) 0.0340(11) Uani 1 1 d . . . C22 C -0.0651(3) 0.6383(5) 0.38426(16) 0.0334(11) Uani 1 1 d . . . H22 H -0.0706 0.7035 0.4049 0.040 Uiso 1 1 calc R . . C23 C -0.0026(3) 0.5390(5) 0.39361(16) 0.0300(10) Uani 1 1 d . . . H23 H 0.0400 0.5255 0.4219 0.036 Uiso 1 1 calc R . . C24 C -0.0132(3) 0.4624(5) 0.35431(16) 0.0309(10) Uani 1 1 d . . . C25 C 0.0304(3) 0.3371(5) 0.35113(17) 0.0351(11) Uani 1 1 d . . . C26 C 0.0630(4) 0.3219(6) 0.3065(2) 0.0486(14) Uani 1 1 d . . . H26A H 0.0123 0.3401 0.2803 0.073 Uiso 1 1 calc R . . H26B H 0.0839 0.2363 0.3041 0.073 Uiso 1 1 calc R . . H26C H 0.1135 0.3796 0.3065 0.073 Uiso 1 1 calc R . . C27 C -0.0422(4) 0.2352(5) 0.3521(2) 0.0493(14) Uani 1 1 d . . . H27A H -0.0637 0.2423 0.3806 0.074 Uiso 1 1 calc R . . H27B H -0.0150 0.1529 0.3506 0.074 Uiso 1 1 calc R . . H27C H -0.0940 0.2460 0.3258 0.074 Uiso 1 1 calc R . . C28 C 0.1111(4) 0.3148(6) 0.3922(2) 0.0502(15) Uani 1 1 d . . . H28A H 0.1569 0.3803 0.3933 0.075 Uiso 1 1 calc R . . H28B H 0.1387 0.2336 0.3890 0.075 Uiso 1 1 calc R . . H28C H 0.0891 0.3161 0.4207 0.075 Uiso 1 1 calc R . . C29 C -0.2040(4) 0.6990(6) 0.3162(2) 0.0439(13) Uani 1 1 d . . . C30 C -0.2186(6) 0.6991(9) 0.2644(2) 0.091(3) Uani 1 1 d . . . H30A H -0.1653 0.7364 0.2558 0.137 Uiso 1 1 calc R . . H30B H -0.2734 0.7475 0.2510 0.137 Uiso 1 1 calc R . . H30C H -0.2263 0.6134 0.2531 0.137 Uiso 1 1 calc R . . C31 C -0.2847(4) 0.6367(8) 0.3299(3) 0.089(3) Uani 1 1 d . . . H31A H -0.2765 0.6407 0.3633 0.133 Uiso 1 1 calc R . . H31B H -0.2882 0.5495 0.3201 0.133 Uiso 1 1 calc R . . H31C H -0.3413 0.6797 0.3152 0.133 Uiso 1 1 calc R . . C32 C -0.1982(5) 0.8324(8) 0.3333(3) 0.089(3) Uani 1 1 d . . . H32A H -0.1800 0.8329 0.3669 0.134 Uiso 1 1 calc R . . H32B H -0.2581 0.8724 0.3233 0.134 Uiso 1 1 calc R . . H32C H -0.1528 0.8778 0.3208 0.134 Uiso 1 1 calc R . . C33 C 0.4350(3) 0.6109(5) 0.32379(16) 0.0358(11) Uani 1 1 d . . . H33 H 0.4931 0.6503 0.3324 0.043 Uiso 1 1 calc R . . C34 C 0.3983(3) 0.5272(5) 0.35248(16) 0.0358(11) Uani 1 1 d . . . C35 C 0.3104(3) 0.4939(5) 0.32686(16) 0.0347(11) Uani 1 1 d . . . H35 H 0.2689 0.4400 0.3371 0.042 Uiso 1 1 calc R . . C36 C 0.2941(3) 0.5533(5) 0.28375(17) 0.0384(12) Uani 1 1 d . . . H36 H 0.2398 0.5462 0.2603 0.046 Uiso 1 1 calc R . . C37 C 0.3726(4) 0.6262(5) 0.28096(17) 0.0372(12) Uani 1 1 d . . . C38 C 0.3899(4) 0.6942(6) 0.23929(18) 0.0451(14) Uani 1 1 d . . . C39 C 0.4387(5) 0.8166(7) 0.2529(2) 0.0659(19) Uani 1 1 d . . . H39A H 0.4011 0.8697 0.2679 0.099 Uiso 1 1 calc R . . H39B H 0.4492 0.8585 0.2255 0.099 Uiso 1 1 calc R . . H39C H 0.4976 0.8007 0.2742 0.099 Uiso 1 1 calc R . . C40 C 0.3008(5) 0.7204(8) 0.2041(2) 0.069(2) Uani 1 1 d . . . H40A H 0.2696 0.6417 0.1941 0.103 Uiso 1 1 calc R . . H40B H 0.3145 0.7633 0.1775 0.103 Uiso 1 1 calc R . . H40C H 0.2612 0.7730 0.2180 0.103 Uiso 1 1 calc R . . C41 C 0.4492(5) 0.6080(7) 0.2170(2) 0.069(2) Uani 1 1 d . . . H41A H 0.5080 0.5935 0.2385 0.104 Uiso 1 1 calc R . . H41B H 0.4598 0.6472 0.1890 0.104 Uiso 1 1 calc R . . H41C H 0.4176 0.5285 0.2091 0.104 Uiso 1 1 calc R . . C42 C 0.4515(4) 0.4702(5) 0.39713(17) 0.0406(12) Uani 1 1 d . . . C43 C 0.5096(5) 0.5665(7) 0.4276(2) 0.072(2) Uani 1 1 d . . . H43A H 0.5482 0.6099 0.4102 0.108 Uiso 1 1 calc R . . H43B H 0.5484 0.5252 0.4542 0.108 Uiso 1 1 calc R . . H43C H 0.4697 0.6267 0.4381 0.108 Uiso 1 1 calc R . . C44 C 0.5133(5) 0.3695(8) 0.3837(2) 0.070(2) Uani 1 1 d . . . H44A H 0.4753 0.3037 0.3664 0.105 Uiso 1 1 calc R . . H44B H 0.5525 0.3341 0.4114 0.105 Uiso 1 1 calc R . . H44C H 0.5515 0.4066 0.3646 0.105 Uiso 1 1 calc R . . C45 C 0.3882(5) 0.4087(7) 0.4238(2) 0.064(2) Uani 1 1 d . . . H45A H 0.3430 0.4694 0.4291 0.097 Uiso 1 1 calc R . . H45B H 0.4242 0.3787 0.4534 0.097 Uiso 1 1 calc R . . H45C H 0.3567 0.3384 0.4061 0.097 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 Sb 0.02961(17) 0.02881(18) 0.02475(16) 0.00142(12) 0.00452(12) -0.00007(13) Fe1 0.0397(4) 0.0306(4) 0.0274(3) -0.0001(3) 0.0060(3) -0.0020(3) Fe2 0.0291(3) 0.0326(4) 0.0242(3) 0.0004(3) 0.0060(3) 0.0023(3) Fe3 0.0300(3) 0.0353(4) 0.0287(3) 0.0017(3) 0.0058(3) -0.0014(3) C1 0.052(3) 0.030(3) 0.046(3) 0.001(2) 0.015(3) -0.002(2) O1 0.094(3) 0.038(2) 0.052(2) 0.008(2) 0.025(2) 0.007(2) C2 0.051(3) 0.036(3) 0.033(3) -0.002(2) 0.010(2) 0.007(2) O2 0.050(2) 0.055(3) 0.056(3) -0.010(2) 0.007(2) 0.012(2) C3 0.038(3) 0.046(4) 0.033(3) 0.001(2) 0.007(2) 0.005(2) O3 0.066(3) 0.037(3) 0.057(3) 0.0078(19) 0.014(2) 0.006(2) C4 0.032(3) 0.045(3) 0.024(2) -0.001(2) -0.0019(19) 0.003(2) O4 0.044(2) 0.068(3) 0.0263(18) 0.0017(17) 0.0089(16) 0.0044(19) C5 0.047(3) 0.035(3) 0.034(3) 0.005(2) 0.010(2) 0.001(2) O5 0.064(3) 0.054(3) 0.047(2) 0.014(2) 0.013(2) 0.017(2) C6 0.036(3) 0.045(3) 0.048(3) -0.004(3) 0.011(2) -0.008(2) O6 0.052(2) 0.065(3) 0.069(3) -0.020(2) 0.013(2) -0.023(2) C7 0.046(3) 0.034(3) 0.032(3) -0.003(2) 0.010(2) -0.005(2) C8 0.034(3) 0.029(3) 0.031(2) -0.0012(19) 0.002(2) 0.000(2) C9 0.035(3) 0.054(4) 0.023(2) 0.001(2) -0.003(2) 0.004(2) C10 0.044(3) 0.059(4) 0.034(3) -0.002(3) 0.006(2) -0.017(3) C11 0.063(4) 0.047(4) 0.030(3) 0.002(2) 0.003(3) -0.021(3) C12 0.119(7) 0.046(4) 0.056(4) -0.012(3) 0.008(4) -0.036(5) C13A 0.13(3) 0.08(2) 0.034(12) -0.034(12) 0.035(15) -0.055(18) C14A 0.10(2) 0.028(9) 0.11(2) -0.018(11) 0.010(16) 0.007(14) C15A 0.13(2) 0.048(14) 0.064(12) 0.010(9) 0.009(14) -0.054(13) C13B 0.11(3) 0.047(16) 0.12(3) -0.023(16) -0.037(18) -0.016(16) C14B 0.10(2) 0.045(11) 0.12(2) -0.011(12) 0.024(15) 0.020(14) C15B 0.15(3) 0.055(16) 0.090(17) 0.003(12) 0.021(18) -0.063(16) C16 0.042(3) 0.037(3) 0.030(3) 0.002(2) 0.007(2) -0.003(2) C17 0.072(4) 0.035(3) 0.043(3) 0.005(2) 0.005(3) -0.005(3) C18 0.038(3) 0.058(4) 0.036(3) 0.006(3) 0.002(2) -0.009(3) C19 0.044(3) 0.071(4) 0.031(3) 0.009(3) -0.001(2) -0.006(3) C20 0.033(2) 0.041(3) 0.032(2) -0.005(2) 0.008(2) -0.004(2) C21 0.029(2) 0.040(3) 0.034(3) 0.003(2) 0.011(2) 0.001(2) C22 0.039(3) 0.035(3) 0.029(2) -0.003(2) 0.012(2) 0.002(2) C23 0.030(2) 0.033(3) 0.027(2) -0.0008(19) 0.0087(19) -0.002(2) C24 0.030(2) 0.034(3) 0.028(2) -0.001(2) 0.0067(19) 0.003(2) C25 0.037(3) 0.031(3) 0.037(3) -0.008(2) 0.008(2) 0.001(2) C26 0.047(3) 0.049(4) 0.054(3) -0.010(3) 0.019(3) 0.005(3) C27 0.057(4) 0.037(3) 0.060(4) -0.011(3) 0.025(3) -0.009(3) C28 0.051(3) 0.041(4) 0.053(3) -0.003(3) 0.000(3) 0.012(3) C29 0.033(3) 0.050(4) 0.051(3) 0.012(3) 0.013(2) 0.010(2) C30 0.084(5) 0.139(8) 0.050(4) 0.034(5) 0.012(4) 0.060(5) C31 0.029(3) 0.111(7) 0.126(7) 0.062(6) 0.017(4) 0.019(4) C32 0.056(4) 0.076(6) 0.125(8) -0.007(5) 0.001(5) 0.036(4) C33 0.033(3) 0.043(3) 0.030(2) 0.000(2) 0.005(2) -0.002(2) C34 0.041(3) 0.038(3) 0.029(2) 0.007(2) 0.009(2) 0.001(2) C35 0.034(3) 0.037(3) 0.036(3) 0.000(2) 0.014(2) 0.001(2) C36 0.033(3) 0.046(3) 0.036(3) -0.005(2) 0.006(2) 0.004(2) C37 0.040(3) 0.039(3) 0.033(3) 0.003(2) 0.010(2) 0.002(2) C38 0.050(3) 0.054(4) 0.034(3) 0.010(2) 0.016(2) 0.011(3) C39 0.083(5) 0.063(5) 0.055(4) 0.017(3) 0.023(4) -0.009(4) C40 0.067(4) 0.103(6) 0.035(3) 0.025(4) 0.009(3) 0.014(4) C41 0.088(5) 0.077(5) 0.053(4) 0.015(4) 0.040(4) 0.019(4) C42 0.043(3) 0.046(3) 0.032(3) 0.009(2) 0.008(2) 0.011(2) C43 0.086(5) 0.075(5) 0.041(3) 0.010(3) -0.016(3) -0.006(4) C44 0.064(4) 0.092(6) 0.050(4) 0.012(4) 0.006(3) 0.039(4) C45 0.061(4) 0.078(5) 0.058(4) 0.040(4) 0.022(3) 0.021(4) _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 Sb Fe2 2.6622(11) . ? Sb Fe3 2.6838(10) . ? Sb Fe1 2.6851(9) . ? Fe1 C2 1.746(6) . ? Fe1 C1 1.758(6) . ? Fe1 C7 2.109(5) . ? Fe1 C10 2.111(6) . ? Fe1 C11 2.136(5) . ? Fe1 C9 2.139(5) . ? Fe1 C8 2.147(5) . ? Fe2 C3 1.744(6) . ? Fe2 C4 1.746(5) . ? Fe2 C22 2.101(5) . ? Fe2 C20 2.114(5) . ? Fe2 C23 2.120(5) . ? Fe2 C21 2.140(5) . ? Fe2 C24 2.141(5) . ? Fe3 C6 1.738(6) . ? Fe3 C5 1.746(5) . ? Fe3 C33 2.106(5) . ? Fe3 C36 2.109(5) . ? Fe3 C35 2.124(5) . ? Fe3 C37 2.137(5) . ? Fe3 C34 2.150(5) . ? C1 O1 1.144(6) . ? C2 O2 1.156(7) . ? C3 O3 1.167(7) . ? C4 O4 1.167(6) . ? C5 O5 1.155(6) . ? C6 O6 1.170(7) . ? C7 C11 1.403(8) . ? C7 C8 1.420(7) . ? C8 C9 1.432(7) . ? C8 C16 1.507(7) . ? C9 C10 1.412(8) . ? C10 C11 1.435(9) . ? C11 C12 1.515(9) . ? C12 C14A 1.30(3) . ? C12 C15B 1.46(3) . ? C12 C13B 1.51(4) . ? C12 C13A 1.55(3) . ? C12 C15A 1.71(3) . ? C12 C14B 1.76(3) . ? C16 C17 1.535(8) . ? C16 C18 1.536(7) . ? C16 C19 1.551(7) . ? C20 C21 1.413(7) . ? C20 C24 1.432(7) . ? C21 C22 1.440(7) . ? C21 C29 1.519(7) . ? C22 C23 1.406(7) . ? C23 C24 1.415(6) . ? C24 C25 1.510(7) . ? C25 C26 1.532(7) . ? C25 C28 1.536(7) . ? C25 C27 1.551(7) . ? C29 C30 1.515(9) . ? C29 C32 1.518(10) . ? C29 C31 1.519(9) . ? C33 C37 1.415(7) . ? C33 C34 1.437(7) . ? C34 C35 1.414(7) . ? C34 C42 1.522(7) . ? C35 C36 1.410(7) . ? C36 C37 1.434(7) . ? C37 C38 1.518(7) . ? C38 C39 1.516(9) . ? C38 C40 1.530(8) . ? C38 C41 1.539(9) . ? C42 C43 1.518(9) . ? C42 C45 1.524(8) . ? C42 C44 1.537(8) . ? 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 Fe2 Sb Fe3 111.76(3) . . ? Fe2 Sb Fe1 110.18(3) . . ? Fe3 Sb Fe1 111.92(3) . . ? C2 Fe1 C1 91.2(3) . . ? C2 Fe1 C7 92.0(2) . . ? C1 Fe1 C7 133.6(2) . . ? C2 Fe1 C10 155.4(2) . . ? C1 Fe1 C10 98.1(2) . . ? C7 Fe1 C10 65.1(2) . . ? C2 Fe1 C11 116.4(3) . . ? C1 Fe1 C11 100.6(2) . . ? C7 Fe1 C11 38.6(2) . . ? C10 Fe1 C11 39.5(2) . . ? C2 Fe1 C9 140.4(2) . . ? C1 Fe1 C9 128.2(2) . . ? C7 Fe1 C9 65.0(2) . . ? C10 Fe1 C9 38.8(2) . . ? C11 Fe1 C9 65.6(2) . . ? C2 Fe1 C8 103.1(2) . . ? C1 Fe1 C8 163.4(2) . . ? C7 Fe1 C8 38.97(19) . . ? C10 Fe1 C8 65.4(2) . . ? C11 Fe1 C8 65.6(2) . . ? C9 Fe1 C8 39.02(19) . . ? C2 Fe1 Sb 94.03(18) . . ? C1 Fe1 Sb 86.75(18) . . ? C7 Fe1 Sb 139.05(15) . . ? C10 Fe1 Sb 109.17(17) . . ? C11 Fe1 Sb 148.28(19) . . ? C9 Fe1 Sb 85.49(15) . . ? C8 Fe1 Sb 100.43(13) . . ? C3 Fe2 C4 92.4(2) . . ? C3 Fe2 C22 99.2(2) . . ? C4 Fe2 C22 158.1(2) . . ? C3 Fe2 C20 132.4(2) . . ? C4 Fe2 C20 93.3(2) . . ? C22 Fe2 C20 65.20(19) . . ? C3 Fe2 C23 130.3(2) . . ? C4 Fe2 C23 136.8(2) . . ? C22 Fe2 C23 38.92(18) . . ? C20 Fe2 C23 64.83(19) . . ? C3 Fe2 C21 100.0(2) . . ? C4 Fe2 C21 120.0(2) . . ? C22 Fe2 C21 39.69(18) . . ? C20 Fe2 C21 38.79(19) . . ? C23 Fe2 C21 65.78(18) . . ? C3 Fe2 C24 164.5(2) . . ? C4 Fe2 C24 100.7(2) . . ? C22 Fe2 C24 65.75(19) . . ? C20 Fe2 C24 39.33(18) . . ? C23 Fe2 C24 38.79(17) . . ? C21 Fe2 C24 66.25(19) . . ? C3 Fe2 Sb 86.85(17) . . ? C4 Fe2 Sb 91.46(16) . . ? C22 Fe2 Sb 107.64(14) . . ? C20 Fe2 Sb 140.15(14) . . ? C23 Fe2 Sb 85.21(13) . . ? C21 Fe2 Sb 147.15(13) . . ? C24 Fe2 Sb 100.98(12) . . ? C6 Fe3 C5 93.1(3) . . ? C6 Fe3 C33 92.5(2) . . ? C5 Fe3 C33 132.6(2) . . ? C6 Fe3 C36 156.7(2) . . ? C5 Fe3 C36 97.5(2) . . ? C33 Fe3 C36 65.1(2) . . ? C6 Fe3 C35 138.6(2) . . ? C5 Fe3 C35 128.0(2) . . ? C33 Fe3 C35 65.0(2) . . ? C36 Fe3 C35 38.92(19) . . ? C6 Fe3 C37 118.2(2) . . ? C5 Fe3 C37 99.2(2) . . ? C33 Fe3 C37 38.95(18) . . ? C36 Fe3 C37 39.5(2) . . ? C35 Fe3 C37 65.86(19) . . ? C6 Fe3 C34 102.1(2) . . ? C5 Fe3 C34 162.7(2) . . ? C33 Fe3 C34 39.45(19) . . ? C36 Fe3 C34 65.4(2) . . ? C35 Fe3 C34 38.62(19) . . ? C37 Fe3 C34 66.23(19) . . ? C6 Fe3 Sb 90.62(18) . . ? C5 Fe3 Sb 85.72(18) . . ? C33 Fe3 Sb 141.26(14) . . ? C36 Fe3 Sb 110.82(15) . . ? C35 Fe3 Sb 87.82(13) . . ? C37 Fe3 Sb 150.15(15) . . ? C34 Fe3 Sb 102.30(13) . . ? O1 C1 Fe1 176.9(5) . . ? O2 C2 Fe1 172.3(5) . . ? O3 C3 Fe2 178.5(5) . . ? O4 C4 Fe2 174.7(4) . . ? O5 C5 Fe3 176.3(5) . . ? O6 C6 Fe3 173.9(5) . . ? C11 C7 C8 110.5(5) . . ? C11 C7 Fe1 71.7(3) . . ? C8 C7 Fe1 72.0(3) . . ? C7 C8 C9 106.4(5) . . ? C7 C8 C16 124.6(5) . . ? C9 C8 C16 128.0(5) . . ? C7 C8 Fe1 69.1(3) . . ? C9 C8 Fe1 70.2(3) . . ? C16 C8 Fe1 134.3(3) . . ? C10 C9 C8 108.1(5) . . ? C10 C9 Fe1 69.5(3) . . ? C8 C9 Fe1 70.8(3) . . ? C9 C10 C11 108.8(5) . . ? C9 C10 Fe1 71.7(3) . . ? C11 C10 Fe1 71.2(3) . . ? C7 C11 C10 106.2(5) . . ? C7 C11 C12 124.8(6) . . ? C10 C11 C12 128.5(6) . . ? C7 C11 Fe1 69.7(3) . . ? C10 C11 Fe1 69.3(3) . . ? C12 C11 Fe1 131.8(5) . . ? C14A C12 C15B 84(2) . . ? C14A C12 C13B 118(2) . . ? C15B C12 C13B 117(2) . . ? C14A C12 C11 115.4(15) . . ? C15B C12 C11 116.8(14) . . ? C13B C12 C11 104.7(18) . . ? C14A C12 C13A 113(2) . . ? C15B C12 C13A 116.8(18) . . ? C13B C12 C13A 6(3) . . ? C11 C12 C13A 109.2(17) . . ? C14A C12 C15A 113.6(18) . . ? C15B C12 C15A 29.8(12) . . ? C13B C12 C15A 99(2) . . ? C11 C12 C15A 103.9(11) . . ? C13A C12 C15A 100.5(17) . . ? C14A C12 C14B 19(3) . . ? C15B C12 C14B 102.7(17) . . ? C13B C12 C14B 106(2) . . ? C11 C12 C14B 108.2(14) . . ? C13A C12 C14B 101(2) . . ? C15A C12 C14B 132.0(15) . . ? C8 C16 C17 112.4(4) . . ? C8 C16 C18 110.9(4) . . ? C17 C16 C18 109.8(5) . . ? C8 C16 C19 106.7(4) . . ? C17 C16 C19 108.4(5) . . ? C18 C16 C19 108.4(4) . . ? C21 C20 C24 110.6(4) . . ? C21 C20 Fe2 71.6(3) . . ? C24 C20 Fe2 71.3(3) . . ? C20 C21 C22 105.5(4) . . ? C20 C21 C29 127.2(5) . . ? C22 C21 C29 126.7(5) . . ? C20 C21 Fe2 69.6(3) . . ? C22 C21 Fe2 68.7(3) . . ? C29 C21 Fe2 132.5(4) . . ? C23 C22 C21 108.7(4) . . ? C23 C22 Fe2 71.3(3) . . ? C21 C22 Fe2 71.6(3) . . ? C22 C23 C24 109.4(4) . . ? C22 C23 Fe2 69.8(3) . . ? C24 C23 Fe2 71.4(3) . . ? C23 C24 C20 105.7(4) . . ? C23 C24 C25 127.1(4) . . ? C20 C24 C25 126.4(4) . . ? C23 C24 Fe2 69.8(3) . . ? C20 C24 Fe2 69.3(3) . . ? C25 C24 Fe2 133.1(3) . . ? C24 C25 C26 112.2(4) . . ? C24 C25 C28 111.3(4) . . ? C26 C25 C28 109.4(4) . . ? C24 C25 C27 108.2(4) . . ? C26 C25 C27 107.9(4) . . ? C28 C25 C27 107.7(5) . . ? C30 C29 C32 109.2(6) . . ? C30 C29 C21 110.8(5) . . ? C32 C29 C21 111.8(5) . . ? C30 C29 C31 109.7(7) . . ? C32 C29 C31 108.3(6) . . ? C21 C29 C31 106.9(5) . . ? C37 C33 C34 110.4(4) . . ? C37 C33 Fe3 71.7(3) . . ? C34 C33 Fe3 71.9(3) . . ? C35 C34 C33 105.8(4) . . ? C35 C34 C42 127.9(5) . . ? C33 C34 C42 125.4(5) . . ? C35 C34 Fe3 69.7(3) . . ? C33 C34 Fe3 68.6(3) . . ? C42 C34 Fe3 134.3(4) . . ? C36 C35 C34 109.1(5) . . ? C36 C35 Fe3 70.0(3) . . ? C34 C35 Fe3 71.7(3) . . ? C35 C36 C37 109.1(4) . . ? C35 C36 Fe3 71.1(3) . . ? C37 C36 Fe3 71.3(3) . . ? C33 C37 C36 105.5(4) . . ? C33 C37 C38 126.8(5) . . ? C36 C37 C38 127.4(5) . . ? C33 C37 Fe3 69.3(3) . . ? C36 C37 Fe3 69.2(3) . . ? C38 C37 Fe3 130.6(4) . . ? C39 C38 C37 111.1(5) . . ? C39 C38 C40 108.6(6) . . ? C37 C38 C40 111.6(5) . . ? C39 C38 C41 110.3(6) . . ? C37 C38 C41 106.9(5) . . ? C40 C38 C41 108.3(5) . . ? C43 C42 C34 111.6(5) . . ? C43 C42 C45 108.8(5) . . ? C34 C42 C45 111.6(5) . . ? C43 C42 C44 109.8(6) . . ? C34 C42 C44 106.4(4) . . ? C45 C42 C44 108.5(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.765 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.116 data_tet1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Bi Cl2 Fe O2' _chemical_formula_weight 569.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 20.936(3) _cell_length_b 20.936(3) _cell_length_c 8.8426(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3875.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 1522 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.85 _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 10.092 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _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 'Stoe IPDS' _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 11852 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.82 _reflns_number_total 3727 _reflns_number_gt 3267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS-XP' _computing_publication_material 'SHELXL-97' _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^)+(0.0347P)^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 riding _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 -0.035(9) _refine_ls_number_reflns 3727 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.005 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi Bi 0.230337(13) 0.247505(13) 0.35640(3) 0.02595(8) Uani 1 1 d . . . Fe Fe 0.10958(5) 0.27296(5) 0.34829(17) 0.0301(2) Uani 1 1 d . . . Cl1 Cl 0.26686(10) 0.33550(10) 0.1669(3) 0.0343(5) Uani 1 1 d . . . Cl2 Cl 0.26420(12) 0.32952(10) 0.5745(3) 0.0412(5) Uani 1 1 d . . . C1 C 0.1126(4) 0.2836(4) 0.1507(13) 0.044(2) Uani 1 1 d . . . O1 O 0.1157(4) 0.2905(4) 0.0218(9) 0.061(2) Uani 1 1 d . . . C2 C 0.1299(4) 0.3540(4) 0.3762(12) 0.040(2) Uani 1 1 d . . . O2 O 0.1414(3) 0.4069(3) 0.3955(9) 0.060(2) Uani 1 1 d . . . C3 C 0.0116(3) 0.2471(4) 0.3712(13) 0.039(2) Uani 1 1 d . . . H3 H -0.0211 0.2624 0.3061 0.046 Uiso 1 1 calc R . . C4 C 0.0490(4) 0.1904(4) 0.3483(16) 0.043(2) Uani 1 1 d . . . C5 C 0.0925(5) 0.1866(5) 0.4641(14) 0.054(3) Uani 1 1 d . . . H5 H 0.1233 0.1537 0.4771 0.064 Uiso 1 1 calc R . . C6 C 0.0837(4) 0.2400(4) 0.5612(11) 0.036(2) Uani 1 1 d . . . H6 H 0.1086 0.2497 0.6481 0.044 Uiso 1 1 calc R . . C7 C 0.0318(4) 0.2760(5) 0.5065(11) 0.036(2) Uani 1 1 d . . . C8 C -0.0025(4) 0.3301(5) 0.5860(11) 0.042(2) Uani 1 1 d . . . C9 C -0.0583(5) 0.2981(7) 0.6736(17) 0.074(4) Uani 1 1 d . . . H9A H -0.0862 0.3312 0.7158 0.112 Uiso 1 1 calc R . . H9B H -0.0410 0.2719 0.7557 0.112 Uiso 1 1 calc R . . H9C H -0.0829 0.2710 0.6044 0.112 Uiso 1 1 calc R . . C10 C 0.0407(6) 0.3650(6) 0.7004(13) 0.058(3) Uani 1 1 d . . . H10A H 0.0152 0.3958 0.7581 0.087 Uiso 1 1 calc R . . H10B H 0.0747 0.3876 0.6461 0.087 Uiso 1 1 calc R . . H10C H 0.0597 0.3338 0.7698 0.087 Uiso 1 1 calc R . . C11 C -0.0315(6) 0.3770(6) 0.4749(15) 0.068(3) Uani 1 1 d . . . H11A H -0.0577 0.4081 0.5297 0.101 Uiso 1 1 calc R . . H11B H -0.0581 0.3539 0.4021 0.101 Uiso 1 1 calc R . . H11C H 0.0027 0.3994 0.4210 0.101 Uiso 1 1 calc R . . C12 C 0.0334(7) 0.1383(6) 0.232(2) 0.085(5) Uani 1 1 d . . . C13 C 0.0904(8) 0.0887(8) 0.226(3) 0.155(11) Uani 1 1 d . . . H13A H 0.1307 0.1115 0.2091 0.233 Uiso 1 1 calc R . . H13B H 0.0833 0.0584 0.1433 0.233 Uiso 1 1 calc R . . H13C H 0.0927 0.0655 0.3221 0.233 Uiso 1 1 calc R . . C14 C -0.0230(7) 0.1024(6) 0.2988(19) 0.098(6) Uani 1 1 d . . . H14A H -0.0089 0.0784 0.3879 0.147 Uiso 1 1 calc R . . H14B H -0.0402 0.0727 0.2233 0.147 Uiso 1 1 calc R . . H14C H -0.0562 0.1329 0.3283 0.147 Uiso 1 1 calc R . . C15 C 0.0167(14) 0.1658(10) 0.079(2) 0.177(13) Uani 1 1 d . . . H15A H 0.0036 0.1312 0.0109 0.265 Uiso 1 1 calc R . . H15B H 0.0540 0.1876 0.0367 0.265 Uiso 1 1 calc R . . H15C H -0.0185 0.1963 0.0901 0.265 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 Bi 0.02658(16) 0.02984(16) 0.02142(12) 0.00141(17) -0.00037(12) 0.00112(17) Fe 0.0269(5) 0.0339(6) 0.0297(6) -0.0009(7) 0.0001(6) 0.0004(4) Cl1 0.0436(11) 0.0300(10) 0.0293(13) 0.0009(9) 0.0085(10) -0.0028(8) Cl2 0.0581(15) 0.0338(11) 0.0316(12) -0.0009(10) -0.0131(11) -0.0033(9) C1 0.042(5) 0.056(5) 0.034(6) 0.004(5) -0.027(6) 0.009(4) O1 0.058(5) 0.084(6) 0.041(5) 0.010(4) -0.011(4) 0.006(4) C2 0.041(4) 0.035(5) 0.044(6) 0.000(4) 0.006(5) 0.008(4) O2 0.066(4) 0.037(4) 0.078(7) 0.007(3) 0.015(4) 0.001(3) C3 0.017(3) 0.050(5) 0.049(6) -0.013(5) -0.001(4) 0.000(3) C4 0.026(4) 0.039(5) 0.066(7) -0.008(6) 0.004(5) -0.015(4) C5 0.039(5) 0.033(5) 0.089(9) 0.018(6) 0.035(6) -0.007(4) C6 0.023(4) 0.053(5) 0.033(5) 0.008(4) -0.002(4) -0.002(4) C7 0.026(4) 0.050(5) 0.031(5) -0.002(4) 0.003(4) -0.005(4) C8 0.028(5) 0.064(6) 0.034(5) -0.018(5) 0.007(4) -0.006(4) C9 0.056(7) 0.090(9) 0.077(11) -0.022(7) 0.043(7) -0.005(7) C10 0.065(7) 0.067(7) 0.041(6) -0.022(5) 0.001(5) -0.008(6) C11 0.062(7) 0.072(8) 0.069(9) -0.027(7) -0.002(6) 0.014(6) C12 0.071(8) 0.064(8) 0.121(14) -0.055(9) 0.044(9) -0.009(6) C13 0.093(11) 0.114(13) 0.26(3) -0.119(15) 0.105(15) -0.034(10) C14 0.094(10) 0.063(8) 0.137(15) -0.059(9) 0.047(9) -0.051(8) C15 0.31(3) 0.143(17) 0.080(13) -0.070(13) 0.030(17) -0.15(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 Bi Fe 2.5847(11) . ? Bi Cl1 2.605(2) . ? Bi Cl2 2.678(2) . ? Bi Cl2 2.971(3) 6_554 ? Fe C1 1.762(12) . ? Fe C2 1.766(9) . ? Fe C6 2.077(9) . ? Fe C5 2.109(9) . ? Fe C3 2.131(7) . ? Fe C4 2.145(8) . ? Fe C7 2.147(9) . ? Cl2 Bi 2.971(3) 6 ? C1 O1 1.150(13) . ? C2 O2 1.146(11) . ? C3 C7 1.406(14) . ? C3 C4 1.436(12) . ? C4 C5 1.372(17) . ? C4 C12 1.536(17) . ? C5 C6 1.422(14) . ? C6 C7 1.408(12) . ? C7 C8 1.515(13) . ? C8 C11 1.516(16) . ? C8 C10 1.541(13) . ? C8 C9 1.553(14) . ? C12 C15 1.51(3) . ? C12 C14 1.520(18) . ? C12 C13 1.58(2) . ? 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 Fe Bi Cl1 97.09(6) . . ? Fe Bi Cl2 98.44(6) . . ? Cl1 Bi Cl2 86.10(7) . . ? Fe Bi Cl2 97.25(6) . 6_554 ? Cl1 Bi Cl2 80.37(7) . 6_554 ? Cl2 Bi Cl2 160.41(4) . 6_554 ? C1 Fe C2 90.5(5) . . ? C1 Fe C6 161.8(4) . . ? C2 Fe C6 104.8(4) . . ? C1 Fe C5 126.6(5) . . ? C2 Fe C5 142.8(5) . . ? C6 Fe C5 39.7(4) . . ? C1 Fe C3 99.3(4) . . ? C2 Fe C3 117.5(4) . . ? C6 Fe C3 65.1(4) . . ? C5 Fe C3 64.7(4) . . ? C1 Fe C4 97.1(5) . . ? C2 Fe C4 156.4(4) . . ? C6 Fe C4 65.0(5) . . ? C5 Fe C4 37.6(5) . . ? C3 Fe C4 39.2(3) . . ? C1 Fe C7 132.0(4) . . ? C2 Fe C7 93.6(4) . . ? C6 Fe C7 38.9(3) . . ? C5 Fe C7 65.2(4) . . ? C3 Fe C7 38.4(4) . . ? C4 Fe C7 64.9(4) . . ? C1 Fe Bi 91.1(3) . . ? C2 Fe Bi 87.6(3) . . ? C6 Fe Bi 99.3(2) . . ? C5 Fe Bi 88.6(3) . . ? C3 Fe Bi 152.4(3) . . ? C4 Fe Bi 114.4(2) . . ? C7 Fe Bi 136.8(3) . . ? Bi Cl2 Bi 105.45(7) . 6 ? O1 C1 Fe 178.9(8) . . ? O2 C2 Fe 178.1(8) . . ? C7 C3 C4 108.2(9) . . ? C7 C3 Fe 71.5(5) . . ? C4 C3 Fe 70.9(4) . . ? C5 C4 C3 107.7(10) . . ? C5 C4 C12 126.9(10) . . ? C3 C4 C12 124.5(11) . . ? C5 C4 Fe 69.8(5) . . ? C3 C4 Fe 69.9(4) . . ? C12 C4 Fe 134.3(9) . . ? C4 C5 C6 108.6(8) . . ? C4 C5 Fe 72.6(6) . . ? C6 C5 Fe 69.0(5) . . ? C7 C6 C5 108.2(9) . . ? C7 C6 Fe 73.3(5) . . ? C5 C6 Fe 71.3(5) . . ? C3 C7 C6 107.1(8) . . ? C3 C7 C8 125.0(8) . . ? C6 C7 C8 127.4(9) . . ? C3 C7 Fe 70.2(5) . . ? C6 C7 Fe 67.9(5) . . ? C8 C7 Fe 133.2(7) . . ? C11 C8 C7 111.9(8) . . ? C11 C8 C10 110.7(9) . . ? C7 C8 C10 112.3(8) . . ? C11 C8 C9 107.6(9) . . ? C7 C8 C9 105.4(8) . . ? C10 C8 C9 108.6(9) . . ? C15 C12 C14 110.9(16) . . ? C15 C12 C4 112.3(12) . . ? C14 C12 C4 104.7(11) . . ? C15 C12 C13 113.4(16) . . ? C14 C12 C13 105.9(13) . . ? C4 C12 C13 109.1(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.855 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.133 data_sbfe3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H31 Fe3 O5 Sb' _chemical_formula_weight 736.83 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9597(14) _cell_length_b 13.363(3) _cell_length_c 15.702(3) _cell_angle_alpha 73.79(3) _cell_angle_beta 89.82(3) _cell_angle_gamma 88.65(3) _cell_volume 1401.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 1291 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 25.83 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 2.510 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4209 _exptl_absorpt_correction_T_max 0.8831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _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 'STOE IPDS' _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 8651 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.83 _reflns_number_total 5017 _reflns_number_gt 4011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS-XP' _computing_publication_material 'SHELXL-97' _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^)+(0.0546P)^2^+2.3856P] 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 5017 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb Sb 0.14282(5) 0.23925(2) 0.69490(2) 0.02204(11) Uani 1 1 d . . . Fe1 Fe 0.27007(11) 0.36326(5) 0.78761(4) 0.02248(17) Uani 1 1 d . . . Fe2 Fe 0.32185(12) 0.24021(5) 0.55060(5) 0.02557(18) Uani 1 1 d . . . Fe3 Fe 0.32306(11) 0.07184(5) 0.68686(5) 0.02518(18) Uani 1 1 d . . . C1 C 0.5087(9) 0.3287(4) 0.7785(4) 0.0286(12) Uani 1 1 d . . . O1 O 0.6730(7) 0.3149(4) 0.7735(3) 0.0506(12) Uani 1 1 d . . . C2 C 0.2712(9) 0.4544(4) 0.6822(4) 0.0327(13) Uani 1 1 d . . . O2 O 0.2780(8) 0.5165(3) 0.6151(3) 0.0546(13) Uani 1 1 d . . . C3 C 0.5063(9) 0.3121(4) 0.5753(3) 0.0325(13) Uani 1 1 d . . . O3 O 0.6358(7) 0.3625(3) 0.5839(3) 0.0428(10) Uani 1 1 d . . . C4 C 0.5114(9) 0.0923(4) 0.7519(4) 0.0316(13) Uani 1 1 d . . . O4 O 0.6436(7) 0.0935(3) 0.7969(3) 0.0458(11) Uani 1 1 d . . . O5 O 0.6254(7) 0.0852(3) 0.5575(3) 0.0420(10) Uani 1 1 d . . . C5 C 0.4849(8) 0.1193(4) 0.5844(3) 0.0277(11) Uani 1 1 d . . . C6 C 0.3045(8) 0.3872(4) 0.9150(3) 0.0263(11) Uani 1 1 d . . . H6 H 0.4249 0.3970 0.9395 0.032 Uiso 1 1 calc R . . C7 C 0.2178(8) 0.2883(4) 0.9260(3) 0.0250(11) Uani 1 1 d . . . C8 C 0.0416(8) 0.3099(4) 0.8781(3) 0.0268(11) Uani 1 1 d . . . H8 H -0.0482 0.2593 0.8731 0.032 Uiso 1 1 calc R . . C9 C 0.0213(8) 0.4189(4) 0.8389(3) 0.0267(11) Uani 1 1 d . . . H9 H -0.0832 0.4534 0.8029 0.032 Uiso 1 1 calc R . . C10 C 0.1855(8) 0.4680(4) 0.8627(3) 0.0268(11) Uani 1 1 d . . . C11 C 0.2177(10) 0.5837(4) 0.8450(4) 0.0343(13) Uani 1 1 d . . . C12 C 0.1726(12) 0.6117(5) 0.9320(4) 0.0476(17) Uani 1 1 d . . . H12A H 0.1968 0.6857 0.9240 0.071 Uiso 1 1 calc R . . H12B H 0.2550 0.5693 0.9797 0.071 Uiso 1 1 calc R . . H12C H 0.0375 0.5978 0.9476 0.071 Uiso 1 1 calc R . . C13 C 0.4280(11) 0.6084(5) 0.8208(5) 0.0476(17) Uani 1 1 d . . . H13A H 0.4454 0.6838 0.8069 0.071 Uiso 1 1 calc R . . H13B H 0.4625 0.5845 0.7691 0.071 Uiso 1 1 calc R . . H13C H 0.5108 0.5727 0.8710 0.071 Uiso 1 1 calc R . . C14 C 0.0868(12) 0.6486(4) 0.7724(5) 0.0497(18) Uani 1 1 d . . . H14A H 0.1049 0.7228 0.7663 0.075 Uiso 1 1 calc R . . H14B H -0.0473 0.6313 0.7876 0.075 Uiso 1 1 calc R . . H14C H 0.1183 0.6338 0.7161 0.075 Uiso 1 1 calc R . . C15 C 0.2866(9) 0.1853(4) 0.9885(4) 0.0315(12) Uani 1 1 d . . . C16 C 0.1851(13) 0.0954(5) 0.9668(5) 0.060(2) Uani 1 1 d . . . H16A H 0.2154 0.0952 0.9058 0.090 Uiso 1 1 calc R . . H16B H 0.0459 0.1040 0.9727 0.090 Uiso 1 1 calc R . . H16C H 0.2289 0.0293 1.0079 0.090 Uiso 1 1 calc R . . C17 C 0.2316(12) 0.1896(5) 1.0834(4) 0.0538(19) Uani 1 1 d . . . H17A H 0.0914 0.1928 1.0884 0.081 Uiso 1 1 calc R . . H17B H 0.2863 0.2516 1.0946 0.081 Uiso 1 1 calc R . . H17C H 0.2825 0.1270 1.1269 0.081 Uiso 1 1 calc R . . C18 C 0.4994(10) 0.1686(5) 0.9849(4) 0.0434(15) Uani 1 1 d . . . H18A H 0.5363 0.1681 0.9248 0.065 Uiso 1 1 calc R . . H18B H 0.5364 0.1016 1.0268 0.065 Uiso 1 1 calc R . . H18C H 0.5648 0.2250 1.0008 0.065 Uiso 1 1 calc R . . C19 C 0.2568(11) 0.3608(5) 0.4358(4) 0.0466(17) Uani 1 1 d . . . H19 H 0.3036 0.4295 0.4247 0.056 Uiso 1 1 calc R . . C20 C 0.3503(11) 0.2764(5) 0.4123(4) 0.0456(16) Uani 1 1 d . . . H20 H 0.4707 0.2779 0.3833 0.055 Uiso 1 1 calc R . . C21 C 0.2302(12) 0.1904(5) 0.4404(4) 0.0515(19) Uani 1 1 d . . . H21 H 0.2552 0.1229 0.4334 0.062 Uiso 1 1 calc R . . C22 C 0.0676(11) 0.2208(6) 0.4804(4) 0.0507(18) Uani 1 1 d . . . H22 H -0.0369 0.1779 0.5051 0.061 Uiso 1 1 calc R . . C23 C 0.0865(11) 0.3256(5) 0.4775(4) 0.0485(17) Uani 1 1 d . . . H23 H -0.0032 0.3660 0.5004 0.058 Uiso 1 1 calc R . . C24 C 0.2401(16) -0.0516(6) 0.6350(5) 0.070(3) Uani 1 1 d . . . H24 H 0.2717 -0.0567 0.5774 0.085 Uiso 1 1 calc R . . C25 C 0.0728(14) -0.0033(6) 0.6587(6) 0.066(3) Uani 1 1 d . . . H25 H -0.0282 0.0305 0.6200 0.080 Uiso 1 1 calc R . . C26 C 0.0847(11) -0.0150(5) 0.7498(6) 0.056(2) Uani 1 1 d . . . H26 H -0.0080 0.0090 0.7846 0.067 Uiso 1 1 calc R . . C27 C 0.2533(12) -0.0669(5) 0.7799(5) 0.054(2) Uani 1 1 d . . . H27 H 0.2973 -0.0844 0.8395 0.065 Uiso 1 1 calc R . . C28 C 0.3495(12) -0.0901(5) 0.7116(6) 0.058(2) Uani 1 1 d . . . H28 H 0.4699 -0.1262 0.7157 0.070 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 Sb 0.0195(2) 0.02328(17) 0.02600(18) -0.01136(12) 0.00121(13) -0.00026(12) Fe1 0.0248(5) 0.0189(3) 0.0239(4) -0.0064(3) -0.0006(3) -0.0002(3) Fe2 0.0280(5) 0.0252(4) 0.0240(4) -0.0075(3) 0.0015(3) -0.0023(3) Fe3 0.0288(5) 0.0208(3) 0.0272(4) -0.0087(3) 0.0031(3) -0.0019(3) C1 0.027(4) 0.028(3) 0.031(3) -0.010(2) -0.003(2) -0.002(2) O1 0.031(3) 0.067(3) 0.056(3) -0.021(2) 0.000(2) 0.001(2) C2 0.038(4) 0.026(3) 0.034(3) -0.010(2) 0.001(2) 0.006(2) O2 0.078(4) 0.037(2) 0.038(2) 0.007(2) 0.006(2) 0.009(2) C3 0.043(4) 0.031(3) 0.022(2) -0.006(2) 0.007(2) 0.001(2) O3 0.034(3) 0.050(2) 0.045(2) -0.0123(19) 0.0017(19) -0.018(2) C4 0.042(4) 0.020(2) 0.033(3) -0.009(2) 0.005(3) 0.004(2) O4 0.037(3) 0.053(3) 0.051(3) -0.020(2) -0.015(2) 0.006(2) O5 0.039(3) 0.043(2) 0.048(2) -0.0208(19) 0.015(2) 0.0041(19) C5 0.026(3) 0.031(3) 0.031(3) -0.014(2) -0.002(2) -0.002(2) C6 0.031(3) 0.027(2) 0.021(2) -0.0081(19) -0.001(2) -0.001(2) C7 0.030(3) 0.026(2) 0.019(2) -0.0054(19) -0.001(2) 0.004(2) C8 0.030(3) 0.023(2) 0.029(3) -0.010(2) 0.003(2) -0.003(2) C9 0.024(3) 0.024(2) 0.032(3) -0.009(2) 0.002(2) 0.002(2) C10 0.037(3) 0.022(2) 0.023(2) -0.0092(19) 0.003(2) 0.001(2) C11 0.050(4) 0.018(2) 0.035(3) -0.008(2) 0.001(3) -0.004(2) C12 0.073(5) 0.027(3) 0.049(4) -0.022(3) 0.004(3) -0.001(3) C13 0.059(5) 0.029(3) 0.054(4) -0.010(3) 0.008(3) -0.017(3) C14 0.071(5) 0.024(3) 0.051(4) -0.007(3) -0.015(3) 0.006(3) C15 0.038(4) 0.023(2) 0.031(3) -0.002(2) -0.002(2) 0.001(2) C16 0.078(6) 0.021(3) 0.074(5) -0.001(3) -0.026(4) -0.004(3) C17 0.074(6) 0.044(4) 0.034(3) 0.005(3) 0.004(3) 0.018(3) C18 0.039(4) 0.041(3) 0.044(3) -0.002(3) -0.012(3) 0.013(3) C19 0.066(5) 0.037(3) 0.029(3) 0.004(2) -0.014(3) -0.005(3) C20 0.058(5) 0.051(4) 0.025(3) -0.006(3) 0.002(3) 0.001(3) C21 0.083(6) 0.044(4) 0.028(3) -0.012(3) -0.014(3) -0.004(3) C22 0.039(5) 0.069(5) 0.038(3) -0.005(3) -0.014(3) -0.017(3) C23 0.061(5) 0.048(4) 0.034(3) -0.009(3) -0.004(3) 0.013(3) C24 0.128(9) 0.044(4) 0.053(4) -0.034(4) 0.035(5) -0.057(5) C25 0.075(7) 0.037(4) 0.076(5) 0.005(4) -0.028(5) -0.031(4) C26 0.051(5) 0.033(3) 0.088(6) -0.024(3) 0.029(4) -0.021(3) C27 0.067(6) 0.036(3) 0.049(4) 0.005(3) -0.012(4) -0.017(3) C28 0.056(5) 0.021(3) 0.098(6) -0.017(3) 0.008(4) -0.001(3) _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 Sb Fe3 2.5726(10) . ? Sb Fe2 2.5793(10) . ? Sb Fe1 2.6597(10) . ? Fe1 C1 1.729(6) . ? Fe1 C2 1.759(6) . ? Fe1 C9 2.112(5) . ? Fe1 C6 2.127(5) . ? Fe1 C8 2.128(5) . ? Fe1 C10 2.139(5) . ? Fe1 C7 2.157(5) . ? Fe2 C3 1.729(6) . ? Fe2 C5 1.902(6) . ? Fe2 C19 2.098(6) . ? Fe2 C20 2.098(6) . ? Fe2 C23 2.121(7) . ? Fe2 C21 2.125(6) . ? Fe2 C22 2.147(7) . ? Fe2 Fe3 2.6364(14) . ? Fe3 C4 1.737(7) . ? Fe3 C5 1.927(5) . ? Fe3 C27 2.081(6) . ? Fe3 C28 2.093(6) . ? Fe3 C24 2.124(6) . ? Fe3 C26 2.125(6) . ? Fe3 C25 2.139(7) . ? C1 O1 1.160(7) . ? C2 O2 1.147(7) . ? C3 O3 1.168(7) . ? C4 O4 1.165(7) . ? O5 C5 1.194(7) . ? C6 C10 1.412(8) . ? C6 C7 1.431(7) . ? C7 C8 1.422(8) . ? C7 C15 1.518(7) . ? C8 C9 1.418(7) . ? C9 C10 1.433(8) . ? C10 C11 1.515(7) . ? C11 C14 1.517(9) . ? C11 C13 1.531(9) . ? C11 C12 1.543(8) . ? C15 C18 1.496(9) . ? C15 C16 1.526(9) . ? C15 C17 1.552(8) . ? C19 C23 1.380(11) . ? C19 C20 1.424(10) . ? C20 C21 1.405(10) . ? C21 C22 1.398(11) . ? C22 C23 1.398(10) . ? C24 C28 1.391(12) . ? C24 C25 1.415(13) . ? C25 C26 1.399(12) . ? C26 C27 1.365(11) . ? C27 C28 1.365(11) . ? 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 Fe3 Sb Fe2 61.56(4) . . ? Fe3 Sb Fe1 123.13(3) . . ? Fe2 Sb Fe1 117.51(3) . . ? C1 Fe1 C2 92.1(3) . . ? C1 Fe1 C9 159.1(2) . . ? C2 Fe1 C9 98.5(2) . . ? C1 Fe1 C6 94.5(2) . . ? C2 Fe1 C6 129.5(2) . . ? C9 Fe1 C6 65.0(2) . . ? C1 Fe1 C8 136.5(2) . . ? C2 Fe1 C8 131.0(3) . . ? C9 Fe1 C8 39.08(19) . . ? C6 Fe1 C8 64.7(2) . . ? C1 Fe1 C10 121.5(2) . . ? C2 Fe1 C10 97.8(2) . . ? C9 Fe1 C10 39.4(2) . . ? C6 Fe1 C10 38.6(2) . . ? C8 Fe1 C10 65.58(19) . . ? C1 Fe1 C7 101.0(2) . . ? C2 Fe1 C7 162.8(2) . . ? C9 Fe1 C7 65.6(2) . . ? C6 Fe1 C7 39.01(19) . . ? C8 Fe1 C7 38.8(2) . . ? C10 Fe1 C7 65.80(18) . . ? C1 Fe1 Sb 93.82(18) . . ? C2 Fe1 Sb 82.21(19) . . ? C9 Fe1 Sb 105.34(15) . . ? C6 Fe1 Sb 146.76(14) . . ? C8 Fe1 Sb 87.61(14) . . ? C10 Fe1 Sb 144.59(16) . . ? C7 Fe1 Sb 107.76(14) . . ? C3 Fe2 C5 89.0(3) . . ? C3 Fe2 C19 90.1(3) . . ? C5 Fe2 C19 138.1(3) . . ? C3 Fe2 C20 100.2(3) . . ? C5 Fe2 C20 99.5(3) . . ? C19 Fe2 C20 39.7(3) . . ? C3 Fe2 C23 116.6(3) . . ? C5 Fe2 C23 151.3(2) . . ? C19 Fe2 C23 38.2(3) . . ? C20 Fe2 C23 65.1(3) . . ? C3 Fe2 C21 137.5(3) . . ? C5 Fe2 C21 88.4(3) . . ? C19 Fe2 C21 65.1(3) . . ? C20 Fe2 C21 38.9(3) . . ? C23 Fe2 C21 64.3(3) . . ? C3 Fe2 C22 153.6(3) . . ? C5 Fe2 C22 114.0(3) . . ? C19 Fe2 C22 64.3(3) . . ? C20 Fe2 C22 64.8(3) . . ? C23 Fe2 C22 38.3(3) . . ? C21 Fe2 C22 38.2(3) . . ? C3 Fe2 Sb 91.91(17) . . ? C5 Fe2 Sb 103.71(16) . . ? C19 Fe2 Sb 118.2(2) . . ? C20 Fe2 Sb 154.0(2) . . ? C23 Fe2 Sb 88.84(18) . . ? C21 Fe2 Sb 129.8(2) . . ? C22 Fe2 Sb 94.7(2) . . ? C3 Fe2 Fe3 103.33(18) . . ? C5 Fe2 Fe3 46.88(16) . . ? C19 Fe2 Fe3 166.2(2) . . ? C20 Fe2 Fe3 137.64(19) . . ? C23 Fe2 Fe3 129.6(2) . . ? C21 Fe2 Fe3 105.42(18) . . ? C22 Fe2 Fe3 101.94(19) . . ? Sb Fe2 Fe3 59.10(3) . . ? C4 Fe3 C5 88.5(2) . . ? C4 Fe3 C27 92.0(3) . . ? C5 Fe3 C27 139.1(3) . . ? C4 Fe3 C28 99.6(3) . . ? C5 Fe3 C28 101.5(3) . . ? C27 Fe3 C28 38.2(3) . . ? C4 Fe3 C24 135.5(4) . . ? C5 Fe3 C24 87.8(2) . . ? C27 Fe3 C24 64.0(3) . . ? C28 Fe3 C24 38.5(3) . . ? C4 Fe3 C26 118.9(3) . . ? C5 Fe3 C26 149.9(3) . . ? C27 Fe3 C26 37.9(3) . . ? C28 Fe3 C26 64.1(3) . . ? C24 Fe3 C26 64.3(3) . . ? C4 Fe3 C25 155.5(3) . . ? C5 Fe3 C25 112.2(3) . . ? C27 Fe3 C25 63.9(3) . . ? C28 Fe3 C25 64.6(3) . . ? C24 Fe3 C25 38.8(4) . . ? C26 Fe3 C25 38.3(3) . . ? C4 Fe3 Sb 92.55(17) . . ? C5 Fe3 Sb 103.20(16) . . ? C27 Fe3 Sb 117.6(2) . . ? C28 Fe3 Sb 152.7(2) . . ? C24 Fe3 Sb 131.4(3) . . ? C26 Fe3 Sb 88.6(2) . . ? C25 Fe3 Sb 95.1(3) . . ? C4 Fe3 Fe2 103.16(17) . . ? C5 Fe3 Fe2 46.09(17) . . ? C27 Fe3 Fe2 164.6(2) . . ? C28 Fe3 Fe2 138.9(3) . . ? C24 Fe3 Fe2 105.7(2) . . ? C26 Fe3 Fe2 128.3(2) . . ? C25 Fe3 Fe2 100.8(2) . . ? Sb Fe3 Fe2 59.34(3) . . ? O1 C1 Fe1 173.3(5) . . ? O2 C2 Fe1 176.8(6) . . ? O3 C3 Fe2 173.8(5) . . ? O4 C4 Fe3 171.8(5) . . ? O5 C5 Fe2 138.3(4) . . ? O5 C5 Fe3 134.6(4) . . ? Fe2 C5 Fe3 87.0(2) . . ? C10 C6 C7 110.3(5) . . ? C10 C6 Fe1 71.1(3) . . ? C7 C6 Fe1 71.6(3) . . ? C8 C7 C6 105.9(4) . . ? C8 C7 C15 127.5(5) . . ? C6 C7 C15 125.9(5) . . ? C8 C7 Fe1 69.5(3) . . ? C6 C7 Fe1 69.4(3) . . ? C15 C7 Fe1 133.0(4) . . ? C9 C8 C7 109.1(5) . . ? C9 C8 Fe1 69.9(3) . . ? C7 C8 Fe1 71.7(3) . . ? C8 C9 C10 108.3(5) . . ? C8 C9 Fe1 71.1(3) . . ? C10 C9 Fe1 71.3(3) . . ? C6 C10 C9 106.4(4) . . ? C6 C10 C11 125.8(5) . . ? C9 C10 C11 127.5(5) . . ? C6 C10 Fe1 70.2(3) . . ? C9 C10 Fe1 69.3(3) . . ? C11 C10 Fe1 130.2(4) . . ? C10 C11 C14 112.2(5) . . ? C10 C11 C13 110.4(5) . . ? C14 C11 C13 109.9(5) . . ? C10 C11 C12 106.9(4) . . ? C14 C11 C12 108.8(5) . . ? C13 C11 C12 108.5(5) . . ? C18 C15 C7 112.7(5) . . ? C18 C15 C16 109.3(6) . . ? C7 C15 C16 109.9(5) . . ? C18 C15 C17 108.8(5) . . ? C7 C15 C17 106.2(4) . . ? C16 C15 C17 109.8(6) . . ? C23 C19 C20 108.2(6) . . ? C23 C19 Fe2 71.8(4) . . ? C20 C19 Fe2 70.2(3) . . ? C21 C20 C19 106.7(7) . . ? C21 C20 Fe2 71.6(3) . . ? C19 C20 Fe2 70.1(3) . . ? C22 C21 C20 108.5(6) . . ? C22 C21 Fe2 71.7(4) . . ? C20 C21 Fe2 69.5(4) . . ? C21 C22 C23 107.8(6) . . ? C21 C22 Fe2 70.1(4) . . ? C23 C22 Fe2 69.9(4) . . ? C19 C23 C22 108.8(7) . . ? C19 C23 Fe2 70.0(4) . . ? C22 C23 Fe2 71.9(4) . . ? C28 C24 C25 107.3(7) . . ? C28 C24 Fe3 69.5(4) . . ? C25 C24 Fe3 71.1(4) . . ? C26 C25 C24 107.0(8) . . ? C26 C25 Fe3 70.3(4) . . ? C24 C25 Fe3 70.1(4) . . ? C27 C26 C25 107.7(7) . . ? C27 C26 Fe3 69.3(4) . . ? C25 C26 Fe3 71.4(4) . . ? C26 C27 C28 110.1(7) . . ? C26 C27 Fe3 72.8(4) . . ? C28 C27 Fe3 71.4(4) . . ? C27 C28 C24 107.9(7) . . ? C27 C28 Fe3 70.5(4) . . ? C24 C28 Fe3 72.0(4) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.880 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.137 data_fesb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cl2 Fe O2 Sb' _chemical_formula_weight 481.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.919(2) _cell_length_b 10.089(2) _cell_length_c 15.006(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.68(3) _cell_angle_gamma 90.00 _cell_volume 1798.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 631 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.07 _exptl_crystal_description stick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.606 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _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 'STOE IPDS' _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 12507 _diffrn_reflns_av_R_equivalents 0.2769 _diffrn_reflns_av_sigmaI/netI 0.2446 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.07 _reflns_number_total 3387 _reflns_number_gt 1341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS-XP' _computing_publication_material 'SHELXL-97' _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^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3387 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2047 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1613 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb Sb 0.03511(7) 0.14358(10) 0.75178(8) 0.0367(3) Uani 1 1 d . . . Fe Fe 0.22503(14) 0.11280(18) 0.69404(14) 0.0301(5) Uani 1 1 d . . . Cl1 Cl 0.0568(3) 0.3577(4) 0.8284(3) 0.0477(10) Uani 1 1 d . . . Cl2 Cl 0.0535(3) 0.0271(4) 0.8916(3) 0.0556(12) Uani 1 1 d . . . C1 C 0.2870(12) 0.1846(14) 0.7900(10) 0.038(4) Uani 1 1 d . . . O1 O 0.3319(9) 0.2297(11) 0.8549(8) 0.059(3) Uani 1 1 d . . . C2 C 0.2331(12) -0.0424(15) 0.7395(11) 0.041(4) Uani 1 1 d . . . O2 O 0.2412(8) -0.1496(11) 0.7721(8) 0.059(3) Uani 1 1 d . . . C3 C 0.3443(9) 0.1369(13) 0.5963(10) 0.036(3) Uani 1 1 d . . . H3 H 0.4228 0.1207 0.6060 0.043 Uiso 1 1 calc R . . C4 C 0.2871(10) 0.2595(12) 0.6096(11) 0.033(4) Uani 1 1 d . . . C5 C 0.1678(9) 0.2410(12) 0.5878(10) 0.028(3) Uani 1 1 d . . . H5 H 0.1105 0.3061 0.5902 0.034 Uiso 1 1 calc R . . C6 C 0.1535(10) 0.1072(13) 0.5625(10) 0.036(4) Uani 1 1 d . . . H6 H 0.0831 0.0660 0.5460 0.044 Uiso 1 1 calc R . . C7 C 0.2587(11) 0.0437(13) 0.5652(11) 0.040(4) Uani 1 1 d . . . C8 C 0.2830(11) -0.0944(13) 0.5255(12) 0.039(4) Uani 1 1 d . . . C9 C 0.3029(13) -0.0715(16) 0.4275(13) 0.058(5) Uani 1 1 d . . . H9A H 0.3249 -0.1552 0.4007 0.088 Uiso 1 1 calc R . . H9B H 0.3630 -0.0061 0.4234 0.088 Uiso 1 1 calc R . . H9C H 0.2335 -0.0386 0.3954 0.088 Uiso 1 1 calc R . . C10 C 0.3902(11) -0.1542(15) 0.5734(11) 0.044(4) Uani 1 1 d . . . H10A H 0.4082 -0.2377 0.5445 0.066 Uiso 1 1 calc R . . H10B H 0.3779 -0.1709 0.6362 0.066 Uiso 1 1 calc R . . H10C H 0.4529 -0.0920 0.5702 0.066 Uiso 1 1 calc R . . C11 C 0.1841(12) -0.1916(14) 0.5326(13) 0.054(5) Uani 1 1 d . . . H11A H 0.1689 -0.2014 0.5955 0.081 Uiso 1 1 calc R . . H11B H 0.2038 -0.2781 0.5086 0.081 Uiso 1 1 calc R . . H11C H 0.1169 -0.1570 0.4983 0.081 Uiso 1 1 calc R . . C12 C 0.3431(10) 0.3955(11) 0.6263(10) 0.029(3) Uani 1 1 d . . . C13 C 0.4609(11) 0.3764(15) 0.6757(11) 0.048(4) Uani 1 1 d . . . H13A H 0.4957 0.4631 0.6881 0.072 Uiso 1 1 calc R . . H13B H 0.5081 0.3243 0.6382 0.072 Uiso 1 1 calc R . . H13C H 0.4536 0.3295 0.7321 0.072 Uiso 1 1 calc R . . C15 C 0.2709(13) 0.4840(13) 0.6795(12) 0.051(5) Uani 1 1 d . . . H15A H 0.2600 0.4422 0.7371 0.076 Uiso 1 1 calc R . . H15B H 0.1977 0.4974 0.6462 0.076 Uiso 1 1 calc R . . H15C H 0.3083 0.5698 0.6898 0.076 Uiso 1 1 calc R . . C14 C 0.3567(13) 0.4562(13) 0.5336(11) 0.046(4) Uani 1 1 d . . . H14A H 0.2826 0.4649 0.5008 0.068 Uiso 1 1 calc R . . H14B H 0.4044 0.3984 0.5003 0.068 Uiso 1 1 calc R . . H14C H 0.3918 0.5438 0.5409 0.068 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 Sb 0.0272(5) 0.0425(6) 0.0408(7) 0.0016(6) 0.0046(4) 0.0001(5) Fe 0.0226(9) 0.0323(11) 0.0351(14) 0.0042(9) 0.0001(9) -0.0004(8) Cl1 0.0426(19) 0.047(2) 0.054(3) -0.011(2) 0.0103(17) 0.003(2) Cl2 0.054(2) 0.066(3) 0.047(3) 0.014(2) 0.008(2) -0.009(2) C1 0.041(8) 0.057(10) 0.013(9) 0.003(7) -0.003(7) -0.010(7) O1 0.053(7) 0.073(8) 0.047(9) 0.007(6) -0.023(6) -0.019(6) C2 0.039(8) 0.041(9) 0.041(11) 0.015(8) 0.001(7) 0.004(7) O2 0.056(6) 0.046(6) 0.075(9) 0.025(7) 0.009(6) 0.015(6) C3 0.020(6) 0.027(7) 0.059(11) 0.000(8) -0.006(6) -0.005(7) C4 0.027(7) 0.027(7) 0.045(11) -0.006(7) 0.009(7) -0.001(6) C5 0.015(6) 0.019(7) 0.052(11) -0.003(6) 0.008(6) 0.006(5) C6 0.023(7) 0.039(8) 0.048(11) -0.001(7) 0.006(7) -0.006(6) C7 0.024(7) 0.033(8) 0.065(13) -0.004(7) 0.006(7) 0.022(6) C8 0.029(7) 0.025(7) 0.060(13) -0.008(7) -0.004(8) 0.003(6) C9 0.048(10) 0.057(11) 0.072(16) -0.008(9) 0.011(9) 0.001(8) C10 0.042(8) 0.037(8) 0.053(12) 0.002(8) -0.004(7) 0.004(8) C11 0.040(8) 0.050(10) 0.071(15) -0.011(9) 0.007(8) -0.005(7) C12 0.030(7) 0.019(7) 0.040(10) 0.001(6) 0.009(6) -0.002(5) C13 0.042(8) 0.042(9) 0.060(12) -0.014(8) -0.003(7) -0.014(7) C15 0.053(10) 0.025(8) 0.075(14) -0.025(8) 0.015(9) -0.010(7) C14 0.056(10) 0.030(8) 0.053(12) 0.002(8) 0.015(8) -0.022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb Cl2 2.399(4) . ? Sb Cl1 2.451(4) . ? Sb Fe 2.508(2) . ? Fe C2 1.708(15) . ? Fe C1 1.724(14) . ? Fe C6 2.087(15) . ? Fe C4 2.121(15) . ? Fe C5 2.122(14) . ? Fe C7 2.124(16) . ? Fe C3 2.138(14) . ? C1 O1 1.165(16) . ? C2 O2 1.188(16) . ? C3 C4 1.434(18) . ? C3 C7 1.436(18) . ? C4 C5 1.444(16) . ? C4 C12 1.537(17) . ? C5 C6 1.410(17) . ? C6 C7 1.406(17) . ? C7 C8 1.552(18) . ? C8 C9 1.53(2) . ? C8 C10 1.538(17) . ? C8 C11 1.543(19) . ? C12 C15 1.513(19) . ? C12 C14 1.54(2) . ? C12 C13 1.545(17) . ? 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 Cl2 Sb Cl1 91.30(15) . . ? Cl2 Sb Fe 102.76(12) . . ? Cl1 Sb Fe 101.98(10) . . ? C2 Fe C1 92.6(7) . . ? C2 Fe C6 111.0(6) . . ? C1 Fe C6 156.4(6) . . ? C2 Fe C4 150.2(6) . . ? C1 Fe C4 93.4(6) . . ? C6 Fe C4 65.7(5) . . ? C2 Fe C5 149.7(6) . . ? C1 Fe C5 117.4(6) . . ? C6 Fe C5 39.1(5) . . ? C4 Fe C5 39.8(5) . . ? C2 Fe C7 93.1(7) . . ? C1 Fe C7 143.0(6) . . ? C6 Fe C7 39.0(5) . . ? C4 Fe C7 65.4(5) . . ? C5 Fe C7 65.8(5) . . ? C2 Fe C3 111.1(6) . . ? C1 Fe C3 105.2(6) . . ? C6 Fe C3 66.2(5) . . ? C4 Fe C3 39.3(5) . . ? C5 Fe C3 66.8(5) . . ? C7 Fe C3 39.4(5) . . ? C2 Fe Sb 89.9(5) . . ? C1 Fe Sb 89.8(5) . . ? C6 Fe Sb 91.1(4) . . ? C4 Fe Sb 119.3(3) . . ? C5 Fe Sb 86.6(3) . . ? C7 Fe Sb 126.7(4) . . ? C3 Fe Sb 153.1(3) . . ? O1 C1 Fe 177.5(14) . . ? O2 C2 Fe 178.4(13) . . ? C4 C3 C7 106.1(10) . . ? C4 C3 Fe 69.7(8) . . ? C7 C3 Fe 69.7(8) . . ? C3 C4 C5 109.1(10) . . ? C3 C4 C12 126.0(10) . . ? C5 C4 C12 123.9(11) . . ? C3 C4 Fe 71.0(8) . . ? C5 C4 Fe 70.1(8) . . ? C12 C4 Fe 133.9(10) . . ? C6 C5 C4 106.3(10) . . ? C6 C5 Fe 69.1(8) . . ? C4 C5 Fe 70.1(8) . . ? C7 C6 C5 109.9(12) . . ? C7 C6 Fe 71.9(9) . . ? C5 C6 Fe 71.8(8) . . ? C6 C7 C3 108.6(11) . . ? C6 C7 C8 126.2(12) . . ? C3 C7 C8 124.3(11) . . ? C6 C7 Fe 69.1(9) . . ? C3 C7 Fe 70.9(9) . . ? C8 C7 Fe 134.4(11) . . ? C9 C8 C10 108.7(12) . . ? C9 C8 C11 110.0(13) . . ? C10 C8 C11 109.2(12) . . ? C9 C8 C7 106.5(13) . . ? C10 C8 C7 110.3(12) . . ? C11 C8 C7 112.1(12) . . ? C15 C12 C4 110.8(11) . . ? C15 C12 C14 110.4(12) . . ? C4 C12 C14 106.5(11) . . ? C15 C12 C13 110.7(12) . . ? C4 C12 C13 109.4(10) . . ? C14 C12 C13 108.9(12) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.912 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.194 data_bife3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30.67 H24 Bi1.33 Fe4 N1.33 O8' _chemical_formula_weight 1041.22 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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)/n 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 8.144(2) _cell_length_b 18.352(4) _cell_length_c 16.518(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.53(3) _cell_angle_gamma 90.00 _cell_volume 2466.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(1) _cell_measurement_reflns_used 1333 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 26.04 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.103 _exptl_crystal_density_method ? _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 8.881 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10636 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.04 _reflns_number_total 4566 _reflns_number_observed 3903 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4566 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_obs 0.0520 _refine_ls_wR_factor_all 0.1362 _refine_ls_wR_factor_obs 0.1319 _refine_ls_goodness_of_fit_all 0.991 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 0.991 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Bi Bi 0.06375(3) 0.080925(13) 0.217535(15) 0.02507(14) Uani 1 d . . Fe1 Fe -0.03030(14) -0.06165(6) 0.22188(6) 0.0277(2) Uani 1 d . . Fe2 Fe 0.35967(15) 0.09031(5) 0.14867(6) 0.0282(3) Uani 1 d . . Fe3 Fe 0.10145(14) 0.13449(5) 0.37059(6) 0.0293(3) Uani 1 d . . C1 C 0.1717(12) -0.0888(4) 0.2516(5) 0.036(2) Uani 1 d . . O1 O 0.2974(9) -0.1114(4) 0.2682(5) 0.060(2) Uani 1 d . . C2 C -0.0910(11) -0.0511(4) 0.3204(5) 0.035(2) Uani 1 d . . O2 O -0.1366(10) -0.0486(4) 0.3864(4) 0.056(2) Uani 1 d . . O3 O 0.5144(8) 0.0311(4) 0.2958(4) 0.048(2) Uani 1 d . . O4 O 0.3209(9) -0.0509(3) 0.0717(4) 0.051(2) Uani 1 d . . O5 O 0.4190(10) 0.1995(4) 0.3463(5) 0.060(2) Uani 1 d . . O6 O 0.2457(9) -0.0018(3) 0.4256(4) 0.051(2) Uani 1 d . . C3 C -0.2635(11) -0.1023(5) 0.1838(6) 0.041(2) Uani 1 d . . H3 H -0.3522(11) -0.1108(5) 0.2181(6) 0.050 Uiso 1 calc R . C4 C -0.2289(11) -0.0364(5) 0.1411(5) 0.039(2) Uani 1 d . . H4 H -0.2915(11) 0.0073(5) 0.1421(5) 0.047 Uiso 1 calc R . C5 C -0.0875(11) -0.0474(5) 0.0979(5) 0.041(2) Uani 1 d . . H5 H -0.0372(11) -0.0123(5) 0.0646(5) 0.049 Uiso 1 calc R . C6 C -0.0314(11) -0.1198(5) 0.1122(5) 0.040(2) Uani 1 d . . H6 H 0.0621(11) -0.1419(5) 0.0900(5) 0.048 Uiso 1 calc R . C7 C -0.1385(12) -0.1523(4) 0.1644(6) 0.044(2) Uani 1 d . . H7 H -0.1294(12) -0.2009(4) 0.1841(6) 0.053 Uiso 1 calc R . C8 C 0.4491(10) 0.0545(4) 0.2383(5) 0.034(2) Uani 1 d . . C9 C 0.3313(10) 0.0055(4) 0.1050(5) 0.034(2) Uani 1 d . . C10 C 0.4859(13) 0.1899(4) 0.1551(5) 0.044(2) Uani 1 d . . H10 H 0.5538(13) 0.2048(4) 0.2003(5) 0.052 Uiso 1 calc R . C11 C 0.5389(13) 0.1496(5) 0.0881(5) 0.044(2) Uani 1 d . . H11 H 0.6471(13) 0.1326(5) 0.0797(5) 0.053 Uiso 1 calc R . C12 C 0.3981(12) 0.1399(5) 0.0363(5) 0.043(2) Uani 1 d . . H12 H 0.3951(12) 0.1150(5) -0.0142(5) 0.051 Uiso 1 calc R . C13 C 0.2650(13) 0.1725(4) 0.0710(5) 0.043(2) Uani 1 d . . H13 H 0.1553(13) 0.1734(4) 0.0490(5) 0.051 Uiso 1 calc R . C14 C 0.3208(12) 0.2039(4) 0.1445(5) 0.039(2) Uani 1 d . . H14 H 0.2557(12) 0.2303(4) 0.1807(5) 0.047 Uiso 1 calc R . C15 C 0.2895(11) 0.1717(4) 0.3523(5) 0.036(2) Uani 1 d . . C16 C 0.1843(11) 0.0517(4) 0.4023(4) 0.034(2) Uani 1 d . . C17 C -0.0923(19) 0.2061(8) 0.3410(8) 0.074(4) Uani 1 d . . H17 H -0.1130(19) 0.2278(8) 0.2893(8) 0.089 Uiso 1 calc R . C18 C -0.1549(14) 0.1419(9) 0.3663(9) 0.080(5) Uani 1 d . . H18 H -0.2246(14) 0.1097(9) 0.3357(9) 0.096 Uiso 1 calc R . C19 C -0.0961(16) 0.1325(6) 0.4464(9) 0.077(4) Uani 1 d . . H19 H -0.1222(16) 0.0922(6) 0.4796(9) 0.092 Uiso 1 calc R . C21 C 0.0074(18) 0.2349(6) 0.4039(9) 0.073(4) Uani 1 d . . H21 H 0.0685(18) 0.2789(6) 0.4018(9) 0.087 Uiso 1 calc R . C20 C 0.0024(16) 0.1881(7) 0.4703(7) 0.064(3) Uani 1 d . . H20 H 0.0572(16) 0.1942(7) 0.5218(7) 0.077 Uiso 1 calc R . C22 C 0.5058(16) -0.1347(7) 0.4452(8) 0.070(3) Uani 1 d . . H22A H 0.4495(101) -0.0980(30) 0.4109(8) 0.105 Uiso 1 calc R . H22B H 0.5905(22) -0.1110(38) 0.4800(42) 0.105 Uiso 1 calc R . H22C H 0.4260(88) -0.1588(11) 0.4789(43) 0.105 Uiso 1 calc R . C23 C 0.5796(14) -0.1868(6) 0.3959(7) 0.059(3) Uani 1 d . . N N 0.6370(17) -0.2315(8) 0.3572(10) 0.100(4) Uani 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 Bi 0.0299(2) 0.0257(2) 0.0197(2) -0.00007(8) 0.00322(13) 0.00067(9) Fe1 0.0318(6) 0.0295(5) 0.0220(5) 0.0010(4) 0.0026(4) -0.0034(4) Fe2 0.0340(6) 0.0304(5) 0.0205(5) 0.0007(4) 0.0066(5) -0.0033(4) Fe3 0.0362(6) 0.0298(5) 0.0223(5) -0.0039(4) 0.0054(5) 0.0032(4) C1 0.047(5) 0.030(4) 0.031(4) 0.007(3) 0.000(4) -0.002(3) O1 0.048(4) 0.064(4) 0.067(5) 0.009(4) -0.008(4) 0.023(4) C2 0.041(4) 0.035(4) 0.031(4) 0.001(3) 0.007(4) -0.012(3) O2 0.073(5) 0.071(4) 0.026(3) 0.000(3) 0.016(3) -0.023(4) O3 0.046(4) 0.069(4) 0.030(3) 0.008(3) -0.007(3) 0.008(3) O4 0.061(4) 0.039(3) 0.053(4) -0.022(3) 0.020(3) -0.004(3) O5 0.060(5) 0.073(5) 0.048(4) -0.017(3) 0.005(4) -0.020(4) O6 0.059(4) 0.051(3) 0.042(4) 0.007(3) 0.000(3) 0.011(3) C3 0.029(4) 0.049(4) 0.046(5) -0.004(4) -0.002(4) -0.008(4) C4 0.037(4) 0.044(4) 0.036(4) 0.001(3) -0.008(4) 0.002(4) C5 0.046(5) 0.058(5) 0.019(3) -0.005(3) -0.003(4) -0.020(4) C6 0.037(4) 0.046(4) 0.038(4) -0.019(4) 0.006(4) 0.000(4) C7 0.052(5) 0.029(4) 0.050(5) -0.009(3) -0.007(5) -0.001(4) C8 0.035(4) 0.037(4) 0.030(4) -0.001(3) 0.004(3) -0.002(3) C9 0.033(4) 0.043(4) 0.025(4) 0.000(3) 0.008(3) -0.001(3) C10 0.060(6) 0.034(4) 0.036(4) 0.003(3) -0.003(4) -0.021(4) C11 0.050(5) 0.045(4) 0.039(5) 0.011(3) 0.014(4) -0.009(4) C12 0.057(6) 0.052(5) 0.020(4) 0.001(3) 0.010(4) -0.009(4) C13 0.054(5) 0.040(4) 0.035(4) 0.013(3) 0.002(4) -0.004(4) C14 0.055(5) 0.025(3) 0.038(4) 0.002(3) 0.014(4) 0.001(3) C15 0.045(5) 0.033(4) 0.029(4) -0.010(3) 0.004(4) -0.009(3) C16 0.047(5) 0.039(4) 0.016(3) 0.001(3) -0.005(3) 0.006(4) C17 0.098(10) 0.073(8) 0.051(6) -0.006(6) 0.014(7) 0.046(8) C18 0.037(5) 0.120(11) 0.082(9) -0.069(9) 0.004(6) 0.029(6) C19 0.074(8) 0.061(6) 0.101(10) 0.008(7) 0.070(8) 0.012(6) C21 0.088(9) 0.036(5) 0.097(10) -0.016(5) 0.044(8) 0.016(5) C20 0.067(7) 0.077(7) 0.047(6) -0.029(5) 0.001(6) 0.031(6) C22 0.063(7) 0.092(8) 0.055(6) -0.019(6) -0.002(6) 0.026(7) C23 0.051(6) 0.065(6) 0.060(6) 0.005(5) -0.003(5) 0.010(5) N 0.087(9) 0.106(9) 0.107(11) -0.030(8) 0.017(9) 0.027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi Fe2 2.7155(14) . ? Bi Fe3 2.7172(12) . ? Bi Fe1 2.7282(12) . ? Fe1 C2 1.732(8) . ? Fe1 C1 1.768(10) . ? Fe1 C7 2.092(8) . ? Fe1 C5 2.096(8) . ? Fe1 C4 2.102(8) . ? Fe1 C6 2.103(8) . ? Fe1 C3 2.111(8) . ? Fe2 C9 1.726(8) . ? Fe2 C8 1.749(8) . ? Fe2 C10 2.096(8) . ? Fe2 C12 2.103(8) . ? Fe2 C13 2.104(8) . ? Fe2 C11 2.109(9) . ? Fe2 C14 2.109(7) . ? Fe3 C15 1.716(9) . ? Fe3 C16 1.733(8) . ? Fe3 C21 2.079(9) . ? Fe3 C19 2.082(11) . ? Fe3 C18 2.090(11) . ? Fe3 C17 2.095(12) . ? Fe3 C20 2.110(10) . ? C1 O1 1.127(11) . ? C2 O2 1.169(11) . ? O3 C8 1.150(10) . ? O4 C9 1.175(10) . ? O5 C15 1.180(11) . ? O6 C16 1.160(10) . ? C3 C7 1.419(13) . ? C3 C4 1.434(13) . ? C4 C5 1.397(13) . ? C5 C6 1.422(13) . ? C6 C7 1.388(14) . ? C10 C14 1.372(14) . ? C10 C11 1.414(14) . ? C11 C12 1.412(13) . ? C12 C13 1.385(14) . ? C13 C14 1.401(12) . ? C17 C18 1.36(2) . ? C17 C21 1.39(2) . ? C18 C19 1.40(2) . ? C19 C20 1.35(2) . ? C21 C20 1.40(2) . ? C22 C23 1.41(2) . ? C23 N 1.15(2) . ? 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 Fe2 Bi Fe3 107.51(4) . . ? Fe2 Bi Fe1 109.10(3) . . ? Fe3 Bi Fe1 110.05(3) . . ? C2 Fe1 C1 94.1(4) . . ? C2 Fe1 C7 112.6(4) . . ? C1 Fe1 C7 105.6(4) . . ? C2 Fe1 C5 147.5(4) . . ? C1 Fe1 C5 118.1(4) . . ? C7 Fe1 C5 65.5(4) . . ? C2 Fe1 C4 109.1(4) . . ? C1 Fe1 C4 156.8(4) . . ? C7 Fe1 C4 65.8(3) . . ? C5 Fe1 C4 38.9(4) . . ? C2 Fe1 C6 151.1(4) . . ? C1 Fe1 C6 93.7(4) . . ? C7 Fe1 C6 38.6(4) . . ? C5 Fe1 C6 39.6(4) . . ? C4 Fe1 C6 65.9(4) . . ? C2 Fe1 C3 91.7(4) . . ? C1 Fe1 C3 142.9(4) . . ? C7 Fe1 C3 39.5(4) . . ? C5 Fe1 C3 66.1(4) . . ? C4 Fe1 C3 39.8(4) . . ? C6 Fe1 C3 66.1(4) . . ? C2 Fe1 Bi 90.5(3) . . ? C1 Fe1 Bi 91.1(2) . . ? C7 Fe1 Bi 149.8(3) . . ? C5 Fe1 Bi 84.5(2) . . ? C4 Fe1 Bi 88.9(2) . . ? C6 Fe1 Bi 117.0(3) . . ? C3 Fe1 Bi 125.5(3) . . ? C9 Fe2 C8 93.3(4) . . ? C9 Fe2 C10 149.6(4) . . ? C8 Fe2 C10 95.7(4) . . ? C9 Fe2 C12 92.5(4) . . ? C8 Fe2 C12 146.8(4) . . ? C10 Fe2 C12 64.9(3) . . ? C9 Fe2 C13 110.7(4) . . ? C8 Fe2 C13 155.9(4) . . ? C10 Fe2 C13 64.6(4) . . ? C12 Fe2 C13 38.4(4) . . ? C9 Fe2 C11 110.5(4) . . ? C8 Fe2 C11 108.9(4) . . ? C10 Fe2 C11 39.3(4) . . ? C12 Fe2 C11 39.2(4) . . ? C13 Fe2 C11 65.4(4) . . ? C9 Fe2 C14 149.3(4) . . ? C8 Fe2 C14 117.1(4) . . ? C10 Fe2 C14 38.1(4) . . ? C12 Fe2 C14 64.6(3) . . ? C13 Fe2 C14 38.8(3) . . ? C11 Fe2 C14 65.2(4) . . ? C9 Fe2 Bi 90.7(3) . . ? C8 Fe2 Bi 88.0(3) . . ? C10 Fe2 Bi 118.4(3) . . ? C12 Fe2 Bi 124.5(3) . . ? C13 Fe2 Bi 89.6(3) . . ? C11 Fe2 Bi 151.3(3) . . ? C14 Fe2 Bi 86.7(3) . . ? C15 Fe3 C16 93.6(4) . . ? C15 Fe3 C21 92.0(5) . . ? C16 Fe3 C21 147.1(5) . . ? C15 Fe3 C19 146.3(5) . . ? C16 Fe3 C19 96.0(4) . . ? C21 Fe3 C19 63.5(5) . . ? C15 Fe3 C18 150.0(6) . . ? C16 Fe3 C18 116.2(6) . . ? C21 Fe3 C18 64.7(6) . . ? C19 Fe3 C18 39.1(6) . . ? C15 Fe3 C17 112.2(6) . . ? C16 Fe3 C17 154.1(6) . . ? C21 Fe3 C17 39.0(5) . . ? C19 Fe3 C17 63.7(6) . . ? C18 Fe3 C17 37.9(6) . . ? C15 Fe3 C20 109.0(5) . . ? C16 Fe3 C20 109.3(4) . . ? C21 Fe3 C20 38.9(5) . . ? C19 Fe3 C20 37.5(5) . . ? C18 Fe3 C20 65.2(4) . . ? C17 Fe3 C20 65.1(5) . . ? C15 Fe3 Bi 92.6(3) . . ? C16 Fe3 Bi 89.5(2) . . ? C21 Fe3 Bi 122.6(4) . . ? C19 Fe3 Bi 119.6(5) . . ? C18 Fe3 Bi 85.4(3) . . ? C17 Fe3 Bi 87.5(3) . . ? C20 Fe3 Bi 149.8(3) . . ? O1 C1 Fe1 174.6(8) . . ? O2 C2 Fe1 175.4(7) . . ? C7 C3 C4 106.0(9) . . ? C7 C3 Fe1 69.5(5) . . ? C4 C3 Fe1 69.8(5) . . ? C5 C4 C3 108.3(8) . . ? C5 C4 Fe1 70.3(5) . . ? C3 C4 Fe1 70.4(5) . . ? C4 C5 C6 108.4(8) . . ? C4 C5 Fe1 70.8(5) . . ? C6 C5 Fe1 70.5(5) . . ? C7 C6 C5 107.4(7) . . ? C7 C6 Fe1 70.2(5) . . ? C5 C6 Fe1 69.9(4) . . ? C6 C7 C3 109.8(8) . . ? C6 C7 Fe1 71.1(5) . . ? C3 C7 Fe1 71.0(5) . . ? O3 C8 Fe2 177.0(8) . . ? O4 C9 Fe2 175.2(8) . . ? C14 C10 C11 109.3(8) . . ? C14 C10 Fe2 71.5(5) . . ? C11 C10 Fe2 70.8(5) . . ? C12 C11 C10 105.8(9) . . ? C12 C11 Fe2 70.2(5) . . ? C10 C11 Fe2 69.9(5) . . ? C13 C12 C11 108.9(8) . . ? C13 C12 Fe2 70.8(5) . . ? C11 C12 Fe2 70.6(5) . . ? C12 C13 C14 107.9(8) . . ? C12 C13 Fe2 70.7(5) . . ? C14 C13 Fe2 70.8(5) . . ? C10 C14 C13 108.2(9) . . ? C10 C14 Fe2 70.5(5) . . ? C13 C14 Fe2 70.4(4) . . ? O5 C15 Fe3 174.5(7) . . ? O6 C16 Fe3 176.7(7) . . ? C18 C17 C21 108.3(12) . . ? C18 C17 Fe3 70.9(7) . . ? C21 C17 Fe3 69.9(7) . . ? C17 C18 C19 106.3(11) . . ? C17 C18 Fe3 71.3(8) . . ? C19 C18 Fe3 70.1(6) . . ? C20 C19 C18 111.0(12) . . ? C20 C19 Fe3 72.4(7) . . ? C18 C19 Fe3 70.7(7) . . ? C17 C21 C20 108.4(12) . . ? C17 C21 Fe3 71.1(6) . . ? C20 C21 Fe3 71.7(6) . . ? C19 C20 C21 105.9(11) . . ? C19 C20 Fe3 70.2(6) . . ? C21 C20 Fe3 69.4(6) . . ? N C23 C22 177.4(16) . . ? _refine_diff_density_max 2.711 _refine_diff_density_min -3.512 _refine_diff_density_rms 0.254 data_bife2cl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H42 Bi Cl Fe2 O4' _chemical_formula_weight 822.77 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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)/n 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 10.479(2) _cell_length_b 15.405(3) _cell_length_c 20.248(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.84(3) _cell_angle_gamma 90.00 _cell_volume 3229.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 1230 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.85 _exptl_crystal_description route _exptl_crystal_colour green _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method ? _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 6.435 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20177 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.85 _reflns_number_total 5830 _reflns_number_observed 5080 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SIEMENS-XP' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+11.9601P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5830 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_obs 0.0513 _refine_ls_wR_factor_all 0.1409 _refine_ls_wR_factor_obs 0.1371 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Bi Bi 0.83034(3) 0.227895(15) 0.109607(13) 0.03088(13) Uani 1 d . . Fe1 Fe 1.01553(11) 0.27614(6) 0.04174(5) 0.0281(2) Uani 1 d . . Fe2 Fe 0.84611(11) 0.06138(6) 0.14832(5) 0.0290(2) Uani 1 d . . Cl Cl 0.9252(2) 0.30212(12) 0.22201(10) 0.0446(5) Uani 1 d . . C1 C 0.9963(8) 0.3819(4) 0.0699(4) 0.035(2) Uani 1 d . . O1 O 0.9911(8) 0.4527(4) 0.0869(3) 0.058(2) Uani 1 d . . C2 C 1.1256(8) 0.2474(5) 0.1142(4) 0.037(2) Uani 1 d . . O2 O 1.2024(8) 0.2322(5) 0.1594(4) 0.062(2) Uani 1 d . . C3 C 0.9973(9) 0.0504(5) 0.1211(4) 0.044(2) Uani 1 d . . O3 O 1.0919(8) 0.0400(5) 0.1011(5) 0.074(2) Uani 1 d . . C4 C 0.7656(10) 0.0302(5) 0.0688(4) 0.043(2) Uani 1 d . . O4 O 0.7138(8) 0.0059(4) 0.0183(3) 0.062(2) Uani 1 d . . C5 C 1.0109(7) 0.3191(4) -0.0571(3) 0.0285(14) Uani 1 d . . H5 H 1.0048(7) 0.3783(4) -0.0705(3) 0.034 Uiso 1 calc R . C6 C 1.1281(8) 0.2752(4) -0.0361(4) 0.032(2) Uani 1 d . . C7 C 1.0921(7) 0.1888(5) -0.0206(4) 0.0316(15) Uani 1 d . . H7 H 1.1504(7) 0.1434(5) -0.0051(4) 0.038 Uiso 1 calc R . C8 C 0.9579(8) 0.1820(4) -0.0319(4) 0.034(2) Uani 1 d . . H8 H 0.9100(8) 0.1313(4) -0.0250(4) 0.041 Uiso 1 calc R . C9 C 0.9035(7) 0.2638(4) -0.0557(4) 0.030(2) Uani 1 d . . C10 C 1.2636(8) 0.3091(5) -0.0384(4) 0.039(2) Uani 1 d . . C11 C 1.2748(10) 0.4026(7) -0.0131(8) 0.079(4) Uani 1 d . . H11A H 1.2536(96) 0.4049(12) 0.0324(20) 0.118 Uiso 1 calc R . H11B H 1.2147(72) 0.4395(13) -0.0425(30) 0.118 Uiso 1 calc R . H11C H 1.3633(27) 0.4233(23) -0.0128(50) 0.118 Uiso 1 calc R . C12 C 1.3653(9) 0.2576(7) 0.0075(5) 0.052(2) Uani 1 d . . H12A H 1.3495(43) 0.2629(40) 0.0537(7) 0.078 Uiso 1 calc R . H12B H 1.4513(11) 0.2804(32) 0.0039(28) 0.078 Uiso 1 calc R . H12C H 1.3606(49) 0.1963(11) -0.0058(24) 0.078 Uiso 1 calc R . C13 C 1.2891(11) 0.3015(11) -0.1092(5) 0.081(4) Uani 1 d . . H13A H 1.3621(65) 0.3389(53) -0.1154(15) 0.121 Uiso 1 calc R . H13B H 1.2122(36) 0.3197(66) -0.1399(6) 0.121 Uiso 1 calc R . H13C H 1.3097(100) 0.2411(16) -0.1185(17) 0.121 Uiso 1 calc R . C14 C 0.7632(8) 0.2835(5) -0.0833(4) 0.037(2) Uani 1 d . . C15 C 0.6726(10) 0.2126(7) -0.0663(6) 0.056(2) Uani 1 d . . H15A H 0.5865(22) 0.2215(31) -0.0921(30) 0.085 Uiso 1 calc R . H15B H 0.6670(61) 0.2147(34) -0.0185(9) 0.085 Uiso 1 calc R . H15C H 0.7058(43) 0.1558(7) -0.0774(38) 0.085 Uiso 1 calc R . C16 C 0.7215(9) 0.3718(6) -0.0572(6) 0.053(2) Uani 1 d . . H16A H 0.7212(69) 0.3680(15) -0.0089(8) 0.079 Uiso 1 calc R . H16B H 0.6346(30) 0.3864(24) -0.0797(27) 0.079 Uiso 1 calc R . H16C H 0.7823(42) 0.4169(10) -0.0664(33) 0.079 Uiso 1 calc R . C17 C 0.7530(10) 0.2862(9) -0.1597(5) 0.066(3) Uani 1 d . . H17A H 0.6623(13) 0.2928(58) -0.1798(6) 0.098 Uiso 1 calc R . H17B H 0.7872(78) 0.2321(24) -0.1755(7) 0.098 Uiso 1 calc R . H17C H 0.8030(69) 0.3354(34) -0.1726(6) 0.098 Uiso 1 calc R . C18 C 0.7666(7) -0.0308(4) 0.2075(4) 0.0308(15) Uani 1 d . . H18 H 0.7378(7) -0.0866(4) 0.1918(4) 0.037 Uiso 1 calc R . C19 C 0.8906(7) -0.0120(4) 0.2385(4) 0.032(2) Uani 1 d . . C20 C 0.8949(7) 0.0790(4) 0.2512(4) 0.0308(15) Uani 1 d . . H20 H 0.9687(7) 0.1111(4) 0.2704(4) 0.037 Uiso 1 calc R . C21 C 0.7696(8) 0.1132(5) 0.2303(3) 0.032(2) Uani 1 d . . H21 H 0.7446(8) 0.1720(5) 0.2341(3) 0.039 Uiso 1 calc R . C22 C 0.6882(7) 0.0450(4) 0.2026(4) 0.0297(15) Uani 1 d . . C23 C 0.9953(8) -0.0770(5) 0.2645(4) 0.042(2) Uani 1 d . . C24 C 1.1320(10) -0.0397(8) 0.2674(7) 0.078(4) Uani 1 d . . H24A H 1.1455(36) -0.0223(61) 0.2224(10) 0.117 Uiso 1 calc R . H24B H 1.1957(10) -0.0839(23) 0.2846(49) 0.117 Uiso 1 calc R . H24C H 1.1421(33) 0.0110(40) 0.2970(40) 0.117 Uiso 1 calc R . C25 C 0.9799(11) -0.1608(6) 0.2236(6) 0.061(3) Uani 1 d . . H25A H 1.0455(54) -0.2028(21) 0.2429(27) 0.092 Uiso 1 calc R . H25B H 0.9905(83) -0.1483(12) 0.1773(12) 0.092 Uiso 1 calc R . H25C H 0.8937(32) -0.1851(30) 0.2246(36) 0.092 Uiso 1 calc R . C26 C 0.9734(12) -0.0975(7) 0.3358(5) 0.064(3) Uani 1 d . . H26A H 1.0407(50) -0.1374(45) 0.3566(16) 0.096 Uiso 1 calc R . H26B H 0.8885(37) -0.1246(52) 0.3346(6) 0.096 Uiso 1 calc R . H26C H 0.9771(85) -0.0437(10) 0.3618(13) 0.096 Uiso 1 calc R . C27 C 0.5435(8) 0.0500(5) 0.1831(4) 0.039(2) Uani 1 d . . C28 C 0.5032(10) 0.1304(6) 0.1400(5) 0.053(2) Uani 1 d . . H28A H 0.4089(10) 0.1355(29) 0.1328(33) 0.080 Uiso 1 calc R . H28B H 0.5337(66) 0.1245(24) 0.0969(16) 0.080 Uiso 1 calc R . H28C H 0.5413(61) 0.1824(8) 0.1630(18) 0.080 Uiso 1 calc R . C29 C 0.4885(9) -0.0295(6) 0.1433(5) 0.052(2) Uani 1 d . . H29A H 0.3942(11) -0.0251(24) 0.1340(32) 0.079 Uiso 1 calc R . H29B H 0.5131(61) -0.0822(7) 0.1693(16) 0.079 Uiso 1 calc R . H29C H 0.5231(57) -0.0320(27) 0.1010(17) 0.079 Uiso 1 calc R . C30 C 0.4845(9) 0.0540(7) 0.2478(5) 0.054(2) Uani 1 d . . H30A H 0.3902(10) 0.0509(50) 0.2370(6) 0.081 Uiso 1 calc R . H30B H 0.5093(61) 0.1086(23) 0.2711(20) 0.081 Uiso 1 calc R . H30C H 0.5162(58) 0.0051(29) 0.2766(17) 0.081 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi 0.0357(2) 0.0222(2) 0.0372(2) 0.00136(9) 0.01360(14) 0.00271(9) Fe1 0.0329(6) 0.0223(5) 0.0306(5) 0.0011(4) 0.0092(5) 0.0010(3) Fe2 0.0399(6) 0.0203(4) 0.0284(5) 0.0003(4) 0.0104(5) 0.0001(4) Cl 0.0641(14) 0.0303(9) 0.0437(10) -0.0146(8) 0.0223(10) -0.0112(8) C1 0.041(4) 0.025(3) 0.039(4) 0.002(3) 0.007(4) -0.001(3) O1 0.091(5) 0.025(3) 0.059(4) -0.007(3) 0.010(4) -0.005(3) C2 0.027(4) 0.044(4) 0.039(4) 0.001(3) 0.007(4) -0.002(3) O2 0.052(5) 0.088(6) 0.043(4) 0.004(3) -0.003(4) 0.016(4) C3 0.054(5) 0.035(4) 0.050(5) 0.014(3) 0.031(4) 0.014(3) O3 0.072(5) 0.057(4) 0.104(6) 0.025(4) 0.048(5) 0.033(4) C4 0.068(6) 0.023(3) 0.039(4) -0.001(3) 0.014(4) 0.002(3) O4 0.101(6) 0.045(3) 0.035(3) -0.006(3) -0.002(4) -0.002(3) C5 0.030(4) 0.026(3) 0.030(3) 0.006(3) 0.007(3) 0.003(3) C6 0.034(4) 0.033(4) 0.027(4) 0.004(3) 0.002(3) 0.003(3) C7 0.033(4) 0.031(3) 0.031(3) 0.002(3) 0.007(3) 0.007(3) C8 0.043(4) 0.024(3) 0.039(4) -0.006(3) 0.012(4) 0.001(3) C9 0.029(4) 0.029(3) 0.034(4) 0.001(3) 0.008(3) 0.001(3) C10 0.027(4) 0.046(4) 0.044(4) 0.011(4) 0.001(4) 0.000(3) C11 0.037(5) 0.046(5) 0.150(13) 0.011(6) 0.006(7) -0.011(4) C12 0.034(5) 0.072(6) 0.048(5) 0.007(5) -0.002(4) 0.002(4) C13 0.039(6) 0.164(13) 0.041(5) 0.022(7) 0.008(5) -0.014(7) C14 0.029(4) 0.037(4) 0.045(5) -0.004(3) 0.005(4) 0.002(3) C15 0.035(5) 0.060(5) 0.074(7) -0.013(5) 0.010(5) -0.007(4) C16 0.039(5) 0.040(4) 0.076(7) -0.004(4) 0.001(5) 0.010(4) C17 0.032(5) 0.113(9) 0.047(6) 0.006(5) -0.009(5) 0.010(5) C18 0.036(4) 0.024(3) 0.033(4) 0.006(3) 0.005(3) 0.001(3) C19 0.035(4) 0.028(3) 0.033(4) 0.005(3) 0.009(3) 0.000(3) C20 0.034(4) 0.029(3) 0.031(4) -0.003(3) 0.007(3) -0.005(3) C21 0.043(4) 0.030(3) 0.026(3) 0.001(3) 0.010(3) 0.002(3) C22 0.035(4) 0.029(3) 0.026(3) 0.002(3) 0.007(3) -0.002(3) C23 0.034(5) 0.039(4) 0.049(5) 0.011(3) -0.004(4) 0.004(3) C24 0.039(6) 0.078(7) 0.114(10) 0.039(7) -0.001(7) 0.000(5) C25 0.062(7) 0.052(5) 0.066(6) -0.002(5) -0.003(5) 0.028(5) C26 0.070(7) 0.058(6) 0.061(6) 0.021(5) -0.004(6) 0.015(5) C27 0.035(4) 0.031(4) 0.051(5) 0.011(3) 0.003(4) 0.000(3) C28 0.048(5) 0.038(4) 0.071(6) 0.020(4) 0.002(5) 0.010(4) C29 0.040(5) 0.051(5) 0.061(6) -0.002(4) -0.012(5) -0.005(4) C30 0.038(5) 0.067(6) 0.061(6) 0.006(5) 0.015(5) 0.002(4) _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 Bi Cl 2.604(2) . ? Bi Fe1 2.6507(12) . ? Bi Fe2 2.6799(11) . ? Fe1 C1 1.747(7) . ? Fe1 C2 1.778(9) . ? Fe1 C7 2.088(7) . ? Fe1 C5 2.102(7) . ? Fe1 C8 2.102(7) . ? Fe1 C6 2.109(8) . ? Fe1 C9 2.144(8) . ? Fe2 C3 1.764(8) . ? Fe2 C4 1.766(9) . ? Fe2 C20 2.085(7) . ? Fe2 C21 2.108(7) . ? Fe2 C18 2.111(7) . ? Fe2 C19 2.136(7) . ? Fe2 C22 2.138(7) . ? C1 O1 1.148(9) . ? C2 O2 1.146(11) . ? C3 O3 1.138(10) . ? C4 O4 1.144(11) . ? C5 C6 1.409(10) . ? C5 C9 1.415(10) . ? C6 C7 1.430(10) . ? C6 C10 1.520(11) . ? C7 C8 1.394(11) . ? C8 C9 1.436(10) . ? C9 C14 1.521(12) . ? C10 C13 1.502(13) . ? C10 C12 1.525(12) . ? C10 C11 1.528(14) . ? C14 C15 1.521(12) . ? C14 C17 1.535(14) . ? C14 C16 1.545(11) . ? C18 C19 1.385(11) . ? C18 C22 1.422(10) . ? C19 C20 1.424(10) . ? C19 C23 1.518(10) . ? C20 C21 1.418(11) . ? C21 C22 1.414(10) . ? C22 C27 1.509(11) . ? C23 C25 1.528(13) . ? C23 C26 1.529(14) . ? C23 C24 1.536(13) . ? C27 C29 1.529(12) . ? C27 C30 1.533(12) . ? C27 C28 1.536(11) . ? 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 Cl Bi Fe1 96.79(5) . . ? Cl Bi Fe2 99.59(5) . . ? Fe1 Bi Fe2 113.76(3) . . ? C1 Fe1 C2 93.2(4) . . ? C1 Fe1 C7 150.7(3) . . ? C2 Fe1 C7 94.5(3) . . ? C1 Fe1 C5 91.7(3) . . ? C2 Fe1 C5 141.4(3) . . ? C7 Fe1 C5 65.3(3) . . ? C1 Fe1 C8 147.1(3) . . ? C2 Fe1 C8 119.6(3) . . ? C7 Fe1 C8 38.9(3) . . ? C5 Fe1 C8 65.1(3) . . ? C1 Fe1 C6 110.9(3) . . ? C2 Fe1 C6 104.4(3) . . ? C7 Fe1 C6 39.9(3) . . ? C5 Fe1 C6 39.1(3) . . ? C8 Fe1 C6 66.3(3) . . ? C1 Fe1 C9 108.0(3) . . ? C2 Fe1 C9 158.7(3) . . ? C7 Fe1 C9 66.0(3) . . ? C5 Fe1 C9 38.9(3) . . ? C8 Fe1 C9 39.5(3) . . ? C6 Fe1 C9 66.5(3) . . ? C1 Fe1 Bi 87.8(3) . . ? C2 Fe1 Bi 86.3(3) . . ? C7 Fe1 Bi 120.9(2) . . ? C5 Fe1 Bi 132.1(2) . . ? C8 Fe1 Bi 91.2(2) . . ? C6 Fe1 Bi 157.5(2) . . ? C9 Fe1 Bi 96.4(2) . . ? C3 Fe2 C4 90.9(4) . . ? C3 Fe2 C20 103.3(4) . . ? C4 Fe2 C20 162.9(3) . . ? C3 Fe2 C21 138.7(4) . . ? C4 Fe2 C21 129.4(4) . . ? C20 Fe2 C21 39.5(3) . . ? C3 Fe2 C18 124.4(3) . . ? C4 Fe2 C18 99.2(3) . . ? C20 Fe2 C18 65.0(3) . . ? C21 Fe2 C18 64.9(3) . . ? C3 Fe2 C19 97.3(3) . . ? C4 Fe2 C19 130.3(3) . . ? C20 Fe2 C19 39.4(3) . . ? C21 Fe2 C19 65.6(3) . . ? C18 Fe2 C19 38.0(3) . . ? C3 Fe2 C22 162.3(3) . . ? C4 Fe2 C22 97.9(4) . . ? C20 Fe2 C22 65.9(3) . . ? C21 Fe2 C22 38.9(3) . . ? C18 Fe2 C22 39.1(3) . . ? C19 Fe2 C22 65.3(3) . . ? C3 Fe2 Bi 91.1(2) . . ? C4 Fe2 Bi 89.7(2) . . ? C20 Fe2 Bi 99.4(2) . . ? C21 Fe2 Bi 81.6(2) . . ? C18 Fe2 Bi 142.9(2) . . ? C19 Fe2 Bi 138.7(2) . . ? C22 Fe2 Bi 104.2(2) . . ? O1 C1 Fe1 175.5(8) . . ? O2 C2 Fe1 175.5(8) . . ? O3 C3 Fe2 176.2(10) . . ? O4 C4 Fe2 176.7(7) . . ? C6 C5 C9 111.3(6) . . ? C6 C5 Fe1 70.7(4) . . ? C9 C5 Fe1 72.1(4) . . ? C5 C6 C7 105.4(7) . . ? C5 C6 C10 126.9(6) . . ? C7 C6 C10 127.2(7) . . ? C5 C6 Fe1 70.2(4) . . ? C7 C6 Fe1 69.3(4) . . ? C10 C6 Fe1 130.8(6) . . ? C8 C7 C6 109.1(6) . . ? C8 C7 Fe1 71.1(4) . . ? C6 C7 Fe1 70.9(4) . . ? C7 C8 C9 109.1(6) . . ? C7 C8 Fe1 70.0(4) . . ? C9 C8 Fe1 71.8(4) . . ? C5 C9 C8 105.1(7) . . ? C5 C9 C14 126.8(6) . . ? C8 C9 C14 127.6(7) . . ? C5 C9 Fe1 68.9(4) . . ? C8 C9 Fe1 68.7(4) . . ? C14 C9 Fe1 133.0(5) . . ? C13 C10 C6 107.9(8) . . ? C13 C10 C12 109.3(9) . . ? C6 C10 C12 111.8(7) . . ? C13 C10 C11 112.2(10) . . ? C6 C10 C11 109.7(7) . . ? C12 C10 C11 106.0(8) . . ? C9 C14 C15 112.0(7) . . ? C9 C14 C17 106.8(7) . . ? C15 C14 C17 107.3(8) . . ? C9 C14 C16 111.0(7) . . ? C15 C14 C16 109.6(7) . . ? C17 C14 C16 110.0(8) . . ? C19 C18 C22 110.6(6) . . ? C19 C18 Fe2 72.0(4) . . ? C22 C18 Fe2 71.5(4) . . ? C18 C19 C20 106.8(6) . . ? C18 C19 C23 126.6(7) . . ? C20 C19 C23 125.8(7) . . ? C18 C19 Fe2 70.0(4) . . ? C20 C19 Fe2 68.4(4) . . ? C23 C19 Fe2 134.1(5) . . ? C21 C20 C19 108.1(6) . . ? C21 C20 Fe2 71.1(4) . . ? C19 C20 Fe2 72.2(4) . . ? C22 C21 C20 108.4(6) . . ? C22 C21 Fe2 71.7(4) . . ? C20 C21 Fe2 69.4(4) . . ? C21 C22 C18 106.0(7) . . ? C21 C22 C27 125.9(6) . . ? C18 C22 C27 127.4(7) . . ? C21 C22 Fe2 69.4(4) . . ? C18 C22 Fe2 69.4(4) . . ? C27 C22 Fe2 133.3(5) . . ? C19 C23 C25 111.0(7) . . ? C19 C23 C26 105.0(7) . . ? C25 C23 C26 108.5(8) . . ? C19 C23 C24 112.7(7) . . ? C25 C23 C24 110.9(9) . . ? C26 C23 C24 108.4(9) . . ? C22 C27 C29 112.3(7) . . ? C22 C27 C30 107.4(7) . . ? C29 C27 C30 108.3(7) . . ? C22 C27 C28 111.6(7) . . ? C29 C27 C28 107.3(8) . . ? C30 C27 C28 109.9(7) . . ? _refine_diff_density_max 6.613 _refine_diff_density_min -1.982 _refine_diff_density_rms 0.196