Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Aldridge, Simon' 'Coombs, D.L.' 'Jones, Cameron' _publ_contact_author_name 'Dr Simon Aldridge' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UK ; _publ_contact_author_email 'ALDRIDGES@CARDIFF.AC.UK' _publ_section_title ; [( 5-C5H5)Fe(CO)2]2B(2,4,6-Me3C6H2): Synthesis, Spectroscopic and Structural Charecterization of a Transition Metal Complex Containing an Unsupported Bridging Borylene Ligand ; data_cj158 _database_code_CSD 179292 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 B Br Fe O2' _chemical_formula_weight 400.88 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' 'B' 'B' 0.0013 0.0007 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.3150(17) _cell_length_b 15.283(3) _cell_length_c 14.113(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.89(3) _cell_angle_gamma 90.00 _cell_volume 1733.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 3.177 _exptl_absorpt_correction_type sortav _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.54 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius CCD' _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 31913 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3963 _reflns_number_gt 3356 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+4.7821P] 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 3963 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.31200(5) 0.24324(3) 0.40883(3) 0.05372(15) Uani 1 1 d . . . Fe1 Fe 0.02046(5) 0.19074(3) 0.31447(3) 0.02383(12) Uani 1 1 d . . . O1 O -0.0283(4) 0.37742(18) 0.3266(2) 0.0616(8) Uani 1 1 d . . . O2 O 0.0825(4) 0.1520(2) 0.52132(19) 0.0657(9) Uani 1 1 d . . . C1 C -0.0081(4) 0.3039(2) 0.3232(3) 0.0359(8) Uani 1 1 d . . . C2 C 0.0565(5) 0.1687(2) 0.4399(3) 0.0383(8) Uani 1 1 d . . . C3 C -0.3582(4) 0.1358(2) 0.2299(2) 0.0244(6) Uani 1 1 d . . . C4 C -0.3950(4) 0.0472(2) 0.2410(2) 0.0291(7) Uani 1 1 d . . . C5 C -0.5199(4) 0.0062(2) 0.1702(2) 0.0326(7) Uani 1 1 d . . . H5 H -0.5427 -0.0525 0.1783 0.039 Uiso 1 1 calc R . . C6 C -0.6115(4) 0.0501(2) 0.0880(2) 0.0308(7) Uani 1 1 d . . . C7 C -0.5758(4) 0.1381(2) 0.0782(2) 0.0286(7) Uani 1 1 d . . . H7 H -0.6362 0.1688 0.0237 0.034 Uiso 1 1 calc R . . C8 C -0.4522(4) 0.1817(2) 0.1477(2) 0.0254(6) Uani 1 1 d . . . C9 C -0.3036(5) -0.0034(3) 0.3308(3) 0.0496(11) Uani 1 1 d . . . H9A H -0.3307 -0.0644 0.3216 0.074 Uiso 1 1 calc R . . H9B H -0.3363 0.0178 0.3871 0.074 Uiso 1 1 calc R . . H9C H -0.1858 0.0043 0.3407 0.074 Uiso 1 1 calc R . . C10 C -0.7470(5) 0.0039(3) 0.0125(3) 0.0434(9) Uani 1 1 d . . . H10A H -0.8009 -0.0381 0.0446 0.065 Uiso 1 1 calc R . . H10B H -0.6990 -0.0256 -0.0337 0.065 Uiso 1 1 calc R . . H10C H -0.8271 0.0460 -0.0213 0.065 Uiso 1 1 calc R . . C11 C -0.4251(5) 0.2784(2) 0.1369(3) 0.0352(8) Uani 1 1 d . . . H11A H -0.4988 0.2991 0.0771 0.053 Uiso 1 1 calc R . . H11B H -0.3119 0.2886 0.1352 0.053 Uiso 1 1 calc R . . H11C H -0.4474 0.3091 0.1915 0.053 Uiso 1 1 calc R . . C12 C 0.2512(4) 0.1588(3) 0.2842(3) 0.0419(9) Uani 1 1 d . . . H12 H 0.3558 0.1743 0.3227 0.050 Uiso 1 1 calc R . . C13 C 0.1529(5) 0.2080(3) 0.2072(3) 0.0450(9) Uani 1 1 d . . . H13 H 0.1811 0.2621 0.1859 0.054 Uiso 1 1 calc R . . C14 C 0.0033(5) 0.1619(3) 0.1669(2) 0.0383(8) Uani 1 1 d . . . H14 H -0.0835 0.1801 0.1150 0.046 Uiso 1 1 calc R . . C15 C 0.0097(4) 0.0834(2) 0.2197(2) 0.0326(7) Uani 1 1 d . . . H15 H -0.0722 0.0405 0.2084 0.039 Uiso 1 1 calc R . . C16 C 0.1628(4) 0.0810(2) 0.2932(3) 0.0357(8) Uani 1 1 d . . . C17 C 0.2264(6) 0.0069(3) 0.3630(3) 0.0566(12) Uani 1 1 d . . . H17A H 0.2830 -0.0348 0.3322 0.085 Uiso 1 1 calc R . . H17B H 0.1345 -0.0212 0.3803 0.085 Uiso 1 1 calc R . . H17C H 0.3021 0.0293 0.4211 0.085 Uiso 1 1 calc R . . B1 B -0.2175(4) 0.1835(2) 0.3086(2) 0.0259(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0355(2) 0.0898(4) 0.0403(2) -0.0338(2) 0.01775(17) -0.0124(2) Fe1 0.0229(2) 0.0246(2) 0.0232(2) -0.00151(17) 0.00459(17) -0.00061(17) O1 0.083(2) 0.0267(15) 0.076(2) -0.0045(14) 0.0232(18) -0.0031(14) O2 0.095(3) 0.070(2) 0.0262(14) 0.0055(13) 0.0049(15) 0.0279(19) C1 0.041(2) 0.0267(17) 0.0393(19) -0.0036(14) 0.0100(16) -0.0050(15) C2 0.043(2) 0.0353(19) 0.0315(18) -0.0024(14) 0.0010(15) 0.0095(15) C3 0.0232(14) 0.0308(16) 0.0200(14) -0.0020(12) 0.0069(12) -0.0019(12) C4 0.0279(16) 0.0325(17) 0.0251(15) 0.0034(13) 0.0035(13) -0.0051(13) C5 0.0313(17) 0.0306(17) 0.0354(18) -0.0017(14) 0.0077(14) -0.0071(14) C6 0.0235(15) 0.0418(19) 0.0268(16) -0.0076(14) 0.0061(13) -0.0022(14) C7 0.0240(15) 0.0376(18) 0.0236(15) 0.0004(13) 0.0050(12) 0.0062(13) C8 0.0241(15) 0.0291(16) 0.0249(14) -0.0009(12) 0.0100(12) 0.0033(12) C9 0.049(2) 0.046(2) 0.043(2) 0.0209(18) -0.0071(18) -0.0175(18) C10 0.0336(19) 0.056(2) 0.0357(19) -0.0110(17) 0.0010(15) -0.0077(17) C11 0.0396(19) 0.0297(17) 0.0363(18) 0.0027(14) 0.0096(15) 0.0057(14) C12 0.0248(17) 0.060(2) 0.043(2) -0.0103(18) 0.0115(15) -0.0001(16) C13 0.053(2) 0.047(2) 0.045(2) 0.0007(17) 0.0302(19) -0.0023(18) C14 0.044(2) 0.048(2) 0.0236(16) -0.0030(15) 0.0107(15) 0.0119(17) C15 0.0297(17) 0.0353(18) 0.0321(17) -0.0106(14) 0.0063(14) 0.0043(14) C16 0.0329(18) 0.0389(19) 0.0345(18) -0.0039(15) 0.0072(14) 0.0121(15) C17 0.059(3) 0.054(3) 0.051(2) 0.002(2) 0.003(2) 0.026(2) B1 0.0281(17) 0.0287(18) 0.0224(16) -0.0033(13) 0.0092(14) -0.0044(14) _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 Br1 B1 2.005(3) . ? Fe1 C2 1.751(4) . ? Fe1 C1 1.754(4) . ? Fe1 B1 1.962(4) . ? Fe1 C14 2.097(3) . ? Fe1 C15 2.104(3) . ? Fe1 C13 2.105(4) . ? Fe1 C16 2.118(3) . ? Fe1 C12 2.126(3) . ? O1 C1 1.139(4) . ? O2 C2 1.142(4) . ? C3 C4 1.405(4) . ? C3 C8 1.408(4) . ? C3 B1 1.571(4) . ? C4 C5 1.392(4) . ? C4 C9 1.512(5) . ? C5 C6 1.386(5) . ? C6 C7 1.393(5) . ? C6 C10 1.512(4) . ? C7 C8 1.394(4) . ? C8 C11 1.510(5) . ? C12 C13 1.400(6) . ? C12 C16 1.421(5) . ? C13 C14 1.416(6) . ? C14 C15 1.405(5) . ? C15 C16 1.421(5) . ? C16 C17 1.505(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 96.28(17) . . ? C2 Fe1 B1 86.59(16) . . ? C1 Fe1 B1 84.55(16) . . ? C2 Fe1 C14 156.06(16) . . ? C1 Fe1 C14 107.54(16) . . ? B1 Fe1 C14 97.81(15) . . ? C2 Fe1 C15 117.49(15) . . ? C1 Fe1 C15 145.98(15) . . ? B1 Fe1 C15 92.97(14) . . ? C14 Fe1 C15 39.07(14) . . ? C2 Fe1 C13 140.02(17) . . ? C1 Fe1 C13 91.85(17) . . ? B1 Fe1 C13 133.23(16) . . ? C14 Fe1 C13 39.38(15) . . ? C15 Fe1 C13 65.48(15) . . ? C2 Fe1 C16 91.98(15) . . ? C1 Fe1 C16 151.79(16) . . ? B1 Fe1 C16 122.93(15) . . ? C14 Fe1 C16 65.83(14) . . ? C15 Fe1 C16 39.33(13) . . ? C13 Fe1 C16 65.34(15) . . ? C2 Fe1 C12 103.30(16) . . ? C1 Fe1 C12 112.70(17) . . ? B1 Fe1 C12 158.54(15) . . ? C14 Fe1 C12 65.62(15) . . ? C15 Fe1 C12 65.58(14) . . ? C13 Fe1 C12 38.63(15) . . ? C16 Fe1 C12 39.11(15) . . ? O1 C1 Fe1 178.4(4) . . ? O2 C2 Fe1 177.9(3) . . ? C4 C3 C8 118.7(3) . . ? C4 C3 B1 120.8(3) . . ? C8 C3 B1 120.4(3) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 C9 119.5(3) . . ? C3 C4 C9 120.6(3) . . ? C6 C5 C4 122.1(3) . . ? C5 C6 C7 117.7(3) . . ? C5 C6 C10 120.9(3) . . ? C7 C6 C10 121.4(3) . . ? C6 C7 C8 121.9(3) . . ? C7 C8 C3 119.7(3) . . ? C7 C8 C11 119.9(3) . . ? C3 C8 C11 120.4(3) . . ? C13 C12 C16 107.9(3) . . ? C13 C12 Fe1 69.9(2) . . ? C16 C12 Fe1 70.14(19) . . ? C12 C13 C14 108.8(3) . . ? C12 C13 Fe1 71.5(2) . . ? C14 C13 Fe1 70.0(2) . . ? C15 C14 C13 107.6(3) . . ? C15 C14 Fe1 70.71(19) . . ? C13 C14 Fe1 70.6(2) . . ? C14 C15 C16 108.3(3) . . ? C14 C15 Fe1 70.22(19) . . ? C16 C15 Fe1 70.89(19) . . ? C12 C16 C15 107.4(3) . . ? C12 C16 C17 125.8(3) . . ? C15 C16 C17 126.6(4) . . ? C12 C16 Fe1 70.8(2) . . ? C15 C16 Fe1 69.77(18) . . ? C17 C16 Fe1 128.2(3) . . ? C3 B1 Fe1 128.0(2) . . ? C3 B1 Br1 110.8(2) . . ? Fe1 B1 Br1 121.24(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.941 _refine_diff_density_min -1.813 _refine_diff_density_rms 0.083 data_c:\bono\mesb\s92 _database_code_CSD 179293 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H21 B Fe2 O4' _chemical_formula_weight 483.91 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' 'B' 'B' 0.0013 0.0007 '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' _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 11.938(2) _cell_length_b 12.404(3) _cell_length_c 15.431(3) _cell_angle_alpha 111.56(3) _cell_angle_beta 97.15(3) _cell_angle_gamma 90.83(3) _cell_volume 2104.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min o.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type 'Sortav (Blessing, 1995)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Kappa-CCD _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 29366 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7309 _reflns_number_gt 5744 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+17.9586P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7309 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2712 _refine_ls_wR_factor_gt 0.2638 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28084(10) 0.47996(10) 0.11866(8) 0.0268(4) Uani 1 1 d . . . O1 O 0.5095(5) 0.4173(6) 0.0877(4) 0.0428(16) Uani 1 1 d . . . C1 C 0.3612(6) 0.7333(7) 0.2521(5) 0.0252(17) Uani 1 1 d . . . B1 B 0.3640(7) 0.6028(8) 0.2441(6) 0.0257(19) Uani 1 1 d . . . Fe2 Fe 0.45275(9) 0.58338(10) 0.36236(8) 0.0238(3) Uani 1 1 d . . . O2 O 0.2386(6) 0.3117(6) 0.2032(5) 0.0435(16) Uani 1 1 d . . . C2 C 0.4392(7) 0.7814(7) 0.2128(5) 0.0252(17) Uani 1 1 d . . . B2 B 0.1394(8) 0.8360(8) -0.2414(6) 0.027(2) Uani 1 1 d . . . Fe3 Fe 0.04827(9) 0.70846(10) -0.36050(8) 0.0238(3) Uani 1 1 d . . . O3 O 0.4979(5) 0.3436(6) 0.2601(5) 0.0387(15) Uani 1 1 d . . . C3 C 0.4370(7) 0.8970(8) 0.2226(6) 0.033(2) Uani 1 1 d . . . H3 H 0.4892 0.9264 0.1955 0.040 Uiso 1 1 calc R . . Fe4 Fe 0.22943(10) 0.83006(11) -0.11968(8) 0.0277(4) Uani 1 1 d . . . O4 O 0.2271(5) 0.5242(6) 0.3875(4) 0.0364(14) Uani 1 1 d . . . C4 C 0.3608(8) 0.9704(8) 0.2708(6) 0.035(2) Uani 1 1 d . . . O5 O 0.2730(5) 0.6313(5) -0.3900(4) 0.0349(14) Uani 1 1 d . . . C5 C 0.2839(7) 0.9231(8) 0.3090(6) 0.0315(19) Uani 1 1 d . . . H5 H 0.2316 0.9706 0.3419 0.038 Uiso 1 1 calc R . . O6 O 0.0048(5) 0.5625(6) -0.2571(4) 0.0392(15) Uani 1 1 d . . . C6 C 0.2812(7) 0.8085(8) 0.3007(6) 0.0305(19) Uani 1 1 d . . . O7 O 0.2658(5) 0.5848(6) -0.2099(5) 0.0402(15) Uani 1 1 d . . . C7 C 0.5270(7) 0.7081(8) 0.1585(6) 0.034(2) Uani 1 1 d . . . H7A H 0.4948 0.6687 0.0939 0.050 Uiso 1 1 calc R . . H7B H 0.5500 0.6520 0.1854 0.050 Uiso 1 1 calc R . . H7C H 0.5915 0.7574 0.1620 0.050 Uiso 1 1 calc R . . O8 O 0.0078(6) 0.7850(6) -0.0775(5) 0.0468(17) Uani 1 1 d . . . C8 C 0.3596(9) 1.0964(8) 0.2798(7) 0.044(2) Uani 1 1 d . . . H8A H 0.4320 1.1214 0.2705 0.066 Uiso 1 1 calc R . . H8B H 0.3438 1.1437 0.3414 0.066 Uiso 1 1 calc R . . H8C H 0.3022 1.1036 0.2332 0.066 Uiso 1 1 calc R . . C9 C 0.1949(7) 0.7641(8) 0.3463(6) 0.033(2) Uani 1 1 d . . . H9A H 0.2302 0.7630 0.4053 0.050 Uiso 1 1 calc R . . H9B H 0.1665 0.6869 0.3056 0.050 Uiso 1 1 calc R . . H9C H 0.1335 0.8144 0.3568 0.050 Uiso 1 1 calc R . . C10 C 0.1543(10) 0.4085(10) 0.0004(8) 0.058(3) Uani 1 1 d . . . H10 H 0.1347 0.3295 -0.0312 0.069 Uiso 1 1 calc R . . C11 C 0.2365(9) 0.4730(12) -0.0204(7) 0.054(3) Uani 1 1 d . . . H11 H 0.2824 0.4447 -0.0674 0.065 Uiso 1 1 calc R . . C12 C 0.2373(9) 0.5853(11) 0.0406(8) 0.050(3) Uani 1 1 d . . . H12 H 0.2830 0.6468 0.0409 0.060 Uiso 1 1 calc R . . C13 C 0.1611(8) 0.5939(9) 0.1011(7) 0.043(2) Uani 1 1 d . . . H13 H 0.1473 0.6612 0.1500 0.052 Uiso 1 1 calc R . . C14 C 0.1067(8) 0.4832(11) 0.0769(8) 0.050(3) Uani 1 1 d . . . H14 H 0.0503 0.4637 0.1060 0.060 Uiso 1 1 calc R . . C15 C 0.4182(8) 0.4441(8) 0.1018(6) 0.0313(19) Uani 1 1 d . . . C16 C 0.2554(7) 0.3817(8) 0.1718(6) 0.0310(19) Uani 1 1 d . . . C17 C 0.6256(7) 0.6362(8) 0.4024(6) 0.036(2) Uani 1 1 d . . . H17 H 0.6810 0.5984 0.3670 0.043 Uiso 1 1 calc R . . C18 C 0.5680(7) 0.7284(7) 0.3918(6) 0.0316(19) Uani 1 1 d . . . H18 H 0.5791 0.7639 0.3496 0.038 Uiso 1 1 calc R . . C19 C 0.4910(8) 0.7574(8) 0.4558(6) 0.037(2) Uani 1 1 d . . . H19 H 0.4413 0.8162 0.4632 0.045 Uiso 1 1 calc R . . C20 C 0.4994(7) 0.6852(8) 0.5074(6) 0.033(2) Uani 1 1 d . . . H20 H 0.4559 0.6867 0.5538 0.040 Uiso 1 1 calc R . . C21 C 0.5864(7) 0.6087(8) 0.4762(6) 0.034(2) Uani 1 1 d . . . H21 H 0.6123 0.5526 0.4991 0.041 Uiso 1 1 calc R . . C22 C 0.3156(7) 0.5493(7) 0.3753(5) 0.0272(18) Uani 1 1 d . . . C23 C 0.4786(7) 0.4395(8) 0.2972(6) 0.0296(19) Uani 1 1 d . . . C24 C 0.1381(7) 0.9615(7) -0.2481(5) 0.0266(17) Uani 1 1 d . . . C25 C 0.2135(7) 0.9942(8) -0.2992(6) 0.0296(18) Uani 1 1 d . . . C26 C 0.2100(7) 1.1037(7) -0.3055(6) 0.0324(19) Uani 1 1 d . . . H26 H 0.2608 1.1242 -0.3387 0.039 Uiso 1 1 calc R . . C27 C 0.1330(8) 1.1831(8) -0.2635(6) 0.036(2) Uani 1 1 d . . . C28 C 0.0582(7) 1.1492(8) -0.2143(6) 0.034(2) Uani 1 1 d . . . H28 H 0.0051 1.2003 -0.1867 0.041 Uiso 1 1 calc R . . C29 C 0.0599(7) 1.0413(8) -0.2050(6) 0.0307(19) Uani 1 1 d . . . C30 C 0.3006(7) 0.9141(8) -0.3469(6) 0.034(2) Uani 1 1 d . . . H30A H 0.2658 0.8594 -0.4067 0.050 Uiso 1 1 calc R . . H30B H 0.3304 0.8729 -0.3081 0.050 Uiso 1 1 calc R . . H30C H 0.3610 0.9590 -0.3560 0.050 Uiso 1 1 calc R . . C31 C 0.1303(9) 1.2991(9) -0.2729(8) 0.050(3) Uani 1 1 d . . . H31A H 0.1977 1.3459 -0.2382 0.075 Uiso 1 1 calc R . . H31B H 0.0653 1.3372 -0.2484 0.075 Uiso 1 1 calc R . . H31C H 0.1263 1.2886 -0.3381 0.075 Uiso 1 1 calc R . . C32 C -0.0242(8) 1.0133(9) -0.1504(6) 0.039(2) Uani 1 1 d . . . H32A H -0.0798 1.0702 -0.1386 0.059 Uiso 1 1 calc R . . H32B H 0.0142 1.0143 -0.0916 0.059 Uiso 1 1 calc R . . H32C H -0.0607 0.9377 -0.1860 0.059 Uiso 1 1 calc R . . C33 C -0.1262(7) 0.7177(8) -0.3998(6) 0.0310(19) Uani 1 1 d . . . H33 H -0.1813 0.7078 -0.3652 0.037 Uiso 1 1 calc R . . C34 C -0.0854(7) 0.6293(8) -0.4743(6) 0.0306(18) Uani 1 1 d . . . H34 H -0.1110 0.5514 -0.4989 0.037 Uiso 1 1 calc R . . C35 C 0.0002(7) 0.6787(8) -0.5051(6) 0.0307(19) Uani 1 1 d . . . H35 H 0.0427 0.6391 -0.5523 0.037 Uiso 1 1 calc R . . C36 C 0.0110(7) 0.8027(8) -0.4503(6) 0.034(2) Uani 1 1 d . . . H36 H 0.0608 0.8571 -0.4562 0.041 Uiso 1 1 calc R . . C37 C -0.0681(7) 0.8251(8) -0.3866(6) 0.035(2) Uani 1 1 d . . . H37 H -0.0804 0.8976 -0.3432 0.041 Uiso 1 1 calc R . . C38 C 0.1847(7) 0.6649(7) -0.3757(6) 0.0290(18) Uani 1 1 d . . . C39 C 0.0232(7) 0.6233(7) -0.2955(6) 0.0296(18) Uani 1 1 d . . . C40 C 0.2967(9) 0.9256(10) 0.0227(7) 0.048(3) Uani 1 1 d . . . H40 H 0.2665 0.9206 0.0739 0.058 Uiso 1 1 calc R . . C41 C 0.3787(7) 0.8604(9) -0.0210(7) 0.041(2) Uani 1 1 d . . . H41 H 0.4141 0.8038 -0.0036 0.049 Uiso 1 1 calc R . . C42 C 0.4019(7) 0.8909(10) -0.0956(7) 0.046(3) Uani 1 1 d . . . H42 H 0.4534 0.8575 -0.1369 0.055 Uiso 1 1 calc R . . C43 C 0.3326(9) 0.9821(9) -0.0968(7) 0.048(3) Uani 1 1 d . . . H43 H 0.3315 1.0212 -0.1381 0.057 Uiso 1 1 calc R . . C44 C 0.2655(8) 1.0027(9) -0.0243(7) 0.047(3) Uani 1 1 d . . . H44 H 0.2108 1.0568 -0.0097 0.057 Uiso 1 1 calc R . . C45 C 0.0951(7) 0.8029(7) -0.0961(6) 0.0310(19) Uani 1 1 d . . . C46 C 0.2504(7) 0.6806(9) -0.1771(6) 0.034(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0226(6) 0.0308(7) 0.0255(6) 0.0107(5) -0.0027(5) 0.0028(5) O1 0.032(4) 0.057(4) 0.037(4) 0.014(3) 0.004(3) 0.017(3) C1 0.017(4) 0.034(5) 0.026(4) 0.015(3) -0.004(3) 0.005(3) B1 0.019(4) 0.032(5) 0.027(5) 0.012(4) 0.003(4) 0.005(4) Fe2 0.0177(6) 0.0273(7) 0.0266(6) 0.0118(5) -0.0020(4) 0.0001(5) O2 0.044(4) 0.041(4) 0.048(4) 0.023(3) -0.002(3) -0.004(3) C2 0.022(4) 0.029(4) 0.024(4) 0.012(3) -0.005(3) 0.001(3) B2 0.021(4) 0.031(5) 0.024(5) 0.004(4) 0.007(4) 0.001(4) Fe3 0.0175(6) 0.0241(6) 0.0280(6) 0.0090(5) -0.0017(4) 0.0008(4) O3 0.031(3) 0.033(4) 0.047(4) 0.011(3) -0.003(3) 0.004(3) C3 0.026(4) 0.044(5) 0.029(4) 0.016(4) -0.006(3) -0.007(4) Fe4 0.0237(7) 0.0303(7) 0.0265(7) 0.0094(5) -0.0022(5) -0.0029(5) O4 0.027(3) 0.045(4) 0.039(3) 0.018(3) 0.003(3) -0.002(3) C4 0.039(5) 0.028(5) 0.035(5) 0.010(4) -0.001(4) 0.001(4) O5 0.025(3) 0.041(4) 0.036(3) 0.011(3) 0.005(3) 0.008(3) C5 0.026(4) 0.032(5) 0.034(5) 0.009(4) 0.000(3) 0.012(4) O6 0.038(4) 0.039(4) 0.043(4) 0.021(3) 0.001(3) -0.002(3) C6 0.030(5) 0.035(5) 0.026(4) 0.012(4) 0.000(3) 0.003(4) O7 0.035(4) 0.033(4) 0.051(4) 0.017(3) -0.002(3) 0.011(3) C7 0.029(5) 0.041(5) 0.033(5) 0.015(4) 0.005(4) 0.004(4) O8 0.037(4) 0.053(4) 0.045(4) 0.010(3) 0.011(3) -0.008(3) C8 0.047(6) 0.030(5) 0.054(6) 0.018(4) -0.004(5) 0.002(4) C9 0.021(4) 0.041(5) 0.040(5) 0.017(4) 0.005(4) 0.008(4) C10 0.065(8) 0.040(6) 0.050(6) 0.010(5) -0.032(6) 0.005(5) C11 0.042(6) 0.096(10) 0.029(5) 0.028(6) 0.001(4) 0.024(6) C12 0.038(6) 0.064(7) 0.057(7) 0.039(6) -0.013(5) -0.002(5) C13 0.035(5) 0.045(6) 0.041(5) 0.011(4) -0.015(4) 0.018(4) C14 0.026(5) 0.082(8) 0.055(6) 0.045(6) -0.006(4) -0.002(5) C15 0.036(5) 0.032(5) 0.024(4) 0.011(4) -0.001(4) 0.010(4) C16 0.018(4) 0.036(5) 0.034(5) 0.011(4) -0.008(3) 0.003(3) C17 0.025(4) 0.041(5) 0.035(5) 0.008(4) 0.001(4) -0.008(4) C18 0.027(4) 0.031(5) 0.040(5) 0.020(4) -0.006(4) -0.007(4) C19 0.037(5) 0.030(5) 0.037(5) 0.007(4) -0.005(4) 0.001(4) C20 0.025(4) 0.043(5) 0.025(4) 0.007(4) -0.005(3) -0.007(4) C21 0.026(4) 0.039(5) 0.033(5) 0.014(4) -0.012(4) -0.006(4) C22 0.023(4) 0.031(4) 0.025(4) 0.009(3) -0.002(3) 0.000(3) C23 0.023(4) 0.035(5) 0.033(4) 0.017(4) -0.001(3) 0.000(4) C24 0.028(4) 0.025(4) 0.024(4) 0.007(3) 0.000(3) 0.001(3) C25 0.024(4) 0.036(5) 0.025(4) 0.009(4) -0.003(3) -0.002(4) C26 0.028(5) 0.029(5) 0.040(5) 0.017(4) -0.007(4) -0.008(4) C27 0.037(5) 0.026(5) 0.039(5) 0.010(4) -0.011(4) -0.005(4) C28 0.027(5) 0.026(4) 0.040(5) 0.006(4) -0.007(4) 0.002(4) C29 0.022(4) 0.034(5) 0.028(4) 0.004(4) -0.002(3) -0.004(4) C30 0.030(5) 0.033(5) 0.037(5) 0.012(4) 0.007(4) -0.005(4) C31 0.051(6) 0.036(5) 0.062(7) 0.024(5) -0.015(5) -0.002(5) C32 0.037(5) 0.041(5) 0.036(5) 0.009(4) 0.010(4) 0.006(4) C33 0.015(4) 0.039(5) 0.037(5) 0.014(4) -0.004(3) -0.002(3) C34 0.024(4) 0.028(4) 0.035(5) 0.009(4) -0.007(3) -0.002(3) C35 0.020(4) 0.043(5) 0.026(4) 0.012(4) -0.005(3) 0.004(4) C36 0.029(5) 0.042(5) 0.035(5) 0.020(4) -0.005(4) -0.001(4) C37 0.025(4) 0.035(5) 0.036(5) 0.008(4) -0.007(4) 0.008(4) C38 0.030(5) 0.028(4) 0.027(4) 0.009(3) 0.003(3) -0.001(4) C39 0.021(4) 0.030(5) 0.035(5) 0.010(4) -0.001(3) 0.001(3) C40 0.052(6) 0.059(7) 0.026(5) 0.008(4) 0.001(4) -0.014(5) C41 0.021(4) 0.048(6) 0.049(6) 0.020(5) -0.015(4) -0.004(4) C42 0.018(4) 0.065(7) 0.039(5) 0.005(5) -0.004(4) -0.019(4) C43 0.047(6) 0.049(6) 0.044(6) 0.022(5) -0.018(5) -0.021(5) C44 0.027(5) 0.035(5) 0.058(6) -0.001(5) -0.017(4) -0.001(4) C45 0.030(5) 0.027(4) 0.033(5) 0.011(4) -0.003(4) -0.004(4) C46 0.025(4) 0.049(6) 0.029(4) 0.017(4) -0.001(3) -0.001(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 Fe1 C15 1.731(9) . ? Fe1 C16 1.743(9) . ? Fe1 C13 2.088(9) . ? Fe1 B1 2.089(10) . ? Fe1 C14 2.104(10) . ? Fe1 C12 2.109(10) . ? Fe1 C11 2.116(9) . ? Fe1 C10 2.118(10) . ? O1 C15 1.168(11) . ? C1 C2 1.409(11) . ? C1 C6 1.426(12) . ? C1 B1 1.577(13) . ? B1 Fe2 2.089(9) . ? Fe2 C22 1.739(8) . ? Fe2 C23 1.751(9) . ? Fe2 C17 2.101(9) . ? Fe2 C19 2.114(9) . ? Fe2 C20 2.122(8) . ? Fe2 C18 2.123(8) . ? Fe2 C21 2.147(8) . ? O2 C16 1.164(11) . ? C2 C3 1.387(12) . ? C2 C7 1.520(12) . ? B2 C24 1.597(13) . ? B2 Fe4 2.071(10) . ? B2 Fe3 2.093(9) . ? Fe3 C38 1.740(9) . ? Fe3 C39 1.748(9) . ? Fe3 C33 2.112(8) . ? Fe3 C35 2.125(8) . ? Fe3 C37 2.129(9) . ? Fe3 C36 2.130(9) . ? Fe3 C34 2.141(8) . ? O3 C23 1.156(11) . ? C3 C4 1.380(13) . ? Fe4 C45 1.743(9) . ? Fe4 C46 1.774(10) . ? Fe4 C44 2.106(9) . ? Fe4 C40 2.120(9) . ? Fe4 C42 2.123(9) . ? Fe4 C41 2.126(8) . ? Fe4 C43 2.129(10) . ? O4 C22 1.153(10) . ? C4 C5 1.382(13) . ? C4 C8 1.517(13) . ? O5 C38 1.156(10) . ? C5 C6 1.379(13) . ? O6 C39 1.150(10) . ? C6 C9 1.519(12) . ? O7 C46 1.135(11) . ? O8 C45 1.154(10) . ? C10 C11 1.398(17) . ? C10 C14 1.398(16) . ? C11 C12 1.364(17) . ? C12 C13 1.361(15) . ? C13 C14 1.407(15) . ? C17 C18 1.393(13) . ? C17 C21 1.430(13) . ? C18 C19 1.387(13) . ? C19 C20 1.398(13) . ? C20 C21 1.424(13) . ? C24 C29 1.411(12) . ? C24 C25 1.414(11) . ? C25 C26 1.398(12) . ? C25 C30 1.515(12) . ? C26 C27 1.393(13) . ? C27 C28 1.394(13) . ? C27 C31 1.498(13) . ? C28 C29 1.399(13) . ? C29 C32 1.501(12) . ? C33 C34 1.411(12) . ? C33 C37 1.427(13) . ? C34 C35 1.401(12) . ? C35 C36 1.452(13) . ? C36 C37 1.404(13) . ? C40 C41 1.361(15) . ? C40 C44 1.426(16) . ? C41 C42 1.392(14) . ? C42 C43 1.417(16) . ? C43 C44 1.406(15) . ? 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 C15 Fe1 C16 95.7(4) . . ? C15 Fe1 C13 142.0(4) . . ? C16 Fe1 C13 122.2(4) . . ? C15 Fe1 B1 81.8(4) . . ? C16 Fe1 B1 92.7(4) . . ? C13 Fe1 B1 93.3(4) . . ? C15 Fe1 C14 155.4(4) . . ? C16 Fe1 C14 91.5(4) . . ? C13 Fe1 C14 39.2(4) . . ? B1 Fe1 C14 121.4(4) . . ? C15 Fe1 C12 105.9(4) . . ? C16 Fe1 C12 155.8(4) . . ? C13 Fe1 C12 37.8(4) . . ? B1 Fe1 C12 101.0(4) . . ? C14 Fe1 C12 64.3(4) . . ? C15 Fe1 C11 93.3(4) . . ? C16 Fe1 C11 132.0(5) . . ? C13 Fe1 C11 64.1(4) . . ? B1 Fe1 C11 135.3(5) . . ? C14 Fe1 C11 64.9(4) . . ? C12 Fe1 C11 37.7(5) . . ? C15 Fe1 C10 116.9(4) . . ? C16 Fe1 C10 97.0(4) . . ? C13 Fe1 C10 64.6(4) . . ? B1 Fe1 C10 157.8(4) . . ? C14 Fe1 C10 38.7(4) . . ? C12 Fe1 C10 63.6(4) . . ? C11 Fe1 C10 38.6(5) . . ? C2 C1 C6 116.8(8) . . ? C2 C1 B1 121.3(7) . . ? C6 C1 B1 121.9(7) . . ? C1 B1 Fe1 115.6(6) . . ? C1 B1 Fe2 113.4(6) . . ? Fe1 B1 Fe2 131.0(5) . . ? C22 Fe2 C23 94.3(4) . . ? C22 Fe2 B1 80.1(4) . . ? C23 Fe2 B1 91.9(4) . . ? C22 Fe2 C17 157.8(4) . . ? C23 Fe2 C17 93.4(4) . . ? B1 Fe2 C17 120.4(4) . . ? C22 Fe2 C19 105.3(4) . . ? C23 Fe2 C19 157.3(4) . . ? B1 Fe2 C19 102.4(4) . . ? C17 Fe2 C19 64.2(4) . . ? C22 Fe2 C20 94.2(4) . . ? C23 Fe2 C20 130.3(4) . . ? B1 Fe2 C20 137.8(4) . . ? C17 Fe2 C20 65.2(3) . . ? C19 Fe2 C20 38.5(4) . . ? C22 Fe2 C18 141.1(4) . . ? C23 Fe2 C18 124.3(4) . . ? B1 Fe2 C18 93.8(4) . . ? C17 Fe2 C18 38.5(4) . . ? C19 Fe2 C18 38.2(4) . . ? C20 Fe2 C18 64.9(3) . . ? C22 Fe2 C21 119.0(4) . . ? C23 Fe2 C21 96.0(4) . . ? B1 Fe2 C21 158.5(4) . . ? C17 Fe2 C21 39.3(3) . . ? C19 Fe2 C21 64.7(4) . . ? C20 Fe2 C21 39.0(4) . . ? C18 Fe2 C21 65.3(3) . . ? C3 C2 C1 120.4(8) . . ? C3 C2 C7 118.6(7) . . ? C1 C2 C7 121.0(7) . . ? C24 B2 Fe4 115.2(6) . . ? C24 B2 Fe3 112.1(6) . . ? Fe4 B2 Fe3 132.7(5) . . ? C38 Fe3 C39 94.4(4) . . ? C38 Fe3 B2 80.2(4) . . ? C39 Fe3 B2 91.1(4) . . ? C38 Fe3 C33 156.9(4) . . ? C39 Fe3 C33 92.7(4) . . ? B2 Fe3 C33 121.6(3) . . ? C38 Fe3 C35 93.8(4) . . ? C39 Fe3 C35 130.8(4) . . ? B2 Fe3 C35 138.1(4) . . ? C33 Fe3 C35 65.2(3) . . ? C38 Fe3 C37 141.8(4) . . ? C39 Fe3 C37 123.6(4) . . ? B2 Fe3 C37 94.2(4) . . ? C33 Fe3 C37 39.3(3) . . ? C35 Fe3 C37 65.4(3) . . ? C38 Fe3 C36 105.2(4) . . ? C39 Fe3 C36 158.2(4) . . ? B2 Fe3 C36 101.4(4) . . ? C33 Fe3 C36 65.5(3) . . ? C35 Fe3 C36 39.9(4) . . ? C37 Fe3 C36 38.5(3) . . ? C38 Fe3 C34 118.4(4) . . ? C39 Fe3 C34 97.1(4) . . ? B2 Fe3 C34 158.8(4) . . ? C33 Fe3 C34 38.8(3) . . ? C35 Fe3 C34 38.3(3) . . ? C37 Fe3 C34 65.1(3) . . ? C36 Fe3 C34 65.4(3) . . ? C4 C3 C2 122.8(8) . . ? C45 Fe4 C46 93.5(4) . . ? C45 Fe4 B2 83.0(4) . . ? C46 Fe4 B2 91.4(4) . . ? C45 Fe4 C44 100.3(4) . . ? C46 Fe4 C44 157.9(4) . . ? B2 Fe4 C44 107.3(4) . . ? C45 Fe4 C40 95.3(4) . . ? C46 Fe4 C40 122.5(4) . . ? B2 Fe4 C40 146.1(4) . . ? C44 Fe4 C40 39.4(4) . . ? C45 Fe4 C42 159.6(4) . . ? C46 Fe4 C42 96.8(4) . . ? B2 Fe4 C42 114.2(4) . . ? C44 Fe4 C42 65.1(4) . . ? C40 Fe4 C42 64.3(4) . . ? C45 Fe4 C41 123.6(4) . . ? C46 Fe4 C41 93.8(4) . . ? B2 Fe4 C41 152.4(4) . . ? C44 Fe4 C41 64.2(4) . . ? C40 Fe4 C41 37.4(4) . . ? C42 Fe4 C41 38.3(4) . . ? C45 Fe4 C43 135.0(4) . . ? C46 Fe4 C43 131.4(4) . . ? B2 Fe4 C43 92.5(4) . . ? C44 Fe4 C43 38.8(4) . . ? C40 Fe4 C43 65.0(4) . . ? C42 Fe4 C43 38.9(4) . . ? C41 Fe4 C43 64.2(4) . . ? C3 C4 C5 116.8(8) . . ? C3 C4 C8 121.8(9) . . ? C5 C4 C8 121.4(8) . . ? C6 C5 C4 123.0(8) . . ? C5 C6 C1 120.2(8) . . ? C5 C6 C9 119.5(8) . . ? C1 C6 C9 120.3(8) . . ? C11 C10 C14 108.1(10) . . ? C11 C10 Fe1 70.6(6) . . ? C14 C10 Fe1 70.1(6) . . ? C12 C11 C10 107.5(10) . . ? C12 C11 Fe1 70.9(6) . . ? C10 C11 Fe1 70.8(6) . . ? C13 C12 C11 109.8(10) . . ? C13 C12 Fe1 70.2(6) . . ? C11 C12 Fe1 71.4(6) . . ? C12 C13 C14 108.2(10) . . ? C12 C13 Fe1 71.9(6) . . ? C14 C13 Fe1 71.0(6) . . ? C10 C14 C13 106.4(9) . . ? C10 C14 Fe1 71.2(6) . . ? C13 C14 Fe1 69.7(5) . . ? O1 C15 Fe1 177.8(8) . . ? O2 C16 Fe1 176.7(8) . . ? C18 C17 C21 109.4(8) . . ? C18 C17 Fe2 71.6(5) . . ? C21 C17 Fe2 72.1(5) . . ? C19 C18 C17 107.3(8) . . ? C19 C18 Fe2 70.5(5) . . ? C17 C18 Fe2 69.9(5) . . ? C18 C19 C20 109.8(8) . . ? C18 C19 Fe2 71.3(5) . . ? C20 C19 Fe2 71.1(5) . . ? C19 C20 C21 107.8(8) . . ? C19 C20 Fe2 70.4(5) . . ? C21 C20 Fe2 71.5(5) . . ? C20 C21 C17 105.7(8) . . ? C20 C21 Fe2 69.6(5) . . ? C17 C21 Fe2 68.6(5) . . ? O4 C22 Fe2 176.2(7) . . ? O3 C23 Fe2 175.2(8) . . ? C29 C24 C25 118.4(8) . . ? C29 C24 B2 120.8(7) . . ? C25 C24 B2 120.8(7) . . ? C26 C25 C24 120.0(8) . . ? C26 C25 C30 118.3(8) . . ? C24 C25 C30 121.7(8) . . ? C27 C26 C25 122.2(8) . . ? C26 C27 C28 117.2(8) . . ? C26 C27 C31 120.8(9) . . ? C28 C27 C31 121.9(9) . . ? C27 C28 C29 122.5(8) . . ? C28 C29 C24 119.7(8) . . ? C28 C29 C32 118.3(8) . . ? C24 C29 C32 122.0(8) . . ? C34 C33 C37 108.0(7) . . ? C34 C33 Fe3 71.7(5) . . ? C37 C33 Fe3 71.0(5) . . ? C35 C34 C33 108.5(8) . . ? C35 C34 Fe3 70.2(5) . . ? C33 C34 Fe3 69.5(4) . . ? C34 C35 C36 107.9(8) . . ? C34 C35 Fe3 71.5(5) . . ? C36 C35 Fe3 70.2(5) . . ? C37 C36 C35 107.1(8) . . ? C37 C36 Fe3 70.7(5) . . ? C35 C36 Fe3 69.8(5) . . ? C36 C37 C33 108.4(8) . . ? C36 C37 Fe3 70.8(5) . . ? C33 C37 Fe3 69.7(5) . . ? O5 C38 Fe3 176.5(8) . . ? O6 C39 Fe3 176.4(8) . . ? C41 C40 C44 107.6(9) . . ? C41 C40 Fe4 71.5(5) . . ? C44 C40 Fe4 69.8(5) . . ? C40 C41 C42 110.2(10) . . ? C40 C41 Fe4 71.1(6) . . ? C42 C41 Fe4 70.8(5) . . ? C41 C42 C43 107.2(9) . . ? C41 C42 Fe4 71.0(5) . . ? C43 C42 Fe4 70.8(5) . . ? C44 C43 C42 107.4(9) . . ? C44 C43 Fe4 69.7(6) . . ? C42 C43 Fe4 70.3(5) . . ? C43 C44 C40 107.5(9) . . ? C43 C44 Fe4 71.5(6) . . ? C40 C44 Fe4 70.8(6) . . ? O8 C45 Fe4 177.7(8) . . ? O7 C46 Fe4 176.9(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.578 (near Fe3) _refine_diff_density_min -0.997 _refine_diff_density_rms 0.203