Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'D.L. Coombs' 'S. Aldridge' 'C. Jones' _publ_contact_author_name 'Dr Simon Aldridge' _publ_contact_author_address ; Dr Simon Aldridge 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 ; Synthetic, structural and reaction chemistry of transition metal complexes containing the mesitylborylene ligand ; data_c_bono_soln_s92_1 _database_code_CSD 187963 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 B Br Fe O2' _chemical_formula_weight 386.86 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.628(2) _cell_length_b 15.439(3) _cell_length_c 17.803(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3196.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 3.443 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 1.36 _exptl_absorpt_correction_T_max 0.83 _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 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 21250 _diffrn_reflns_av_R_equivalents 0.1467 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3641 _reflns_number_gt 2300 _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^)+(0.0432P)^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 3641 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 0.15216(4) 0.11670(3) 0.71229(2) 0.02740(15) Uani 1 1 d . . . Fe1 Fe 0.32566(5) -0.05604(4) 0.66292(3) 0.01837(16) Uani 1 1 d . . . C2 C 0.3318(3) -0.0283(3) 0.7588(3) 0.0250(10) Uani 1 1 d . . . O2 O 0.3357(3) -0.0110(2) 0.82139(18) 0.0393(8) Uani 1 1 d . . . C6 C 0.3267(4) 0.2400(3) 0.4553(2) 0.0223(9) Uani 1 1 d . . . B1 B 0.2666(4) 0.0608(3) 0.6426(2) 0.0196(10) Uani 1 1 d . . . C12 C 0.3807(4) -0.0947(3) 0.5558(2) 0.0254(10) Uani 1 1 d . . . H12 H 0.3383 -0.0866 0.5121 0.030 Uiso 1 1 calc R . . C14 C 0.5041(4) -0.0722(3) 0.6536(2) 0.0269(10) Uani 1 1 d . . . H14 H 0.5572 -0.0465 0.6856 0.032 Uiso 1 1 calc R . . C3 C 0.2903(3) 0.1222(2) 0.5746(2) 0.0171(8) Uani 1 1 d . . . C8 C 0.3806(3) 0.1832(2) 0.5779(2) 0.0176(9) Uani 1 1 d . . . C4 C 0.2200(3) 0.1204(2) 0.5106(2) 0.0193(9) Uani 1 1 d . . . C13 C 0.4607(3) -0.0359(3) 0.5866(2) 0.0237(9) Uani 1 1 d . . . H13 H 0.4812 0.0174 0.5664 0.028 Uiso 1 1 calc R . . C7 C 0.3967(3) 0.2409(3) 0.5177(2) 0.0222(9) Uani 1 1 d . . . H7 H 0.4564 0.2808 0.5202 0.027 Uiso 1 1 calc R . . C10 C 0.3431(4) 0.3046(3) 0.3921(2) 0.0321(11) Uani 1 1 d . . . H10A H 0.3186 0.2791 0.3456 0.048 Uiso 1 1 calc R . . H10B H 0.4228 0.3201 0.3886 0.048 Uiso 1 1 calc R . . H10C H 0.2981 0.3555 0.4020 0.048 Uiso 1 1 calc R . . C16 C 0.3763(3) -0.1687(3) 0.6036(2) 0.0246(10) Uani 1 1 d . . . H16 H 0.3308 -0.2175 0.5963 0.030 Uiso 1 1 calc R . . C5 C 0.2389(3) 0.1790(3) 0.4523(2) 0.0233(10) Uani 1 1 d . . . H5 H 0.1915 0.1773 0.4103 0.028 Uiso 1 1 calc R . . C11 C 0.4575(4) 0.1875(3) 0.6458(2) 0.0291(10) Uani 1 1 d . . . H11A H 0.4125 0.2024 0.6891 0.044 Uiso 1 1 calc R . . H11B H 0.5156 0.2308 0.6380 0.044 Uiso 1 1 calc R . . H11C H 0.4933 0.1323 0.6535 0.044 Uiso 1 1 calc R . . C15 C 0.4523(4) -0.1552(3) 0.6635(2) 0.0263(10) Uani 1 1 d . . . H15 H 0.4664 -0.1935 0.7027 0.032 Uiso 1 1 calc R . . O1 O 0.0840(3) -0.1030(2) 0.66322(17) 0.0345(8) Uani 1 1 d . . . C1 C 0.1794(4) -0.0845(3) 0.6636(2) 0.0245(10) Uani 1 1 d . . . C9 C 0.1216(4) 0.0573(3) 0.5049(2) 0.0260(10) Uani 1 1 d . . . H9A H 0.1507 -0.0008 0.5077 0.039 Uiso 1 1 calc R . . H9B H 0.0825 0.0654 0.4580 0.039 Uiso 1 1 calc R . . H9C H 0.0688 0.0671 0.5455 0.039 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 Br1 0.0348(3) 0.0245(2) 0.0229(2) 0.00153(18) 0.00861(18) 0.00851(19) Fe1 0.0215(3) 0.0171(3) 0.0166(3) 0.0001(2) 0.0022(2) 0.0004(2) C2 0.029(2) 0.021(2) 0.024(3) 0.0040(19) -0.0025(19) 0.0041(18) O2 0.056(2) 0.043(2) 0.0185(18) -0.0019(15) -0.0025(15) 0.0114(17) C6 0.028(2) 0.020(2) 0.018(2) 0.0056(17) 0.0078(17) 0.0053(19) B1 0.014(2) 0.027(3) 0.018(2) -0.004(2) -0.0001(17) -0.002(2) C12 0.024(2) 0.036(3) 0.016(2) -0.0054(19) 0.0059(17) 0.0083(19) C14 0.027(2) 0.023(2) 0.030(3) -0.001(2) 0.0027(18) -0.0010(19) C3 0.020(2) 0.018(2) 0.014(2) -0.0018(17) 0.0011(16) 0.0033(16) C8 0.016(2) 0.016(2) 0.021(2) -0.0048(17) -0.0011(16) 0.0035(16) C4 0.018(2) 0.019(2) 0.021(2) 0.0005(18) -0.0006(16) 0.0043(17) C13 0.024(2) 0.022(2) 0.026(2) -0.0005(18) 0.0060(18) -0.0004(18) C7 0.020(2) 0.018(2) 0.029(3) 0.0017(18) 0.0033(18) -0.0002(17) C10 0.037(3) 0.031(3) 0.028(3) 0.008(2) 0.007(2) 0.005(2) C16 0.024(2) 0.019(2) 0.032(3) -0.0035(18) 0.0096(19) -0.0028(18) C5 0.025(2) 0.027(2) 0.017(2) -0.0005(18) -0.0020(17) 0.0044(19) C11 0.032(2) 0.025(2) 0.030(3) 0.0031(19) -0.008(2) 0.000(2) C15 0.027(2) 0.023(2) 0.029(3) 0.0032(19) 0.0068(19) 0.0107(19) O1 0.0244(19) 0.0325(19) 0.047(2) -0.0080(15) 0.0092(14) -0.0060(14) C1 0.032(3) 0.019(2) 0.023(2) -0.0032(18) 0.0067(18) -0.0001(19) C9 0.027(2) 0.028(2) 0.024(2) -0.0034(19) -0.0008(19) 0.0017(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 B1 2.013(4) . ? Fe1 C1 1.757(5) . ? Fe1 C2 1.761(5) . ? Fe1 B1 1.964(5) . ? Fe1 C14 2.096(4) . ? Fe1 C12 2.098(4) . ? Fe1 C13 2.099(4) . ? Fe1 C16 2.118(4) . ? Fe1 C15 2.123(4) . ? C2 O2 1.147(5) . ? C6 C7 1.378(6) . ? C6 C5 1.390(6) . ? C6 C10 1.515(6) . ? B1 C3 1.563(6) . ? C12 C13 1.411(6) . ? C12 C16 1.425(6) . ? C14 C13 1.410(6) . ? C14 C15 1.427(6) . ? C3 C4 1.402(5) . ? C3 C8 1.411(5) . ? C8 C7 1.405(5) . ? C8 C11 1.505(5) . ? C4 C5 1.395(5) . ? C4 C9 1.505(6) . ? C16 C15 1.400(6) . ? O1 C1 1.145(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 C1 Fe1 C2 95.38(19) . . ? C1 Fe1 B1 83.80(19) . . ? C2 Fe1 B1 88.25(19) . . ? C1 Fe1 C14 158.30(18) . . ? C2 Fe1 C14 93.77(17) . . ? B1 Fe1 C14 116.15(17) . . ? C1 Fe1 C12 103.29(18) . . ? C2 Fe1 C12 159.66(18) . . ? B1 Fe1 C12 101.59(17) . . ? C14 Fe1 C12 65.93(17) . . ? C1 Fe1 C13 139.94(17) . . ? C2 Fe1 C13 124.11(17) . . ? B1 Fe1 C13 90.38(17) . . ? C14 Fe1 C13 39.27(16) . . ? C12 Fe1 C13 39.29(16) . . ? C1 Fe1 C16 93.85(18) . . ? C2 Fe1 C16 132.18(18) . . ? B1 Fe1 C16 139.43(18) . . ? C14 Fe1 C16 65.65(16) . . ? C12 Fe1 C16 39.50(16) . . ? C13 Fe1 C16 65.87(16) . . ? C1 Fe1 C15 119.41(18) . . ? C2 Fe1 C15 98.19(18) . . ? B1 Fe1 C15 154.88(18) . . ? C14 Fe1 C15 39.53(16) . . ? C12 Fe1 C15 65.65(16) . . ? C13 Fe1 C15 65.87(16) . . ? C16 Fe1 C15 38.54(16) . . ? O2 C2 Fe1 179.4(4) . . ? C7 C6 C5 118.1(4) . . ? C7 C6 C10 121.2(4) . . ? C5 C6 C10 120.7(4) . . ? C3 B1 Fe1 129.7(3) . . ? C3 B1 Br1 109.5(3) . . ? Fe1 B1 Br1 120.8(2) . . ? C13 C12 C16 107.9(4) . . ? C13 C12 Fe1 70.4(2) . . ? C16 C12 Fe1 71.0(2) . . ? C13 C14 C15 108.1(4) . . ? C13 C14 Fe1 70.5(2) . . ? C15 C14 Fe1 71.3(2) . . ? C4 C3 C8 118.8(3) . . ? C4 C3 B1 120.9(3) . . ? C8 C3 B1 120.3(3) . . ? C7 C8 C3 119.4(4) . . ? C7 C8 C11 120.2(4) . . ? C3 C8 C11 120.3(4) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 C9 119.3(4) . . ? C3 C4 C9 120.7(4) . . ? C14 C13 C12 108.0(4) . . ? C14 C13 Fe1 70.2(2) . . ? C12 C13 Fe1 70.3(2) . . ? C6 C7 C8 122.0(4) . . ? C15 C16 C12 108.2(4) . . ? C15 C16 Fe1 71.0(2) . . ? C12 C16 Fe1 69.5(2) . . ? C6 C5 C4 121.9(4) . . ? C16 C15 C14 107.8(4) . . ? C16 C15 Fe1 70.5(2) . . ? C14 C15 Fe1 69.2(2) . . ? O1 C1 Fe1 179.3(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.770 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.123 data_cj172 _database_code_CSD 187964 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 B Fe2 O3' _chemical_formula_weight 455.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 8.0990(16) _cell_length_b 10.959(2) _cell_length_c 11.035(2) _cell_angle_alpha 80.39(3) _cell_angle_beta 84.48(3) _cell_angle_gamma 84.96(3) _cell_volume 958.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type Sortav (Blessing 1995) _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.88 _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 rotating anode _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Nonius 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 10805 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4221 _reflns_number_gt 3121 _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^)+(0.0914P)^2^+2.2854P] 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 4221 _refine_ls_number_parameters 256 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.084 _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 0.31641(7) 0.10286(6) 0.79361(6) 0.0170(2) Uani 1 1 d . . . Fe2 Fe 0.07023(8) 0.26175(6) 0.78039(6) 0.0195(2) Uani 1 1 d . . . O1 O 0.1200(5) 0.1243(4) 1.0248(3) 0.0326(8) Uani 1 1 d . . . O2 O 0.5361(4) 0.2744(3) 0.8531(3) 0.0287(8) Uani 1 1 d . . . O3 O -0.1559(4) 0.0868(3) 0.7354(3) 0.0290(8) Uani 1 1 d . . . C1 C 0.1517(6) 0.1493(4) 0.9180(4) 0.0193(9) Uani 1 1 d . . . C2 C 0.4490(6) 0.2068(4) 0.8285(4) 0.0214(10) Uani 1 1 d . . . C3 C -0.0649(6) 0.1546(4) 0.7534(4) 0.0222(10) Uani 1 1 d . . . C4 C 0.2884(5) 0.2578(4) 0.5116(4) 0.0170(9) Uani 1 1 d . . . C5 C 0.1813(6) 0.2439(4) 0.4208(4) 0.0206(9) Uani 1 1 d . . . C6 C 0.2288(6) 0.2780(4) 0.2968(4) 0.0241(10) Uani 1 1 d . . . H6 H 0.1576 0.2665 0.2391 0.029 Uiso 1 1 calc R . . C7 C 0.3787(6) 0.3286(4) 0.2558(4) 0.0238(10) Uani 1 1 d . . . C8 C 0.4832(6) 0.3424(4) 0.3441(4) 0.0244(10) Uani 1 1 d . . . H8 H 0.5848 0.3757 0.3181 0.029 Uiso 1 1 calc R . . C9 C 0.4431(5) 0.3088(4) 0.4687(4) 0.0190(9) Uani 1 1 d . . . C10 C 0.0142(6) 0.1928(5) 0.4568(5) 0.0318(12) Uani 1 1 d . . . H10A H -0.0422 0.1934 0.3841 0.048 Uiso 1 1 calc R . . H10B H -0.0507 0.2431 0.5099 0.048 Uiso 1 1 calc R . . H10C H 0.0289 0.1092 0.4995 0.048 Uiso 1 1 calc R . . C11 C 0.4260(8) 0.3677(5) 0.1209(5) 0.0347(13) Uani 1 1 d . . . H11A H 0.3870 0.4528 0.0967 0.052 Uiso 1 1 calc R . . H11B H 0.3764 0.3163 0.0741 0.052 Uiso 1 1 calc R . . H11C H 0.5448 0.3590 0.1055 0.052 Uiso 1 1 calc R . . C12 C 0.5661(6) 0.3294(5) 0.5568(5) 0.0255(10) Uani 1 1 d . . . H12A H 0.6597 0.3681 0.5109 0.038 Uiso 1 1 calc R . . H12B H 0.6033 0.2510 0.6025 0.038 Uiso 1 1 calc R . . H12C H 0.5135 0.3820 0.6128 0.038 Uiso 1 1 calc R . . C13 C 0.4888(6) -0.0505(4) 0.8305(5) 0.0304(12) Uani 1 1 d . . . H13 H 0.5830 -0.0499 0.8723 0.036 Uiso 1 1 calc R . . C14 C 0.4772(6) -0.0189(4) 0.7019(5) 0.0267(11) Uani 1 1 d . . . H14 H 0.5635 0.0064 0.6438 0.032 Uiso 1 1 calc R . . C15 C 0.3127(6) -0.0321(4) 0.6762(5) 0.0241(10) Uani 1 1 d . . . H15 H 0.2720 -0.0177 0.5987 0.029 Uiso 1 1 calc R . . C16 C 0.2210(6) -0.0713(4) 0.7896(5) 0.0239(10) Uani 1 1 d . . . H16 H 0.1089 -0.0864 0.7997 0.029 Uiso 1 1 calc R . . C17 C 0.3278(6) -0.0837(4) 0.8841(5) 0.0267(11) Uani 1 1 d . . . H17 H 0.2989 -0.1092 0.9675 0.032 Uiso 1 1 calc R . . C18 C 0.1582(9) 0.4306(6) 0.8085(8) 0.0563(18) Uani 1 1 d U . . H18 H 0.2686 0.4420 0.8174 0.068 Uiso 1 1 calc R . . C19 C 0.0912(11) 0.4456(5) 0.6970(7) 0.065(2) Uani 1 1 d U . . H19 H 0.1415 0.4682 0.6180 0.078 Uiso 1 1 calc R . . C20 C -0.0934(10) 0.4145(6) 0.7388(8) 0.0583(19) Uani 1 1 d U . . H20 H -0.1819 0.4132 0.6912 0.070 Uiso 1 1 calc R . . C21 C -0.0887(9) 0.3904(6) 0.8619(7) 0.055(2) Uani 1 1 d . . . H21 H -0.1808 0.3689 0.9159 0.066 Uiso 1 1 calc R . . C22 C 0.0528(12) 0.3996(6) 0.8974(8) 0.062(2) Uani 1 1 d . . . H22 H 0.0764 0.3851 0.9797 0.074 Uiso 1 1 calc R . . B1 B 0.2393(6) 0.2180(4) 0.6516(5) 0.0167(10) 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 0.0164(3) 0.0184(3) 0.0156(4) -0.0014(2) -0.0009(3) -0.0007(2) Fe2 0.0164(3) 0.0182(4) 0.0230(4) -0.0029(3) 0.0008(3) -0.0004(2) O1 0.032(2) 0.045(2) 0.0190(19) -0.0037(15) 0.0053(15) -0.0005(16) O2 0.0273(18) 0.036(2) 0.0272(19) -0.0120(15) -0.0036(15) -0.0105(15) O3 0.0231(18) 0.0285(19) 0.035(2) 0.0014(15) -0.0072(15) -0.0078(15) C1 0.019(2) 0.019(2) 0.020(2) -0.0040(17) 0.0021(18) -0.0061(17) C2 0.024(2) 0.026(2) 0.014(2) -0.0033(18) -0.0012(18) 0.0009(19) C3 0.019(2) 0.023(2) 0.022(2) 0.0009(18) 0.0007(19) 0.0013(19) C4 0.020(2) 0.0109(19) 0.019(2) -0.0008(16) -0.0018(18) -0.0004(16) C5 0.024(2) 0.019(2) 0.019(2) -0.0024(17) -0.0043(19) 0.0002(18) C6 0.036(3) 0.021(2) 0.016(2) -0.0039(18) -0.009(2) 0.004(2) C7 0.039(3) 0.014(2) 0.015(2) 0.0031(17) 0.004(2) 0.0050(19) C8 0.027(2) 0.019(2) 0.023(2) 0.0021(18) 0.007(2) -0.0004(19) C9 0.019(2) 0.015(2) 0.022(2) -0.0005(17) 0.0015(18) -0.0003(17) C10 0.029(3) 0.047(3) 0.022(3) -0.001(2) -0.009(2) -0.014(2) C11 0.051(3) 0.031(3) 0.016(3) 0.001(2) 0.007(2) 0.009(2) C12 0.021(2) 0.031(3) 0.024(3) 0.001(2) -0.003(2) -0.010(2) C13 0.028(3) 0.020(2) 0.045(3) -0.006(2) -0.015(2) 0.004(2) C14 0.024(2) 0.018(2) 0.037(3) -0.007(2) 0.006(2) -0.0016(19) C15 0.028(3) 0.019(2) 0.025(3) -0.0056(18) -0.002(2) -0.0001(19) C16 0.021(2) 0.022(2) 0.027(3) -0.0022(19) 0.003(2) -0.0039(18) C17 0.034(3) 0.022(2) 0.021(2) 0.0047(19) -0.006(2) 0.002(2) C18 0.044(3) 0.040(3) 0.087(4) -0.013(3) -0.017(3) -0.002(3) C19 0.111(4) 0.022(3) 0.048(3) 0.001(2) 0.042(3) 0.009(3) C20 0.069(4) 0.034(3) 0.083(4) -0.026(3) -0.054(3) 0.016(3) C21 0.050(4) 0.032(3) 0.075(5) -0.013(3) 0.025(4) 0.009(3) C22 0.098(7) 0.034(4) 0.060(5) -0.022(3) -0.022(5) 0.007(4) B1 0.017(2) 0.016(2) 0.018(3) -0.0033(19) -0.0004(19) -0.0044(18) _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 C2 1.743(5) . ? Fe1 C1 1.919(5) . ? Fe1 B1 1.956(5) . ? Fe1 C14 2.096(5) . ? Fe1 C13 2.100(5) . ? Fe1 C17 2.118(5) . ? Fe1 C15 2.127(5) . ? Fe1 C16 2.130(5) . ? Fe1 Fe2 2.5278(12) . ? Fe2 C3 1.752(5) . ? Fe2 C1 1.920(5) . ? Fe2 B1 1.966(5) . ? Fe2 C20 2.060(6) . ? Fe2 C21 2.082(6) . ? Fe2 C19 2.085(6) . ? Fe2 C18 2.120(7) . ? Fe2 C22 2.133(7) . ? O1 C1 1.173(6) . ? O2 C2 1.147(6) . ? O3 C3 1.144(6) . ? C4 C5 1.421(6) . ? C4 C9 1.423(6) . ? C4 B1 1.556(7) . ? C5 C6 1.383(7) . ? C5 C10 1.503(7) . ? C6 C7 1.384(7) . ? C7 C8 1.385(7) . ? C7 C11 1.501(6) . ? C8 C9 1.378(7) . ? C9 C12 1.512(6) . ? C13 C14 1.414(8) . ? C13 C17 1.430(8) . ? C14 C15 1.413(7) . ? C15 C16 1.414(7) . ? C16 C17 1.400(7) . ? C18 C22 1.259(11) . ? C18 C19 1.371(11) . ? C19 C20 1.571(12) . ? C20 C21 1.344(11) . ? C21 C22 1.264(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 C2 Fe1 C1 90.4(2) . . ? C2 Fe1 B1 93.1(2) . . ? C1 Fe1 B1 98.8(2) . . ? C2 Fe1 C14 103.3(2) . . ? C1 Fe1 C14 156.2(2) . . ? B1 Fe1 C14 99.7(2) . . ? C2 Fe1 C13 93.4(2) . . ? C1 Fe1 C13 121.7(2) . . ? B1 Fe1 C13 138.8(2) . . ? C14 Fe1 C13 39.4(2) . . ? C2 Fe1 C17 120.3(2) . . ? C1 Fe1 C17 90.7(2) . . ? B1 Fe1 C17 145.3(2) . . ? C14 Fe1 C17 65.6(2) . . ? C13 Fe1 C17 39.6(2) . . ? C2 Fe1 C15 139.9(2) . . ? C1 Fe1 C15 129.64(19) . . ? B1 Fe1 C15 83.7(2) . . ? C14 Fe1 C15 39.09(19) . . ? C13 Fe1 C15 65.8(2) . . ? C17 Fe1 C15 65.0(2) . . ? C2 Fe1 C16 158.0(2) . . ? C1 Fe1 C16 94.90(19) . . ? B1 Fe1 C16 107.1(2) . . ? C14 Fe1 C16 65.37(19) . . ? C13 Fe1 C16 65.73(19) . . ? C17 Fe1 C16 38.5(2) . . ? C15 Fe1 C16 38.79(18) . . ? C2 Fe1 Fe2 93.29(16) . . ? C1 Fe1 Fe2 48.82(14) . . ? B1 Fe1 Fe2 50.03(15) . . ? C14 Fe1 Fe2 146.64(15) . . ? C13 Fe1 Fe2 168.45(16) . . ? C17 Fe1 Fe2 128.99(15) . . ? C15 Fe1 Fe2 113.73(14) . . ? C16 Fe1 Fe2 106.26(14) . . ? C3 Fe2 C1 91.5(2) . . ? C3 Fe2 B1 93.2(2) . . ? C1 Fe2 B1 98.5(2) . . ? C3 Fe2 C20 94.9(2) . . ? C1 Fe2 C20 141.6(3) . . ? B1 Fe2 C20 118.8(3) . . ? C3 Fe2 C21 103.0(3) . . ? C1 Fe2 C21 103.9(3) . . ? B1 Fe2 C21 151.8(2) . . ? C20 Fe2 C21 37.9(3) . . ? C3 Fe2 C19 129.4(3) . . ? C1 Fe2 C19 138.6(3) . . ? B1 Fe2 C19 86.4(2) . . ? C20 Fe2 C19 44.5(3) . . ? C21 Fe2 C19 65.5(3) . . ? C3 Fe2 C18 160.5(2) . . ? C1 Fe2 C18 101.1(3) . . ? B1 Fe2 C18 99.4(3) . . ? C20 Fe2 C18 66.0(3) . . ? C21 Fe2 C18 59.7(3) . . ? C19 Fe2 C18 38.1(3) . . ? C3 Fe2 C22 134.0(3) . . ? C1 Fe2 C22 86.0(3) . . ? B1 Fe2 C22 132.6(3) . . ? C20 Fe2 C22 62.7(3) . . ? C21 Fe2 C22 34.9(3) . . ? C19 Fe2 C22 62.3(3) . . ? C18 Fe2 C22 34.4(3) . . ? C3 Fe2 Fe1 93.02(15) . . ? C1 Fe2 Fe1 48.81(14) . . ? B1 Fe2 Fe1 49.71(15) . . ? C20 Fe2 Fe1 166.5(3) . . ? C21 Fe2 Fe1 149.1(3) . . ? C19 Fe2 Fe1 122.5(2) . . ? C18 Fe2 Fe1 106.43(19) . . ? C22 Fe2 Fe1 118.0(2) . . ? O1 C1 Fe1 138.8(4) . . ? O1 C1 Fe2 138.8(4) . . ? Fe1 C1 Fe2 82.36(18) . . ? O2 C2 Fe1 179.0(4) . . ? O3 C3 Fe2 178.4(4) . . ? C5 C4 C9 117.1(4) . . ? C5 C4 B1 121.5(4) . . ? C9 C4 B1 121.5(4) . . ? C6 C5 C4 120.5(4) . . ? C6 C5 C10 118.5(4) . . ? C4 C5 C10 121.1(4) . . ? C5 C6 C7 122.2(4) . . ? C6 C7 C8 117.4(4) . . ? C6 C7 C11 121.3(5) . . ? C8 C7 C11 121.2(5) . . ? C9 C8 C7 122.8(5) . . ? C8 C9 C4 120.0(4) . . ? C8 C9 C12 118.2(4) . . ? C4 C9 C12 121.8(4) . . ? C14 C13 C17 106.8(4) . . ? C14 C13 Fe1 70.2(3) . . ? C17 C13 Fe1 70.9(3) . . ? C15 C14 C13 108.7(4) . . ? C15 C14 Fe1 71.6(3) . . ? C13 C14 Fe1 70.5(3) . . ? C14 C15 C16 107.7(4) . . ? C14 C15 Fe1 69.3(3) . . ? C16 C15 Fe1 70.7(3) . . ? C17 C16 C15 108.4(4) . . ? C17 C16 Fe1 70.3(3) . . ? C15 C16 Fe1 70.5(3) . . ? C16 C17 C13 108.4(4) . . ? C16 C17 Fe1 71.2(3) . . ? C13 C17 Fe1 69.5(3) . . ? C22 C18 C19 112.1(7) . . ? C22 C18 Fe2 73.3(5) . . ? C19 C18 Fe2 69.6(4) . . ? C18 C19 C20 101.2(6) . . ? C18 C19 Fe2 72.4(4) . . ? C20 C19 Fe2 66.9(3) . . ? C21 C20 C19 100.9(6) . . ? C21 C20 Fe2 72.0(4) . . ? C19 C20 Fe2 68.6(3) . . ? C22 C21 C20 113.6(7) . . ? C22 C21 Fe2 74.8(4) . . ? C20 C21 Fe2 70.2(4) . . ? C18 C22 C21 112.1(8) . . ? C18 C22 Fe2 72.2(5) . . ? C21 C22 Fe2 70.4(4) . . ? C4 B1 Fe1 140.1(3) . . ? C4 B1 Fe2 139.6(3) . . ? Fe1 B1 Fe2 80.26(19) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.549 (near Fe1) _refine_diff_density_min -0.680 _refine_diff_density_rms 0.135 data_c_bono_soln_s92_2 _database_code_CSD 187965 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H25 B Fe2 O4' _chemical_formula_weight 511.96 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.3720(19) _cell_length_b 21.143(4) _cell_length_c 11.672(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.39(3) _cell_angle_gamma 90.00 _cell_volume 2312.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type sortav (Blessing) _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.93 _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 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 10628 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.23 _reflns_number_total 2079 _reflns_number_gt 1769 _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^)+(0.0292P)^2^+2.0499P] 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 2079 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.05199(3) 0.108045(14) 0.59295(3) 0.03540(13) Uani 1 1 d . . . O1 O -0.2457(2) 0.07159(9) 0.58909(19) 0.0674(6) Uani 1 1 d . . . O2 O 0.1517(2) -0.00885(9) 0.69365(16) 0.0623(5) Uani 1 1 d . . . C1 C -0.1279(3) 0.08684(11) 0.5929(2) 0.0445(6) Uani 1 1 d . . . C2 C 0.1105(2) 0.03846(11) 0.6578(2) 0.0423(6) Uani 1 1 d . . . C3 C 0.1916(3) 0.18292(12) 0.5502(2) 0.0484(6) Uani 1 1 d . . . H3 H 0.2273 0.2124 0.6022 0.058 Uiso 1 1 calc R . . C4 C 0.0639(3) 0.18878(12) 0.4882(2) 0.0535(7) Uani 1 1 d . . . H4 H 0.0000 0.2223 0.4925 0.064 Uiso 1 1 calc R . . C5 C 0.0494(3) 0.13486(14) 0.4182(2) 0.0567(7) Uani 1 1 d . . . H5 H -0.0255 0.1267 0.3677 0.068 Uiso 1 1 calc R . . C6 C 0.1672(3) 0.09572(13) 0.4379(2) 0.0550(7) Uani 1 1 d . . . H6 H 0.1841 0.0570 0.4027 0.066 Uiso 1 1 calc R . . C7 C 0.2572(3) 0.12542(13) 0.5213(2) 0.0497(6) Uani 1 1 d . . . C8 C 0.3995(3) 0.10201(18) 0.5631(3) 0.0848(11) Uani 1 1 d . . . H8A H 0.4740 0.1214 0.5192 0.127 Uiso 1 1 calc R . . H8B H 0.4042 0.0569 0.5542 0.127 Uiso 1 1 calc R . . H8C H 0.4115 0.1127 0.6425 0.127 Uiso 1 1 calc R . . C9 C 0.0000 0.22431(14) 0.7500 0.0366(7) Uani 1 2 d S . . C10 C 0.1199(2) 0.25929(10) 0.7878(2) 0.0414(5) Uani 1 1 d . . . C11 C 0.1177(3) 0.32496(11) 0.7872(2) 0.0513(6) Uani 1 1 d . . . H11 H 0.1980 0.3468 0.8126 0.062 Uiso 1 1 calc R . . C12 C 0.0000 0.35909(16) 0.7500 0.0535(9) Uani 1 2 d S . . C13 C 0.2537(3) 0.22646(12) 0.8303(2) 0.0528(6) Uani 1 1 d . . . H13A H 0.3348 0.2533 0.8176 0.079 Uiso 1 1 calc R . . H13B H 0.2660 0.1874 0.7894 0.079 Uiso 1 1 calc R . . H13C H 0.2453 0.2178 0.9107 0.079 Uiso 1 1 calc R . . C14 C 0.0000 0.43069(17) 0.7500 0.0773(14) Uani 1 2 d S . . H14A H 0.0632 0.4458 0.6917 0.116 Uiso 0.50 1 calc PR . . H14B H 0.0316 0.4458 0.8235 0.116 Uiso 0.50 1 calc PR . . H14C H -0.0948 0.4458 0.7348 0.116 Uiso 0.50 1 calc PR . . B1 B 0.0000 0.14959(16) 0.7500 0.0343(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0387(2) 0.0394(2) 0.0280(2) 0.00171(12) 0.00027(13) -0.00303(13) O1 0.0438(12) 0.0709(13) 0.0874(16) -0.0009(11) -0.0117(10) -0.0114(9) O2 0.0752(13) 0.0538(11) 0.0581(12) 0.0113(9) 0.0056(10) 0.0168(9) C1 0.0515(17) 0.0431(13) 0.0390(14) 0.0015(10) -0.0053(11) -0.0015(11) C2 0.0424(14) 0.0505(15) 0.0342(13) -0.0007(10) 0.0071(10) 0.0012(11) C3 0.0574(16) 0.0508(14) 0.0372(14) 0.0036(11) 0.0081(12) -0.0166(12) C4 0.0634(18) 0.0544(15) 0.0427(15) 0.0175(12) 0.0053(13) 0.0000(12) C5 0.0630(18) 0.0767(18) 0.0303(14) 0.0086(12) -0.0042(12) -0.0105(14) C6 0.0717(19) 0.0566(15) 0.0369(14) -0.0045(11) 0.0187(13) -0.0084(13) C7 0.0418(14) 0.0675(16) 0.0399(14) 0.0082(12) 0.0114(11) -0.0043(11) C8 0.052(2) 0.122(3) 0.081(2) 0.019(2) 0.0130(18) 0.0058(18) C9 0.0394(18) 0.0396(17) 0.0307(17) 0.000 0.0012(13) 0.000 C10 0.0419(14) 0.0433(13) 0.0390(14) -0.0053(10) 0.0019(10) -0.0028(10) C11 0.0524(16) 0.0462(14) 0.0555(16) -0.0108(11) 0.0128(12) -0.0113(11) C12 0.060(2) 0.0384(19) 0.063(2) 0.000 0.0256(19) 0.000 C13 0.0456(15) 0.0577(15) 0.0551(17) -0.0059(12) -0.0100(12) -0.0074(12) C14 0.085(3) 0.042(2) 0.105(4) 0.000 0.039(3) 0.000 B1 0.0274(18) 0.043(2) 0.0323(19) 0.000 -0.0037(14) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.742(2) . ? Fe1 C1 1.745(3) . ? Fe1 B1 2.0931(15) . ? Fe1 C4 2.103(2) . ? Fe1 C3 2.116(2) . ? Fe1 C5 2.117(2) . ? Fe1 C6 2.130(3) . ? Fe1 C7 2.134(3) . ? O1 C1 1.151(3) . ? O2 C2 1.150(3) . ? C3 C4 1.400(4) . ? C3 C7 1.405(4) . ? C4 C5 1.409(4) . ? C5 C6 1.397(4) . ? C6 C7 1.429(4) . ? C7 C8 1.501(4) . ? C9 C10 1.414(3) 2_556 ? C9 C10 1.414(3) . ? C9 B1 1.580(5) . ? C10 C11 1.389(3) . ? C10 C13 1.514(3) . ? C11 C12 1.385(3) . ? C12 C11 1.385(3) 2_556 ? C12 C14 1.514(5) . ? B1 Fe1 2.0931(15) 2_556 ? 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 94.83(11) . . ? C2 Fe1 B1 92.76(11) . . ? C1 Fe1 B1 82.95(9) . . ? C2 Fe1 C4 157.04(11) . . ? C1 Fe1 C4 105.28(11) . . ? B1 Fe1 C4 100.49(11) . . ? C2 Fe1 C3 122.78(11) . . ? C1 Fe1 C3 142.33(11) . . ? B1 Fe1 C3 92.32(10) . . ? C4 Fe1 C3 38.76(10) . . ? C2 Fe1 C5 130.30(11) . . ? C1 Fe1 C5 93.66(11) . . ? B1 Fe1 C5 136.90(12) . . ? C4 Fe1 C5 39.00(10) . . ? C3 Fe1 C5 64.88(10) . . ? C2 Fe1 C6 96.11(11) . . ? C1 Fe1 C6 117.63(12) . . ? B1 Fe1 C6 156.63(10) . . ? C4 Fe1 C6 64.92(11) . . ? C3 Fe1 C6 64.74(10) . . ? C5 Fe1 C6 38.42(11) . . ? C2 Fe1 C7 91.96(11) . . ? C1 Fe1 C7 156.56(11) . . ? B1 Fe1 C7 119.14(9) . . ? C4 Fe1 C7 65.22(11) . . ? C3 Fe1 C7 38.59(10) . . ? C5 Fe1 C7 65.20(11) . . ? C6 Fe1 C7 39.16(11) . . ? O1 C1 Fe1 177.4(2) . . ? O2 C2 Fe1 175.5(2) . . ? C4 C3 C7 109.0(2) . . ? C4 C3 Fe1 70.12(14) . . ? C7 C3 Fe1 71.42(14) . . ? C3 C4 C5 107.9(2) . . ? C3 C4 Fe1 71.11(13) . . ? C5 C4 Fe1 71.03(14) . . ? C6 C5 C4 108.1(2) . . ? C6 C5 Fe1 71.30(15) . . ? C4 C5 Fe1 69.97(14) . . ? C5 C6 C7 108.3(2) . . ? C5 C6 Fe1 70.29(15) . . ? C7 C6 Fe1 70.59(14) . . ? C3 C7 C6 106.7(2) . . ? C3 C7 C8 126.6(3) . . ? C6 C7 C8 126.6(3) . . ? C3 C7 Fe1 69.99(14) . . ? C6 C7 Fe1 70.26(15) . . ? C8 C7 Fe1 128.1(2) . . ? C10 C9 C10 116.9(3) 2_556 . ? C10 C9 B1 121.55(14) 2_556 . ? C10 C9 B1 121.55(14) . . ? C11 C10 C9 120.6(2) . . ? C11 C10 C13 118.2(2) . . ? C9 C10 C13 121.2(2) . . ? C12 C11 C10 122.3(3) . . ? C11 C12 C11 117.2(3) . 2_556 ? C11 C12 C14 121.39(16) . . ? C11 C12 C14 121.39(16) 2_556 . ? C9 B1 Fe1 114.81(9) . . ? C9 B1 Fe1 114.81(9) . 2_556 ? Fe1 B1 Fe1 130.38(17) . 2_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.256 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.087 data_cj180 _database_code_CSD 187966 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H29 B Fe O3' _chemical_formula_weight 456.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 17.798(4) _cell_length_b 10.551(2) _cell_length_c 12.427(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.57(3) _cell_angle_gamma 90.00 _cell_volume 2332.7(8) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type Sortav (blessing) _exptl_absorpt_correction_T_min 0.72 _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 Nonius 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 42154 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4273 _reflns_number_gt 3554 _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^)+(0.0404P)^2^+1.4164P] 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 4273 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.420765(16) 0.60412(3) 0.23824(2) 0.02396(11) Uani 1 1 d . . . O1 O 0.34248(10) 0.81657(17) 0.33107(15) 0.0466(4) Uani 1 1 d . . . O3 O 0.27885(9) 0.67359(14) 0.12579(13) 0.0362(4) Uani 1 1 d . . . O2 O 0.44804(11) 0.72962(19) 0.03641(14) 0.0554(5) Uani 1 1 d . . . C1 C 0.20735(12) 0.6735(2) 0.07862(18) 0.0304(5) Uani 1 1 d . . . C2 C 0.19243(14) 0.6206(3) -0.0203(2) 0.0488(7) Uani 1 1 d . . . H2 H 0.2297 0.5761 -0.0553 0.059 Uiso 1 1 calc R . . C3 C 0.12118(14) 0.6338(3) -0.06816(19) 0.0486(7) Uani 1 1 d . . . H3 H 0.1117 0.5970 -0.1352 0.058 Uiso 1 1 calc R . . C4 C 0.06396(12) 0.6997(2) -0.01956(17) 0.0284(5) Uani 1 1 d . . . C5 C 0.08082(14) 0.7486(2) 0.08121(19) 0.0386(6) Uani 1 1 d . . . H5 H 0.0437 0.7920 0.1173 0.046 Uiso 1 1 calc R . . C6 C 0.15123(14) 0.7353(2) 0.1305(2) 0.0408(6) Uani 1 1 d . . . H6 H 0.1603 0.7685 0.1990 0.049 Uiso 1 1 calc R . . C7 C -0.01303(12) 0.7199(2) -0.07562(18) 0.0333(5) Uani 1 1 d . . . C8 C -0.03264(14) 0.6121(2) -0.1530(2) 0.0420(6) Uani 1 1 d . . . H8A H -0.0818 0.6260 -0.1844 0.063 Uiso 1 1 calc R . . H8B H -0.0320 0.5332 -0.1144 0.063 Uiso 1 1 calc R . . H8C H 0.0036 0.6091 -0.2088 0.063 Uiso 1 1 calc R . . C9 C -0.07563(14) 0.7277(4) 0.0076(2) 0.0635(9) Uani 1 1 d . . . H9A H -0.0676 0.8007 0.0525 0.095 Uiso 1 1 calc R . . H9B H -0.0746 0.6526 0.0513 0.095 Uiso 1 1 calc R . . H9C H -0.1236 0.7344 -0.0292 0.095 Uiso 1 1 calc R . . C10 C -0.01052(15) 0.8449(2) -0.1383(2) 0.0467(6) Uani 1 1 d . . . H10A H 0.0007 0.9132 -0.0895 0.070 Uiso 1 1 calc R . . H10B H -0.0584 0.8597 -0.1735 0.070 Uiso 1 1 calc R . . H10C H 0.0277 0.8400 -0.1912 0.070 Uiso 1 1 calc R . . C11 C 0.28721(11) 0.4313(2) 0.15832(16) 0.0263(5) Uani 1 1 d . . . C12 C 0.31004(12) 0.3457(2) 0.07871(17) 0.0298(5) Uani 1 1 d . . . C13 C 0.29107(13) 0.2178(2) 0.08649(19) 0.0352(5) Uani 1 1 d . . . H13 H 0.3066 0.1622 0.0335 0.042 Uiso 1 1 calc R . . C14 C 0.24993(13) 0.1714(2) 0.1704(2) 0.0367(6) Uani 1 1 d . . . C15 C 0.22604(12) 0.2563(2) 0.24744(19) 0.0354(5) Uani 1 1 d . . . H15 H 0.1976 0.2265 0.3038 0.042 Uiso 1 1 calc R . . C16 C 0.24350(12) 0.3851(2) 0.24286(18) 0.0303(5) Uani 1 1 d . . . C17 C 0.35532(14) 0.3900(2) -0.01566(18) 0.0385(6) Uani 1 1 d . . . H17A H 0.3245 0.3871 -0.0802 0.058 Uiso 1 1 calc R . . H17B H 0.3981 0.3357 -0.0234 0.058 Uiso 1 1 calc R . . H17C H 0.3720 0.4754 -0.0031 0.058 Uiso 1 1 calc R . . C18 C 0.23055(17) 0.0320(2) 0.1762(3) 0.0553(7) Uani 1 1 d . . . H18A H 0.1912 0.0131 0.1243 0.083 Uiso 1 1 calc R . . H18B H 0.2139 0.0121 0.2471 0.083 Uiso 1 1 calc R . . H18C H 0.2742 -0.0175 0.1609 0.083 Uiso 1 1 calc R . . C19 C 0.21652(13) 0.4738(2) 0.32821(19) 0.0388(6) Uani 1 1 d . . . H19A H 0.1938 0.4259 0.3843 0.058 Uiso 1 1 calc R . . H19B H 0.1802 0.5313 0.2970 0.058 Uiso 1 1 calc R . . H19C H 0.2584 0.5209 0.3578 0.058 Uiso 1 1 calc R . . C20 C 0.42838(16) 0.4204(2) 0.3043(3) 0.0538(8) Uani 1 1 d . . . H20 H 0.3899 0.3608 0.3036 0.065 Uiso 1 1 calc R . . C21 C 0.44268(14) 0.5098(3) 0.3844(2) 0.0431(6) Uani 1 1 d . . . H21 H 0.4144 0.5221 0.4453 0.052 Uiso 1 1 calc R . . C22 C 0.50752(13) 0.5790(2) 0.35746(18) 0.0334(5) Uani 1 1 d . . . H22 H 0.5300 0.6433 0.3981 0.040 Uiso 1 1 calc R . . C23 C 0.53163(13) 0.5338(2) 0.25966(19) 0.0392(6) Uani 1 1 d . . . H23 H 0.5732 0.5627 0.2230 0.047 Uiso 1 1 calc R . . C24 C 0.48177(17) 0.4354(3) 0.2249(2) 0.0528(8) Uani 1 1 d . . . H24 H 0.4843 0.3897 0.1612 0.063 Uiso 1 1 calc R . . C25 C 0.37349(12) 0.7321(2) 0.29433(18) 0.0314(5) Uani 1 1 d . . . C26 C 0.43655(12) 0.6801(2) 0.11734(19) 0.0341(5) Uani 1 1 d . . . B1 B 0.31873(14) 0.5708(2) 0.16485(19) 0.0273(5) 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 0.02065(18) 0.02500(18) 0.02588(18) 0.00394(12) -0.00594(12) -0.00073(12) O1 0.0390(10) 0.0415(10) 0.0590(11) -0.0102(9) -0.0071(8) 0.0103(8) O3 0.0274(8) 0.0293(8) 0.0510(10) 0.0091(7) -0.0168(7) -0.0053(7) O2 0.0507(12) 0.0753(14) 0.0398(10) 0.0250(10) -0.0069(8) -0.0198(10) C1 0.0247(11) 0.0273(11) 0.0384(12) 0.0091(9) -0.0112(9) -0.0042(9) C2 0.0238(13) 0.088(2) 0.0341(13) -0.0033(13) 0.0002(10) 0.0117(13) C3 0.0278(13) 0.092(2) 0.0260(12) -0.0109(12) -0.0053(10) 0.0104(13) C4 0.0226(11) 0.0339(11) 0.0286(11) 0.0059(9) -0.0018(9) -0.0003(9) C5 0.0331(13) 0.0379(13) 0.0445(14) -0.0097(11) -0.0071(10) 0.0122(11) C6 0.0430(15) 0.0353(13) 0.0432(14) -0.0124(10) -0.0172(11) 0.0086(11) C7 0.0221(11) 0.0436(13) 0.0340(12) 0.0027(10) -0.0040(9) 0.0039(10) C8 0.0294(13) 0.0450(15) 0.0507(15) 0.0022(11) -0.0145(11) -0.0017(11) C9 0.0230(14) 0.115(3) 0.0530(17) 0.0001(17) 0.0011(12) 0.0083(15) C10 0.0390(15) 0.0419(14) 0.0580(17) 0.0064(12) -0.0191(12) 0.0088(12) C11 0.0193(11) 0.0313(11) 0.0278(11) 0.0065(9) -0.0061(8) -0.0030(9) C12 0.0238(11) 0.0336(12) 0.0315(12) 0.0012(9) -0.0079(9) -0.0040(9) C13 0.0306(12) 0.0331(12) 0.0414(13) -0.0025(10) -0.0085(10) 0.0002(10) C14 0.0268(12) 0.0303(12) 0.0522(15) 0.0101(11) -0.0124(11) -0.0048(10) C15 0.0232(11) 0.0411(13) 0.0415(13) 0.0194(11) -0.0056(10) -0.0061(10) C16 0.0199(11) 0.0374(12) 0.0331(12) 0.0072(9) -0.0052(9) -0.0011(9) C17 0.0369(14) 0.0461(14) 0.0325(12) -0.0046(10) 0.0002(10) -0.0081(11) C18 0.0524(17) 0.0340(14) 0.079(2) 0.0129(13) -0.0131(15) -0.0083(12) C19 0.0315(13) 0.0470(14) 0.0381(13) 0.0074(11) 0.0045(10) -0.0012(11) C20 0.0404(16) 0.0305(13) 0.088(2) 0.0254(14) -0.0349(15) -0.0052(11) C21 0.0325(13) 0.0575(16) 0.0392(13) 0.0243(12) -0.0037(10) 0.0098(12) C22 0.0288(12) 0.0349(12) 0.0357(12) 0.0033(10) -0.0152(10) 0.0030(10) C23 0.0259(12) 0.0506(15) 0.0413(14) 0.0091(11) 0.0012(10) 0.0119(11) C24 0.0648(19) 0.0411(14) 0.0507(16) -0.0147(12) -0.0285(14) 0.0291(14) C25 0.0269(12) 0.0322(12) 0.0347(12) 0.0025(10) -0.0081(9) -0.0025(10) C26 0.0238(12) 0.0401(13) 0.0379(13) 0.0054(10) -0.0085(9) -0.0065(10) B1 0.0215(12) 0.0329(13) 0.0273(12) 0.0031(10) -0.0024(10) -0.0021(10) _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 C26 1.733(2) . ? Fe1 C25 1.746(2) . ? Fe1 B1 2.040(2) . ? Fe1 C24 2.094(2) . ? Fe1 C21 2.098(2) . ? Fe1 C20 2.108(2) . ? Fe1 C23 2.118(2) . ? Fe1 C22 2.127(2) . ? O1 C25 1.149(3) . ? O3 B1 1.377(3) . ? O3 C1 1.386(3) . ? O2 C26 1.157(3) . ? C1 C6 1.369(3) . ? C1 C2 1.370(3) . ? C2 C3 1.393(3) . ? C3 C4 1.385(3) . ? C4 C5 1.380(3) . ? C4 C7 1.535(3) . ? C5 C6 1.387(3) . ? C7 C8 1.524(3) . ? C7 C10 1.532(3) . ? C7 C9 1.543(3) . ? C11 C12 1.408(3) . ? C11 C16 1.411(3) . ? C11 B1 1.577(3) . ? C12 C13 1.394(3) . ? C12 C17 1.515(3) . ? C13 C14 1.380(3) . ? C14 C15 1.386(4) . ? C14 C18 1.513(3) . ? C15 C16 1.396(3) . ? C16 C19 1.503(3) . ? C20 C21 1.390(4) . ? C20 C24 1.397(4) . ? C21 C22 1.413(3) . ? C22 C23 1.384(3) . ? C23 C24 1.425(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 Fe1 C25 94.58(11) . . ? C26 Fe1 B1 81.69(10) . . ? C25 Fe1 B1 83.05(10) . . ? C26 Fe1 C24 103.17(12) . . ? C25 Fe1 C24 160.99(11) . . ? B1 Fe1 C24 105.98(11) . . ? C26 Fe1 C21 159.94(10) . . ? C25 Fe1 C21 95.82(11) . . ? B1 Fe1 C21 116.57(10) . . ? C24 Fe1 C21 65.22(11) . . ? C26 Fe1 C20 138.83(13) . . ? C25 Fe1 C20 125.60(12) . . ? B1 Fe1 C20 93.58(10) . . ? C24 Fe1 C20 38.85(12) . . ? C21 Fe1 C20 38.59(11) . . ? C26 Fe1 C23 95.65(10) . . ? C25 Fe1 C23 132.70(10) . . ? B1 Fe1 C23 144.15(10) . . ? C24 Fe1 C23 39.54(11) . . ? C21 Fe1 C23 64.83(10) . . ? C20 Fe1 C23 65.12(10) . . ? C26 Fe1 C22 122.00(10) . . ? C25 Fe1 C22 99.62(9) . . ? B1 Fe1 C22 155.52(9) . . ? C24 Fe1 C22 65.22(10) . . ? C21 Fe1 C22 39.08(9) . . ? C20 Fe1 C22 64.93(9) . . ? C23 Fe1 C22 38.07(9) . . ? B1 O3 C1 127.36(17) . . ? C6 C1 C2 119.4(2) . . ? C6 C1 O3 118.3(2) . . ? C2 C1 O3 122.2(2) . . ? C1 C2 C3 119.6(2) . . ? C4 C3 C2 122.4(2) . . ? C5 C4 C3 116.1(2) . . ? C5 C4 C7 121.9(2) . . ? C3 C4 C7 122.0(2) . . ? C4 C5 C6 122.3(2) . . ? C1 C6 C5 120.2(2) . . ? C8 C7 C10 109.3(2) . . ? C8 C7 C4 111.61(19) . . ? C10 C7 C4 108.20(19) . . ? C8 C7 C9 107.8(2) . . ? C10 C7 C9 109.1(2) . . ? C4 C7 C9 110.80(19) . . ? C12 C11 C16 118.52(19) . . ? C12 C11 B1 121.74(19) . . ? C16 C11 B1 119.12(19) . . ? C13 C12 C11 119.8(2) . . ? C13 C12 C17 119.2(2) . . ? C11 C12 C17 121.0(2) . . ? C14 C13 C12 122.0(2) . . ? C13 C14 C15 118.1(2) . . ? C13 C14 C18 120.5(2) . . ? C15 C14 C18 121.3(2) . . ? C14 C15 C16 121.9(2) . . ? C15 C16 C11 119.6(2) . . ? C15 C16 C19 120.1(2) . . ? C11 C16 C19 120.2(2) . . ? C21 C20 C24 108.3(2) . . ? C21 C20 Fe1 70.33(14) . . ? C24 C20 Fe1 70.03(14) . . ? C20 C21 C22 108.4(2) . . ? C20 C21 Fe1 71.09(14) . . ? C22 C21 Fe1 71.57(13) . . ? C23 C22 C21 107.8(2) . . ? C23 C22 Fe1 70.62(13) . . ? C21 C22 Fe1 69.36(13) . . ? C22 C23 C24 108.1(2) . . ? C22 C23 Fe1 71.32(13) . . ? C24 C23 Fe1 69.31(14) . . ? C20 C24 C23 107.4(2) . . ? C20 C24 Fe1 71.13(15) . . ? C23 C24 Fe1 71.15(14) . . ? O1 C25 Fe1 179.8(2) . . ? O2 C26 Fe1 178.9(2) . . ? O3 B1 C11 122.55(19) . . ? O3 B1 Fe1 117.74(16) . . ? C11 B1 Fe1 119.67(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.263 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.055 data_cj_181 _database_code_CSD 187967 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 B Br Fe O2' _chemical_formula_weight 456.99 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6640(19) _cell_length_b 17.437(4) _cell_length_c 13.127(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.41(3) _cell_angle_gamma 90.00 _cell_volume 2073.2(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 colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 2.666 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.59 _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 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 34838 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4735 _reflns_number_gt 4107 _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^)+(0.0259P)^2^+1.8866P] 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 4735 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.87675(2) 0.189942(14) 0.42478(2) 0.03309(8) Uani 1 1 d . . . Fe1 Fe 0.50760(3) 0.154604(16) 0.28560(2) 0.01459(8) Uani 1 1 d . . . O1 O 0.5826(2) 0.15860(10) 0.51903(13) 0.0369(4) Uani 1 1 d . . . O2 O 0.5953(2) 0.31089(10) 0.26230(16) 0.0432(5) Uani 1 1 d . . . C1 C 0.7939(2) 0.06734(11) 0.26507(16) 0.0168(4) Uani 1 1 d . . . C2 C 0.8307(2) 0.08265(13) 0.17213(18) 0.0232(4) Uani 1 1 d . . . C3 C 0.9015(3) 0.02650(15) 0.13272(19) 0.0308(5) Uani 1 1 d . . . H3 H 0.9222 0.0365 0.0699 0.037 Uiso 1 1 calc R . . C4 C 0.9423(3) -0.04381(14) 0.1839(2) 0.0305(5) Uani 1 1 d . . . C5 C 0.9095(2) -0.05763(13) 0.27761(19) 0.0260(5) Uani 1 1 d . . . H5 H 0.9377 -0.1040 0.3140 0.031 Uiso 1 1 calc R . . C6 C 0.8356(2) -0.00366(12) 0.31796(17) 0.0199(4) Uani 1 1 d . . . C7 C 0.8017(3) 0.16058(15) 0.1186(2) 0.0341(6) Uani 1 1 d . . . H7A H 0.8853 0.1933 0.1518 0.051 Uiso 1 1 calc R . . H7B H 0.7156 0.1827 0.1274 0.051 Uiso 1 1 calc R . . H7C H 0.7859 0.1553 0.0426 0.051 Uiso 1 1 calc R . . C8 C 1.0204(3) -0.10345(18) 0.1401(3) 0.0502(8) Uani 1 1 d . . . H8A H 0.9571 -0.1193 0.0691 0.075 Uiso 1 1 calc R . . H8B H 1.0442 -0.1470 0.1878 0.075 Uiso 1 1 calc R . . H8C H 1.1095 -0.0820 0.1355 0.075 Uiso 1 1 calc R . . C9 C 0.8018(2) -0.02200(13) 0.41955(18) 0.0281(5) Uani 1 1 d . . . H9A H 0.6970 -0.0269 0.4014 0.042 Uiso 1 1 calc R . . H9B H 0.8381 0.0186 0.4715 0.042 Uiso 1 1 calc R . . H9C H 0.8490 -0.0693 0.4501 0.042 Uiso 1 1 calc R . . C10 C 0.4124(2) 0.05989(12) 0.17939(16) 0.0195(4) Uani 1 1 d . . . C11 C 0.3566(2) 0.06259(12) 0.26646(17) 0.0211(4) Uani 1 1 d . . . C12 C 0.2816(2) 0.13451(14) 0.26079(18) 0.0253(5) Uani 1 1 d . . . C13 C 0.2935(2) 0.17620(13) 0.17205(18) 0.0266(5) Uani 1 1 d . . . C14 C 0.3768(2) 0.13050(13) 0.12218(16) 0.0217(4) Uani 1 1 d . . . C15 C 0.4759(2) -0.00917(13) 0.14429(19) 0.0268(5) Uani 1 1 d . . . H15A H 0.3981 -0.0376 0.0919 0.040 Uiso 1 1 calc R . . H15B H 0.5237 -0.0410 0.2062 0.040 Uiso 1 1 calc R . . H15C H 0.5465 0.0068 0.1121 0.040 Uiso 1 1 calc R . . C16 C 0.3592(3) -0.00128(14) 0.34363(19) 0.0322(5) Uani 1 1 d . . . H16A H 0.2645 -0.0260 0.3208 0.048 Uiso 1 1 calc R . . H16B H 0.3811 0.0192 0.4154 0.048 Uiso 1 1 calc R . . H16C H 0.4336 -0.0379 0.3440 0.048 Uiso 1 1 calc R . . C17 C 0.1982(3) 0.15702(18) 0.3340(2) 0.0410(6) Uani 1 1 d . . . H17A H 0.1809 0.2113 0.3290 0.061 Uiso 1 1 calc R . . H17B H 0.2551 0.1436 0.4077 0.061 Uiso 1 1 calc R . . H17C H 0.1054 0.1305 0.3119 0.061 Uiso 1 1 calc R . . C18 C 0.2270(3) 0.25322(17) 0.1333(2) 0.0470(7) Uani 1 1 d . . . H18A H 0.1284 0.2467 0.0826 0.071 Uiso 1 1 calc R . . H18B H 0.2856 0.2794 0.0984 0.071 Uiso 1 1 calc R . . H18C H 0.2243 0.2829 0.1942 0.071 Uiso 1 1 calc R . . C19 C 0.4014(3) 0.14945(15) 0.01821(18) 0.0326(5) Uani 1 1 d . . . H19A H 0.4910 0.1257 0.0182 0.049 Uiso 1 1 calc R . . H19B H 0.4089 0.2040 0.0122 0.049 Uiso 1 1 calc R . . H19C H 0.3199 0.1307 -0.0423 0.049 Uiso 1 1 calc R . . C20 C 0.5574(2) 0.15723(12) 0.42714(17) 0.0214(4) Uani 1 1 d . . . C21 C 0.5632(2) 0.24857(13) 0.27202(18) 0.0257(5) Uani 1 1 d . . . B1 B 0.7165(2) 0.12931(13) 0.31348(18) 0.0173(4) 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 0.01729(12) 0.03517(14) 0.04150(15) -0.01956(11) 0.00354(9) -0.00458(9) Fe1 0.01359(14) 0.01490(14) 0.01451(14) -0.00061(10) 0.00393(10) 0.00165(10) O1 0.0507(11) 0.0423(10) 0.0179(8) -0.0025(7) 0.0121(8) -0.0048(8) O2 0.0568(12) 0.0191(9) 0.0520(12) 0.0054(8) 0.0167(10) -0.0030(8) C1 0.0119(9) 0.0192(10) 0.0185(10) -0.0013(8) 0.0042(7) -0.0014(7) C2 0.0194(10) 0.0268(11) 0.0242(11) 0.0014(9) 0.0086(8) -0.0023(9) C3 0.0316(12) 0.0406(14) 0.0275(12) -0.0034(10) 0.0194(10) 0.0002(11) C4 0.0264(12) 0.0315(13) 0.0373(13) -0.0111(10) 0.0157(10) 0.0004(10) C5 0.0224(11) 0.0195(11) 0.0362(13) -0.0012(9) 0.0102(9) 0.0022(8) C6 0.0160(9) 0.0192(10) 0.0245(11) -0.0006(8) 0.0071(8) -0.0013(8) C7 0.0353(13) 0.0351(14) 0.0374(14) 0.0123(11) 0.0195(11) 0.0029(11) C8 0.0511(18) 0.0480(17) 0.0610(19) -0.0163(15) 0.0313(15) 0.0105(14) C9 0.0293(12) 0.0286(12) 0.0292(12) 0.0097(9) 0.0135(10) 0.0060(10) C10 0.0157(9) 0.0216(10) 0.0187(10) -0.0042(8) 0.0031(8) -0.0037(8) C11 0.0153(10) 0.0271(11) 0.0199(10) -0.0039(8) 0.0048(8) -0.0067(8) C12 0.0118(9) 0.0373(13) 0.0244(11) -0.0065(9) 0.0035(8) -0.0001(9) C13 0.0175(10) 0.0298(12) 0.0246(11) -0.0025(9) -0.0025(8) 0.0064(9) C14 0.0196(10) 0.0251(11) 0.0167(10) -0.0017(8) 0.0016(8) 0.0001(8) C15 0.0259(11) 0.0230(11) 0.0294(12) -0.0100(9) 0.0071(9) -0.0046(9) C16 0.0320(13) 0.0355(13) 0.0290(12) 0.0015(10) 0.0103(10) -0.0138(10) C17 0.0207(12) 0.0632(18) 0.0426(15) -0.0144(13) 0.0156(11) 0.0005(12) C18 0.0390(15) 0.0417(16) 0.0457(16) 0.0032(13) -0.0038(12) 0.0225(12) C19 0.0401(14) 0.0367(14) 0.0182(11) 0.0000(9) 0.0066(10) -0.0048(11) C20 0.0219(10) 0.0186(10) 0.0242(11) -0.0005(8) 0.0086(8) -0.0014(8) C21 0.0278(11) 0.0231(11) 0.0251(11) 0.0008(9) 0.0078(9) 0.0029(9) B1 0.0178(11) 0.0166(11) 0.0163(11) -0.0004(8) 0.0045(8) -0.0016(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 Br1 B1 2.018(2) . ? Fe1 C20 1.750(2) . ? Fe1 C21 1.753(2) . ? Fe1 B1 1.972(2) . ? Fe1 C14 2.118(2) . ? Fe1 C13 2.120(2) . ? Fe1 C12 2.122(2) . ? Fe1 C11 2.124(2) . ? Fe1 C10 2.150(2) . ? O1 C20 1.144(3) . ? O2 C21 1.149(3) . ? C1 C6 1.408(3) . ? C1 C2 1.411(3) . ? C1 B1 1.569(3) . ? C2 C3 1.393(3) . ? C2 C7 1.510(3) . ? C3 C4 1.388(4) . ? C4 C5 1.394(3) . ? C4 C8 1.512(3) . ? C5 C6 1.393(3) . ? C6 C9 1.513(3) . ? C10 C14 1.421(3) . ? C10 C11 1.424(3) . ? C10 C15 1.495(3) . ? C11 C12 1.438(3) . ? C11 C16 1.500(3) . ? C12 C13 1.412(3) . ? C12 C17 1.505(3) . ? C13 C14 1.442(3) . ? C13 C18 1.499(3) . ? C14 C19 1.501(3) . ? 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 C20 Fe1 C21 95.92(10) . . ? C20 Fe1 B1 85.66(10) . . ? C21 Fe1 B1 84.12(10) . . ? C20 Fe1 C14 157.92(9) . . ? C21 Fe1 C14 100.28(9) . . ? B1 Fe1 C14 110.75(9) . . ? C20 Fe1 C13 125.55(10) . . ? C21 Fe1 C13 91.21(10) . . ? B1 Fe1 C13 148.78(9) . . ? C14 Fe1 C13 39.79(9) . . ? C20 Fe1 C12 93.11(10) . . ? C21 Fe1 C12 118.33(10) . . ? B1 Fe1 C12 157.49(9) . . ? C14 Fe1 C12 65.99(9) . . ? C13 Fe1 C12 38.87(9) . . ? C20 Fe1 C11 93.92(9) . . ? C21 Fe1 C11 156.43(9) . . ? B1 Fe1 C11 118.01(9) . . ? C14 Fe1 C11 65.64(8) . . ? C13 Fe1 C11 65.75(9) . . ? C12 Fe1 C11 39.58(9) . . ? C20 Fe1 C10 127.26(9) . . ? C21 Fe1 C10 136.82(9) . . ? B1 Fe1 C10 97.32(9) . . ? C14 Fe1 C10 38.87(8) . . ? C13 Fe1 C10 65.70(8) . . ? C12 Fe1 C10 65.72(8) . . ? C11 Fe1 C10 38.92(8) . . ? C6 C1 C2 118.54(18) . . ? C6 C1 B1 120.05(18) . . ? C2 C1 B1 121.31(18) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 C7 119.7(2) . . ? C1 C2 C7 120.71(19) . . ? C4 C3 C2 122.3(2) . . ? C3 C4 C5 117.8(2) . . ? C3 C4 C8 121.2(2) . . ? C5 C4 C8 120.9(2) . . ? C6 C5 C4 121.6(2) . . ? C5 C6 C1 120.21(19) . . ? C5 C6 C9 119.28(19) . . ? C1 C6 C9 120.51(18) . . ? C14 C10 C11 107.82(18) . . ? C14 C10 C15 125.78(19) . . ? C11 C10 C15 125.8(2) . . ? C14 C10 Fe1 69.33(12) . . ? C11 C10 Fe1 69.53(12) . . ? C15 C10 Fe1 133.61(14) . . ? C10 C11 C12 108.22(19) . . ? C10 C11 C16 126.6(2) . . ? C12 C11 C16 124.9(2) . . ? C10 C11 Fe1 71.55(12) . . ? C12 C11 Fe1 70.15(12) . . ? C16 C11 Fe1 129.22(15) . . ? C13 C12 C11 107.87(19) . . ? C13 C12 C17 127.5(2) . . ? C11 C12 C17 124.5(2) . . ? C13 C12 Fe1 70.46(12) . . ? C11 C12 Fe1 70.26(11) . . ? C17 C12 Fe1 127.61(16) . . ? C12 C13 C14 108.02(19) . . ? C12 C13 C18 126.3(2) . . ? C14 C13 C18 125.6(2) . . ? C12 C13 Fe1 70.66(12) . . ? C14 C13 Fe1 70.04(12) . . ? C18 C13 Fe1 126.56(17) . . ? C10 C14 C13 108.03(19) . . ? C10 C14 C19 125.8(2) . . ? C13 C14 C19 125.5(2) . . ? C10 C14 Fe1 71.80(11) . . ? C13 C14 Fe1 70.17(12) . . ? C19 C14 Fe1 130.50(16) . . ? O1 C20 Fe1 176.59(19) . . ? O2 C21 Fe1 177.9(2) . . ? C1 B1 Fe1 132.87(15) . . ? C1 B1 Br1 107.49(14) . . ? Fe1 B1 Br1 119.64(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.480 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.072 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