# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Fc2B2(OH)2 _database_code_depnum_ccdc_archive 'CCDC 892505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 B2 Fe2 O2' _chemical_formula_sum 'C20 H18 B2 Fe2 O2' _chemical_formula_weight 423.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.88640(10) _cell_length_b 9.77070(10) _cell_length_c 10.07860(10) _cell_angle_alpha 106.2430(10) _cell_angle_beta 91.6240(10) _cell_angle_gamma 96.6060(10) _cell_volume 832.898(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4061 _cell_measurement_theta_min 7.02 _cell_measurement_theta_max 67.14 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 14.048 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.0363 _exptl_absorpt_correction_T_max 0.3645 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7289 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 7.02 _diffrn_reflns_theta_max 68.08 _reflns_number_total 2782 _reflns_number_gt 2499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0745P)^2^+0.9969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2782 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Fe2 Fe 0.67833(7) 0.28742(6) 0.46186(5) 0.0277(2) Uani 1 1 d . . . Fe1 Fe 0.15049(6) 0.24966(6) 0.98352(5) 0.02368(19) Uani 1 1 d . . . O2 O 0.7721(3) 0.7019(3) 0.5164(3) 0.0330(6) Uani 1 1 d . . . H2 H 0.7697 0.7786 0.5797 0.049 Uiso 1 1 calc R . . O1 O -0.1531(3) -0.0380(3) 0.7303(3) 0.0304(6) Uani 1 1 d . . . H1 H -0.1627 0.0418 0.7170 0.046 Uiso 1 1 calc R . . B2 B 0.6420(5) 0.6113(5) 0.5119(4) 0.0295(9) Uani 1 1 d . . . B1 B -0.0833(5) -0.0162(5) 0.8597(4) 0.0251(8) Uani 1 1 d . . . C11 C 0.6212(4) 0.4607(4) 0.4031(4) 0.0289(8) Uani 1 1 d . . . C12 C 0.4888(4) 0.3547(4) 0.3919(4) 0.0284(8) Uani 1 1 d . . . C13 C 0.5216(5) 0.2224(4) 0.2964(4) 0.0313(8) Uani 1 1 d . . . H13 H 0.4525 0.1294 0.2685 0.038 Uiso 1 1 calc R . . C14 C 0.6694(5) 0.2468(4) 0.2494(4) 0.0329(9) Uani 1 1 d . . . H14 H 0.7223 0.1739 0.1834 0.039 Uiso 1 1 calc R . . C15 C 0.7299(5) 0.3924(4) 0.3154(4) 0.0313(8) Uani 1 1 d . . . H15 H 0.8330 0.4387 0.3034 0.038 Uiso 1 1 calc R . . C16 C 0.8671(5) 0.3206(5) 0.5939(4) 0.0364(9) Uani 1 1 d . . . H16 H 0.9611 0.3882 0.5960 0.044 Uiso 1 1 calc R . . C17 C 0.7373(5) 0.3541(5) 0.6696(4) 0.0343(9) Uani 1 1 d . . . H17 H 0.7239 0.4495 0.7346 0.041 Uiso 1 1 calc R . . C18 C 0.6302(5) 0.2279(5) 0.6377(4) 0.0351(9) Uani 1 1 d . . . H18 H 0.5279 0.2193 0.6757 0.042 Uiso 1 1 calc R . . C19 C 0.6922(5) 0.1173(5) 0.5406(4) 0.0385(10) Uani 1 1 d . . . H19 H 0.6423 0.0165 0.4988 0.046 Uiso 1 1 calc R . . C20 C 0.8394(5) 0.1753(5) 0.5145(4) 0.0364(9) Uani 1 1 d . . . H20 H 0.9107 0.1221 0.4504 0.044 Uiso 1 1 calc R . . C1 C -0.0560(4) 0.1297(4) 0.9714(4) 0.0256(7) Uani 1 1 d . . . C2 C 0.0266(4) 0.1461(4) 1.1036(3) 0.0246(7) Uani 1 1 d . . . C3 C 0.0555(4) 0.2955(4) 1.1721(4) 0.0274(8) Uani 1 1 d . . . H3 H 0.1123 0.3397 1.2641 0.033 Uiso 1 1 calc R . . C4 C -0.0064(4) 0.3724(4) 1.0872(4) 0.0286(8) Uani 1 1 d . . . H4 H -0.0013 0.4792 1.1094 0.034 Uiso 1 1 calc R . . C5 C -0.0763(4) 0.2702(4) 0.9646(4) 0.0288(8) Uani 1 1 d . . . H5 H -0.1282 0.2935 0.8858 0.035 Uiso 1 1 calc R . . C6 C 0.3552(5) 0.1683(5) 0.9531(4) 0.0341(9) Uani 1 1 d . . . H6 H 0.3895 0.0927 0.9921 0.041 Uiso 1 1 calc R . . C7 C 0.3795(4) 0.3177(4) 1.0173(4) 0.0325(9) Uani 1 1 d . . . H7 H 0.4345 0.3662 1.1094 0.039 Uiso 1 1 calc R . . C8 C 0.3119(5) 0.3881(5) 0.9289(4) 0.0354(9) Uani 1 1 d . . . H8 H 0.3121 0.4942 0.9470 0.042 Uiso 1 1 calc R . . C9 C 0.2440(5) 0.2788(5) 0.8092(4) 0.0349(9) Uani 1 1 d . . . H9 H 0.1881 0.2950 0.7285 0.042 Uiso 1 1 calc R . . C10 C 0.2705(5) 0.1432(5) 0.8248(4) 0.0346(9) Uani 1 1 d . . . H10 H 0.2362 0.0473 0.7573 0.042 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 Fe2 0.0332(3) 0.0265(4) 0.0230(3) 0.0076(2) -0.0059(2) 0.0025(2) Fe1 0.0315(3) 0.0195(3) 0.0200(3) 0.0085(2) -0.0054(2) -0.0026(2) O2 0.0416(16) 0.0293(16) 0.0251(13) 0.0061(11) -0.0044(11) -0.0020(11) O1 0.0444(16) 0.0201(14) 0.0250(13) 0.0076(10) -0.0125(11) -0.0019(11) B2 0.041(2) 0.026(2) 0.0226(19) 0.0114(17) -0.0093(17) 0.0026(18) B1 0.029(2) 0.024(2) 0.0216(18) 0.0102(16) -0.0030(15) -0.0050(16) C11 0.038(2) 0.030(2) 0.0213(16) 0.0110(15) -0.0039(14) 0.0048(16) C12 0.039(2) 0.026(2) 0.0197(16) 0.0074(14) -0.0097(15) 0.0032(16) C13 0.043(2) 0.028(2) 0.0205(17) 0.0049(15) -0.0111(15) 0.0024(16) C14 0.045(2) 0.030(2) 0.0220(17) 0.0053(15) -0.0041(15) 0.0052(17) C15 0.038(2) 0.031(2) 0.0255(18) 0.0116(16) -0.0008(15) 0.0006(16) C16 0.038(2) 0.042(3) 0.0294(19) 0.0143(18) -0.0122(16) 0.0003(18) C17 0.046(2) 0.033(2) 0.0225(17) 0.0083(15) -0.0109(16) 0.0025(17) C18 0.029(2) 0.051(3) 0.0308(19) 0.0232(19) -0.0024(15) 0.0007(17) C19 0.046(2) 0.031(2) 0.042(2) 0.0188(19) -0.0117(18) 0.0006(17) C20 0.041(2) 0.037(3) 0.034(2) 0.0126(18) -0.0065(17) 0.0102(18) C1 0.0258(18) 0.026(2) 0.0255(17) 0.0109(15) -0.0030(14) -0.0016(14) C2 0.0314(19) 0.023(2) 0.0183(16) 0.0078(14) -0.0044(13) -0.0036(14) C3 0.039(2) 0.023(2) 0.0197(16) 0.0059(14) -0.0026(14) 0.0020(15) C4 0.037(2) 0.023(2) 0.0251(17) 0.0062(15) -0.0033(15) 0.0049(15) C5 0.033(2) 0.029(2) 0.0267(18) 0.0110(15) -0.0048(14) 0.0038(15) C6 0.035(2) 0.036(2) 0.035(2) 0.0165(18) 0.0027(16) 0.0065(17) C7 0.0277(19) 0.035(2) 0.035(2) 0.0147(17) -0.0062(15) -0.0065(16) C8 0.041(2) 0.030(2) 0.038(2) 0.0181(18) -0.0035(17) -0.0068(16) C9 0.037(2) 0.041(3) 0.0290(19) 0.0179(17) -0.0003(16) -0.0027(17) C10 0.042(2) 0.032(2) 0.0264(18) 0.0056(16) 0.0048(16) -0.0015(17) _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 Fe2 C17 2.045(4) . ? Fe2 C19 2.047(4) . ? Fe2 C20 2.043(4) . ? Fe2 C16 2.049(4) . ? Fe2 C11 2.053(4) . ? Fe2 C13 2.048(4) . ? Fe2 C18 2.056(4) . ? Fe2 C15 2.054(4) . ? Fe2 C12 2.053(4) . ? Fe2 C14 2.063(4) . ? Fe1 C9 2.042(4) . ? Fe1 C1 2.041(4) . ? Fe1 C2 2.050(4) . ? Fe1 C10 2.049(4) . ? Fe1 C8 2.051(4) . ? Fe1 C5 2.057(4) . ? Fe1 C3 2.056(4) . ? Fe1 C7 2.055(4) . ? Fe1 C4 2.059(4) . ? Fe1 C6 2.065(4) . ? O2 B2 1.364(5) . ? O2 H2 0.8400 . ? O1 B1 1.379(5) . ? O1 H1 0.8400 . ? B2 C12 1.541(6) 2_666 ? B2 C11 1.558(6) . ? B1 C1 1.538(6) . ? B1 C2 1.550(5) 2_557 ? C11 C15 1.424(6) . ? C11 C12 1.455(6) . ? C12 C13 1.446(5) . ? C12 B2 1.541(6) 2_666 ? C13 C14 1.426(6) . ? C13 H13 1.0000 . ? C14 C15 1.425(6) . ? C14 H14 1.0000 . ? C15 H15 1.0000 . ? C16 C20 1.410(6) . ? C16 C17 1.420(6) . ? C16 H16 1.0000 . ? C17 C18 1.421(6) . ? C17 H17 1.0000 . ? C18 C19 1.416(6) . ? C18 H18 1.0000 . ? C19 C20 1.426(6) . ? C19 H19 1.0000 . ? C20 H20 1.0000 . ? C1 C5 1.426(5) . ? C1 C2 1.462(5) . ? C2 C3 1.418(5) . ? C2 B1 1.550(5) 2_557 ? C3 C4 1.424(5) . ? C3 H3 1.0000 . ? C4 C5 1.425(5) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 C7 1.410(6) . ? C6 C10 1.422(6) . ? C6 H6 1.0000 . ? C7 C8 1.427(5) . ? C7 H7 1.0000 . ? C8 C9 1.432(6) . ? C8 H8 1.0000 . ? C9 C10 1.422(6) . ? C9 H9 1.0000 . ? C10 H10 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Fe2 C19 68.35(17) . . ? C17 Fe2 C20 68.11(16) . . ? C19 Fe2 C20 40.83(18) . . ? C17 Fe2 C16 40.61(17) . . ? C19 Fe2 C16 68.39(17) . . ? C20 Fe2 C16 40.33(17) . . ? C17 Fe2 C11 108.21(16) . . ? C19 Fe2 C11 167.70(17) . . ? C20 Fe2 C11 150.18(17) . . ? C16 Fe2 C11 117.28(17) . . ? C17 Fe2 C13 152.32(18) . . ? C19 Fe2 C13 107.95(17) . . ? C20 Fe2 C13 128.08(17) . . ? C16 Fe2 C13 165.75(17) . . ? C11 Fe2 C13 69.25(16) . . ? C17 Fe2 C18 40.56(17) . . ? C19 Fe2 C18 40.40(18) . . ? C20 Fe2 C18 68.03(17) . . ? C16 Fe2 C18 68.13(17) . . ? C11 Fe2 C18 129.51(17) . . ? C13 Fe2 C18 118.68(17) . . ? C17 Fe2 C15 128.54(17) . . ? C19 Fe2 C15 150.72(18) . . ? C20 Fe2 C15 117.13(17) . . ? C16 Fe2 C15 107.62(17) . . ? C11 Fe2 C15 40.56(16) . . ? C13 Fe2 C15 68.41(16) . . ? C18 Fe2 C15 167.23(17) . . ? C17 Fe2 C12 118.30(16) . . ? C19 Fe2 C12 128.67(17) . . ? C20 Fe2 C12 166.99(17) . . ? C16 Fe2 C12 151.57(17) . . ? C11 Fe2 C12 41.50(15) . . ? C13 Fe2 C12 41.28(15) . . ? C18 Fe2 C12 108.75(16) . . ? C15 Fe2 C12 68.87(16) . . ? C17 Fe2 C14 166.12(18) . . ? C19 Fe2 C14 117.60(17) . . ? C20 Fe2 C14 107.50(16) . . ? C16 Fe2 C14 127.70(17) . . ? C11 Fe2 C14 68.62(15) . . ? C13 Fe2 C14 40.60(17) . . ? C18 Fe2 C14 151.55(18) . . ? C15 Fe2 C14 40.50(17) . . ? C12 Fe2 C14 68.94(15) . . ? C9 Fe1 C1 120.68(16) . . ? C9 Fe1 C2 157.74(16) . . ? C1 Fe1 C2 41.87(13) . . ? C9 Fe1 C10 40.69(17) . . ? C1 Fe1 C10 107.48(16) . . ? C2 Fe1 C10 122.42(16) . . ? C9 Fe1 C8 40.95(17) . . ? C1 Fe1 C8 156.14(15) . . ? C2 Fe1 C8 160.18(16) . . ? C10 Fe1 C8 68.57(18) . . ? C9 Fe1 C5 106.86(16) . . ? C1 Fe1 C5 40.71(15) . . ? C2 Fe1 C5 68.92(14) . . ? C10 Fe1 C5 124.22(16) . . ? C8 Fe1 C5 120.69(16) . . ? C9 Fe1 C3 160.11(17) . . ? C1 Fe1 C3 68.98(15) . . ? C2 Fe1 C3 40.42(15) . . ? C10 Fe1 C3 157.92(16) . . ? C8 Fe1 C3 123.62(17) . . ? C5 Fe1 C3 68.17(15) . . ? C9 Fe1 C7 68.38(16) . . ? C1 Fe1 C7 161.62(15) . . ? C2 Fe1 C7 124.20(15) . . ? C10 Fe1 C7 68.03(17) . . ? C8 Fe1 C7 40.68(16) . . ? C5 Fe1 C7 156.58(16) . . ? C3 Fe1 C7 108.08(16) . . ? C9 Fe1 C4 123.33(16) . . ? C1 Fe1 C4 68.77(15) . . ? C2 Fe1 C4 68.52(15) . . ? C10 Fe1 C4 160.35(16) . . ? C8 Fe1 C4 106.62(17) . . ? C5 Fe1 C4 40.52(15) . . ? C3 Fe1 C4 40.50(14) . . ? C7 Fe1 C4 121.55(16) . . ? C9 Fe1 C6 68.10(16) . . ? C1 Fe1 C6 125.17(16) . . ? C2 Fe1 C6 108.57(15) . . ? C10 Fe1 C6 40.45(16) . . ? C8 Fe1 C6 68.02(17) . . ? C5 Fe1 C6 161.46(17) . . ? C3 Fe1 C6 122.63(15) . . ? C7 Fe1 C6 40.02(17) . . ? C4 Fe1 C6 157.20(16) . . ? B2 O2 H2 109.5 . . ? B1 O1 H1 109.5 . . ? O2 B2 C12 125.0(4) . 2_666 ? O2 B2 C11 118.9(4) . . ? C12 B2 C11 116.1(4) 2_666 . ? O1 B1 C1 124.4(3) . . ? O1 B1 C2 118.5(3) . 2_557 ? C1 B1 C2 117.1(3) . 2_557 ? C15 C11 C12 107.6(3) . . ? C15 C11 B2 128.5(4) . . ? C12 C11 B2 123.2(3) . . ? C15 C11 Fe2 69.8(2) . . ? C12 C11 Fe2 69.2(2) . . ? B2 C11 Fe2 118.8(2) . . ? C11 C12 C13 106.9(3) . . ? C11 C12 B2 120.6(3) . 2_666 ? C13 C12 B2 131.8(4) . 2_666 ? C11 C12 Fe2 69.3(2) . . ? C13 C12 Fe2 69.2(2) . . ? B2 C12 Fe2 119.4(2) 2_666 . ? C14 C13 C12 108.4(4) . . ? C14 C13 Fe2 70.2(2) . . ? C12 C13 Fe2 69.5(2) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Fe2 C13 H13 125.8 . . ? C13 C14 C15 108.0(4) . . ? C13 C14 Fe2 69.2(2) . . ? C15 C14 Fe2 69.4(2) . . ? C13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Fe2 C14 H14 126.0 . . ? C11 C15 C14 109.1(4) . . ? C11 C15 Fe2 69.7(2) . . ? C14 C15 Fe2 70.1(2) . . ? C11 C15 H15 125.5 . . ? C14 C15 H15 125.5 . . ? Fe2 C15 H15 125.5 . . ? C20 C16 C17 107.9(4) . . ? C20 C16 Fe2 69.6(2) . . ? C17 C16 Fe2 69.5(2) . . ? C20 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Fe2 C16 H16 126.1 . . ? C16 C17 C18 108.0(4) . . ? C16 C17 Fe2 69.8(2) . . ? C18 C17 Fe2 70.1(2) . . ? C16 C17 H17 126.0 . . ? C18 C17 H17 126.0 . . ? Fe2 C17 H17 126.0 . . ? C19 C18 C17 108.2(4) . . ? C19 C18 Fe2 69.5(2) . . ? C17 C18 Fe2 69.3(2) . . ? C19 C18 H18 125.9 . . ? C17 C18 H18 125.9 . . ? Fe2 C18 H18 125.9 . . ? C18 C19 C20 107.5(4) . . ? C18 C19 Fe2 70.1(2) . . ? C20 C19 Fe2 69.4(2) . . ? C18 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? Fe2 C19 H19 126.2 . . ? C16 C20 C19 108.4(4) . . ? C16 C20 Fe2 70.1(2) . . ? C19 C20 Fe2 69.7(2) . . ? C16 C20 H20 125.8 . . ? C19 C20 H20 125.8 . . ? Fe2 C20 H20 125.8 . . ? C5 C1 C2 107.2(3) . . ? C5 C1 B1 130.7(3) . . ? C2 C1 B1 121.3(3) . . ? C5 C1 Fe1 70.2(2) . . ? C2 C1 Fe1 69.4(2) . . ? B1 C1 Fe1 117.4(3) . . ? C3 C2 C1 107.3(3) . . ? C3 C2 B1 130.7(3) . 2_557 ? C1 C2 B1 121.6(3) . 2_557 ? C3 C2 Fe1 70.0(2) . . ? C1 C2 Fe1 68.7(2) . . ? B1 C2 Fe1 120.3(3) 2_557 . ? C2 C3 C4 108.9(3) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C3 Fe1 69.9(2) . . ? C2 C3 H3 125.5 . . ? C4 C3 H3 125.5 . . ? Fe1 C3 H3 125.5 . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Fe1 69.6(2) . . ? C5 C4 Fe1 69.7(2) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 126.0 . . ? C1 C5 C4 108.6(3) . . ? C1 C5 Fe1 69.1(2) . . ? C4 C5 Fe1 69.8(2) . . ? C1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Fe1 C5 H5 125.7 . . ? C7 C6 C10 108.3(4) . . ? C7 C6 Fe1 69.6(2) . . ? C10 C6 Fe1 69.2(2) . . ? C7 C6 H6 125.8 . . ? C10 C6 H6 125.8 . . ? Fe1 C6 H6 125.8 . . ? C6 C7 C8 108.5(3) . . ? C6 C7 Fe1 70.4(2) . . ? C8 C7 Fe1 69.5(2) . . ? C6 C7 H7 125.8 . . ? C8 C7 H7 125.8 . . ? Fe1 C7 H7 125.8 . . ? C7 C8 C9 107.3(4) . . ? C7 C8 Fe1 69.8(2) . . ? C9 C8 Fe1 69.2(2) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? Fe1 C8 H8 126.4 . . ? C10 C9 C8 108.0(3) . . ? C10 C9 Fe1 69.9(2) . . ? C8 C9 Fe1 69.9(2) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe1 C9 H9 126.0 . . ? C6 C10 C9 107.9(4) . . ? C6 C10 Fe1 70.4(2) . . ? C9 C10 Fe1 69.4(2) . . ? C6 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 2.03 2.830(4) 159.0 1_665 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 68.08 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.860 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.102 # Attachment '- Fc2B2O2H2_THF.cif' data_fc2b2(OH)2_acetone _database_code_depnum_ccdc_archive 'CCDC 892506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 B2 Fe2 O2, C3 H6 O ' _chemical_formula_sum 'C23 H24 B2 Fe2 O3' _chemical_formula_weight 481.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6092(2) _cell_length_b 10.8863(3) _cell_length_c 10.9983(2) _cell_angle_alpha 100.0450(10) _cell_angle_beta 116.1300(10) _cell_angle_gamma 106.5510(10) _cell_volume 1024.66(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6689 _cell_measurement_theta_min 4.52 _cell_measurement_theta_max 67.51 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 11.531 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.1220 _exptl_absorpt_correction_T_max 0.2307 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8732 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 67.93 _reflns_number_total 3442 _reflns_number_gt 3266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0525P)^2^+0.9777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3442 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Fe1 Fe 0.08291(4) 0.38502(4) 0.20322(4) 0.01912(12) Uani 1 1 d . . . Fe2 Fe 0.77076(4) 0.83365(4) 0.23519(4) 0.01914(12) Uani 1 1 d . . . O1 O -0.1977(2) 0.23119(18) -0.22641(18) 0.0254(4) Uani 1 1 d . . . H1 H -0.2406 0.1760 -0.1976 0.038 Uiso 1 1 calc R . . O2 O 0.8097(2) 1.14011(19) 0.52075(18) 0.0263(4) Uani 1 1 d . . . H2 H 0.8208 1.1580 0.6032 0.039 Uiso 1 1 calc R . . O3 O 0.3867(3) -0.0150(2) 0.1958(2) 0.0459(5) Uani 1 1 d . . . B2 B 0.8986(3) 1.0733(3) 0.5140(3) 0.0198(5) Uani 1 1 d . . . B1 B -0.1064(3) 0.3570(3) -0.1174(3) 0.0218(6) Uani 1 1 d . . . C1 C -0.0968(3) 0.3920(3) 0.0303(3) 0.0212(5) Uani 1 1 d . . . C2 C 0.0047(3) 0.5276(3) 0.1416(3) 0.0219(5) Uani 1 1 d . . . C3 C 0.0068(3) 0.5199(3) 0.2715(3) 0.0247(5) Uani 1 1 d . . . H3 H 0.0674 0.5966 0.3665 0.030 Uiso 1 1 calc R . . C4 C -0.0897(3) 0.3840(3) 0.2430(3) 0.0258(5) Uani 1 1 d . . . H4 H -0.1078 0.3490 0.3146 0.031 Uiso 1 1 calc R . . C5 C -0.1530(3) 0.3057(3) 0.0961(3) 0.0235(5) Uani 1 1 d . . . H5 H -0.2232 0.2063 0.0473 0.028 Uiso 1 1 calc R . . C6 C 0.2880(3) 0.4157(3) 0.3773(3) 0.0284(6) Uani 1 1 d . . . H6 H 0.3354 0.4772 0.4787 0.034 Uiso 1 1 calc R . . C7 C 0.1841(3) 0.2758(3) 0.3154(3) 0.0269(5) Uani 1 1 d . . . H7 H 0.1459 0.2215 0.3660 0.032 Uiso 1 1 calc R . . C8 C 0.1444(3) 0.2264(3) 0.1696(3) 0.0259(5) Uani 1 1 d . . . H8 H 0.0733 0.1313 0.0994 0.031 Uiso 1 1 calc R . . C9 C 0.2237(3) 0.3360(3) 0.1407(3) 0.0264(5) Uani 1 1 d . . . H9 H 0.2175 0.3316 0.0465 0.032 Uiso 1 1 calc R . . C10 C 0.3122(3) 0.4528(3) 0.2687(3) 0.0280(6) Uani 1 1 d . . . H10 H 0.3791 0.5453 0.2806 0.034 Uiso 1 1 calc R . . C12 C 0.9972(3) 0.9640(2) 0.3595(2) 0.0203(5) Uani 1 1 d . . . C13 C 0.9525(3) 0.9210(2) 0.2100(3) 0.0221(5) Uani 1 1 d . . . H13 H 0.9972 0.8703 0.1676 0.027 Uiso 1 1 calc R . . C14 C 0.8308(3) 0.9587(3) 0.1315(3) 0.0237(5) Uani 1 1 d . . . H14 H 0.7754 0.9392 0.0249 0.028 Uiso 1 1 calc R . . C15 C 0.7995(3) 1.0267(3) 0.2307(3) 0.0227(5) Uani 1 1 d . . . H15 H 0.7182 1.0631 0.2053 0.027 Uiso 1 1 calc R . . C16 C 0.6461(3) 0.7397(3) 0.3162(3) 0.0303(6) Uani 1 1 d . . . H16 H 0.6498 0.7835 0.4062 0.036 Uiso 1 1 calc R . . C17 C 0.5466(3) 0.7344(3) 0.1755(3) 0.0333(6) Uani 1 1 d . . . H17 H 0.4675 0.7735 0.1488 0.040 Uiso 1 1 calc R . . C18 C 0.5792(3) 0.6640(3) 0.0791(3) 0.0317(6) Uani 1 1 d . . . H18 H 0.5271 0.6448 -0.0275 0.038 Uiso 1 1 calc R . . C19 C 0.6985(3) 0.6251(3) 0.1611(3) 0.0279(5) Uani 1 1 d . . . H19 H 0.7458 0.5745 0.1225 0.033 Uiso 1 1 calc R . . C20 C 0.7392(3) 0.6717(3) 0.3073(3) 0.0266(5) Uani 1 1 d . . . H20 H 0.8206 0.6599 0.3900 0.032 Uiso 1 1 calc R . . C11 C 0.9008(3) 1.0314(2) 0.3723(3) 0.0208(5) Uani 1 1 d . . . C22 C 0.4604(4) 0.1386(4) 0.4212(4) 0.0447(7) Uani 1 1 d . . . H22A H 0.3982 0.0567 0.4274 0.067 Uiso 1 1 calc R . . H22B H 0.4172 0.2068 0.4234 0.067 Uiso 1 1 calc R . . H22C H 0.5663 0.1764 0.5032 0.067 Uiso 1 1 calc R . . C21 C 0.4594(3) 0.1020(3) 0.2840(3) 0.0369(7) Uani 1 1 d . . . C23 C 0.5471(4) 0.2161(4) 0.2563(4) 0.0443(8) Uani 1 1 d . . . H23A H 0.5352 0.1812 0.1617 0.066 Uiso 1 1 calc R . . H23B H 0.6563 0.2550 0.3316 0.066 Uiso 1 1 calc R . . H23C H 0.5074 0.2871 0.2572 0.066 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 Fe1 0.0225(2) 0.0186(2) 0.0211(2) 0.00850(15) 0.01367(16) 0.00984(15) Fe2 0.0209(2) 0.0160(2) 0.0198(2) 0.00542(14) 0.01086(15) 0.00671(15) O1 0.0317(9) 0.0216(10) 0.0270(9) 0.0083(7) 0.0182(7) 0.0112(7) O2 0.0326(9) 0.0291(10) 0.0239(8) 0.0081(7) 0.0168(7) 0.0182(8) O3 0.0510(13) 0.0389(14) 0.0469(13) 0.0124(10) 0.0281(11) 0.0142(10) B2 0.0210(12) 0.0139(13) 0.0222(13) 0.0039(10) 0.0119(10) 0.0042(10) B1 0.0242(13) 0.0225(15) 0.0256(13) 0.0106(11) 0.0142(11) 0.0151(11) C1 0.0228(11) 0.0220(13) 0.0251(12) 0.0106(10) 0.0137(10) 0.0135(10) C2 0.0281(12) 0.0225(14) 0.0233(11) 0.0093(10) 0.0161(10) 0.0158(10) C3 0.0300(13) 0.0255(14) 0.0274(12) 0.0108(10) 0.0186(10) 0.0157(11) C4 0.0278(12) 0.0308(15) 0.0298(13) 0.0141(11) 0.0199(11) 0.0161(11) C5 0.0216(11) 0.0261(14) 0.0272(12) 0.0105(10) 0.0139(10) 0.0123(10) C6 0.0245(12) 0.0320(15) 0.0256(12) 0.0080(11) 0.0094(10) 0.0147(11) C7 0.0290(13) 0.0292(15) 0.0310(13) 0.0167(11) 0.0173(11) 0.0165(11) C8 0.0273(12) 0.0253(14) 0.0309(13) 0.0115(10) 0.0165(11) 0.0151(10) C9 0.0285(13) 0.0312(15) 0.0318(13) 0.0151(11) 0.0205(11) 0.0176(11) C10 0.0223(12) 0.0254(15) 0.0404(14) 0.0137(11) 0.0180(11) 0.0110(10) C12 0.0208(11) 0.0150(12) 0.0238(12) 0.0040(9) 0.0133(9) 0.0046(9) C13 0.0272(12) 0.0183(13) 0.0230(12) 0.0069(9) 0.0156(10) 0.0080(10) C14 0.0304(13) 0.0209(13) 0.0237(12) 0.0094(10) 0.0167(10) 0.0100(10) C15 0.0271(12) 0.0175(13) 0.0256(12) 0.0082(9) 0.0147(10) 0.0097(10) C16 0.0324(14) 0.0251(15) 0.0369(14) 0.0113(11) 0.0237(12) 0.0066(11) C17 0.0210(12) 0.0275(15) 0.0476(16) 0.0145(12) 0.0167(12) 0.0062(10) C18 0.0286(13) 0.0195(14) 0.0289(13) 0.0048(10) 0.0080(11) 0.0001(10) C19 0.0321(13) 0.0163(13) 0.0319(13) 0.0062(10) 0.0170(11) 0.0061(10) C20 0.0277(12) 0.0194(14) 0.0322(13) 0.0135(10) 0.0158(11) 0.0061(10) C11 0.0220(11) 0.0159(12) 0.0250(12) 0.0067(9) 0.0129(9) 0.0073(9) C22 0.0434(17) 0.053(2) 0.0463(18) 0.0188(15) 0.0264(15) 0.0245(15) C21 0.0348(15) 0.0377(19) 0.0379(15) 0.0132(13) 0.0171(13) 0.0174(13) C23 0.0364(16) 0.049(2) 0.0493(18) 0.0221(15) 0.0225(14) 0.0170(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 Fe1 C7 2.040(3) . ? Fe1 C8 2.043(3) . ? Fe1 C2 2.040(2) . ? Fe1 C1 2.048(2) . ? Fe1 C6 2.051(2) . ? Fe1 C3 2.049(3) . ? Fe1 C5 2.053(2) . ? Fe1 C9 2.054(2) . ? Fe1 C10 2.056(2) . ? Fe1 C4 2.059(2) . ? Fe2 C12 2.035(2) . ? Fe2 C11 2.038(2) . ? Fe2 C17 2.042(3) . ? Fe2 C18 2.042(3) . ? Fe2 C16 2.043(3) . ? Fe2 C15 2.048(3) . ? Fe2 C19 2.054(3) . ? Fe2 C13 2.054(2) . ? Fe2 C20 2.058(3) . ? Fe2 C14 2.061(2) . ? O1 B1 1.378(3) . ? O1 H1 0.8400 . ? O2 B2 1.363(3) . ? O2 H2 0.8400 . ? O3 C21 1.228(4) . ? B2 C11 1.558(3) . ? B2 C12 1.556(4) 2_776 ? B1 C2 1.552(4) 2_565 ? B1 C1 1.553(4) . ? C1 C5 1.435(3) . ? C1 C2 1.462(3) . ? C2 C3 1.437(3) . ? C2 B1 1.552(4) 2_565 ? C3 C4 1.424(4) . ? C3 H3 1.0000 . ? C4 C5 1.423(4) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 C7 1.420(4) . ? C6 C10 1.426(4) . ? C6 H6 1.0000 . ? C7 C8 1.419(4) . ? C7 H7 1.0000 . ? C8 C9 1.424(4) . ? C8 H8 1.0000 . ? C9 C10 1.419(4) . ? C9 H9 1.0000 . ? C10 H10 1.0000 . ? C12 C13 1.438(3) . ? C12 C11 1.457(3) . ? C12 B2 1.556(4) 2_776 ? C13 C14 1.423(3) . ? C13 H13 1.0000 . ? C14 C15 1.424(3) . ? C14 H14 1.0000 . ? C15 C11 1.432(3) . ? C15 H15 1.0000 . ? C16 C20 1.418(4) . ? C16 C17 1.417(4) . ? C16 H16 1.0000 . ? C17 C18 1.422(4) . ? C17 H17 1.0000 . ? C18 C19 1.425(4) . ? C18 H18 1.0000 . ? C19 C20 1.417(4) . ? C19 H19 1.0000 . ? C20 H20 1.0000 . ? C22 C21 1.486(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21 C23 1.492(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Fe1 C8 40.69(10) . . ? C7 Fe1 C2 165.64(10) . . ? C8 Fe1 C2 152.89(10) . . ? C7 Fe1 C1 150.28(11) . . ? C8 Fe1 C1 117.85(10) . . ? C2 Fe1 C1 41.91(10) . . ? C7 Fe1 C6 40.63(11) . . ? C8 Fe1 C6 68.35(11) . . ? C2 Fe1 C6 128.40(11) . . ? C1 Fe1 C6 168.35(11) . . ? C7 Fe1 C3 126.49(10) . . ? C8 Fe1 C3 164.64(10) . . ? C2 Fe1 C3 41.15(9) . . ? C1 Fe1 C3 69.51(10) . . ? C6 Fe1 C3 107.11(10) . . ? C7 Fe1 C5 116.08(10) . . ? C8 Fe1 C5 107.45(10) . . ? C2 Fe1 C5 69.33(10) . . ? C1 Fe1 C5 40.96(10) . . ? C6 Fe1 C5 149.33(11) . . ? C3 Fe1 C5 68.51(10) . . ? C7 Fe1 C9 68.38(10) . . ? C8 Fe1 C9 40.67(10) . . ? C2 Fe1 C9 119.59(10) . . ? C1 Fe1 C9 109.38(10) . . ? C6 Fe1 C9 68.23(10) . . ? C3 Fe1 C9 152.89(11) . . ? C5 Fe1 C9 129.40(10) . . ? C7 Fe1 C10 68.32(11) . . ? C8 Fe1 C10 68.21(11) . . ? C2 Fe1 C10 109.21(10) . . ? C1 Fe1 C10 130.32(10) . . ? C6 Fe1 C10 40.63(11) . . ? C3 Fe1 C10 118.60(11) . . ? C5 Fe1 C10 168.25(11) . . ? C9 Fe1 C10 40.37(11) . . ? C7 Fe1 C4 105.88(10) . . ? C8 Fe1 C4 126.96(11) . . ? C2 Fe1 C4 68.99(10) . . ? C1 Fe1 C4 68.93(10) . . ? C6 Fe1 C4 116.24(10) . . ? C3 Fe1 C4 40.56(11) . . ? C5 Fe1 C4 40.50(10) . . ? C9 Fe1 C4 166.15(11) . . ? C10 Fe1 C4 150.82(11) . . ? C12 Fe2 C11 41.92(9) . . ? C12 Fe2 C17 159.68(11) . . ? C11 Fe2 C17 121.97(11) . . ? C12 Fe2 C18 158.21(11) . . ? C11 Fe2 C18 158.48(11) . . ? C17 Fe2 C18 40.76(12) . . ? C12 Fe2 C16 123.55(10) . . ? C11 Fe2 C16 106.72(10) . . ? C17 Fe2 C16 40.60(12) . . ? C18 Fe2 C16 68.39(11) . . ? C12 Fe2 C15 69.44(10) . . ? C11 Fe2 C15 41.01(9) . . ? C17 Fe2 C15 106.33(11) . . ? C18 Fe2 C15 122.34(11) . . ? C16 Fe2 C15 121.70(11) . . ? C12 Fe2 C19 122.50(10) . . ? C11 Fe2 C19 158.83(10) . . ? C17 Fe2 C19 68.36(12) . . ? C18 Fe2 C19 40.71(11) . . ? C16 Fe2 C19 68.11(11) . . ? C15 Fe2 C19 159.33(10) . . ? C12 Fe2 C13 41.17(9) . . ? C11 Fe2 C13 69.37(9) . . ? C17 Fe2 C13 157.36(11) . . ? C18 Fe2 C13 122.10(11) . . ? C16 Fe2 C13 160.92(11) . . ? C15 Fe2 C13 68.35(10) . . ? C19 Fe2 C13 108.42(10) . . ? C12 Fe2 C20 107.97(10) . . ? C11 Fe2 C20 122.55(10) . . ? C17 Fe2 C20 68.16(11) . . ? C18 Fe2 C20 68.19(11) . . ? C16 Fe2 C20 40.45(11) . . ? C15 Fe2 C20 158.14(10) . . ? C19 Fe2 C20 40.32(11) . . ? C13 Fe2 C20 124.84(10) . . ? C12 Fe2 C14 69.14(10) . . ? C11 Fe2 C14 69.03(10) . . ? C17 Fe2 C14 121.32(11) . . ? C18 Fe2 C14 106.93(11) . . ? C16 Fe2 C14 157.21(11) . . ? C15 Fe2 C14 40.54(10) . . ? C19 Fe2 C14 123.80(10) . . ? C13 Fe2 C14 40.45(10) . . ? C20 Fe2 C14 160.49(11) . . ? B1 O1 H1 109.5 . . ? B2 O2 H2 109.5 . . ? O2 B2 C11 119.4(2) . . ? O2 B2 C12 124.5(2) . 2_776 ? C11 B2 C12 116.1(2) . 2_776 ? O1 B1 C2 118.6(2) . 2_565 ? O1 B1 C1 124.4(2) . . ? C2 B1 C1 117.0(2) 2_565 . ? C5 C1 C2 107.0(2) . . ? C5 C1 B1 131.0(2) . . ? C2 C1 B1 121.2(2) . . ? C5 C1 Fe1 69.69(13) . . ? C2 C1 Fe1 68.74(13) . . ? B1 C1 Fe1 118.07(16) . . ? C3 C2 C1 107.3(2) . . ? C3 C2 B1 130.1(2) . 2_565 ? C1 C2 B1 121.8(2) . 2_565 ? C3 C2 Fe1 69.76(14) . . ? C1 C2 Fe1 69.35(13) . . ? B1 C2 Fe1 118.28(16) 2_565 . ? C4 C3 C2 108.5(2) . . ? C4 C3 Fe1 70.09(14) . . ? C2 C3 Fe1 69.09(14) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe1 C3 H3 125.8 . . ? C3 C4 C5 108.4(2) . . ? C3 C4 Fe1 69.35(14) . . ? C5 C4 Fe1 69.53(13) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 108.8(2) . . ? C4 C5 Fe1 69.97(14) . . ? C1 C5 Fe1 69.35(13) . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C7 C6 C10 107.8(2) . . ? C7 C6 Fe1 69.26(14) . . ? C10 C6 Fe1 69.90(14) . . ? C7 C6 H6 126.1 . . ? C10 C6 H6 126.1 . . ? Fe1 C6 H6 126.1 . . ? C6 C7 C8 108.2(2) . . ? C6 C7 Fe1 70.11(14) . . ? C8 C7 Fe1 69.80(14) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 125.9 . . ? C7 C8 C9 108.0(2) . . ? C7 C8 Fe1 69.51(15) . . ? C9 C8 Fe1 70.08(14) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe1 C8 H8 126.0 . . ? C10 C9 C8 107.9(2) . . ? C10 C9 Fe1 69.89(14) . . ? C8 C9 Fe1 69.25(14) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe1 C9 H9 126.0 . . ? C9 C10 C6 108.1(2) . . ? C9 C10 Fe1 69.74(14) . . ? C6 C10 Fe1 69.47(14) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe1 C10 H10 126.0 . . ? C13 C12 C11 107.1(2) . . ? C13 C12 B2 130.1(2) . 2_776 ? C11 C12 B2 121.7(2) . 2_776 ? C13 C12 Fe2 70.11(13) . . ? C11 C12 Fe2 69.16(13) . . ? B2 C12 Fe2 116.79(16) 2_776 . ? C14 C13 C12 108.7(2) . . ? C14 C13 Fe2 70.05(14) . . ? C12 C13 Fe2 68.72(13) . . ? C14 C13 H13 125.6 . . ? C12 C13 H13 125.6 . . ? Fe2 C13 H13 125.6 . . ? C15 C14 C13 108.1(2) . . ? C15 C14 Fe2 69.24(14) . . ? C13 C14 Fe2 69.50(14) . . ? C15 C14 H14 125.9 . . ? C13 C14 H14 125.9 . . ? Fe2 C14 H14 125.9 . . ? C14 C15 C11 108.9(2) . . ? C14 C15 Fe2 70.21(15) . . ? C11 C15 Fe2 69.13(14) . . ? C14 C15 H15 125.6 . . ? C11 C15 H15 125.6 . . ? Fe2 C15 H15 125.6 . . ? C20 C16 C17 108.2(2) . . ? C20 C16 Fe2 70.33(14) . . ? C17 C16 Fe2 69.63(15) . . ? C20 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Fe2 C16 H16 125.9 . . ? C18 C17 C16 107.9(3) . . ? C18 C17 Fe2 69.65(15) . . ? C16 C17 Fe2 69.76(14) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Fe2 C17 H17 126.0 . . ? C17 C18 C19 107.8(2) . . ? C17 C18 Fe2 69.59(15) . . ? C19 C18 Fe2 70.08(15) . . ? C17 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? Fe2 C18 H18 126.1 . . ? C20 C19 C18 108.0(2) . . ? C20 C19 Fe2 70.00(15) . . ? C18 C19 Fe2 69.22(15) . . ? C20 C19 H19 126.0 . . ? C18 C19 H19 126.0 . . ? Fe2 C19 H19 126.0 . . ? C19 C20 C16 108.1(2) . . ? C19 C20 Fe2 69.68(15) . . ? C16 C20 Fe2 69.22(15) . . ? C19 C20 H20 126.0 . . ? C16 C20 H20 126.0 . . ? Fe2 C20 H20 126.0 . . ? C15 C11 C12 107.2(2) . . ? C15 C11 B2 129.8(2) . . ? C12 C11 B2 122.2(2) . . ? C15 C11 Fe2 69.86(14) . . ? C12 C11 Fe2 68.92(13) . . ? B2 C11 Fe2 118.18(16) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C21 C22 122.1(3) . . ? O3 C21 C23 121.4(3) . . ? C22 C21 C23 116.5(3) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 B1 C1 C5 11.5(4) . . . . ? C2 B1 C1 C5 -168.0(2) 2_565 . . . ? O1 B1 C1 C2 179.1(2) . . . . ? C2 B1 C1 C2 -0.4(4) 2_565 . . . ? O1 B1 C1 Fe1 98.2(3) . . . . ? C2 B1 C1 Fe1 -81.4(2) 2_565 . . . ? C7 Fe1 C1 C5 48.3(3) . . . . ? C8 Fe1 C1 C5 84.76(16) . . . . ? C2 Fe1 C1 C5 -118.5(2) . . . . ? C6 Fe1 C1 C5 -155.5(5) . . . . ? C3 Fe1 C1 C5 -80.44(15) . . . . ? C9 Fe1 C1 C5 128.41(15) . . . . ? C10 Fe1 C1 C5 168.89(15) . . . . ? C4 Fe1 C1 C5 -36.93(15) . . . . ? C7 Fe1 C1 C2 166.82(19) . . . . ? C8 Fe1 C1 C2 -156.72(14) . . . . ? C6 Fe1 C1 C2 -37.0(5) . . . . ? C3 Fe1 C1 C2 38.08(14) . . . . ? C5 Fe1 C1 C2 118.5(2) . . . . ? C9 Fe1 C1 C2 -113.06(15) . . . . ? C10 Fe1 C1 C2 -72.59(18) . . . . ? C4 Fe1 C1 C2 81.60(15) . . . . ? C7 Fe1 C1 B1 -78.2(3) . . . . ? C8 Fe1 C1 B1 -41.7(2) . . . . ? C2 Fe1 C1 B1 115.0(2) . . . . ? C6 Fe1 C1 B1 78.0(5) . . . . ? C3 Fe1 C1 B1 153.1(2) . . . . ? C5 Fe1 C1 B1 -126.5(3) . . . . ? C9 Fe1 C1 B1 1.9(2) . . . . ? C10 Fe1 C1 B1 42.4(3) . . . . ? C4 Fe1 C1 B1 -163.4(2) . . . . ? C5 C1 C2 C3 -0.2(3) . . . . ? B1 C1 C2 C3 -170.4(2) . . . . ? Fe1 C1 C2 C3 -59.67(16) . . . . ? C5 C1 C2 B1 170.7(2) . . . 2_565 ? B1 C1 C2 B1 0.5(4) . . . 2_565 ? Fe1 C1 C2 B1 111.2(2) . . . 2_565 ? C5 C1 C2 Fe1 59.48(16) . . . . ? B1 C1 C2 Fe1 -110.8(2) . . . . ? C7 Fe1 C2 C3 -34.3(5) . . . . ? C8 Fe1 C2 C3 168.7(2) . . . . ? C1 Fe1 C2 C3 118.6(2) . . . . ? C6 Fe1 C2 C3 -70.33(18) . . . . ? C5 Fe1 C2 C3 80.60(16) . . . . ? C9 Fe1 C2 C3 -154.93(15) . . . . ? C10 Fe1 C2 C3 -111.81(16) . . . . ? C4 Fe1 C2 C3 37.12(15) . . . . ? C7 Fe1 C2 C1 -152.9(4) . . . . ? C8 Fe1 C2 C1 50.1(3) . . . . ? C6 Fe1 C2 C1 171.08(14) . . . . ? C3 Fe1 C2 C1 -118.6(2) . . . . ? C5 Fe1 C2 C1 -37.99(13) . . . . ? C9 Fe1 C2 C1 86.48(16) . . . . ? C10 Fe1 C2 C1 129.61(14) . . . . ? C4 Fe1 C2 C1 -81.46(15) . . . . ? C7 Fe1 C2 B1 91.2(4) . . . 2_565 ? C8 Fe1 C2 B1 -65.8(3) . . . 2_565 ? C1 Fe1 C2 B1 -115.9(2) . . . 2_565 ? C6 Fe1 C2 B1 55.2(2) . . . 2_565 ? C3 Fe1 C2 B1 125.5(3) . . . 2_565 ? C5 Fe1 C2 B1 -153.9(2) . . . 2_565 ? C9 Fe1 C2 B1 -29.4(2) . . . 2_565 ? C10 Fe1 C2 B1 13.7(2) . . . 2_565 ? C4 Fe1 C2 B1 162.6(2) . . . 2_565 ? C1 C2 C3 C4 0.2(3) . . . . ? B1 C2 C3 C4 -169.7(2) 2_565 . . . ? Fe1 C2 C3 C4 -59.21(17) . . . . ? C1 C2 C3 Fe1 59.41(16) . . . . ? B1 C2 C3 Fe1 -110.5(3) 2_565 . . . ? C7 Fe1 C3 C4 -70.07(18) . . . . ? C8 Fe1 C3 C4 -40.3(4) . . . . ? C2 Fe1 C3 C4 119.9(2) . . . . ? C1 Fe1 C3 C4 81.18(16) . . . . ? C6 Fe1 C3 C4 -110.60(16) . . . . ? C5 Fe1 C3 C4 37.17(14) . . . . ? C9 Fe1 C3 C4 173.9(2) . . . . ? C10 Fe1 C3 C4 -153.17(15) . . . . ? C7 Fe1 C3 C2 169.98(14) . . . . ? C8 Fe1 C3 C2 -160.2(3) . . . . ? C1 Fe1 C3 C2 -38.77(14) . . . . ? C6 Fe1 C3 C2 129.45(15) . . . . ? C5 Fe1 C3 C2 -82.77(15) . . . . ? C9 Fe1 C3 C2 53.9(3) . . . . ? C10 Fe1 C3 C2 86.89(17) . . . . ? C4 Fe1 C3 C2 -119.9(2) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? Fe1 C3 C4 C5 -58.72(17) . . . . ? C2 C3 C4 Fe1 58.59(17) . . . . ? C7 Fe1 C4 C3 128.20(15) . . . . ? C8 Fe1 C4 C3 167.62(14) . . . . ? C2 Fe1 C4 C3 -37.64(14) . . . . ? C1 Fe1 C4 C3 -82.71(16) . . . . ? C6 Fe1 C4 C3 85.89(17) . . . . ? C5 Fe1 C4 C3 -120.0(2) . . . . ? C9 Fe1 C4 C3 -168.3(4) . . . . ? C10 Fe1 C4 C3 54.4(3) . . . . ? C7 Fe1 C4 C5 -111.76(16) . . . . ? C8 Fe1 C4 C5 -72.34(18) . . . . ? C2 Fe1 C4 C5 82.39(16) . . . . ? C1 Fe1 C4 C5 37.33(15) . . . . ? C6 Fe1 C4 C5 -154.07(15) . . . . ? C3 Fe1 C4 C5 120.0(2) . . . . ? C9 Fe1 C4 C5 -48.3(5) . . . . ? C10 Fe1 C4 C5 174.4(2) . . . . ? C3 C4 C5 C1 0.0(3) . . . . ? Fe1 C4 C5 C1 -58.60(16) . . . . ? C3 C4 C5 Fe1 58.61(17) . . . . ? C2 C1 C5 C4 0.1(3) . . . . ? B1 C1 C5 C4 169.1(2) . . . . ? Fe1 C1 C5 C4 58.98(17) . . . . ? C2 C1 C5 Fe1 -58.87(15) . . . . ? B1 C1 C5 Fe1 110.1(3) . . . . ? C7 Fe1 C5 C4 84.03(17) . . . . ? C8 Fe1 C5 C4 127.05(16) . . . . ? C2 Fe1 C5 C4 -81.46(16) . . . . ? C1 Fe1 C5 C4 -120.3(2) . . . . ? C6 Fe1 C5 C4 50.2(3) . . . . ? C3 Fe1 C5 C4 -37.22(15) . . . . ? C9 Fe1 C5 C4 166.63(15) . . . . ? C10 Fe1 C5 C4 -166.5(5) . . . . ? C7 Fe1 C5 C1 -155.66(15) . . . . ? C8 Fe1 C5 C1 -112.64(15) . . . . ? C2 Fe1 C5 C1 38.85(14) . . . . ? C6 Fe1 C5 C1 170.55(19) . . . . ? C3 Fe1 C5 C1 83.08(15) . . . . ? C9 Fe1 C5 C1 -73.06(18) . . . . ? C10 Fe1 C5 C1 -46.2(6) . . . . ? C4 Fe1 C5 C1 120.3(2) . . . . ? C8 Fe1 C6 C7 -37.80(15) . . . . ? C2 Fe1 C6 C7 167.05(15) . . . . ? C1 Fe1 C6 C7 -162.1(4) . . . . ? C3 Fe1 C6 C7 126.64(15) . . . . ? C5 Fe1 C6 C7 50.1(3) . . . . ? C9 Fe1 C6 C7 -81.73(16) . . . . ? C10 Fe1 C6 C7 -119.1(2) . . . . ? C4 Fe1 C6 C7 83.91(17) . . . . ? C7 Fe1 C6 C10 119.1(2) . . . . ? C8 Fe1 C6 C10 81.34(17) . . . . ? C2 Fe1 C6 C10 -73.82(19) . . . . ? C1 Fe1 C6 C10 -43.0(6) . . . . ? C3 Fe1 C6 C10 -114.23(17) . . . . ? C5 Fe1 C6 C10 169.22(19) . . . . ? C9 Fe1 C6 C10 37.41(16) . . . . ? C4 Fe1 C6 C10 -156.96(16) . . . . ? C10 C6 C7 C8 0.2(3) . . . . ? Fe1 C6 C7 C8 59.66(17) . . . . ? C10 C6 C7 Fe1 -59.49(18) . . . . ? C8 Fe1 C7 C6 119.1(2) . . . . ? C2 Fe1 C7 C6 -45.1(5) . . . . ? C1 Fe1 C7 C6 172.81(18) . . . . ? C3 Fe1 C7 C6 -72.53(18) . . . . ? C5 Fe1 C7 C6 -154.18(15) . . . . ? C9 Fe1 C7 C6 81.34(16) . . . . ? C10 Fe1 C7 C6 37.75(16) . . . . ? C4 Fe1 C7 C6 -111.99(16) . . . . ? C2 Fe1 C7 C8 -164.2(4) . . . . ? C1 Fe1 C7 C8 53.7(3) . . . . ? C6 Fe1 C7 C8 -119.1(2) . . . . ? C3 Fe1 C7 C8 168.36(15) . . . . ? C5 Fe1 C7 C8 86.72(16) . . . . ? C9 Fe1 C7 C8 -37.77(15) . . . . ? C10 Fe1 C7 C8 -81.36(16) . . . . ? C4 Fe1 C7 C8 128.90(15) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? Fe1 C7 C8 C9 59.74(17) . . . . ? C6 C7 C8 Fe1 -59.85(17) . . . . ? C2 Fe1 C8 C7 171.5(2) . . . . ? C1 Fe1 C8 C7 -153.13(15) . . . . ? C6 Fe1 C8 C7 37.74(15) . . . . ? C3 Fe1 C8 C7 -37.8(4) . . . . ? C5 Fe1 C8 C7 -109.96(15) . . . . ? C9 Fe1 C8 C7 119.1(2) . . . . ? C10 Fe1 C8 C7 81.64(16) . . . . ? C4 Fe1 C8 C7 -69.51(18) . . . . ? C7 Fe1 C8 C9 -119.1(2) . . . . ? C2 Fe1 C8 C9 52.4(3) . . . . ? C1 Fe1 C8 C9 87.76(16) . . . . ? C6 Fe1 C8 C9 -81.36(16) . . . . ? C3 Fe1 C8 C9 -156.9(4) . . . . ? C5 Fe1 C8 C9 130.94(15) . . . . ? C10 Fe1 C8 C9 -37.47(15) . . . . ? C4 Fe1 C8 C9 171.38(15) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? Fe1 C8 C9 C10 59.39(17) . . . . ? C7 C8 C9 Fe1 -59.38(17) . . . . ? C7 Fe1 C9 C10 -81.52(17) . . . . ? C8 Fe1 C9 C10 -119.3(2) . . . . ? C2 Fe1 C9 C10 85.20(17) . . . . ? C1 Fe1 C9 C10 130.18(16) . . . . ? C6 Fe1 C9 C10 -37.64(16) . . . . ? C3 Fe1 C9 C10 47.5(3) . . . . ? C5 Fe1 C9 C10 171.84(15) . . . . ? C4 Fe1 C9 C10 -149.3(4) . . . . ? C7 Fe1 C9 C8 37.79(15) . . . . ? C2 Fe1 C9 C8 -155.49(15) . . . . ? C1 Fe1 C9 C8 -110.52(16) . . . . ? C6 Fe1 C9 C8 81.67(16) . . . . ? C3 Fe1 C9 C8 166.8(2) . . . . ? C5 Fe1 C9 C8 -68.86(19) . . . . ? C10 Fe1 C9 C8 119.3(2) . . . . ? C4 Fe1 C9 C8 -30.0(5) . . . . ? C8 C9 C10 C6 0.1(3) . . . . ? Fe1 C9 C10 C6 59.08(17) . . . . ? C8 C9 C10 Fe1 -58.99(17) . . . . ? C7 C6 C10 C9 -0.2(3) . . . . ? Fe1 C6 C10 C9 -59.25(17) . . . . ? C7 C6 C10 Fe1 59.10(17) . . . . ? C7 Fe1 C10 C9 81.69(17) . . . . ? C8 Fe1 C10 C9 37.74(15) . . . . ? C2 Fe1 C10 C9 -113.41(16) . . . . ? C1 Fe1 C10 C9 -70.96(19) . . . . ? C6 Fe1 C10 C9 119.4(2) . . . . ? C3 Fe1 C10 C9 -157.50(15) . . . . ? C5 Fe1 C10 C9 -32.6(6) . . . . ? C4 Fe1 C10 C9 165.5(2) . . . . ? C7 Fe1 C10 C6 -37.74(16) . . . . ? C8 Fe1 C10 C6 -81.70(17) . . . . ? C2 Fe1 C10 C6 127.15(16) . . . . ? C1 Fe1 C10 C6 169.60(15) . . . . ? C3 Fe1 C10 C6 83.06(18) . . . . ? C5 Fe1 C10 C6 -152.0(5) . . . . ? C9 Fe1 C10 C6 -119.4(2) . . . . ? C4 Fe1 C10 C6 46.1(3) . . . . ? C11 Fe2 C12 C13 -118.2(2) . . . . ? C17 Fe2 C12 C13 -161.7(3) . . . . ? C18 Fe2 C12 C13 46.7(3) . . . . ? C16 Fe2 C12 C13 164.64(15) . . . . ? C15 Fe2 C12 C13 -80.23(15) . . . . ? C19 Fe2 C12 C13 80.83(17) . . . . ? C20 Fe2 C12 C13 122.78(15) . . . . ? C14 Fe2 C12 C13 -36.75(14) . . . . ? C17 Fe2 C12 C11 -43.5(4) . . . . ? C18 Fe2 C12 C11 164.9(3) . . . . ? C16 Fe2 C12 C11 -77.17(17) . . . . ? C15 Fe2 C12 C11 37.96(14) . . . . ? C19 Fe2 C12 C11 -160.98(14) . . . . ? C13 Fe2 C12 C11 118.2(2) . . . . ? C20 Fe2 C12 C11 -119.03(15) . . . . ? C14 Fe2 C12 C11 81.44(15) . . . . ? C11 Fe2 C12 B2 116.0(2) . . . 2_776 ? C17 Fe2 C12 B2 72.5(4) . . . 2_776 ? C18 Fe2 C12 B2 -79.1(3) . . . 2_776 ? C16 Fe2 C12 B2 38.8(2) . . . 2_776 ? C15 Fe2 C12 B2 153.9(2) . . . 2_776 ? C19 Fe2 C12 B2 -45.0(2) . . . 2_776 ? C13 Fe2 C12 B2 -125.8(2) . . . 2_776 ? C20 Fe2 C12 B2 -3.1(2) . . . 2_776 ? C14 Fe2 C12 B2 -162.6(2) . . . 2_776 ? C11 C12 C13 C14 -0.8(3) . . . . ? B2 C12 C13 C14 167.6(2) 2_776 . . . ? Fe2 C12 C13 C14 58.78(17) . . . . ? C11 C12 C13 Fe2 -59.53(15) . . . . ? B2 C12 C13 Fe2 108.8(3) 2_776 . . . ? C12 Fe2 C13 C14 -120.5(2) . . . . ? C11 Fe2 C13 C14 -81.50(15) . . . . ? C17 Fe2 C13 C14 43.1(3) . . . . ? C18 Fe2 C13 C14 78.11(18) . . . . ? C16 Fe2 C13 C14 -163.0(3) . . . . ? C15 Fe2 C13 C14 -37.39(14) . . . . ? C19 Fe2 C13 C14 120.86(15) . . . . ? C20 Fe2 C13 C14 162.50(15) . . . . ? C11 Fe2 C13 C12 38.99(14) . . . . ? C17 Fe2 C13 C12 163.6(3) . . . . ? C18 Fe2 C13 C12 -161.41(15) . . . . ? C16 Fe2 C13 C12 -42.5(4) . . . . ? C15 Fe2 C13 C12 83.10(15) . . . . ? C19 Fe2 C13 C12 -118.65(15) . . . . ? C20 Fe2 C13 C12 -77.01(17) . . . . ? C14 Fe2 C13 C12 120.5(2) . . . . ? C12 C13 C14 C15 0.7(3) . . . . ? Fe2 C13 C14 C15 58.66(17) . . . . ? C12 C13 C14 Fe2 -57.96(16) . . . . ? C12 Fe2 C14 C15 -82.37(15) . . . . ? C11 Fe2 C14 C15 -37.34(14) . . . . ? C17 Fe2 C14 C15 78.17(18) . . . . ? C18 Fe2 C14 C15 120.30(16) . . . . ? C16 Fe2 C14 C15 45.9(3) . . . . ? C19 Fe2 C14 C15 161.73(15) . . . . ? C13 Fe2 C14 C15 -119.8(2) . . . . ? C20 Fe2 C14 C15 -167.4(3) . . . . ? C12 Fe2 C14 C13 37.38(14) . . . . ? C11 Fe2 C14 C13 82.41(15) . . . . ? C17 Fe2 C14 C13 -162.08(15) . . . . ? C18 Fe2 C14 C13 -119.95(16) . . . . ? C16 Fe2 C14 C13 165.7(2) . . . . ? C15 Fe2 C14 C13 119.8(2) . . . . ? C19 Fe2 C14 C13 -78.52(17) . . . . ? C20 Fe2 C14 C13 -47.6(4) . . . . ? C13 C14 C15 C11 -0.4(3) . . . . ? Fe2 C14 C15 C11 58.45(17) . . . . ? C13 C14 C15 Fe2 -58.82(17) . . . . ? C12 Fe2 C15 C14 81.57(15) . . . . ? C11 Fe2 C15 C14 120.3(2) . . . . ? C17 Fe2 C15 C14 -119.40(16) . . . . ? C18 Fe2 C15 C14 -77.87(18) . . . . ? C16 Fe2 C15 C14 -160.90(15) . . . . ? C19 Fe2 C15 C14 -47.6(3) . . . . ? C13 Fe2 C15 C14 37.30(14) . . . . ? C20 Fe2 C15 C14 168.7(2) . . . . ? C12 Fe2 C15 C11 -38.77(14) . . . . ? C17 Fe2 C15 C11 120.26(15) . . . . ? C18 Fe2 C15 C11 161.79(15) . . . . ? C16 Fe2 C15 C11 78.75(17) . . . . ? C19 Fe2 C15 C11 -167.9(3) . . . . ? C13 Fe2 C15 C11 -83.04(15) . . . . ? C20 Fe2 C15 C11 48.4(3) . . . . ? C14 Fe2 C15 C11 -120.3(2) . . . . ? C12 Fe2 C16 C20 -78.05(18) . . . . ? C11 Fe2 C16 C20 -120.90(16) . . . . ? C17 Fe2 C16 C20 119.1(2) . . . . ? C18 Fe2 C16 C20 81.30(17) . . . . ? C15 Fe2 C16 C20 -163.13(15) . . . . ? C19 Fe2 C16 C20 37.32(15) . . . . ? C13 Fe2 C16 C20 -45.8(4) . . . . ? C14 Fe2 C16 C20 163.6(2) . . . . ? C12 Fe2 C16 C17 162.80(16) . . . . ? C11 Fe2 C16 C17 119.95(17) . . . . ? C18 Fe2 C16 C17 -37.85(18) . . . . ? C15 Fe2 C16 C17 77.72(19) . . . . ? C19 Fe2 C16 C17 -81.83(18) . . . . ? C13 Fe2 C16 C17 -165.0(3) . . . . ? C20 Fe2 C16 C17 -119.1(2) . . . . ? C14 Fe2 C16 C17 44.4(3) . . . . ? C20 C16 C17 C18 -0.6(3) . . . . ? Fe2 C16 C17 C18 59.42(19) . . . . ? C20 C16 C17 Fe2 -59.98(18) . . . . ? C12 Fe2 C17 C18 -164.3(3) . . . . ? C11 Fe2 C17 C18 162.85(16) . . . . ? C16 Fe2 C17 C18 -119.1(2) . . . . ? C15 Fe2 C17 C18 120.92(17) . . . . ? C19 Fe2 C17 C18 -37.93(16) . . . . ? C13 Fe2 C17 C18 48.2(4) . . . . ? C20 Fe2 C17 C18 -81.49(18) . . . . ? C14 Fe2 C17 C18 79.40(19) . . . . ? C12 Fe2 C17 C16 -45.2(4) . . . . ? C11 Fe2 C17 C16 -78.04(19) . . . . ? C18 Fe2 C17 C16 119.1(2) . . . . ? C15 Fe2 C17 C16 -119.97(17) . . . . ? C19 Fe2 C17 C16 81.18(18) . . . . ? C13 Fe2 C17 C16 167.3(3) . . . . ? C20 Fe2 C17 C16 37.62(17) . . . . ? C14 Fe2 C17 C16 -161.49(16) . . . . ? C16 C17 C18 C19 0.4(3) . . . . ? Fe2 C17 C18 C19 59.90(18) . . . . ? C16 C17 C18 Fe2 -59.49(18) . . . . ? C12 Fe2 C18 C17 165.3(3) . . . . ? C11 Fe2 C18 C17 -43.0(4) . . . . ? C16 Fe2 C18 C17 37.71(17) . . . . ? C15 Fe2 C18 C17 -77.01(19) . . . . ? C19 Fe2 C18 C17 118.8(2) . . . . ? C13 Fe2 C18 C17 -160.21(16) . . . . ? C20 Fe2 C18 C17 81.40(18) . . . . ? C14 Fe2 C18 C17 -118.64(17) . . . . ? C12 Fe2 C18 C19 46.5(3) . . . . ? C11 Fe2 C18 C19 -161.8(2) . . . . ? C17 Fe2 C18 C19 -118.8(2) . . . . ? C16 Fe2 C18 C19 -81.12(17) . . . . ? C15 Fe2 C18 C19 164.16(15) . . . . ? C13 Fe2 C18 C19 80.96(18) . . . . ? C20 Fe2 C18 C19 -37.43(16) . . . . ? C14 Fe2 C18 C19 122.53(16) . . . . ? C17 C18 C19 C20 -0.1(3) . . . . ? Fe2 C18 C19 C20 59.49(18) . . . . ? C17 C18 C19 Fe2 -59.59(18) . . . . ? C12 Fe2 C19 C20 79.32(18) . . . . ? C11 Fe2 C19 C20 42.2(3) . . . . ? C17 Fe2 C19 C20 -81.32(17) . . . . ? C18 Fe2 C19 C20 -119.3(2) . . . . ? C16 Fe2 C19 C20 -37.44(16) . . . . ? C15 Fe2 C19 C20 -160.1(3) . . . . ? C13 Fe2 C19 C20 122.56(15) . . . . ? C14 Fe2 C19 C20 164.64(15) . . . . ? C12 Fe2 C19 C18 -161.38(16) . . . . ? C11 Fe2 C19 C18 161.5(3) . . . . ? C17 Fe2 C19 C18 37.98(17) . . . . ? C16 Fe2 C19 C18 81.86(18) . . . . ? C15 Fe2 C19 C18 -40.8(4) . . . . ? C13 Fe2 C19 C18 -118.14(17) . . . . ? C20 Fe2 C19 C18 119.3(2) . . . . ? C14 Fe2 C19 C18 -76.06(19) . . . . ? C18 C19 C20 C16 -0.2(3) . . . . ? Fe2 C19 C20 C16 58.76(17) . . . . ? C18 C19 C20 Fe2 -59.00(18) . . . . ? C17 C16 C20 C19 0.5(3) . . . . ? Fe2 C16 C20 C19 -59.05(17) . . . . ? C17 C16 C20 Fe2 59.54(18) . . . . ? C12 Fe2 C20 C19 -119.39(16) . . . . ? C11 Fe2 C20 C19 -163.26(15) . . . . ? C17 Fe2 C20 C19 81.85(17) . . . . ? C18 Fe2 C20 C19 37.78(16) . . . . ? C16 Fe2 C20 C19 119.6(2) . . . . ? C15 Fe2 C20 C19 161.2(2) . . . . ? C13 Fe2 C20 C19 -76.98(18) . . . . ? C14 Fe2 C20 C19 -41.2(4) . . . . ? C12 Fe2 C20 C16 121.00(16) . . . . ? C11 Fe2 C20 C16 77.14(18) . . . . ? C17 Fe2 C20 C16 -37.76(16) . . . . ? C18 Fe2 C20 C16 -81.83(17) . . . . ? C15 Fe2 C20 C16 41.6(3) . . . . ? C19 Fe2 C20 C16 -119.6(2) . . . . ? C13 Fe2 C20 C16 163.41(15) . . . . ? C14 Fe2 C20 C16 -160.8(3) . . . . ? C14 C15 C11 C12 -0.1(3) . . . . ? Fe2 C15 C11 C12 59.01(16) . . . . ? C14 C15 C11 B2 -169.6(2) . . . . ? Fe2 C15 C11 B2 -110.4(3) . . . . ? C14 C15 C11 Fe2 -59.12(17) . . . . ? C13 C12 C11 C15 0.5(3) . . . . ? B2 C12 C11 C15 -169.0(2) 2_776 . . . ? Fe2 C12 C11 C15 -59.61(16) . . . . ? C13 C12 C11 B2 170.9(2) . . . . ? B2 C12 C11 B2 1.4(4) 2_776 . . . ? Fe2 C12 C11 B2 110.8(2) . . . . ? C13 C12 C11 Fe2 60.13(16) . . . . ? B2 C12 C11 Fe2 -109.4(2) 2_776 . . . ? O2 B2 C11 C15 -14.0(4) . . . . ? C12 B2 C11 C15 166.7(2) 2_776 . . . ? O2 B2 C11 C12 177.9(2) . . . . ? C12 B2 C11 C12 -1.4(4) 2_776 . . . ? O2 B2 C11 Fe2 -100.5(2) . . . . ? C12 B2 C11 Fe2 80.3(2) 2_776 . . . ? C12 Fe2 C11 C15 118.6(2) . . . . ? C17 Fe2 C11 C15 -77.72(17) . . . . ? C18 Fe2 C11 C15 -46.1(3) . . . . ? C16 Fe2 C11 C15 -119.39(15) . . . . ? C19 Fe2 C11 C15 168.2(3) . . . . ? C13 Fe2 C11 C15 80.33(15) . . . . ? C20 Fe2 C11 C15 -160.73(14) . . . . ? C14 Fe2 C11 C15 36.93(14) . . . . ? C17 Fe2 C11 C12 163.63(15) . . . . ? C18 Fe2 C11 C12 -164.7(3) . . . . ? C16 Fe2 C11 C12 121.96(15) . . . . ? C15 Fe2 C11 C12 -118.6(2) . . . . ? C19 Fe2 C11 C12 49.6(3) . . . . ? C13 Fe2 C11 C12 -38.32(13) . . . . ? C20 Fe2 C11 C12 80.63(16) . . . . ? C14 Fe2 C11 C12 -81.72(15) . . . . ? C12 Fe2 C11 B2 -116.2(2) . . . . ? C17 Fe2 C11 B2 47.5(2) . . . . ? C18 Fe2 C11 B2 79.1(3) . . . . ? C16 Fe2 C11 B2 5.8(2) . . . . ? C15 Fe2 C11 B2 125.2(2) . . . . ? C19 Fe2 C11 B2 -66.6(4) . . . . ? C13 Fe2 C11 B2 -154.5(2) . . . . ? C20 Fe2 C11 B2 -35.5(2) . . . . ? C14 Fe2 C11 B2 162.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O3 0.84 1.99 2.803(3) 162.0 2 O2 H2 O1 0.84 2.02 2.828(2) 161.4 1_666 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 67.93 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.709 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.068 # Attachment '- Fc2B2O2Me2.cif' data_fc2b2(OH)2_THF _database_code_depnum_ccdc_archive 'CCDC 892507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 B2 Fe2 O2, C4 H8 O' _chemical_formula_sum 'C24 H26 B2 Fe2 O3' _chemical_formula_weight 495.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.70780(10) _cell_length_b 10.87150(10) _cell_length_c 11.2219(2) _cell_angle_alpha 108.0850(10) _cell_angle_beta 99.0930(10) _cell_angle_gamma 115.6720(10) _cell_volume 1051.97(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5422 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 11.249 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3019 _exptl_absorpt_correction_T_max 0.5065 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8304 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.41 _diffrn_reflns_theta_max 67.19 _reflns_number_total 3460 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0398P)^2^+0.4405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3460 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Fe1 Fe 0.79452(3) 0.92445(3) 0.11508(3) 0.01469(10) Uani 1 1 d . . . Fe2 Fe 0.77143(3) 0.22954(3) 0.66669(3) 0.01488(10) Uani 1 1 d . . . O2 O 0.48415(16) 0.16977(17) 0.34791(15) 0.0200(3) Uani 1 1 d . . . H2 H 0.4014 0.1626 0.3300 0.030 Uiso 1 1 calc R . . O1 O 1.23275(16) 1.18531(17) 0.25972(14) 0.0201(3) Uani 1 1 d . . . H1 H 1.2088 1.2368 0.3133 0.030 Uiso 1 1 calc R . . O3 O 0.23186(19) 0.35324(19) 0.49442(16) 0.0306(4) Uani 1 1 d . . . B1 B 1.1214(3) 1.0991(3) 0.1380(2) 0.0179(5) Uani 1 1 d . . . B2 B 0.4886(3) 0.0915(3) 0.4213(2) 0.0165(5) Uani 1 1 d . . . C5 C 0.9111(2) 1.1556(2) 0.2001(2) 0.0188(5) Uani 1 1 d . . . H5 H 0.9629 1.2222 0.2977 0.023 Uiso 1 1 calc R . . C1 C 0.9739(2) 1.0973(2) 0.1103(2) 0.0162(4) Uani 1 1 d . . . C2 C 0.8589(2) 1.0032(2) -0.0211(2) 0.0174(4) Uani 1 1 d . . . C3 C 0.7294(2) 1.0076(2) -0.0072(2) 0.0197(5) Uani 1 1 d . . . H3 H 0.6320 0.9525 -0.0801 0.024 Uiso 1 1 calc R . . C4 C 0.7617(3) 1.1007(2) 0.1279(2) 0.0208(5) Uani 1 1 d . . . H4 H 0.6912 1.1219 0.1661 0.025 Uiso 1 1 calc R . . C6 C 0.6142(2) 0.7239(2) 0.0802(2) 0.0207(5) Uani 1 1 d . . . H6 H 0.5112 0.6800 0.0210 0.025 Uiso 1 1 calc R . . C10 C 0.7241(3) 0.6976(2) 0.0415(2) 0.0207(5) Uani 1 1 d . . . H10 H 0.7121 0.6327 -0.0501 0.025 Uiso 1 1 calc R . . C9 C 0.8545(3) 0.7816(2) 0.1551(2) 0.0207(5) Uani 1 1 d . . . H9 H 0.9500 0.7856 0.1577 0.025 Uiso 1 1 calc R . . C8 C 0.8253(2) 0.8594(2) 0.2644(2) 0.0200(5) Uani 1 1 d . . . H8 H 0.8968 0.9273 0.3574 0.024 Uiso 1 1 calc R . . C7 C 0.6775(2) 0.8244(2) 0.2188(2) 0.0195(5) Uani 1 1 d . . . H7 H 0.6265 0.8627 0.2740 0.023 Uiso 1 1 calc R . . C12 C 0.6436(2) 0.0048(2) 0.5429(2) 0.0154(4) Uani 1 1 d . . . C11 C 0.6335(2) 0.0941(2) 0.4723(2) 0.0162(4) Uani 1 1 d . . . C15 C 0.7798(2) 0.1891(2) 0.4771(2) 0.0165(4) Uani 1 1 d . . . H15 H 0.8079 0.2651 0.4390 0.020 Uiso 1 1 calc R . . C14 C 0.8792(2) 0.1612(2) 0.5480(2) 0.0171(4) Uani 1 1 d . . . H14 H 0.9882 0.2131 0.5676 0.021 Uiso 1 1 calc R . . C13 C 0.7963(2) 0.0478(2) 0.5881(2) 0.0169(4) Uani 1 1 d . . . H13 H 0.8376 0.0064 0.6406 0.020 Uiso 1 1 calc R . . C19 C 0.9297(3) 0.4198(3) 0.8342(2) 0.0260(5) Uani 1 1 d . . . H19 H 1.0387 0.4695 0.8544 0.031 Uiso 1 1 calc R . . C18 C 0.8430(3) 0.3044(3) 0.8703(2) 0.0230(5) Uani 1 1 d . . . H18 H 0.8804 0.2585 0.9204 0.028 Uiso 1 1 calc R . . C16 C 0.6877(3) 0.3563(3) 0.7567(2) 0.0237(5) Uani 1 1 d . . . H16 H 0.5969 0.3536 0.7133 0.028 Uiso 1 1 calc R . . C24 C 0.3641(3) 0.3772(3) 0.5794(2) 0.0257(5) Uani 1 1 d . . . H24A H 0.4434 0.4058 0.5405 0.031 Uiso 1 1 calc R . . H24B H 0.3450 0.2836 0.5887 0.031 Uiso 1 1 calc R . . C21 C 0.2195(3) 0.4821(3) 0.5545(3) 0.0299(6) Uani 1 1 d . . . H21A H 0.1153 0.4556 0.5271 0.036 Uiso 1 1 calc R . . H21B H 0.2775 0.5633 0.5292 0.036 Uiso 1 1 calc R . . C22 C 0.2812(3) 0.5311(3) 0.7038(3) 0.0329(6) Uani 1 1 d . . . H22A H 0.2070 0.4691 0.7351 0.039 Uiso 1 1 calc R . . H22B H 0.3153 0.6387 0.7550 0.039 Uiso 1 1 calc R . . C23 C 0.4105(3) 0.5036(3) 0.7155(2) 0.0275(5) Uani 1 1 d . . . H23A H 0.5032 0.5954 0.7327 0.033 Uiso 1 1 calc R . . H23B H 0.4241 0.4719 0.7879 0.033 Uiso 1 1 calc R . . C17 C 0.6944(3) 0.2659(2) 0.8231(2) 0.0213(5) Uani 1 1 d . . . H17 H 0.6087 0.1879 0.8338 0.026 Uiso 1 1 calc R . . C20 C 0.8336(3) 0.4521(2) 0.7644(2) 0.0266(5) Uani 1 1 d . . . H20 H 0.8633 0.5284 0.7266 0.032 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 Fe1 0.01267(18) 0.01731(18) 0.01397(17) 0.00712(14) 0.00440(14) 0.00735(14) Fe2 0.01226(18) 0.01518(18) 0.01354(17) 0.00470(14) 0.00302(14) 0.00557(14) O2 0.0124(8) 0.0251(8) 0.0228(8) 0.0143(7) 0.0034(7) 0.0080(7) O1 0.0173(8) 0.0234(8) 0.0168(7) 0.0077(6) 0.0032(6) 0.0096(6) O3 0.0312(10) 0.0321(9) 0.0233(8) 0.0047(7) 0.0018(8) 0.0194(8) B1 0.0170(13) 0.0191(12) 0.0196(12) 0.0135(10) 0.0065(10) 0.0072(10) B2 0.0170(13) 0.0136(11) 0.0112(11) 0.0013(9) 0.0007(10) 0.0058(10) C5 0.0186(12) 0.0163(10) 0.0214(11) 0.0090(9) 0.0075(10) 0.0080(9) C1 0.0162(11) 0.0157(10) 0.0162(10) 0.0090(9) 0.0049(9) 0.0065(9) C2 0.0158(11) 0.0219(11) 0.0176(11) 0.0128(9) 0.0058(9) 0.0092(9) C3 0.0169(12) 0.0244(11) 0.0222(11) 0.0140(10) 0.0059(10) 0.0116(10) C4 0.0213(12) 0.0219(11) 0.0267(12) 0.0131(10) 0.0112(10) 0.0143(10) C6 0.0166(11) 0.0200(11) 0.0213(11) 0.0092(9) 0.0051(9) 0.0062(9) C10 0.0256(13) 0.0161(11) 0.0199(11) 0.0073(9) 0.0080(10) 0.0105(9) C9 0.0205(12) 0.0225(11) 0.0249(11) 0.0143(10) 0.0074(10) 0.0129(10) C8 0.0195(12) 0.0226(11) 0.0179(11) 0.0117(9) 0.0038(9) 0.0097(9) C7 0.0200(12) 0.0216(11) 0.0221(11) 0.0136(9) 0.0120(10) 0.0103(9) C12 0.0152(11) 0.0140(10) 0.0113(9) 0.0023(8) 0.0013(9) 0.0061(9) C11 0.0167(11) 0.0191(10) 0.0114(9) 0.0058(8) 0.0042(9) 0.0087(9) C15 0.0181(11) 0.0161(10) 0.0131(10) 0.0057(8) 0.0058(9) 0.0071(9) C14 0.0140(11) 0.0199(11) 0.0159(10) 0.0057(9) 0.0058(9) 0.0085(9) C13 0.0165(11) 0.0188(10) 0.0148(10) 0.0061(9) 0.0042(9) 0.0097(9) C19 0.0189(12) 0.0237(12) 0.0158(11) -0.0033(9) 0.0023(10) 0.0046(10) C18 0.0225(12) 0.0299(12) 0.0124(10) 0.0046(9) 0.0033(9) 0.0141(10) C16 0.0260(13) 0.0242(12) 0.0218(11) 0.0047(10) 0.0078(10) 0.0171(10) C24 0.0243(13) 0.0311(13) 0.0226(12) 0.0132(10) 0.0050(10) 0.0148(11) C21 0.0254(13) 0.0255(12) 0.0360(14) 0.0120(11) 0.0070(11) 0.0129(11) C22 0.0328(15) 0.0246(13) 0.0340(14) 0.0072(11) 0.0142(12) 0.0117(11) C23 0.0293(14) 0.0216(12) 0.0241(12) 0.0094(10) 0.0042(11) 0.0090(10) C17 0.0204(12) 0.0244(12) 0.0159(11) 0.0051(9) 0.0083(10) 0.0106(10) C20 0.0364(15) 0.0157(11) 0.0207(11) 0.0028(9) 0.0092(11) 0.0113(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 C7 2.043(2) . ? Fe1 C2 2.044(2) . ? Fe1 C8 2.044(2) . ? Fe1 C1 2.047(2) . ? Fe1 C3 2.049(2) . ? Fe1 C5 2.050(2) . ? Fe1 C6 2.054(2) . ? Fe1 C9 2.057(2) . ? Fe1 C4 2.060(2) . ? Fe1 C10 2.064(2) . ? Fe2 C12 2.041(2) . ? Fe2 C13 2.049(2) . ? Fe2 C11 2.052(2) . ? Fe2 C16 2.053(2) . ? Fe2 C18 2.055(2) . ? Fe2 C19 2.056(2) . ? Fe2 C20 2.056(2) . ? Fe2 C17 2.056(2) . ? Fe2 C15 2.060(2) . ? Fe2 C14 2.067(2) . ? O2 B2 1.364(3) . ? O2 H2 0.8400 . ? O1 B1 1.374(3) . ? O1 H1 0.8400 . ? O3 C21 1.427(3) . ? O3 C24 1.443(3) . ? B1 C2 1.545(3) 2_775 ? B1 C1 1.551(3) . ? B2 C11 1.551(3) . ? B2 C12 1.555(3) 2_656 ? C5 C4 1.426(3) . ? C5 C1 1.435(3) . ? C5 H5 1.0000 . ? C1 C2 1.461(3) . ? C2 C3 1.440(3) . ? C2 B1 1.545(3) 2_775 ? C3 C4 1.421(3) . ? C3 H3 1.0000 . ? C4 H4 1.0000 . ? C6 C10 1.426(3) . ? C6 C7 1.429(3) . ? C6 H6 1.0000 . ? C10 C9 1.420(3) . ? C10 H10 1.0000 . ? C9 C8 1.422(3) . ? C9 H9 1.0000 . ? C8 C7 1.419(3) . ? C8 H8 1.0000 . ? C7 H7 1.0000 . ? C12 C13 1.441(3) . ? C12 C11 1.458(3) . ? C12 B2 1.555(3) 2_656 ? C11 C15 1.436(3) . ? C15 C14 1.421(3) . ? C15 H15 1.0000 . ? C14 C13 1.426(3) . ? C14 H14 1.0000 . ? C13 H13 1.0000 . ? C19 C18 1.424(3) . ? C19 C20 1.423(3) . ? C19 H19 1.0000 . ? C18 C17 1.417(3) . ? C18 H18 1.0000 . ? C16 C17 1.422(3) . ? C16 C20 1.423(3) . ? C16 H16 1.0000 . ? C24 C23 1.528(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C21 C22 1.523(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.532(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C17 H17 1.0000 . ? C20 H20 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Fe1 C2 165.31(9) . . ? C7 Fe1 C8 40.62(9) . . ? C2 Fe1 C8 153.31(9) . . ? C7 Fe1 C1 150.75(9) . . ? C2 Fe1 C1 41.83(8) . . ? C8 Fe1 C1 117.94(9) . . ? C7 Fe1 C3 126.28(9) . . ? C2 Fe1 C3 41.19(8) . . ? C8 Fe1 C3 163.93(9) . . ? C1 Fe1 C3 69.43(8) . . ? C7 Fe1 C5 116.39(9) . . ? C2 Fe1 C5 69.35(8) . . ? C8 Fe1 C5 106.95(9) . . ? C1 Fe1 C5 41.00(8) . . ? C3 Fe1 C5 68.46(9) . . ? C7 Fe1 C6 40.84(9) . . ? C2 Fe1 C6 128.03(9) . . ? C8 Fe1 C6 68.37(9) . . ? C1 Fe1 C6 167.42(9) . . ? C3 Fe1 C6 107.55(9) . . ? C5 Fe1 C6 150.43(9) . . ? C7 Fe1 C9 68.33(9) . . ? C2 Fe1 C9 119.94(9) . . ? C8 Fe1 C9 40.57(9) . . ? C1 Fe1 C9 108.83(9) . . ? C3 Fe1 C9 153.97(9) . . ? C5 Fe1 C9 128.22(9) . . ? C6 Fe1 C9 68.19(9) . . ? C7 Fe1 C4 105.91(9) . . ? C2 Fe1 C4 69.02(9) . . ? C8 Fe1 C4 126.26(9) . . ? C1 Fe1 C4 69.00(9) . . ? C3 Fe1 C4 40.45(9) . . ? C5 Fe1 C4 40.60(9) . . ? C6 Fe1 C4 117.16(9) . . ? C9 Fe1 C4 165.01(9) . . ? C7 Fe1 C10 68.30(9) . . ? C2 Fe1 C10 109.32(9) . . ? C8 Fe1 C10 68.05(9) . . ? C1 Fe1 C10 129.48(9) . . ? C3 Fe1 C10 119.68(9) . . ? C5 Fe1 C10 166.94(9) . . ? C6 Fe1 C10 40.52(9) . . ? C9 Fe1 C10 40.32(9) . . ? C4 Fe1 C10 152.06(9) . . ? C12 Fe2 C13 41.24(8) . . ? C12 Fe2 C11 41.72(8) . . ? C13 Fe2 C11 69.25(8) . . ? C12 Fe2 C16 123.15(9) . . ? C13 Fe2 C16 159.78(9) . . ? C11 Fe2 C16 107.63(9) . . ? C12 Fe2 C18 121.17(9) . . ? C13 Fe2 C18 106.89(9) . . ? C11 Fe2 C18 158.08(9) . . ? C16 Fe2 C18 68.13(9) . . ? C12 Fe2 C19 157.18(9) . . ? C13 Fe2 C19 121.57(9) . . ? C11 Fe2 C19 159.89(9) . . ? C16 Fe2 C19 68.25(10) . . ? C18 Fe2 C19 40.53(9) . . ? C12 Fe2 C20 160.18(9) . . ? C13 Fe2 C20 157.71(10) . . ? C11 Fe2 C20 123.65(9) . . ? C16 Fe2 C20 40.53(10) . . ? C18 Fe2 C20 68.04(9) . . ? C19 Fe2 C20 40.51(10) . . ? C12 Fe2 C17 106.81(9) . . ? C13 Fe2 C17 123.18(9) . . ? C11 Fe2 C17 122.55(9) . . ? C16 Fe2 C17 40.48(9) . . ? C18 Fe2 C17 40.31(9) . . ? C19 Fe2 C17 67.98(9) . . ? C20 Fe2 C17 67.92(9) . . ? C12 Fe2 C15 69.13(8) . . ? C13 Fe2 C15 68.10(8) . . ? C11 Fe2 C15 40.88(8) . . ? C16 Fe2 C15 123.42(9) . . ? C18 Fe2 C15 159.41(9) . . ? C19 Fe2 C15 123.68(9) . . ? C20 Fe2 C15 108.57(9) . . ? C17 Fe2 C15 159.12(9) . . ? C12 Fe2 C14 69.16(8) . . ? C13 Fe2 C14 40.54(8) . . ? C11 Fe2 C14 68.85(8) . . ? C16 Fe2 C14 158.62(9) . . ? C18 Fe2 C14 123.07(9) . . ? C19 Fe2 C14 107.39(9) . . ? C20 Fe2 C14 122.63(9) . . ? C17 Fe2 C14 159.22(9) . . ? C15 Fe2 C14 40.27(8) . . ? B2 O2 H2 109.5 . . ? B1 O1 H1 109.5 . . ? C21 O3 C24 107.67(17) . . ? O1 B1 C2 119.3(2) . 2_775 ? O1 B1 C1 123.5(2) . . ? C2 B1 C1 117.15(19) 2_775 . ? O2 B2 C11 119.1(2) . . ? O2 B2 C12 124.7(2) . 2_656 ? C11 B2 C12 116.14(19) . 2_656 ? C4 C5 C1 108.83(19) . . ? C4 C5 Fe1 70.07(12) . . ? C1 C5 Fe1 69.40(12) . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C5 C1 C2 107.12(19) . . ? C5 C1 B1 130.67(19) . . ? C2 C1 B1 121.29(19) . . ? C5 C1 Fe1 69.60(12) . . ? C2 C1 Fe1 68.98(11) . . ? B1 C1 Fe1 117.96(14) . . ? C3 C2 C1 107.08(19) . . ? C3 C2 B1 130.4(2) . 2_775 ? C1 C2 B1 121.56(19) . 2_775 ? C3 C2 Fe1 69.61(12) . . ? C1 C2 Fe1 69.19(11) . . ? B1 C2 Fe1 117.69(14) 2_775 . ? C4 C3 C2 108.75(19) . . ? C4 C3 Fe1 70.15(12) . . ? C2 C3 Fe1 69.21(12) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 125.6 . . ? C3 C4 C5 108.22(19) . . ? C3 C4 Fe1 69.39(12) . . ? C5 C4 Fe1 69.33(12) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 125.9 . . ? C10 C6 C7 107.7(2) . . ? C10 C6 Fe1 70.13(12) . . ? C7 C6 Fe1 69.19(12) . . ? C10 C6 H6 126.1 . . ? C7 C6 H6 126.1 . . ? Fe1 C6 H6 126.1 . . ? C9 C10 C6 108.13(19) . . ? C9 C10 Fe1 69.58(12) . . ? C6 C10 Fe1 69.35(12) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe1 C10 H10 125.9 . . ? C10 C9 C8 107.9(2) . . ? C10 C9 Fe1 70.10(12) . . ? C8 C9 Fe1 69.22(12) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe1 C9 H9 126.0 . . ? C7 C8 C9 108.32(19) . . ? C7 C8 Fe1 69.66(12) . . ? C9 C8 Fe1 70.21(12) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe1 C8 H8 125.8 . . ? C8 C7 C6 107.88(19) . . ? C8 C7 Fe1 69.72(12) . . ? C6 C7 Fe1 69.97(12) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe1 C7 H7 126.1 . . ? C13 C12 C11 107.04(18) . . ? C13 C12 B2 130.51(19) . 2_656 ? C11 C12 B2 121.50(19) . 2_656 ? C13 C12 Fe2 69.69(12) . . ? C11 C12 Fe2 69.54(11) . . ? B2 C12 Fe2 117.15(14) 2_656 . ? C15 C11 C12 107.04(18) . . ? C15 C11 B2 130.27(19) . . ? C12 C11 B2 122.27(19) . . ? C15 C11 Fe2 69.84(12) . . ? C12 C11 Fe2 68.73(11) . . ? B2 C11 Fe2 120.70(14) . . ? C14 C15 C11 109.23(18) . . ? C14 C15 Fe2 70.15(12) . . ? C11 C15 Fe2 69.28(12) . . ? C14 C15 H15 125.4 . . ? C11 C15 H15 125.4 . . ? Fe2 C15 H15 125.4 . . ? C15 C14 C13 107.84(18) . . ? C15 C14 Fe2 69.59(12) . . ? C13 C14 Fe2 69.07(12) . . ? C15 C14 H14 126.1 . . ? C13 C14 H14 126.1 . . ? Fe2 C14 H14 126.1 . . ? C14 C13 C12 108.84(18) . . ? C14 C13 Fe2 70.40(12) . . ? C12 C13 Fe2 69.07(12) . . ? C14 C13 H13 125.6 . . ? C12 C13 H13 125.6 . . ? Fe2 C13 H13 125.6 . . ? C18 C19 C20 107.8(2) . . ? C18 C19 Fe2 69.72(13) . . ? C20 C19 Fe2 69.76(12) . . ? C18 C19 H19 126.1 . . ? C20 C19 H19 126.1 . . ? Fe2 C19 H19 126.1 . . ? C17 C18 C19 108.1(2) . . ? C17 C18 Fe2 69.88(12) . . ? C19 C18 Fe2 69.75(13) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? Fe2 C18 H18 126.0 . . ? C17 C16 C20 107.7(2) . . ? C17 C16 Fe2 69.86(12) . . ? C20 C16 Fe2 69.83(13) . . ? C17 C16 H16 126.2 . . ? C20 C16 H16 126.2 . . ? Fe2 C16 H16 126.2 . . ? O3 C24 C23 107.70(19) . . ? O3 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? O3 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? O3 C21 C22 104.40(19) . . ? O3 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? O3 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? C21 C22 C23 102.3(2) . . ? C21 C22 H22A 111.3 . . ? C23 C22 H22A 111.3 . . ? C21 C22 H22B 111.3 . . ? C23 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? C24 C23 C22 103.38(19) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? C18 C17 C16 108.3(2) . . ? C18 C17 Fe2 69.81(12) . . ? C16 C17 Fe2 69.66(12) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? Fe2 C17 H17 125.8 . . ? C19 C20 C16 108.1(2) . . ? C19 C20 Fe2 69.73(13) . . ? C16 C20 Fe2 69.64(12) . . ? C19 C20 H20 125.9 . . ? C16 C20 H20 125.9 . . ? Fe2 C20 H20 125.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 2.00 2.813(2) 162.4 1_445 O1 H1 O3 0.84 1.94 2.703(2) 150.4 1_665 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 67.19 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.375 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.052 # Attachment '- Fc2B2O2H2_acetone.cif' data_Fc2B2(OMe)2 _database_code_depnum_ccdc_archive 'CCDC 892853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 B2 Fe2 O2' _chemical_formula_sum 'C22 H22 B2 Fe2 O2' _chemical_formula_weight 451.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1632(3) _cell_length_b 11.6968(4) _cell_length_c 16.2939(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.347(2) _cell_angle_gamma 90.00 _cell_volume 1876.56(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6654 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 67.41 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 12.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1222 _exptl_absorpt_correction_T_max 0.1787 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10060 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.67 _diffrn_reflns_theta_max 67.55 _reflns_number_total 3244 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0425P)^2^+1.1855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3244 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Fe2 Fe 1.06391(3) 0.44151(3) 0.16490(2) 0.00889(11) Uani 1 1 d . . . Fe1 Fe 0.76740(3) -0.00808(3) 0.07301(2) 0.00828(11) Uani 1 1 d . . . B2 B 0.8471(3) 0.4767(2) -0.00999(16) 0.0123(5) Uani 1 1 d . . . B1 B 0.4920(2) 0.1109(2) 0.05033(15) 0.0093(5) Uani 1 1 d . . . O1 O 0.47275(14) 0.20066(13) 0.09918(9) 0.0115(3) Uani 1 1 d . . . O2 O 0.71251(16) 0.46840(15) -0.01112(10) 0.0172(4) Uani 1 1 d . . . C1 C 0.6114(2) 0.09125(18) 0.00785(13) 0.0094(4) Uani 1 1 d . . . C2 C 0.6182(2) -0.01575(18) -0.03711(14) 0.0100(4) Uani 1 1 d . . . C3 C 0.7491(2) -0.02021(19) -0.05564(14) 0.0114(4) Uani 1 1 d . . . H3 H 0.7839 -0.0844 -0.0849 0.014 Uiso 1 1 calc R . . C4 C 0.8222(2) 0.08006(19) -0.02330(13) 0.0115(4) Uani 1 1 d . . . H4 H 0.9171 0.0986 -0.0260 0.014 Uiso 1 1 calc R . . C5 C 0.7385(2) 0.14855(18) 0.01544(13) 0.0098(4) Uani 1 1 d . . . H5 H 0.7648 0.2237 0.0441 0.012 Uiso 1 1 calc R . . C10 C 0.8329(2) 0.0158(2) 0.20139(14) 0.0173(5) Uani 1 1 d . . . H10 H 0.8371 0.0904 0.2319 0.021 Uiso 1 1 calc R . . C9 C 0.9380(2) -0.0325(2) 0.16863(16) 0.0201(5) Uani 1 1 d . . . H9 H 1.0293 0.0019 0.1723 0.024 Uiso 1 1 calc R . . C8 C 0.8905(2) -0.1388(2) 0.13048(16) 0.0192(5) Uani 1 1 d . . . H8 H 0.9425 -0.1919 0.1021 0.023 Uiso 1 1 calc R . . C7 C 0.7568(2) -0.1566(2) 0.13911(15) 0.0165(5) Uani 1 1 d . . . H7 H 0.6978 -0.2241 0.1178 0.020 Uiso 1 1 calc R . . C6 C 0.7205(2) -0.0607(2) 0.18251(14) 0.0153(5) Uani 1 1 d . . . H6 H 0.6317 -0.0491 0.1973 0.018 Uiso 1 1 calc R . . C21 C 0.5681(2) 0.2915(2) 0.12517(16) 0.0175(5) Uani 1 1 d . . . H21A H 0.6560 0.2597 0.1554 0.026 Uiso 1 1 calc R . . H21B H 0.5349 0.3435 0.1627 0.026 Uiso 1 1 calc R . . H21C H 0.5788 0.3335 0.0752 0.026 Uiso 1 1 calc R . . C11 C 0.9398(2) 0.53493(19) 0.06978(14) 0.0128(5) Uani 1 1 d . . . C15 C 0.9085(2) 0.55911(19) 0.14879(14) 0.0142(5) Uani 1 1 d . . . H15 H 0.8187 0.5458 0.1619 0.017 Uiso 1 1 calc R . . C14 C 1.0264(2) 0.60188(19) 0.20642(15) 0.0163(5) Uani 1 1 d . . . H14 H 1.0337 0.6244 0.2666 0.020 Uiso 1 1 calc R . . C13 C 1.1328(2) 0.60516(19) 0.16439(14) 0.0147(5) Uani 1 1 d . . . H13 H 1.2278 0.6312 0.1900 0.018 Uiso 1 1 calc R . . C12 C 1.0824(2) 0.56353(19) 0.07942(14) 0.0128(5) Uani 1 1 d . . . C16 C 1.0504(2) 0.27315(19) 0.12987(16) 0.0162(5) Uani 1 1 d . . . H16 H 1.0000 0.2421 0.0737 0.019 Uiso 1 1 calc R . . C20 C 0.9965(2) 0.29012(19) 0.20153(15) 0.0161(5) Uani 1 1 d . . . H20 H 0.9014 0.2730 0.2046 0.019 Uiso 1 1 calc R . . C19 C 1.1018(2) 0.3358(2) 0.26839(15) 0.0177(5) Uani 1 1 d . . . H19 H 1.0938 0.3565 0.3265 0.021 Uiso 1 1 calc R . . C18 C 1.2198(2) 0.3466(2) 0.23735(16) 0.0192(5) Uani 1 1 d . . . H18 H 1.3096 0.3771 0.2698 0.023 Uiso 1 1 calc R . . C17 C 1.1886(2) 0.30791(19) 0.15228(16) 0.0186(5) Uani 1 1 d . . . H17 H 1.2525 0.3062 0.1144 0.022 Uiso 1 1 calc R . . C22 C 0.6138(2) 0.4228(2) -0.08225(16) 0.0216(5) Uani 1 1 d . . . H22A H 0.6154 0.4668 -0.1332 0.032 Uiso 1 1 calc R . . H22B H 0.5233 0.4278 -0.0715 0.032 Uiso 1 1 calc R . . H22C H 0.6353 0.3426 -0.0907 0.032 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 Fe2 0.00881(18) 0.00725(18) 0.00939(18) -0.00059(12) -0.00009(13) 0.00059(12) Fe1 0.00483(18) 0.00919(18) 0.01032(19) 0.00142(12) 0.00090(13) 0.00087(12) B2 0.0145(12) 0.0101(12) 0.0109(12) 0.0046(10) 0.0003(10) 0.0002(10) B1 0.0058(11) 0.0118(12) 0.0079(12) 0.0031(9) -0.0025(9) 0.0024(9) O1 0.0089(7) 0.0119(8) 0.0135(8) -0.0039(6) 0.0024(6) -0.0015(6) O2 0.0123(8) 0.0222(9) 0.0164(9) 0.0008(7) 0.0020(6) -0.0005(7) C1 0.0077(10) 0.0102(10) 0.0081(10) 0.0017(8) -0.0018(8) 0.0013(8) C2 0.0081(10) 0.0108(11) 0.0111(11) 0.0009(8) 0.0023(8) 0.0018(8) C3 0.0102(11) 0.0140(11) 0.0100(11) 0.0017(9) 0.0023(8) 0.0015(9) C4 0.0092(10) 0.0146(11) 0.0111(11) 0.0026(9) 0.0030(8) -0.0001(8) C5 0.0081(10) 0.0096(11) 0.0109(11) 0.0027(8) 0.0012(8) 0.0005(8) C10 0.0198(12) 0.0189(12) 0.0090(11) 0.0040(9) -0.0045(9) -0.0008(10) C9 0.0103(11) 0.0251(13) 0.0211(13) 0.0113(11) -0.0031(9) 0.0013(10) C8 0.0172(12) 0.0184(12) 0.0232(13) 0.0118(10) 0.0070(10) 0.0108(10) C7 0.0191(12) 0.0128(11) 0.0165(12) 0.0072(9) 0.0021(9) 0.0007(9) C6 0.0156(11) 0.0207(12) 0.0099(11) 0.0066(9) 0.0035(9) 0.0009(9) C21 0.0163(12) 0.0147(12) 0.0223(13) -0.0080(10) 0.0065(10) -0.0039(9) C11 0.0137(11) 0.0120(11) 0.0125(11) 0.0036(9) 0.0030(9) 0.0042(9) C15 0.0179(12) 0.0128(11) 0.0112(11) 0.0017(9) 0.0023(9) 0.0072(9) C14 0.0279(13) 0.0074(11) 0.0131(11) 0.0003(9) 0.0045(10) 0.0042(9) C13 0.0212(12) 0.0069(11) 0.0142(12) -0.0006(9) 0.0010(9) -0.0017(9) C12 0.0164(11) 0.0106(11) 0.0098(11) 0.0028(8) 0.0005(9) -0.0002(9) C16 0.0147(11) 0.0102(11) 0.0217(13) -0.0042(9) 0.0006(9) -0.0008(9) C20 0.0135(11) 0.0094(11) 0.0242(13) 0.0020(9) 0.0026(9) -0.0020(9) C19 0.0236(13) 0.0120(11) 0.0148(12) 0.0058(9) -0.0006(9) 0.0015(9) C18 0.0113(11) 0.0121(12) 0.0278(14) 0.0017(10) -0.0075(10) 0.0008(9) C17 0.0135(11) 0.0098(11) 0.0325(14) -0.0001(10) 0.0059(10) 0.0037(9) C22 0.0136(12) 0.0280(14) 0.0199(13) 0.0021(11) -0.0021(10) -0.0033(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 Fe2 C12 2.035(2) . ? Fe2 C20 2.041(2) . ? Fe2 C13 2.039(2) . ? Fe2 C16 2.045(2) . ? Fe2 C19 2.049(2) . ? Fe2 C18 2.052(2) . ? Fe2 C11 2.054(2) . ? Fe2 C17 2.054(2) . ? Fe2 C15 2.062(2) . ? Fe2 C14 2.061(2) . ? Fe1 C1 2.039(2) . ? Fe1 C9 2.044(2) . ? Fe1 C2 2.044(2) . ? Fe1 C5 2.046(2) . ? Fe1 C8 2.049(2) . ? Fe1 C10 2.051(2) . ? Fe1 C6 2.052(2) . ? Fe1 C7 2.060(2) . ? Fe1 C3 2.063(2) . ? Fe1 C4 2.066(2) . ? B2 O2 1.367(3) . ? B2 C12 1.554(3) 3_765 ? B2 C11 1.560(3) . ? B1 O1 1.360(3) . ? B1 C2 1.556(3) 3_655 ? B1 C1 1.556(3) . ? O1 C21 1.430(3) . ? O2 C22 1.435(3) . ? C1 C5 1.433(3) . ? C1 C2 1.460(3) . ? C2 C3 1.436(3) . ? C2 B1 1.556(3) 3_655 ? C3 C4 1.418(3) . ? C3 H3 1.0000 . ? C4 C5 1.425(3) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C10 C6 1.423(3) . ? C10 C9 1.424(4) . ? C10 H10 1.0000 . ? C9 C8 1.420(4) . ? C9 H9 1.0000 . ? C8 C7 1.416(3) . ? C8 H8 1.0000 . ? C7 C6 1.422(3) . ? C7 H7 1.0000 . ? C6 H6 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C11 C15 1.429(3) . ? C11 C12 1.458(3) . ? C15 C14 1.418(3) . ? C15 H15 1.0000 . ? C14 C13 1.416(3) . ? C14 H14 1.0000 . ? C13 C12 1.437(3) . ? C13 H13 1.0000 . ? C12 B2 1.554(3) 3_765 ? C16 C17 1.421(3) . ? C16 C20 1.421(3) . ? C16 H16 1.0000 . ? C20 C19 1.428(3) . ? C20 H20 1.0000 . ? C19 C18 1.418(3) . ? C19 H19 1.0000 . ? C18 C17 1.417(4) . ? C18 H18 1.0000 . ? C17 H17 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Fe2 C20 154.61(9) . . ? C12 Fe2 C13 41.30(9) . . ? C20 Fe2 C13 163.02(10) . . ? C12 Fe2 C16 119.70(9) . . ? C20 Fe2 C16 40.70(10) . . ? C13 Fe2 C16 154.45(10) . . ? C12 Fe2 C19 162.92(9) . . ? C20 Fe2 C19 40.89(9) . . ? C13 Fe2 C19 125.10(9) . . ? C16 Fe2 C19 68.58(10) . . ? C12 Fe2 C18 125.74(10) . . ? C20 Fe2 C18 68.25(9) . . ? C13 Fe2 C18 107.07(9) . . ? C16 Fe2 C18 68.19(9) . . ? C19 Fe2 C18 40.46(10) . . ? C12 Fe2 C11 41.78(9) . . ? C20 Fe2 C11 119.63(9) . . ? C13 Fe2 C11 69.19(9) . . ? C16 Fe2 C11 108.38(9) . . ? C19 Fe2 C11 153.76(9) . . ? C18 Fe2 C11 164.67(10) . . ? C12 Fe2 C17 107.52(10) . . ? C20 Fe2 C17 68.25(9) . . ? C13 Fe2 C17 119.52(9) . . ? C16 Fe2 C17 40.56(9) . . ? C19 Fe2 C17 68.20(10) . . ? C18 Fe2 C17 40.38(10) . . ? C11 Fe2 C17 127.45(10) . . ? C12 Fe2 C15 69.07(9) . . ? C20 Fe2 C15 108.31(9) . . ? C13 Fe2 C15 68.04(9) . . ? C16 Fe2 C15 127.62(9) . . ? C19 Fe2 C15 119.28(10) . . ? C18 Fe2 C15 153.17(10) . . ? C11 Fe2 C15 40.62(9) . . ? C17 Fe2 C15 165.26(10) . . ? C12 Fe2 C14 69.05(9) . . ? C20 Fe2 C14 126.22(10) . . ? C13 Fe2 C14 40.41(9) . . ? C16 Fe2 C14 164.27(10) . . ? C19 Fe2 C14 106.93(9) . . ? C18 Fe2 C14 118.86(10) . . ? C11 Fe2 C14 68.57(9) . . ? C17 Fe2 C14 153.35(10) . . ? C15 Fe2 C14 40.23(9) . . ? C1 Fe1 C9 151.66(10) . . ? C1 Fe1 C2 41.92(8) . . ? C9 Fe1 C2 165.40(10) . . ? C1 Fe1 C5 41.08(8) . . ? C9 Fe1 C5 118.23(9) . . ? C2 Fe1 C5 69.26(8) . . ? C1 Fe1 C8 166.20(10) . . ? C9 Fe1 C8 40.59(10) . . ? C2 Fe1 C8 127.19(10) . . ? C5 Fe1 C8 151.58(9) . . ? C1 Fe1 C10 117.89(9) . . ? C9 Fe1 C10 40.70(10) . . ? C2 Fe1 C10 152.13(9) . . ? C5 Fe1 C10 108.62(9) . . ? C8 Fe1 C10 68.18(10) . . ? C1 Fe1 C6 107.80(9) . . ? C9 Fe1 C6 68.36(10) . . ? C2 Fe1 C6 117.94(9) . . ? C5 Fe1 C6 129.01(9) . . ? C8 Fe1 C6 68.04(9) . . ? C10 Fe1 C6 40.59(9) . . ? C1 Fe1 C7 128.17(9) . . ? C9 Fe1 C7 68.17(10) . . ? C2 Fe1 C7 107.36(9) . . ? C5 Fe1 C7 166.98(9) . . ? C8 Fe1 C7 40.31(9) . . ? C10 Fe1 C7 68.12(10) . . ? C6 Fe1 C7 40.46(9) . . ? C1 Fe1 C3 69.34(9) . . ? C9 Fe1 C3 127.66(10) . . ? C2 Fe1 C3 40.93(8) . . ? C5 Fe1 C3 68.23(9) . . ? C8 Fe1 C3 107.70(9) . . ? C10 Fe1 C3 166.05(9) . . ? C6 Fe1 C3 151.76(9) . . ? C7 Fe1 C3 118.03(9) . . ? C1 Fe1 C4 68.97(8) . . ? C9 Fe1 C4 108.14(9) . . ? C2 Fe1 C4 68.66(9) . . ? C5 Fe1 C4 40.53(8) . . ? C8 Fe1 C4 118.05(9) . . ? C10 Fe1 C4 128.78(9) . . ? C6 Fe1 C4 167.02(9) . . ? C7 Fe1 C4 151.22(9) . . ? C3 Fe1 C4 40.18(9) . . ? O2 B2 C12 127.5(2) . 3_765 ? O2 B2 C11 115.9(2) . . ? C12 B2 C11 116.5(2) 3_765 . ? O1 B1 C2 115.44(19) . 3_655 ? O1 B1 C1 128.0(2) . . ? C2 B1 C1 116.52(19) 3_655 . ? B1 O1 C21 124.14(17) . . ? B2 O2 C22 122.30(19) . . ? C5 C1 C2 106.89(18) . . ? C5 C1 B1 132.7(2) . . ? C2 C1 B1 119.28(19) . . ? C5 C1 Fe1 69.74(12) . . ? C2 C1 Fe1 69.24(12) . . ? B1 C1 Fe1 116.37(14) . . ? C3 C2 C1 107.33(19) . . ? C3 C2 B1 128.1(2) . 3_655 ? C1 C2 B1 124.11(19) . 3_655 ? C3 C2 Fe1 70.24(12) . . ? C1 C2 Fe1 68.84(12) . . ? B1 C2 Fe1 120.32(15) 3_655 . ? C4 C3 C2 108.62(19) . . ? C4 C3 Fe1 70.03(12) . . ? C2 C3 Fe1 68.83(12) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? Fe1 C3 H3 125.7 . . ? C3 C4 C5 108.31(19) . . ? C3 C4 Fe1 69.79(12) . . ? C5 C4 Fe1 68.97(12) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 108.85(19) . . ? C4 C5 Fe1 70.49(12) . . ? C1 C5 Fe1 69.18(12) . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C6 C10 C9 107.8(2) . . ? C6 C10 Fe1 69.74(13) . . ? C9 C10 Fe1 69.38(14) . . ? C6 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.1 . . ? C8 C9 C10 107.8(2) . . ? C8 C9 Fe1 69.92(13) . . ? C10 C9 Fe1 69.93(13) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.1 . . ? C7 C8 C9 108.4(2) . . ? C7 C8 Fe1 70.26(13) . . ? C9 C8 Fe1 69.49(13) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe1 C8 H8 125.8 . . ? C8 C7 C6 107.9(2) . . ? C8 C7 Fe1 69.42(13) . . ? C6 C7 Fe1 69.45(13) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe1 C7 H7 126.1 . . ? C7 C6 C10 108.1(2) . . ? C7 C6 Fe1 70.09(13) . . ? C10 C6 Fe1 69.67(13) . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? Fe1 C6 H6 126.0 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C11 C12 107.1(2) . . ? C15 C11 B2 127.9(2) . . ? C12 C11 B2 124.7(2) . . ? C15 C11 Fe2 69.97(12) . . ? C12 C11 Fe2 68.42(12) . . ? B2 C11 Fe2 121.83(16) . . ? C14 C15 C11 109.1(2) . . ? C14 C15 Fe2 69.88(13) . . ? C11 C15 Fe2 69.41(13) . . ? C14 C15 H15 125.5 . . ? C11 C15 H15 125.5 . . ? Fe2 C15 H15 125.5 . . ? C15 C14 C13 108.1(2) . . ? C15 C14 Fe2 69.89(13) . . ? C13 C14 Fe2 68.94(13) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Fe2 C14 H14 126.0 . . ? C14 C13 C12 108.9(2) . . ? C14 C13 Fe2 70.65(13) . . ? C12 C13 Fe2 69.21(12) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Fe2 C13 H13 125.5 . . ? C13 C12 C11 106.8(2) . . ? C13 C12 B2 133.3(2) . 3_765 ? C11 C12 B2 118.5(2) . 3_765 ? C13 C12 Fe2 69.49(12) . . ? C11 C12 Fe2 69.80(12) . . ? B2 C12 Fe2 115.05(15) 3_765 . ? C17 C16 C20 107.9(2) . . ? C17 C16 Fe2 70.06(13) . . ? C20 C16 Fe2 69.46(13) . . ? C17 C16 H16 126.1 . . ? C20 C16 H16 126.1 . . ? Fe2 C16 H16 126.1 . . ? C16 C20 C19 108.1(2) . . ? C16 C20 Fe2 69.83(13) . . ? C19 C20 Fe2 69.87(13) . . ? C16 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? Fe2 C20 H20 125.9 . . ? C18 C19 C20 107.5(2) . . ? C18 C19 Fe2 69.88(13) . . ? C20 C19 Fe2 69.24(13) . . ? C18 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? Fe2 C19 H19 126.2 . . ? C17 C18 C19 108.5(2) . . ? C17 C18 Fe2 69.90(13) . . ? C19 C18 Fe2 69.66(13) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? Fe2 C18 H18 125.8 . . ? C18 C17 C16 108.0(2) . . ? C18 C17 Fe2 69.71(13) . . ? C16 C17 Fe2 69.38(13) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Fe2 C17 H17 126.0 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 67.55 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.367 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.066