Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name S.Aldridge _publ_contact_author_address ; School of Chemistry Cardiff University Main Building Park Place Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email ALDRIDGES@CARDIFF.AC.UK _publ_section_title ; Fluoride anion binding by cyclic boronic esters: influence of backbone chelate on receptor integrity ; loop_ _publ_author_name S.Aldridge C.Bresner 'Simon J. Coles' 'Natalie D. Coombs' 'Joanne K. Day' 'Ian Fallis' ; M.B.Hursthouse ; # Attachment '3a.cif' data_sa0523 _database_code_depnum_ccdc_archive 'CCDC 604014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0523 _chemical_melting_point ? _chemical_formula_moiety 'C12 H13 B Fe O2' _chemical_formula_sum 'C12 H13 B Fe O2' _chemical_formula_weight 255.88 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' 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p 21 21 21' 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' _cell_length_a 5.81790(10) _cell_length_b 9.9233(2) _cell_length_c 18.4741(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1066.56(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5949 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4892 _exptl_absorpt_correction_T_max 0.7684 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8431 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 26.36 _reflns_number_total 2138 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997' _computing_structure_solution 'Sir-92 (A.Altomare et al. 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0453P)^2^+0.4391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 2138 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C -0.1112(5) 0.9587(3) 0.76820(14) 0.0204(5) Uani 1 1 d . . . H1 H -0.2469 0.9004 0.7570 0.024 Uiso 1 1 calc R . . C2 C -0.1055(5) 1.0649(3) 0.81993(14) 0.0195(5) Uani 1 1 d . . . H2 H -0.2367 1.0939 0.8512 0.023 Uiso 1 1 calc R . . C3 C 0.1221(5) 1.1231(3) 0.82010(14) 0.0196(5) Uani 1 1 d . . . C4 C 0.2535(5) 1.0480(3) 0.76775(14) 0.0216(6) Uani 1 1 d . . . H4 H 0.4192 1.0631 0.7559 0.026 Uiso 1 1 calc R . . C5 C 0.1097(5) 0.9480(3) 0.73601(14) 0.0223(6) Uani 1 1 d . . . H5 H 0.1565 0.8814 0.6982 0.027 Uiso 1 1 calc R . . C6 C 0.2692(5) 0.8984(3) 0.94701(15) 0.0256(6) Uani 1 1 d . . . H6 H 0.3151 0.9733 0.9802 0.031 Uiso 1 1 calc R . . C7 C 0.4131(6) 0.8366(3) 0.89439(17) 0.0320(7) Uani 1 1 d . . . H7 H 0.5776 0.8591 0.8845 0.038 Uiso 1 1 calc R . . C8 C 0.2811(6) 0.7367(3) 0.85894(16) 0.0328(7) Uani 1 1 d . . . H8 H 0.3361 0.6763 0.8192 0.039 Uiso 1 1 calc R . . C9 C 0.0546(5) 0.7372(3) 0.88962(17) 0.0278(7) Uani 1 1 d . . . H9 H -0.0761 0.6773 0.8753 0.033 Uiso 1 1 calc R . . C10 C 0.0505(5) 0.8368(3) 0.94435(16) 0.0241(6) Uani 1 1 d . . . H10 H -0.0849 0.8610 0.9751 0.029 Uiso 1 1 calc R . . C11 C 0.2426(5) 1.3917(3) 0.95855(17) 0.0288(7) Uani 1 1 d . . . H11A H 0.2634 1.3710 1.0105 0.035 Uiso 1 1 calc R . . H11B H 0.1765 1.4832 0.9539 0.035 Uiso 1 1 calc R . . C12 C 0.4714(5) 1.3824(3) 0.91836(16) 0.0264(7) Uani 1 1 d . . . H12A H 0.5087 1.4691 0.8947 0.032 Uiso 1 1 calc R . . H12B H 0.5973 1.3587 0.9521 0.032 Uiso 1 1 calc R . . O1 O 0.0947(4) 1.2931(2) 0.92464(10) 0.0259(5) Uani 1 1 d . . . O2 O 0.4393(3) 1.2776(2) 0.86507(11) 0.0275(5) Uani 1 1 d . . . Fe1 Fe 0.13232(6) 0.92116(3) 0.845642(18) 0.01607(12) Uani 1 1 d . . . B1 B 0.2191(6) 1.2319(3) 0.87092(17) 0.0205(6) 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 C1 0.0195(13) 0.0215(13) 0.0202(13) 0.0010(10) -0.0023(12) -0.0025(12) C2 0.0195(13) 0.0184(12) 0.0204(12) 0.0003(10) -0.0035(11) 0.0029(13) C3 0.0219(13) 0.0165(12) 0.0204(12) 0.0038(10) -0.0026(12) 0.0019(12) C4 0.0247(14) 0.0236(14) 0.0165(12) 0.0042(11) -0.0017(11) -0.0015(12) C5 0.0275(14) 0.0248(14) 0.0146(12) -0.0003(10) 0.0001(12) 0.0009(13) C6 0.0332(15) 0.0242(15) 0.0195(13) 0.0029(12) -0.0071(12) 0.0003(13) C7 0.0222(17) 0.0386(17) 0.0352(16) 0.0164(14) -0.0021(13) 0.0083(14) C8 0.0472(18) 0.0231(14) 0.0281(15) 0.0013(13) 0.0034(14) 0.0196(14) C9 0.0337(16) 0.0152(13) 0.0343(16) 0.0042(13) -0.0039(13) -0.0014(12) C10 0.0255(15) 0.0250(15) 0.0217(14) 0.0089(12) 0.0043(12) 0.0052(12) C11 0.0361(17) 0.0202(14) 0.0300(15) -0.0052(12) -0.0018(14) -0.0034(13) C12 0.0293(15) 0.0208(15) 0.0293(15) -0.0044(12) -0.0043(13) -0.0033(12) O1 0.0254(11) 0.0259(10) 0.0265(10) -0.0050(8) 0.0014(9) -0.0056(10) O2 0.0233(10) 0.0242(10) 0.0351(12) -0.0080(9) 0.0009(9) -0.0022(9) Fe1 0.01746(19) 0.01446(19) 0.01628(19) 0.00030(14) 0.00019(15) 0.00151(16) B1 0.0243(15) 0.0143(14) 0.0230(15) 0.0059(13) -0.0017(12) -0.0002(13) _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 C1 C5 1.420(4) . ? C1 C2 1.423(4) . ? C1 Fe1 2.048(3) . ? C2 C3 1.445(4) . ? C2 Fe1 2.043(3) . ? C3 C4 1.441(4) . ? C3 B1 1.538(4) . ? C3 Fe1 2.060(2) . ? C4 C5 1.424(4) . ? C4 Fe1 2.038(3) . ? C5 Fe1 2.047(3) . ? C6 C10 1.412(4) . ? C6 C7 1.422(4) . ? C6 Fe1 2.048(3) . ? C7 C8 1.415(5) . ? C7 Fe1 2.045(3) . ? C8 C9 1.434(5) . ? C8 Fe1 2.040(3) . ? C9 C10 1.415(4) . ? C9 Fe1 2.049(3) . ? C10 Fe1 2.062(3) . ? C11 O1 1.446(3) . ? C11 C12 1.527(4) . ? C12 O2 1.444(3) . ? O1 B1 1.371(4) . ? O2 B1 1.363(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 C5 C1 C2 108.4(2) . . ? C5 C1 Fe1 69.68(15) . . ? C2 C1 Fe1 69.48(15) . . ? C1 C2 C3 108.6(2) . . ? C1 C2 Fe1 69.80(15) . . ? C3 C2 Fe1 70.00(15) . . ? C4 C3 C2 106.1(2) . . ? C4 C3 B1 125.3(3) . . ? C2 C3 B1 128.2(3) . . ? C4 C3 Fe1 68.58(15) . . ? C2 C3 Fe1 68.77(14) . . ? B1 C3 Fe1 122.16(18) . . ? C5 C4 C3 109.0(3) . . ? C5 C4 Fe1 69.95(15) . . ? C3 C4 Fe1 70.25(15) . . ? C1 C5 C4 107.9(2) . . ? C1 C5 Fe1 69.73(14) . . ? C4 C5 Fe1 69.24(15) . . ? C10 C6 C7 108.6(3) . . ? C10 C6 Fe1 70.45(17) . . ? C7 C6 Fe1 69.59(16) . . ? C8 C7 C6 107.4(3) . . ? C8 C7 Fe1 69.51(17) . . ? C6 C7 Fe1 69.75(17) . . ? C7 C8 C9 108.3(3) . . ? C7 C8 Fe1 69.96(17) . . ? C9 C8 Fe1 69.82(17) . . ? C10 C9 C8 107.4(3) . . ? C10 C9 Fe1 70.37(16) . . ? C8 C9 Fe1 69.10(17) . . ? C6 C10 C9 108.2(3) . . ? C6 C10 Fe1 69.34(16) . . ? C9 C10 Fe1 69.38(16) . . ? O1 C11 C12 105.5(2) . . ? O2 C12 C11 105.2(2) . . ? B1 O1 C11 107.4(2) . . ? B1 O2 C12 107.9(2) . . ? C4 Fe1 C8 119.51(13) . . ? C4 Fe1 C2 68.84(11) . . ? C8 Fe1 C2 160.37(13) . . ? C4 Fe1 C7 106.74(12) . . ? C8 Fe1 C7 40.52(13) . . ? C2 Fe1 C7 158.37(12) . . ? C4 Fe1 C5 40.81(11) . . ? C8 Fe1 C5 105.26(11) . . ? C2 Fe1 C5 68.63(11) . . ? C7 Fe1 C5 122.71(13) . . ? C4 Fe1 C6 125.41(12) . . ? C8 Fe1 C6 68.03(11) . . ? C2 Fe1 C6 123.57(11) . . ? C7 Fe1 C6 40.66(12) . . ? C5 Fe1 C6 160.78(12) . . ? C4 Fe1 C1 68.51(11) . . ? C8 Fe1 C1 122.75(12) . . ? C2 Fe1 C1 40.72(10) . . ? C7 Fe1 C1 159.20(12) . . ? C5 Fe1 C1 40.58(11) . . ? C6 Fe1 C1 158.16(12) . . ? C4 Fe1 C9 155.06(11) . . ? C8 Fe1 C9 41.08(13) . . ? C2 Fe1 C9 124.39(12) . . ? C7 Fe1 C9 68.66(13) . . ? C5 Fe1 C9 119.61(12) . . ? C6 Fe1 C9 67.98(12) . . ? C1 Fe1 C9 106.64(12) . . ? C4 Fe1 C3 41.17(11) . . ? C8 Fe1 C3 155.94(13) . . ? C2 Fe1 C3 41.23(11) . . ? C7 Fe1 C3 121.55(13) . . ? C5 Fe1 C3 69.20(10) . . ? C6 Fe1 C3 109.14(11) . . ? C1 Fe1 C3 69.08(11) . . ? C9 Fe1 C3 162.08(12) . . ? C4 Fe1 C10 162.76(11) . . ? C8 Fe1 C10 68.11(12) . . ? C2 Fe1 C10 109.43(11) . . ? C7 Fe1 C10 68.18(13) . . ? C5 Fe1 C10 155.91(12) . . ? C6 Fe1 C10 40.20(12) . . ? C1 Fe1 C10 122.15(12) . . ? C9 Fe1 C10 40.25(12) . . ? C3 Fe1 C10 126.21(11) . . ? O2 B1 O1 114.0(2) . . ? O2 B1 C3 122.0(3) . . ? O1 B1 C3 124.0(3) . . ? 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 C5 C1 C2 C3 0.5(3) . . . . ? Fe1 C1 C2 C3 59.45(17) . . . . ? C5 C1 C2 Fe1 -58.99(18) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? Fe1 C2 C3 C4 58.65(17) . . . . ? C1 C2 C3 B1 -174.2(2) . . . . ? Fe1 C2 C3 B1 -114.9(3) . . . . ? C1 C2 C3 Fe1 -59.33(17) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? B1 C3 C4 C5 174.4(2) . . . . ? Fe1 C3 C4 C5 59.42(18) . . . . ? C2 C3 C4 Fe1 -58.77(17) . . . . ? B1 C3 C4 Fe1 115.0(3) . . . . ? C2 C1 C5 C4 -0.1(3) . . . . ? Fe1 C1 C5 C4 -58.92(18) . . . . ? C2 C1 C5 Fe1 58.87(17) . . . . ? C3 C4 C5 C1 -0.4(3) . . . . ? Fe1 C4 C5 C1 59.23(17) . . . . ? C3 C4 C5 Fe1 -59.61(18) . . . . ? C10 C6 C7 C8 0.3(3) . . . . ? Fe1 C6 C7 C8 -59.6(2) . . . . ? C10 C6 C7 Fe1 59.9(2) . . . . ? C6 C7 C8 C9 0.2(3) . . . . ? Fe1 C7 C8 C9 -59.5(2) . . . . ? C6 C7 C8 Fe1 59.70(19) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? Fe1 C8 C9 C10 -60.20(19) . . . . ? C7 C8 C9 Fe1 59.6(2) . . . . ? C7 C6 C10 C9 -0.7(3) . . . . ? Fe1 C6 C10 C9 58.7(2) . . . . ? C7 C6 C10 Fe1 -59.32(19) . . . . ? C8 C9 C10 C6 0.8(3) . . . . ? Fe1 C9 C10 C6 -58.6(2) . . . . ? C8 C9 C10 Fe1 59.4(2) . . . . ? O1 C11 C12 O2 -0.9(3) . . . . ? C12 C11 O1 B1 0.2(3) . . . . ? C11 C12 O2 B1 1.3(3) . . . . ? C5 C4 Fe1 C8 78.9(2) . . . . ? C3 C4 Fe1 C8 -161.19(17) . . . . ? C5 C4 Fe1 C2 -81.41(17) . . . . ? C3 C4 Fe1 C2 38.52(16) . . . . ? C5 C4 Fe1 C7 121.00(18) . . . . ? C3 C4 Fe1 C7 -119.08(18) . . . . ? C3 C4 Fe1 C5 119.9(2) . . . . ? C5 C4 Fe1 C6 161.70(17) . . . . ? C3 C4 Fe1 C6 -78.4(2) . . . . ? C5 C4 Fe1 C1 -37.55(16) . . . . ? C3 C4 Fe1 C1 82.38(17) . . . . ? C5 C4 Fe1 C9 45.7(4) . . . . ? C3 C4 Fe1 C9 165.7(3) . . . . ? C5 C4 Fe1 C3 -119.9(2) . . . . ? C5 C4 Fe1 C10 -168.9(4) . . . . ? C3 C4 Fe1 C10 -49.0(4) . . . . ? C7 C8 Fe1 C4 81.2(2) . . . . ? C9 C8 Fe1 C4 -159.46(17) . . . . ? C7 C8 Fe1 C2 -168.2(3) . . . . ? C9 C8 Fe1 C2 -48.9(4) . . . . ? C9 C8 Fe1 C7 119.3(2) . . . . ? C7 C8 Fe1 C5 122.88(19) . . . . ? C9 C8 Fe1 C5 -117.80(18) . . . . ? C7 C8 Fe1 C6 -38.10(18) . . . . ? C9 C8 Fe1 C6 81.23(18) . . . . ? C7 C8 Fe1 C1 163.37(18) . . . . ? C9 C8 Fe1 C1 -77.31(19) . . . . ? C7 C8 Fe1 C9 -119.3(2) . . . . ? C7 C8 Fe1 C3 49.8(3) . . . . ? C9 C8 Fe1 C3 169.2(2) . . . . ? C7 C8 Fe1 C10 -81.6(2) . . . . ? C9 C8 Fe1 C10 37.74(17) . . . . ? C1 C2 Fe1 C4 81.23(17) . . . . ? C3 C2 Fe1 C4 -38.47(15) . . . . ? C1 C2 Fe1 C8 -37.9(4) . . . . ? C3 C2 Fe1 C8 -157.6(3) . . . . ? C1 C2 Fe1 C7 163.3(3) . . . . ? C3 C2 Fe1 C7 43.6(4) . . . . ? C1 C2 Fe1 C5 37.29(16) . . . . ? C3 C2 Fe1 C5 -82.41(16) . . . . ? C1 C2 Fe1 C6 -159.51(17) . . . . ? C3 C2 Fe1 C6 80.78(19) . . . . ? C3 C2 Fe1 C1 -119.7(2) . . . . ? C1 C2 Fe1 C9 -74.74(19) . . . . ? C3 C2 Fe1 C9 165.56(15) . . . . ? C1 C2 Fe1 C3 119.7(2) . . . . ? C1 C2 Fe1 C10 -117.07(17) . . . . ? C3 C2 Fe1 C10 123.23(16) . . . . ? C8 C7 Fe1 C4 -116.09(19) . . . . ? C6 C7 Fe1 C4 125.33(17) . . . . ? C6 C7 Fe1 C8 -118.6(3) . . . . ? C8 C7 Fe1 C2 169.2(3) . . . . ? C6 C7 Fe1 C2 50.7(4) . . . . ? C8 C7 Fe1 C5 -74.3(2) . . . . ? C6 C7 Fe1 C5 167.08(16) . . . . ? C8 C7 Fe1 C6 118.6(3) . . . . ? C8 C7 Fe1 C1 -42.7(4) . . . . ? C6 C7 Fe1 C1 -161.3(3) . . . . ? C8 C7 Fe1 C9 37.95(17) . . . . ? C6 C7 Fe1 C9 -80.63(19) . . . . ? C8 C7 Fe1 C3 -158.55(17) . . . . ? C6 C7 Fe1 C3 82.9(2) . . . . ? C8 C7 Fe1 C10 81.4(2) . . . . ? C6 C7 Fe1 C10 -37.20(16) . . . . ? C1 C5 Fe1 C4 -119.4(2) . . . . ? C1 C5 Fe1 C8 122.92(18) . . . . ? C4 C5 Fe1 C8 -117.73(19) . . . . ? C1 C5 Fe1 C2 -37.41(15) . . . . ? C4 C5 Fe1 C2 81.94(17) . . . . ? C1 C5 Fe1 C7 163.35(17) . . . . ? C4 C5 Fe1 C7 -77.30(19) . . . . ? C1 C5 Fe1 C6 -170.4(3) . . . . ? C4 C5 Fe1 C6 -51.0(4) . . . . ? C4 C5 Fe1 C1 119.4(2) . . . . ? C1 C5 Fe1 C9 80.97(18) . . . . ? C4 C5 Fe1 C9 -159.68(17) . . . . ? C1 C5 Fe1 C3 -81.74(17) . . . . ? C4 C5 Fe1 C3 37.61(17) . . . . ? C1 C5 Fe1 C10 52.6(3) . . . . ? C4 C5 Fe1 C10 172.0(3) . . . . ? C10 C6 Fe1 C4 166.97(16) . . . . ? C7 C6 Fe1 C4 -73.4(2) . . . . ? C10 C6 Fe1 C8 -81.63(19) . . . . ? C7 C6 Fe1 C8 37.97(19) . . . . ? C10 C6 Fe1 C2 80.41(18) . . . . ? C7 C6 Fe1 C2 -160.00(17) . . . . ? C10 C6 Fe1 C7 -119.6(2) . . . . ? C10 C6 Fe1 C5 -154.5(3) . . . . ? C7 C6 Fe1 C5 -34.9(4) . . . . ? C10 C6 Fe1 C1 42.5(3) . . . . ? C7 C6 Fe1 C1 162.1(3) . . . . ? C10 C6 Fe1 C9 -37.16(17) . . . . ? C7 C6 Fe1 C9 82.4(2) . . . . ? C10 C6 Fe1 C3 123.93(17) . . . . ? C7 C6 Fe1 C3 -116.48(19) . . . . ? C7 C6 Fe1 C10 119.6(2) . . . . ? C5 C1 Fe1 C4 37.75(15) . . . . ? C2 C1 Fe1 C4 -82.11(16) . . . . ? C5 C1 Fe1 C8 -74.3(2) . . . . ? C2 C1 Fe1 C8 165.80(17) . . . . ? C5 C1 Fe1 C2 119.9(2) . . . . ? C5 C1 Fe1 C7 -42.8(4) . . . . ? C2 C1 Fe1 C7 -162.6(3) . . . . ? C2 C1 Fe1 C5 -119.9(2) . . . . ? C5 C1 Fe1 C6 171.5(3) . . . . ? C2 C1 Fe1 C6 51.6(4) . . . . ? C5 C1 Fe1 C9 -116.34(17) . . . . ? C2 C1 Fe1 C9 123.81(16) . . . . ? C5 C1 Fe1 C3 82.06(17) . . . . ? C2 C1 Fe1 C3 -37.79(16) . . . . ? C5 C1 Fe1 C10 -157.49(15) . . . . ? C2 C1 Fe1 C10 82.66(18) . . . . ? C10 C9 Fe1 C4 164.9(3) . . . . ? C8 C9 Fe1 C4 46.4(4) . . . . ? C10 C9 Fe1 C8 118.5(3) . . . . ? C10 C9 Fe1 C2 -79.4(2) . . . . ? C8 C9 Fe1 C2 162.15(17) . . . . ? C10 C9 Fe1 C7 81.03(19) . . . . ? C8 C9 Fe1 C7 -37.46(18) . . . . ? C10 C9 Fe1 C5 -162.54(17) . . . . ? C8 C9 Fe1 C5 79.0(2) . . . . ? C10 C9 Fe1 C6 37.12(18) . . . . ? C8 C9 Fe1 C6 -81.37(19) . . . . ? C10 C9 Fe1 C1 -120.43(18) . . . . ? C8 C9 Fe1 C1 121.09(18) . . . . ? C10 C9 Fe1 C3 -47.1(5) . . . . ? C8 C9 Fe1 C3 -165.6(3) . . . . ? C8 C9 Fe1 C10 -118.5(3) . . . . ? C2 C3 Fe1 C4 118.2(2) . . . . ? B1 C3 Fe1 C4 -119.1(3) . . . . ? C4 C3 Fe1 C8 43.5(3) . . . . ? C2 C3 Fe1 C8 161.7(3) . . . . ? B1 C3 Fe1 C8 -75.7(4) . . . . ? C4 C3 Fe1 C2 -118.2(2) . . . . ? B1 C3 Fe1 C2 122.6(3) . . . . ? C4 C3 Fe1 C7 79.13(19) . . . . ? C2 C3 Fe1 C7 -162.66(16) . . . . ? B1 C3 Fe1 C7 -40.0(3) . . . . ? C4 C3 Fe1 C5 -37.29(16) . . . . ? C2 C3 Fe1 C5 80.92(16) . . . . ? B1 C3 Fe1 C5 -156.4(3) . . . . ? C4 C3 Fe1 C6 122.32(17) . . . . ? C2 C3 Fe1 C6 -119.47(16) . . . . ? B1 C3 Fe1 C6 3.2(3) . . . . ? C4 C3 Fe1 C1 -80.86(16) . . . . ? C2 C3 Fe1 C1 37.35(15) . . . . ? B1 C3 Fe1 C1 160.0(3) . . . . ? C4 C3 Fe1 C9 -160.2(4) . . . . ? C2 C3 Fe1 C9 -42.0(4) . . . . ? B1 C3 Fe1 C9 80.7(5) . . . . ? C4 C3 Fe1 C10 163.91(16) . . . . ? C2 C3 Fe1 C10 -77.88(19) . . . . ? B1 C3 Fe1 C10 44.8(3) . . . . ? C6 C10 Fe1 C4 -38.3(5) . . . . ? C9 C10 Fe1 C4 -158.2(4) . . . . ? C6 C10 Fe1 C8 81.43(19) . . . . ? C9 C10 Fe1 C8 -38.49(19) . . . . ? C6 C10 Fe1 C2 -119.40(17) . . . . ? C9 C10 Fe1 C2 120.68(18) . . . . ? C6 C10 Fe1 C7 37.61(17) . . . . ? C9 C10 Fe1 C7 -82.3(2) . . . . ? C6 C10 Fe1 C5 159.7(3) . . . . ? C9 C10 Fe1 C5 39.7(4) . . . . ? C9 C10 Fe1 C6 -119.9(2) . . . . ? C6 C10 Fe1 C1 -162.72(16) . . . . ? C9 C10 Fe1 C1 77.4(2) . . . . ? C6 C10 Fe1 C9 119.9(2) . . . . ? C6 C10 Fe1 C3 -76.3(2) . . . . ? C9 C10 Fe1 C3 163.78(18) . . . . ? C12 O2 B1 O1 -1.3(3) . . . . ? C12 O2 B1 C3 177.6(2) . . . . ? C11 O1 B1 O2 0.7(3) . . . . ? C11 O1 B1 C3 -178.1(2) . . . . ? C4 C3 B1 O2 7.4(4) . . . . ? C2 C3 B1 O2 179.8(2) . . . . ? Fe1 C3 B1 O2 92.6(3) . . . . ? C4 C3 B1 O1 -173.9(2) . . . . ? C2 C3 B1 O1 -1.5(4) . . . . ? Fe1 C3 B1 O1 -88.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.332 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.091 # Attachment '3b.cif' data_sa0418 _database_code_depnum_ccdc_archive 'CCDC 604015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0418 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 B2 Fe O4' _chemical_formula_weight 325.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 7.0116(4) _cell_length_b 10.0523(7) _cell_length_c 9.8912(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.211(3) _cell_angle_gamma 90.00 _cell_volume 675.82(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1376 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7661 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1901 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 26.33 _reflns_number_total 740 _reflns_number_gt 687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir-92 (A. Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0245P)^2^+1.4290P] 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 740 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 C1 C 0.2773(4) 0.0698(4) 0.0803(3) 0.0379(9) Uani 1 1 d . . . H1 H 0.3497 0.1252 0.0330 0.045 Uiso 1 1 calc R . . C2 C 0.1514(4) 0.1140(3) 0.1625(3) 0.0284(7) Uani 1 1 d . . . H2 H 0.1259 0.2042 0.1807 0.034 Uiso 1 1 calc R . . C3 C 0.0683(5) 0.0000 0.2141(4) 0.0216(9) Uani 1 2 d S . . C4 C -0.3129(5) -0.0755(4) 0.4109(3) 0.0463(10) Uani 1 1 d . . . H4A H -0.2764 -0.1104 0.5074 0.056 Uiso 1 1 calc R . . H4B H -0.4443 -0.1104 0.3634 0.056 Uiso 1 1 calc R . . B1 B -0.0923(6) 0.0000 0.2957(5) 0.0236(10) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.0000 0.0179(3) Uani 1 4 d S . . O1 O -0.1682(3) -0.1128(2) 0.3362(2) 0.0420(6) 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 C1 0.0197(13) 0.068(2) 0.0253(16) 0.0011(15) 0.0034(12) -0.0188(15) C2 0.0308(15) 0.0313(18) 0.0207(15) -0.0043(13) 0.0019(12) -0.0126(14) C3 0.0184(18) 0.029(2) 0.0156(19) 0.000 0.0009(15) 0.000 C4 0.0306(15) 0.087(3) 0.0236(16) -0.0051(17) 0.0112(13) -0.0199(18) B1 0.018(2) 0.035(3) 0.014(2) 0.000 -0.0029(17) 0.000 Fe1 0.0137(4) 0.0246(5) 0.0149(4) 0.000 0.0027(3) 0.000 O1 0.0497(14) 0.0432(15) 0.0419(14) -0.0063(11) 0.0282(12) -0.0150(12) _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 C1 C1 1.404(7) 6 ? C1 C2 1.411(4) . ? C1 Fe1 2.036(3) . ? C1 H1 0.9500 . ? C2 C3 1.435(4) . ? C2 Fe1 2.046(3) . ? C2 H2 0.9500 . ? C3 C2 1.435(4) 6 ? C3 B1 1.538(6) . ? C3 Fe1 2.053(4) . ? C4 O1 1.443(4) . ? C4 C4 1.518(8) 6 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? B1 O1 1.355(3) . ? B1 O1 1.355(3) 6 ? Fe1 C1 2.036(3) 6 ? Fe1 C1 2.036(3) 5 ? Fe1 C1 2.036(3) 2 ? Fe1 C2 2.046(3) 5 ? Fe1 C2 2.046(3) 6 ? Fe1 C2 2.046(3) 2 ? Fe1 C3 2.053(4) 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 C1 C2 108.36(19) 6 . ? C1 C1 Fe1 69.83(10) 6 . ? C2 C1 Fe1 70.16(15) . . ? C1 C1 H1 125.8 6 . ? C2 C1 H1 125.8 . . ? Fe1 C1 H1 125.8 . . ? C1 C2 C3 108.6(3) . . ? C1 C2 Fe1 69.40(17) . . ? C3 C2 Fe1 69.76(19) . . ? C1 C2 H2 125.7 . . ? C3 C2 H2 125.7 . . ? Fe1 C2 H2 126.7 . . ? C2 C3 C2 106.0(3) 6 . ? C2 C3 B1 126.86(17) 6 . ? C2 C3 B1 126.86(17) . . ? C2 C3 Fe1 69.25(18) 6 . ? C2 C3 Fe1 69.25(18) . . ? B1 C3 Fe1 121.7(3) . . ? O1 C4 C4 105.08(19) . 6 ? O1 C4 H4A 110.7 . . ? C4 C4 H4A 110.7 6 . ? O1 C4 H4B 110.7 . . ? C4 C4 H4B 110.7 6 . ? H4A C4 H4B 108.8 . . ? O1 B1 O1 113.7(4) . 6 ? O1 B1 C3 123.15(18) . . ? O1 B1 C3 123.15(18) 6 . ? C1 Fe1 C1 40.3(2) . 6 ? C1 Fe1 C1 180.0(2) . 5 ? C1 Fe1 C1 139.7(2) 6 5 ? C1 Fe1 C1 139.7(2) . 2 ? C1 Fe1 C1 180.0(2) 6 2 ? C1 Fe1 C1 40.3(2) 5 2 ? C1 Fe1 C2 139.56(12) . 5 ? C1 Fe1 C2 112.01(13) 6 5 ? C1 Fe1 C2 40.44(12) 5 5 ? C1 Fe1 C2 67.99(13) 2 5 ? C1 Fe1 C2 40.44(12) . . ? C1 Fe1 C2 67.99(13) 6 . ? C1 Fe1 C2 139.56(12) 5 . ? C1 Fe1 C2 112.01(13) 2 . ? C2 Fe1 C2 180.00(19) 5 . ? C1 Fe1 C2 67.99(13) . 6 ? C1 Fe1 C2 40.44(12) 6 6 ? C1 Fe1 C2 112.01(13) 5 6 ? C1 Fe1 C2 139.56(12) 2 6 ? C2 Fe1 C2 111.85(18) 5 6 ? C2 Fe1 C2 68.15(18) . 6 ? C1 Fe1 C2 112.01(13) . 2 ? C1 Fe1 C2 139.56(12) 6 2 ? C1 Fe1 C2 67.99(13) 5 2 ? C1 Fe1 C2 40.44(12) 2 2 ? C2 Fe1 C2 68.15(18) 5 2 ? C2 Fe1 C2 111.85(18) . 2 ? C2 Fe1 C2 180.00(15) 6 2 ? C1 Fe1 C3 68.84(12) . . ? C1 Fe1 C3 68.84(12) 6 . ? C1 Fe1 C3 111.16(12) 5 . ? C1 Fe1 C3 111.16(12) 2 . ? C2 Fe1 C3 139.01(10) 5 . ? C2 Fe1 C3 40.99(10) . . ? C2 Fe1 C3 40.99(10) 6 . ? C2 Fe1 C3 139.01(10) 2 . ? C1 Fe1 C3 111.16(12) . 5 ? C1 Fe1 C3 111.16(12) 6 5 ? C1 Fe1 C3 68.84(12) 5 5 ? C1 Fe1 C3 68.84(12) 2 5 ? C2 Fe1 C3 40.99(10) 5 5 ? C2 Fe1 C3 139.01(10) . 5 ? C2 Fe1 C3 139.01(10) 6 5 ? C2 Fe1 C3 40.99(10) 2 5 ? C3 Fe1 C3 180.0(2) . 5 ? B1 O1 C4 108.1(3) . . ? 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 C1 C1 C2 C3 -0.7(3) 6 . . . ? Fe1 C1 C2 C3 58.9(2) . . . . ? C1 C1 C2 Fe1 -59.61(9) 6 . . . ? C1 C2 C3 C2 1.1(4) . . . 6 ? Fe1 C2 C3 C2 59.8(2) . . . 6 ? C1 C2 C3 B1 -173.4(3) . . . . ? Fe1 C2 C3 B1 -114.7(4) . . . . ? C1 C2 C3 Fe1 -58.7(2) . . . . ? C2 C3 B1 O1 4.0(6) 6 . . . ? C2 C3 B1 O1 177.4(3) . . . . ? Fe1 C3 B1 O1 90.7(4) . . . . ? C2 C3 B1 O1 -177.4(3) 6 . . 6 ? C2 C3 B1 O1 -4.0(6) . . . 6 ? Fe1 C3 B1 O1 -90.7(4) . . . 6 ? C2 C1 Fe1 C1 -119.29(17) . . . 6 ? C1 C1 Fe1 C1 177(100) 6 . . 5 ? C2 C1 Fe1 C1 57(42) . . . 5 ? C1 C1 Fe1 C1 180.0 6 . . 2 ? C2 C1 Fe1 C1 60.71(17) . . . 2 ? C1 C1 Fe1 C2 -60.71(17) 6 . . 5 ? C2 C1 Fe1 C2 180.0 . . . 5 ? C1 C1 Fe1 C2 119.29(17) 6 . . . ? C1 C1 Fe1 C2 37.60(10) 6 . . 6 ? C2 C1 Fe1 C2 -81.7(2) . . . 6 ? C1 C1 Fe1 C2 -142.40(10) 6 . . 2 ? C2 C1 Fe1 C2 98.3(2) . . . 2 ? C1 C1 Fe1 C3 81.83(7) 6 . . . ? C2 C1 Fe1 C3 -37.46(16) . . . . ? C1 C1 Fe1 C3 -98.17(7) 6 . . 5 ? C2 C1 Fe1 C3 142.54(16) . . . 5 ? C3 C2 Fe1 C1 -120.1(3) . . . . ? C1 C2 Fe1 C1 37.5(2) . . . 6 ? C3 C2 Fe1 C1 -82.63(19) . . . 6 ? C1 C2 Fe1 C1 180.0 . . . 5 ? C3 C2 Fe1 C1 59.9(3) . . . 5 ? C1 C2 Fe1 C1 -142.5(2) . . . 2 ? C3 C2 Fe1 C1 97.37(19) . . . 2 ? C1 C2 Fe1 C2 -70(15) . . . 5 ? C3 C2 Fe1 C2 170(15) . . . 5 ? C1 C2 Fe1 C2 81.26(19) . . . 6 ? C3 C2 Fe1 C2 -38.88(19) . . . 6 ? C1 C2 Fe1 C2 -98.74(19) . . . 2 ? C3 C2 Fe1 C2 141.12(19) . . . 2 ? C1 C2 Fe1 C3 120.1(3) . . . . ? C1 C2 Fe1 C3 -59.9(3) . . . 5 ? C3 C2 Fe1 C3 180.0 . . . 5 ? C2 C3 Fe1 C1 -80.4(2) 6 . . . ? C2 C3 Fe1 C1 36.98(19) . . . . ? B1 C3 Fe1 C1 158.30(11) . . . . ? C2 C3 Fe1 C1 -36.98(19) 6 . . 6 ? C2 C3 Fe1 C1 80.4(2) . . . 6 ? B1 C3 Fe1 C1 -158.30(11) . . . 6 ? C2 C3 Fe1 C1 99.6(2) 6 . . 5 ? C2 C3 Fe1 C1 -143.02(19) . . . 5 ? B1 C3 Fe1 C1 -21.70(11) . . . 5 ? C2 C3 Fe1 C1 143.02(19) 6 . . 2 ? C2 C3 Fe1 C1 -99.6(2) . . . 2 ? B1 C3 Fe1 C1 21.70(11) . . . 2 ? C2 C3 Fe1 C2 62.7(3) 6 . . 5 ? C2 C3 Fe1 C2 180.0 . . . 5 ? B1 C3 Fe1 C2 -58.67(16) . . . 5 ? C2 C3 Fe1 C2 -117.3(3) 6 . . . ? B1 C3 Fe1 C2 121.33(16) . . . . ? C2 C3 Fe1 C2 117.3(3) . . . 6 ? B1 C3 Fe1 C2 -121.33(16) . . . 6 ? C2 C3 Fe1 C2 180.0 6 . . 2 ? C2 C3 Fe1 C2 -62.7(3) . . . 2 ? B1 C3 Fe1 C2 58.67(16) . . . 2 ? C2 C3 Fe1 C3 -170(4) 6 . . 5 ? C2 C3 Fe1 C3 -53(4) . . . 5 ? B1 C3 Fe1 C3 69(100) . . . 5 ? O1 B1 O1 C4 0.8(5) 6 . . . ? C3 B1 O1 C4 179.5(3) . . . . ? C4 C4 O1 B1 -0.4(3) 6 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.606 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.108 # Attachment '4.cif' data_s92 _database_code_depnum_ccdc_archive 'CCDC 604016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 B Fe O2' _chemical_formula_weight 408.07 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 Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 9.5746(3) _cell_length_b 9.5746(3) _cell_length_c 18.2224(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1446.70(8) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7956 _exptl_absorpt_correction_T_max 0.8253 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5630 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3585 _reflns_number_gt 3518 _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^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.037(19) _refine_ls_number_reflns 3585 _refine_ls_number_parameters 255 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.003 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 C1 C 0.5629(6) 0.8120(4) 0.78551(17) 0.0406(9) Uani 1 1 d . . . H1 H 0.5047 0.6981 0.7911 0.049 Uiso 1 1 calc R . . C2 C 0.4962(6) 0.9112(6) 0.7704(2) 0.0491(12) Uani 1 1 d . . . H2 H 0.3849 0.8751 0.7638 0.059 Uiso 1 1 calc R . . C3 C 0.6224(7) 1.0729(6) 0.76682(19) 0.0504(13) Uani 1 1 d . . . H3 H 0.6109 1.1643 0.7577 0.060 Uiso 1 1 calc R . . C4 C 0.7680(6) 1.0745(6) 0.7792(2) 0.0425(10) Uani 1 1 d . . . H4 H 0.8725 1.1673 0.7796 0.051 Uiso 1 1 calc R . . C5 C 0.7312(5) 0.9123(5) 0.79085(18) 0.0389(9) Uani 1 1 d . . . H5 H 0.8069 0.8780 0.8005 0.047 Uiso 1 1 calc R . . C6 C 0.5496(4) 0.8661(4) 0.96659(16) 0.0236(6) Uani 1 1 d . . . C7 C 0.4575(5) 0.9403(5) 0.94744(18) 0.0346(8) Uani 1 1 d . . . H7 H 0.3436 0.8864 0.9419 0.042 Uiso 1 1 calc R . . C8 C 0.5639(6) 1.1076(5) 0.9380(2) 0.0436(9) Uani 1 1 d . . . H8 H 0.5338 1.1854 0.9256 0.052 Uiso 1 1 calc R . . C9 C 0.7243(6) 1.1390(4) 0.95021(18) 0.0397(11) Uani 1 1 d . . . H9 H 0.8201 1.2410 0.9471 0.048 Uiso 1 1 calc R . . C10 C 0.7144(4) 0.9904(4) 0.96783(16) 0.0297(7) Uani 1 1 d . . . H10 H 0.8033 0.9758 0.9787 0.036 Uiso 1 1 calc R . . C11 C 0.3095(3) 0.4163(3) 0.99348(16) 0.0204(5) Uani 1 1 d . . . H11 H 0.2327 0.3932 1.0351 0.025 Uiso 1 1 calc R . . C12 C 0.4779(3) 0.4586(3) 1.02542(15) 0.0209(5) Uani 1 1 d . . . H12 H 0.5282 0.4114 0.9931 0.025 Uiso 1 1 calc R . . C13 C 0.2417(3) 0.2733(3) 0.94358(15) 0.0223(6) Uani 1 1 d . . . C14 C 0.1581(4) 0.1207(4) 0.97504(17) 0.0268(6) Uani 1 1 d . . . H14 H 0.1375 0.1110 1.0263 0.032 Uiso 1 1 calc R . . C15 C 0.1047(4) -0.0166(4) 0.93335(17) 0.0305(7) Uani 1 1 d . . . H15 H 0.0473 -0.1197 0.9559 0.037 Uiso 1 1 calc R . . C16 C 0.1343(4) -0.0045(4) 0.85886(19) 0.0328(7) Uani 1 1 d . . . H16 H 0.1001 -0.0989 0.8301 0.039 Uiso 1 1 calc R . . C17 C 0.2145(5) 0.1463(4) 0.82657(19) 0.0385(8) Uani 1 1 d . . . H17 H 0.2324 0.1548 0.7751 0.046 Uiso 1 1 calc R . . C18 C 0.2694(4) 0.2863(4) 0.86832(15) 0.0308(6) Uani 1 1 d . . . H18 H 0.3252 0.3893 0.8456 0.037 Uiso 1 1 calc R . . C19 C 0.4695(3) 0.4001(3) 1.10267(15) 0.0194(5) Uani 1 1 d . . . C20 C 0.4534(3) 0.4838(4) 1.16176(14) 0.0225(5) Uani 1 1 d . . . H20 H 0.4540 0.5821 1.1536 0.027 Uiso 1 1 calc R . . C21 C 0.4364(3) 0.4233(4) 1.23237(14) 0.0233(6) Uani 1 1 d . . . H21 H 0.4264 0.4809 1.2726 0.028 Uiso 1 1 calc R . . C22 C 0.4340(4) 0.2793(4) 1.24459(15) 0.0261(6) Uani 1 1 d . . . H22 H 0.4207 0.2374 1.2929 0.031 Uiso 1 1 calc R . . C23 C 0.4511(4) 0.1968(4) 1.18608(17) 0.0289(6) Uani 1 1 d . . . H23 H 0.4503 0.0984 1.1944 0.035 Uiso 1 1 calc R . . C24 C 0.4695(4) 0.2573(4) 1.11501(15) 0.0250(6) Uani 1 1 d . . . H24 H 0.4820 0.2007 1.0751 0.030 Uiso 1 1 calc R . . B1 B 0.4851(4) 0.6849(4) 0.98056(17) 0.0236(6) Uani 1 1 d . . . O1 O 0.3384(3) 0.5629(2) 0.95726(11) 0.0258(4) Uani 1 1 d . . . O2 O 0.5708(3) 0.6323(2) 1.02114(10) 0.0237(4) Uani 1 1 d . . . Fe1 Fe 0.61807(5) 0.97844(4) 0.866574(17) 0.02255(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 C1 0.057(3) 0.0296(15) 0.0240(15) -0.0060(13) -0.0014(18) 0.013(2) C2 0.050(2) 0.058(3) 0.034(2) -0.009(2) -0.0211(17) 0.023(2) C3 0.096(4) 0.048(2) 0.0206(16) 0.0030(17) -0.003(2) 0.046(3) C4 0.057(3) 0.0319(19) 0.0270(17) 0.0033(16) 0.0135(17) 0.013(2) C5 0.048(2) 0.039(2) 0.0306(17) -0.0011(16) 0.0101(18) 0.0228(19) C6 0.0296(17) 0.0206(14) 0.0229(14) 0.0026(12) 0.0018(13) 0.0144(13) C7 0.047(2) 0.0324(19) 0.0349(17) 0.0098(16) 0.0145(15) 0.0279(19) C8 0.077(3) 0.0285(19) 0.0315(17) 0.0040(16) 0.0149(19) 0.0314(19) C9 0.064(3) 0.0155(14) 0.0235(15) 0.0012(12) -0.0009(18) 0.0075(19) C10 0.0348(19) 0.0303(18) 0.0156(14) -0.0013(12) -0.0070(11) 0.0100(16) C11 0.0189(14) 0.0187(13) 0.0246(12) 0.0033(11) 0.0007(10) 0.0102(11) C12 0.0200(12) 0.0215(14) 0.0218(13) 0.0007(11) 0.0009(10) 0.0107(11) C13 0.0174(12) 0.0251(14) 0.0239(12) 0.0005(11) -0.0019(10) 0.0103(11) C14 0.0219(14) 0.0249(14) 0.0282(15) 0.0016(12) 0.0020(12) 0.0076(12) C15 0.0292(16) 0.0228(14) 0.0361(16) -0.0019(12) -0.0035(14) 0.0105(13) C16 0.0348(18) 0.0300(15) 0.0342(15) -0.0106(12) -0.0104(15) 0.0166(15) C17 0.049(2) 0.0454(19) 0.0193(12) -0.0045(13) -0.0048(14) 0.0223(18) C18 0.0333(15) 0.0278(15) 0.0245(13) 0.0040(11) -0.0021(13) 0.0101(13) C19 0.0165(11) 0.0184(13) 0.0199(11) -0.0011(11) -0.0001(9) 0.0062(11) C20 0.0203(13) 0.0230(12) 0.0246(13) 0.0000(11) -0.0014(11) 0.0111(11) C21 0.0204(12) 0.0264(14) 0.0211(12) -0.0016(11) -0.0023(11) 0.0102(12) C22 0.0244(15) 0.0312(18) 0.0200(13) 0.0048(12) 0.0003(12) 0.0118(14) C23 0.0386(19) 0.0244(16) 0.0283(14) 0.0041(13) -0.0003(14) 0.0192(14) C24 0.0300(16) 0.0245(16) 0.0239(14) 0.0006(12) 0.0014(13) 0.0163(13) B1 0.0318(18) 0.0238(14) 0.0198(13) 0.0043(12) 0.0070(13) 0.0172(14) O1 0.0267(11) 0.0201(10) 0.0319(10) 0.0025(9) -0.0054(9) 0.0127(9) O2 0.0212(9) 0.0206(10) 0.0250(9) 0.0055(8) -0.0003(8) 0.0072(8) Fe1 0.0275(2) 0.0208(2) 0.01849(15) -0.00041(17) -0.00035(16) 0.0114(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.407(6) . ? C1 C2 1.412(7) . ? C1 Fe1 2.039(3) . ? C1 H1 0.9500 . ? C2 C3 1.411(7) . ? C2 Fe1 2.023(4) . ? C2 H2 0.9500 . ? C3 C4 1.404(7) . ? C3 Fe1 2.022(4) . ? C3 H3 0.9500 . ? C4 C5 1.427(6) . ? C4 Fe1 2.031(4) . ? C4 H4 0.9500 . ? C5 Fe1 2.041(3) . ? C5 H5 0.9500 . ? C6 C7 1.425(5) . ? C6 C10 1.425(5) . ? C6 B1 1.544(4) . ? C6 Fe1 2.050(3) . ? C7 C8 1.415(6) . ? C7 Fe1 2.027(3) . ? C7 H7 0.9500 . ? C8 C9 1.427(7) . ? C8 Fe1 2.033(3) . ? C8 H8 0.9500 . ? C9 C10 1.415(5) . ? C9 Fe1 2.039(3) . ? C9 H9 0.9500 . ? C10 Fe1 2.040(3) . ? C10 H10 0.9500 . ? C11 O1 1.447(3) . ? C11 C13 1.495(4) . ? C11 C12 1.565(4) . ? C11 H11 1.0000 . ? C12 O2 1.444(3) . ? C12 C19 1.502(4) . ? C12 H12 1.0000 . ? C13 C18 1.391(4) . ? C13 C14 1.391(4) . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 C16 1.380(5) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C18 1.395(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.386(4) . ? C19 C20 1.396(4) . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? B1 O1 1.370(4) . ? B1 O2 1.373(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 C5 C1 C2 107.6(3) . . ? C5 C1 Fe1 69.87(19) . . ? C2 C1 Fe1 69.1(2) . . ? C5 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? Fe1 C1 H1 126.5 . . ? C1 C2 C3 108.7(4) . . ? C1 C2 Fe1 70.3(2) . . ? C3 C2 Fe1 69.5(2) . . ? C1 C2 H2 125.7 . . ? C3 C2 H2 125.7 . . ? Fe1 C2 H2 126.1 . . ? C4 C3 C2 107.8(5) . . ? C4 C3 Fe1 70.1(2) . . ? C2 C3 Fe1 69.7(2) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe1 C3 H3 125.7 . . ? C3 C4 C5 108.0(5) . . ? C3 C4 Fe1 69.4(2) . . ? C5 C4 Fe1 69.9(2) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 126.3 . . ? C1 C5 C4 107.9(4) . . ? C1 C5 Fe1 69.8(2) . . ? C4 C5 Fe1 69.1(2) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Fe1 C5 H5 126.6 . . ? C7 C6 C10 106.9(3) . . ? C7 C6 B1 126.9(3) . . ? C10 C6 B1 126.1(3) . . ? C7 C6 Fe1 68.65(17) . . ? C10 C6 Fe1 69.24(16) . . ? B1 C6 Fe1 125.4(2) . . ? C8 C7 C6 108.7(3) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 70.43(19) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? Fe1 C7 H7 125.6 . . ? C7 C8 C9 108.0(3) . . ? C7 C8 Fe1 69.4(2) . . ? C9 C8 Fe1 69.7(2) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe1 C8 H8 126.5 . . ? C10 C9 C8 107.5(3) . . ? C10 C9 Fe1 69.75(18) . . ? C8 C9 Fe1 69.3(2) . . ? C10 C9 H9 126.3 . . ? C8 C9 H9 126.3 . . ? Fe1 C9 H9 126.3 . . ? C9 C10 C6 109.0(3) . . ? C9 C10 Fe1 69.64(18) . . ? C6 C10 Fe1 70.00(16) . . ? C9 C10 H10 125.5 . . ? C6 C10 H10 125.5 . . ? Fe1 C10 H10 126.4 . . ? O1 C11 C13 113.3(2) . . ? O1 C11 C12 104.2(2) . . ? C13 C11 C12 112.5(2) . . ? O1 C11 H11 108.9 . . ? C13 C11 H11 108.9 . . ? C12 C11 H11 108.9 . . ? O2 C12 C19 111.6(2) . . ? O2 C12 C11 103.8(2) . . ? C19 C12 C11 113.3(2) . . ? O2 C12 H12 109.3 . . ? C19 C12 H12 109.3 . . ? C11 C12 H12 109.3 . . ? C18 C13 C14 118.9(3) . . ? C18 C13 C11 122.8(3) . . ? C14 C13 C11 118.0(2) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 121.1(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 119.2(3) . . ? C13 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C24 C19 C20 119.7(3) . . ? C24 C19 C12 119.6(2) . . ? C20 C19 C12 120.6(3) . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.9(3) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? O1 B1 O2 113.6(2) . . ? O1 B1 C6 124.8(3) . . ? O2 B1 C6 121.6(3) . . ? B1 O1 C11 107.6(2) . . ? B1 O2 C12 108.3(2) . . ? C2 Fe1 C3 40.8(2) . . ? C2 Fe1 C7 107.91(17) . . ? C3 Fe1 C7 125.33(19) . . ? C2 Fe1 C8 117.76(19) . . ? C3 Fe1 C8 104.92(16) . . ? C7 Fe1 C8 40.79(16) . . ? C2 Fe1 C4 68.2(2) . . ? C3 Fe1 C4 40.56(19) . . ? C7 Fe1 C4 162.30(16) . . ? C8 Fe1 C4 124.33(18) . . ? C2 Fe1 C9 151.40(18) . . ? C3 Fe1 C9 116.35(18) . . ? C7 Fe1 C9 68.89(17) . . ? C8 Fe1 C9 41.0(2) . . ? C4 Fe1 C9 105.77(17) . . ? C2 Fe1 C5 68.09(18) . . ? C3 Fe1 C5 68.63(18) . . ? C7 Fe1 C5 155.28(17) . . ? C8 Fe1 C5 163.34(17) . . ? C4 Fe1 C5 41.02(16) . . ? C9 Fe1 C5 126.69(19) . . ? C2 Fe1 C10 166.77(17) . . ? C3 Fe1 C10 151.72(19) . . ? C7 Fe1 C10 68.51(15) . . ? C8 Fe1 C10 68.48(15) . . ? C4 Fe1 C10 119.13(17) . . ? C9 Fe1 C10 40.61(14) . . ? C5 Fe1 C10 109.48(15) . . ? C2 Fe1 C1 40.66(19) . . ? C3 Fe1 C1 68.76(17) . . ? C7 Fe1 C1 120.61(16) . . ? C8 Fe1 C1 153.4(2) . . ? C4 Fe1 C1 68.53(16) . . ? C9 Fe1 C1 165.31(19) . . ? C5 Fe1 C1 40.35(19) . . ? C10 Fe1 C1 129.19(16) . . ? C2 Fe1 C6 128.35(16) . . ? C3 Fe1 C6 164.51(19) . . ? C7 Fe1 C6 40.92(14) . . ? C8 Fe1 C6 68.81(14) . . ? C4 Fe1 C6 154.59(17) . . ? C9 Fe1 C6 68.86(13) . . ? C5 Fe1 C6 121.22(15) . . ? C10 Fe1 C6 40.76(14) . . ? C1 Fe1 C6 110.11(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.317 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.040 # Attachment '5.cif' data_sa0417 _database_code_depnum_ccdc_archive 'CCDC 604017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0417 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H15 B Fe O2' _chemical_formula_weight 269.91 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b n 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, z+1/2' _cell_length_a 5.8359(3) _cell_length_b 13.8400(7) _cell_length_c 14.7344(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1190.08(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4647 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8062 _exptl_absorpt_correction_T_max 0.8346 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5013 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2299 _reflns_number_gt 1987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir-92 (A. Altomare et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0281P)^2^+0.6506P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 2299 _refine_ls_number_parameters 154 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 1.01544(8) 0.75940(3) 0.99282(7) 0.02068(15) Uani 1 1 d . . . O1 O 1.4520(5) 0.84988(19) 1.16686(18) 0.0315(7) Uani 1 1 d . . . O2 O 1.0801(5) 0.85726(18) 1.23731(19) 0.0309(6) Uani 1 1 d . . . C8 C 1.0090(7) 0.8057(3) 0.8607(3) 0.0328(10) Uani 1 1 d . . . H8 H 1.0610 0.7709 0.8090 0.039 Uiso 1 1 calc R . . C4 C 1.1453(6) 0.6217(2) 0.9988(3) 0.0284(8) Uani 1 1 d . . . H4 H 1.1911 0.5829 0.9488 0.034 Uiso 1 1 calc R . . C10 C 0.7789(7) 0.8662(2) 0.9739(3) 0.0260(9) Uani 1 1 d . . . H10 H 0.6500 0.8789 1.0115 0.031 Uiso 1 1 calc R . . C6 C 0.9985(6) 0.9063(2) 0.9834(4) 0.0265(9) Uani 1 1 d . . . H6 H 1.0435 0.9512 1.0288 0.032 Uiso 1 1 calc R . . B1 B 1.2326(8) 0.8177(3) 1.1770(3) 0.0238(10) Uani 1 1 d . . . C1 C 1.1550(7) 0.7315(3) 1.1181(3) 0.0236(8) Uani 1 1 d . . . C9 C 0.7847(7) 0.8029(2) 0.8974(3) 0.0299(10) Uani 1 1 d . . . H9 H 0.6603 0.7655 0.8751 0.036 Uiso 1 1 calc R . . C12 C 1.3333(8) 0.9971(3) 1.2414(3) 0.0386(10) Uani 1 1 d . . . H12A H 1.2690 1.0259 1.1854 0.046 Uiso 1 1 calc R . . H12B H 1.3873 1.0503 1.2809 0.046 Uiso 1 1 calc R . . C3 C 0.9231(7) 0.6246(2) 1.0381(3) 0.0280(9) Uani 1 1 d . . . H3 H 0.7937 0.5882 1.0190 0.034 Uiso 1 1 calc R . . C11 C 1.1488(8) 0.9404(3) 1.2901(3) 0.0393(11) Uani 1 1 d . . . H11A H 1.2071 0.9188 1.3499 0.047 Uiso 1 1 calc R . . H11B H 1.0143 0.9825 1.3007 0.047 Uiso 1 1 calc R . . C2 C 0.9292(8) 0.6919(3) 1.1111(3) 0.0258(9) Uani 1 1 d . . . H2 H 0.8034 0.7079 1.1491 0.031 Uiso 1 1 calc R . . C7 C 1.1422(7) 0.8692(2) 0.9143(3) 0.0300(9) Uani 1 1 d . . . H7 H 1.2995 0.8843 0.9055 0.036 Uiso 1 1 calc R . . C5 C 1.2864(7) 0.6871(2) 1.0473(3) 0.0267(9) Uani 1 1 d . . . H5 H 1.4434 0.6994 1.0348 0.032 Uiso 1 1 calc R . . C13 C 1.5309(7) 0.9330(3) 1.2174(3) 0.0370(11) Uani 1 1 d . . . H13A H 1.6431 0.9696 1.1806 0.044 Uiso 1 1 calc R . . H13B H 1.6086 0.9113 1.2736 0.044 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 0.0285(3) 0.0151(2) 0.0184(3) 0.0008(4) -0.0016(3) 0.00265(19) O1 0.0362(17) 0.0295(15) 0.0286(17) -0.0088(12) -0.0023(13) 0.0010(13) O2 0.0390(16) 0.0267(14) 0.0269(16) -0.0065(12) 0.0034(14) -0.0003(13) C8 0.053(3) 0.022(2) 0.023(2) 0.0048(16) -0.004(2) 0.0090(19) C4 0.044(2) 0.0158(15) 0.025(2) -0.002(2) -0.008(3) 0.0096(14) C10 0.032(2) 0.0183(16) 0.028(2) 0.0035(15) -0.0001(17) 0.0111(15) C6 0.038(2) 0.0141(13) 0.028(2) 0.009(2) -0.004(2) 0.0016(15) B1 0.030(3) 0.026(2) 0.016(2) 0.0042(17) -0.0035(19) 0.0061(19) C1 0.031(2) 0.0202(17) 0.019(2) 0.0062(15) -0.0043(17) 0.0010(17) C9 0.035(2) 0.0203(19) 0.034(3) 0.0031(18) -0.0147(19) 0.0031(17) C12 0.057(3) 0.0245(18) 0.034(2) -0.0056(16) -0.004(2) -0.002(2) C3 0.037(2) 0.0144(18) 0.032(2) 0.0039(15) -0.006(2) -0.0006(16) C11 0.055(3) 0.032(2) 0.031(3) -0.0106(18) 0.002(2) -0.001(2) C2 0.036(2) 0.0229(19) 0.019(2) 0.0070(15) 0.0011(17) 0.0021(18) C7 0.032(2) 0.0234(19) 0.035(2) 0.0123(18) -0.0006(19) -0.0004(18) C5 0.030(2) 0.0220(18) 0.028(2) 0.0029(16) -0.0042(18) 0.0063(17) C13 0.047(3) 0.029(2) 0.035(3) -0.0064(19) -0.006(2) -0.0134(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 Fe1 C5 2.036(4) . ? Fe1 C9 2.038(4) . ? Fe1 C2 2.041(4) . ? Fe1 C6 2.041(3) . ? Fe1 C10 2.042(3) . ? Fe1 C7 2.049(4) . ? Fe1 C8 2.050(4) . ? Fe1 C4 2.052(3) . ? Fe1 C3 2.053(4) . ? Fe1 C1 2.054(4) . ? O1 B1 1.364(5) . ? O1 C13 1.446(4) . ? O2 B1 1.372(5) . ? O2 C11 1.446(4) . ? C8 C7 1.415(6) . ? C8 C9 1.417(6) . ? C8 H8 0.9500 . ? C4 C5 1.417(5) . ? C4 C3 1.421(6) . ? C4 H4 0.9500 . ? C10 C6 1.404(5) . ? C10 C9 1.428(5) . ? C10 H10 0.9500 . ? C6 C7 1.415(6) . ? C6 H6 0.9500 . ? B1 C1 1.543(6) . ? C1 C2 1.431(6) . ? C1 C5 1.434(5) . ? C9 H9 0.9500 . ? C12 C13 1.497(6) . ? C12 C11 1.513(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C3 C2 1.423(5) . ? C3 H3 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C2 H2 0.9500 . ? C7 H7 0.9500 . ? C5 H5 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? 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 C5 Fe1 C9 158.47(17) . . ? C5 Fe1 C2 68.27(16) . . ? C9 Fe1 C2 124.17(17) . . ? C5 Fe1 C6 123.67(15) . . ? C9 Fe1 C6 68.07(16) . . ? C2 Fe1 C6 120.19(18) . . ? C5 Fe1 C10 159.20(16) . . ? C9 Fe1 C10 40.98(15) . . ? C2 Fe1 C10 106.36(17) . . ? C6 Fe1 C10 40.22(14) . . ? C5 Fe1 C7 107.88(16) . . ? C9 Fe1 C7 68.27(17) . . ? C2 Fe1 C7 155.68(18) . . ? C6 Fe1 C7 40.48(17) . . ? C10 Fe1 C7 68.27(16) . . ? C5 Fe1 C8 122.82(17) . . ? C9 Fe1 C8 40.56(16) . . ? C2 Fe1 C8 161.76(18) . . ? C6 Fe1 C8 67.84(19) . . ? C10 Fe1 C8 68.39(17) . . ? C7 Fe1 C8 40.39(16) . . ? C5 Fe1 C4 40.54(14) . . ? C9 Fe1 C4 123.21(16) . . ? C2 Fe1 C4 68.24(18) . . ? C6 Fe1 C4 161.07(15) . . ? C10 Fe1 C4 158.06(16) . . ? C7 Fe1 C4 125.43(18) . . ? C8 Fe1 C4 109.72(19) . . ? C5 Fe1 C3 68.23(15) . . ? C9 Fe1 C3 108.60(16) . . ? C2 Fe1 C3 40.68(16) . . ? C6 Fe1 C3 156.19(17) . . ? C10 Fe1 C3 121.65(16) . . ? C7 Fe1 C3 162.27(18) . . ? C8 Fe1 C3 125.98(17) . . ? C4 Fe1 C3 40.49(16) . . ? C5 Fe1 C1 41.04(15) . . ? C9 Fe1 C1 159.64(17) . . ? C2 Fe1 C1 40.91(16) . . ? C6 Fe1 C1 105.53(18) . . ? C10 Fe1 C1 121.79(16) . . ? C7 Fe1 C1 120.25(17) . . ? C8 Fe1 C1 156.84(17) . . ? C4 Fe1 C1 68.95(17) . . ? C3 Fe1 C1 69.00(16) . . ? B1 O1 C13 120.2(3) . . ? B1 O2 C11 119.1(3) . . ? C7 C8 C9 108.1(4) . . ? C7 C8 Fe1 69.8(2) . . ? C9 C8 Fe1 69.3(2) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 126.6 . . ? C5 C4 C3 107.9(4) . . ? C5 C4 Fe1 69.13(18) . . ? C3 C4 Fe1 69.78(19) . . ? C5 C4 H4 126.1 . . ? C3 C4 H4 126.1 . . ? Fe1 C4 H4 126.6 . . ? C6 C10 C9 107.4(4) . . ? C6 C10 Fe1 69.84(19) . . ? C9 C10 Fe1 69.3(2) . . ? C6 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Fe1 C10 H10 126.1 . . ? C10 C6 C7 109.0(4) . . ? C10 C6 Fe1 69.94(18) . . ? C7 C6 Fe1 70.1(2) . . ? C10 C6 H6 125.5 . . ? C7 C6 H6 125.5 . . ? Fe1 C6 H6 126.1 . . ? O1 B1 O2 123.3(4) . . ? O1 B1 C1 117.8(3) . . ? O2 B1 C1 118.9(4) . . ? C2 C1 C5 106.0(3) . . ? C2 C1 B1 127.4(4) . . ? C5 C1 B1 125.7(3) . . ? C2 C1 Fe1 69.0(2) . . ? C5 C1 Fe1 68.8(2) . . ? B1 C1 Fe1 118.5(2) . . ? C8 C9 C10 107.8(4) . . ? C8 C9 Fe1 70.2(2) . . ? C10 C9 Fe1 69.7(2) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 125.7 . . ? C13 C12 C11 110.7(3) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C4 C3 C2 107.7(4) . . ? C4 C3 Fe1 69.72(19) . . ? C2 C3 Fe1 69.2(2) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe1 C3 H3 126.5 . . ? O2 C11 C12 110.8(4) . . ? O2 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C3 C2 C1 109.2(4) . . ? C3 C2 Fe1 70.1(2) . . ? C1 C2 Fe1 70.1(2) . . ? C3 C2 H2 125.4 . . ? C1 C2 H2 125.4 . . ? Fe1 C2 H2 126.0 . . ? C8 C7 C6 107.5(4) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 69.5(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe1 C7 H7 126.0 . . ? C4 C5 C1 109.3(4) . . ? C4 C5 Fe1 70.3(2) . . ? C1 C5 Fe1 70.1(2) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Fe1 C5 H5 125.7 . . ? O1 C13 C12 110.3(3) . . ? O1 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? O1 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? 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 C5 Fe1 C8 C7 -78.8(3) . . . . ? C9 Fe1 C8 C7 119.6(3) . . . . ? C2 Fe1 C8 C7 157.9(5) . . . . ? C6 Fe1 C8 C7 37.9(2) . . . . ? C10 Fe1 C8 C7 81.4(3) . . . . ? C4 Fe1 C8 C7 -121.9(2) . . . . ? C3 Fe1 C8 C7 -164.4(2) . . . . ? C1 Fe1 C8 C7 -39.5(5) . . . . ? C5 Fe1 C8 C9 161.6(2) . . . . ? C2 Fe1 C8 C9 38.2(6) . . . . ? C6 Fe1 C8 C9 -81.7(2) . . . . ? C10 Fe1 C8 C9 -38.2(2) . . . . ? C7 Fe1 C8 C9 -119.6(3) . . . . ? C4 Fe1 C8 C9 118.4(2) . . . . ? C3 Fe1 C8 C9 76.0(3) . . . . ? C1 Fe1 C8 C9 -159.2(3) . . . . ? C9 Fe1 C4 C5 160.9(2) . . . . ? C2 Fe1 C4 C5 -81.6(3) . . . . ? C6 Fe1 C4 C5 38.8(8) . . . . ? C10 Fe1 C4 C5 -161.2(5) . . . . ? C7 Fe1 C4 C5 75.4(3) . . . . ? C8 Fe1 C4 C5 117.8(3) . . . . ? C3 Fe1 C4 C5 -119.4(4) . . . . ? C1 Fe1 C4 C5 -37.5(2) . . . . ? C5 Fe1 C4 C3 119.4(4) . . . . ? C9 Fe1 C4 C3 -79.7(3) . . . . ? C2 Fe1 C4 C3 37.8(3) . . . . ? C6 Fe1 C4 C3 158.2(6) . . . . ? C10 Fe1 C4 C3 -41.8(7) . . . . ? C7 Fe1 C4 C3 -165.2(3) . . . . ? C8 Fe1 C4 C3 -122.8(3) . . . . ? C1 Fe1 C4 C3 81.9(3) . . . . ? C5 Fe1 C10 C6 46.0(6) . . . . ? C9 Fe1 C10 C6 -118.6(4) . . . . ? C2 Fe1 C10 C6 117.7(3) . . . . ? C7 Fe1 C10 C6 -37.2(3) . . . . ? C8 Fe1 C10 C6 -80.8(3) . . . . ? C4 Fe1 C10 C6 -170.1(5) . . . . ? C3 Fe1 C10 C6 159.3(3) . . . . ? C1 Fe1 C10 C6 75.8(3) . . . . ? C5 Fe1 C10 C9 164.6(4) . . . . ? C2 Fe1 C10 C9 -123.7(2) . . . . ? C6 Fe1 C10 C9 118.6(4) . . . . ? C7 Fe1 C10 C9 81.4(3) . . . . ? C8 Fe1 C10 C9 37.8(2) . . . . ? C4 Fe1 C10 C9 -51.5(6) . . . . ? C3 Fe1 C10 C9 -82.1(3) . . . . ? C1 Fe1 C10 C9 -165.6(2) . . . . ? C9 C10 C6 C7 -0.1(4) . . . . ? Fe1 C10 C6 C7 59.3(3) . . . . ? C9 C10 C6 Fe1 -59.4(3) . . . . ? C5 Fe1 C6 C10 -162.1(2) . . . . ? C9 Fe1 C6 C10 38.4(3) . . . . ? C2 Fe1 C6 C10 -79.4(3) . . . . ? C7 Fe1 C6 C10 120.1(4) . . . . ? C8 Fe1 C6 C10 82.3(3) . . . . ? C4 Fe1 C6 C10 168.6(6) . . . . ? C3 Fe1 C6 C10 -48.2(6) . . . . ? C1 Fe1 C6 C10 -121.2(3) . . . . ? C5 Fe1 C6 C7 77.7(3) . . . . ? C9 Fe1 C6 C7 -81.8(3) . . . . ? C2 Fe1 C6 C7 160.4(3) . . . . ? C10 Fe1 C6 C7 -120.1(4) . . . . ? C8 Fe1 C6 C7 -37.9(3) . . . . ? C4 Fe1 C6 C7 48.5(8) . . . . ? C3 Fe1 C6 C7 -168.3(4) . . . . ? C1 Fe1 C6 C7 118.7(3) . . . . ? C13 O1 B1 O2 -3.5(6) . . . . ? C13 O1 B1 C1 177.3(3) . . . . ? C11 O2 B1 O1 3.3(5) . . . . ? C11 O2 B1 C1 -177.6(3) . . . . ? O1 B1 C1 C2 -173.7(3) . . . . ? O2 B1 C1 C2 7.1(6) . . . . ? O1 B1 C1 C5 -6.0(6) . . . . ? O2 B1 C1 C5 174.8(3) . . . . ? O1 B1 C1 Fe1 -89.3(4) . . . . ? O2 B1 C1 Fe1 91.5(4) . . . . ? C5 Fe1 C1 C2 -117.7(3) . . . . ? C9 Fe1 C1 C2 49.9(5) . . . . ? C6 Fe1 C1 C2 118.4(2) . . . . ? C10 Fe1 C1 C2 77.9(3) . . . . ? C7 Fe1 C1 C2 159.7(2) . . . . ? C8 Fe1 C1 C2 -171.8(4) . . . . ? C4 Fe1 C1 C2 -80.6(2) . . . . ? C3 Fe1 C1 C2 -37.1(2) . . . . ? C9 Fe1 C1 C5 167.6(4) . . . . ? C2 Fe1 C1 C5 117.7(3) . . . . ? C6 Fe1 C1 C5 -123.9(2) . . . . ? C10 Fe1 C1 C5 -164.4(2) . . . . ? C7 Fe1 C1 C5 -82.6(2) . . . . ? C8 Fe1 C1 C5 -54.1(5) . . . . ? C4 Fe1 C1 C5 37.0(2) . . . . ? C3 Fe1 C1 C5 80.6(2) . . . . ? C5 Fe1 C1 B1 120.2(4) . . . . ? C9 Fe1 C1 B1 -72.3(5) . . . . ? C2 Fe1 C1 B1 -122.2(4) . . . . ? C6 Fe1 C1 B1 -3.7(4) . . . . ? C10 Fe1 C1 B1 -44.2(4) . . . . ? C7 Fe1 C1 B1 37.6(4) . . . . ? C8 Fe1 C1 B1 66.1(5) . . . . ? C4 Fe1 C1 B1 157.2(4) . . . . ? C3 Fe1 C1 B1 -159.3(4) . . . . ? C7 C8 C9 C10 0.6(4) . . . . ? Fe1 C8 C9 C10 59.7(3) . . . . ? C7 C8 C9 Fe1 -59.1(3) . . . . ? C6 C10 C9 C8 -0.3(4) . . . . ? Fe1 C10 C9 C8 -60.1(3) . . . . ? C6 C10 C9 Fe1 59.7(3) . . . . ? C5 Fe1 C9 C8 -46.4(5) . . . . ? C2 Fe1 C9 C8 -166.5(2) . . . . ? C6 Fe1 C9 C8 81.1(3) . . . . ? C10 Fe1 C9 C8 118.8(3) . . . . ? C7 Fe1 C9 C8 37.3(2) . . . . ? C4 Fe1 C9 C8 -81.7(3) . . . . ? C3 Fe1 C9 C8 -124.1(2) . . . . ? C1 Fe1 C9 C8 156.3(4) . . . . ? C5 Fe1 C9 C10 -165.1(4) . . . . ? C2 Fe1 C9 C10 74.8(3) . . . . ? C6 Fe1 C9 C10 -37.7(2) . . . . ? C7 Fe1 C9 C10 -81.4(3) . . . . ? C8 Fe1 C9 C10 -118.8(3) . . . . ? C4 Fe1 C9 C10 159.6(3) . . . . ? C3 Fe1 C9 C10 117.2(2) . . . . ? C1 Fe1 C9 C10 37.6(5) . . . . ? C5 C4 C3 C2 -0.2(4) . . . . ? Fe1 C4 C3 C2 -59.0(3) . . . . ? C5 C4 C3 Fe1 58.8(2) . . . . ? C5 Fe1 C3 C4 -37.6(3) . . . . ? C9 Fe1 C3 C4 119.7(3) . . . . ? C2 Fe1 C3 C4 -119.1(4) . . . . ? C6 Fe1 C3 C4 -162.6(4) . . . . ? C10 Fe1 C3 C4 163.0(3) . . . . ? C7 Fe1 C3 C4 43.0(7) . . . . ? C8 Fe1 C3 C4 78.0(3) . . . . ? C1 Fe1 C3 C4 -81.8(3) . . . . ? C5 Fe1 C3 C2 81.5(3) . . . . ? C9 Fe1 C3 C2 -121.2(3) . . . . ? C6 Fe1 C3 C2 -43.5(5) . . . . ? C10 Fe1 C3 C2 -77.9(3) . . . . ? C7 Fe1 C3 C2 162.1(5) . . . . ? C8 Fe1 C3 C2 -162.9(3) . . . . ? C4 Fe1 C3 C2 119.1(4) . . . . ? C1 Fe1 C3 C2 37.3(2) . . . . ? B1 O2 C11 C12 25.9(5) . . . . ? C13 C12 C11 O2 -54.3(5) . . . . ? C4 C3 C2 C1 0.0(4) . . . . ? Fe1 C3 C2 C1 -59.3(2) . . . . ? C4 C3 C2 Fe1 59.3(3) . . . . ? C5 C1 C2 C3 0.2(4) . . . . ? B1 C1 C2 C3 169.8(3) . . . . ? Fe1 C1 C2 C3 59.4(3) . . . . ? C5 C1 C2 Fe1 -59.2(2) . . . . ? B1 C1 C2 Fe1 110.5(4) . . . . ? C5 Fe1 C2 C3 -81.5(2) . . . . ? C9 Fe1 C2 C3 78.6(3) . . . . ? C6 Fe1 C2 C3 161.2(2) . . . . ? C10 Fe1 C2 C3 119.8(2) . . . . ? C7 Fe1 C2 C3 -166.9(4) . . . . ? C8 Fe1 C2 C3 49.5(6) . . . . ? C4 Fe1 C2 C3 -37.7(2) . . . . ? C1 Fe1 C2 C3 -120.2(3) . . . . ? C5 Fe1 C2 C1 38.7(2) . . . . ? C9 Fe1 C2 C1 -161.2(2) . . . . ? C6 Fe1 C2 C1 -78.6(3) . . . . ? C10 Fe1 C2 C1 -120.0(2) . . . . ? C7 Fe1 C2 C1 -46.7(5) . . . . ? C8 Fe1 C2 C1 169.6(5) . . . . ? C4 Fe1 C2 C1 82.5(2) . . . . ? C3 Fe1 C2 C1 120.2(3) . . . . ? C9 C8 C7 C6 -0.7(4) . . . . ? Fe1 C8 C7 C6 -59.5(3) . . . . ? C9 C8 C7 Fe1 58.8(3) . . . . ? C10 C6 C7 C8 0.5(4) . . . . ? Fe1 C6 C7 C8 59.7(3) . . . . ? C10 C6 C7 Fe1 -59.3(3) . . . . ? C5 Fe1 C7 C8 120.0(2) . . . . ? C9 Fe1 C7 C8 -37.5(2) . . . . ? C2 Fe1 C7 C8 -163.4(4) . . . . ? C6 Fe1 C7 C8 -118.7(4) . . . . ? C10 Fe1 C7 C8 -81.8(3) . . . . ? C4 Fe1 C7 C8 78.6(3) . . . . ? C3 Fe1 C7 C8 45.7(7) . . . . ? C1 Fe1 C7 C8 163.2(2) . . . . ? C5 Fe1 C7 C6 -121.3(3) . . . . ? C9 Fe1 C7 C6 81.2(3) . . . . ? C2 Fe1 C7 C6 -44.7(5) . . . . ? C10 Fe1 C7 C6 37.0(2) . . . . ? C8 Fe1 C7 C6 118.7(4) . . . . ? C4 Fe1 C7 C6 -162.7(3) . . . . ? C3 Fe1 C7 C6 164.4(5) . . . . ? C1 Fe1 C7 C6 -78.1(3) . . . . ? C3 C4 C5 C1 0.3(4) . . . . ? Fe1 C4 C5 C1 59.5(3) . . . . ? C3 C4 C5 Fe1 -59.2(3) . . . . ? C2 C1 C5 C4 -0.3(4) . . . . ? B1 C1 C5 C4 -170.2(3) . . . . ? Fe1 C1 C5 C4 -59.6(3) . . . . ? C2 C1 C5 Fe1 59.3(2) . . . . ? B1 C1 C5 Fe1 -110.5(4) . . . . ? C9 Fe1 C5 C4 -48.1(5) . . . . ? C2 Fe1 C5 C4 81.5(3) . . . . ? C6 Fe1 C5 C4 -165.9(3) . . . . ? C10 Fe1 C5 C4 160.2(5) . . . . ? C7 Fe1 C5 C4 -124.1(3) . . . . ? C8 Fe1 C5 C4 -82.2(3) . . . . ? C3 Fe1 C5 C4 37.5(3) . . . . ? C1 Fe1 C5 C4 120.1(3) . . . . ? C9 Fe1 C5 C1 -168.2(4) . . . . ? C2 Fe1 C5 C1 -38.6(2) . . . . ? C6 Fe1 C5 C1 74.0(3) . . . . ? C10 Fe1 C5 C1 40.1(5) . . . . ? C7 Fe1 C5 C1 115.8(2) . . . . ? C8 Fe1 C5 C1 157.7(2) . . . . ? C4 Fe1 C5 C1 -120.1(3) . . . . ? C3 Fe1 C5 C1 -82.6(2) . . . . ? B1 O1 C13 C12 -25.8(5) . . . . ? C11 C12 C13 O1 53.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.470 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.063 # Attachment '6.cif' data_sa0504 _database_code_depnum_ccdc_archive 'CCDC 604018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0504 _chemical_melting_point ? _chemical_formula_moiety 'C64 H70 B2 Fe2 O4' _chemical_formula_sum 'C64 H70 B2 Fe2 O4' _chemical_formula_weight 1036.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 23.2880(3) _cell_length_b 17.4224(4) _cell_length_c 17.8722(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.1080(10) _cell_angle_gamma 90.00 _cell_volume 6142.23(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31417 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8014 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details 'Sortav (Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37841 _diffrn_reflns_av_R_equivalents 0.2506 _diffrn_reflns_av_sigmaI/netI 0.1181 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6254 _reflns_number_gt 4731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997' _computing_structure_solution 'Sir-92 (A.Altomare et al. 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1570P)^2^+41.4686P] 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 6254 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.3128 _refine_ls_wR_factor_gt 0.2913 _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 C1 C 0.7396(3) 0.2163(4) 0.8137(5) 0.0516(17) Uani 1 1 d . . . H1 H 0.7348 0.1651 0.7930 0.062 Uiso 1 1 calc R . . C2 C 0.7622(3) 0.2401(4) 0.9012(5) 0.0512(16) Uani 1 1 d . . . H2 H 0.7754 0.2072 0.9502 0.061 Uiso 1 1 calc R . . C3 C 0.7617(3) 0.3206(4) 0.9026(5) 0.0531(17) Uani 1 1 d . . . H3 H 0.7744 0.3515 0.9528 0.064 Uiso 1 1 calc R . . C4 C 0.7399(3) 0.3472(4) 0.8198(5) 0.0534(17) Uani 1 1 d . . . H4 H 0.7351 0.3997 0.8031 0.064 Uiso 1 1 calc R . . C5 C 0.7257(4) 0.2845(5) 0.7635(5) 0.061(2) Uani 1 1 d . . . H5 H 0.7096 0.2872 0.7023 0.073 Uiso 1 1 calc R . . C6 C 0.6040(2) 0.2469(3) 0.8581(3) 0.0329(11) Uani 1 1 d . . . H6 H 0.6171 0.2184 0.9102 0.039 Uiso 1 1 calc R . . C7 C 0.5807(2) 0.2147(3) 0.7726(3) 0.0307(11) Uani 1 1 d . . . C8 C 0.5666(3) 0.2773(3) 0.7147(4) 0.0369(12) Uani 1 1 d . . . H8 H 0.5505 0.2733 0.6536 0.044 Uiso 1 1 calc R . . C9 C 0.6042(3) 0.3273(4) 0.8523(4) 0.0433(14) Uani 1 1 d . . . H9 H 0.6178 0.3624 0.8996 0.052 Uiso 1 1 calc R . . C10 C 0.5804(3) 0.3471(4) 0.7626(4) 0.0444(14) Uani 1 1 d . . . H10 H 0.5749 0.3975 0.7394 0.053 Uiso 1 1 calc R . . C11 C 0.5492(2) 0.0234(3) 0.6528(3) 0.0264(10) Uani 1 1 d . . . C12 C 0.4859(2) -0.0029(3) 0.5856(3) 0.0257(10) Uani 1 1 d . . . C13 C 0.6037(2) -0.0270(3) 0.7005(3) 0.0282(10) Uani 1 1 d . . . C14 C 0.4790(2) -0.0810(3) 0.5671(3) 0.0253(10) Uani 1 1 d . . . H14 H 0.4363 -0.0993 0.5206 0.030 Uiso 1 1 calc R . . C15 C 0.5310(2) -0.1337(3) 0.6127(3) 0.0279(10) Uani 1 1 d . . . C16 C 0.5938(3) -0.1038(3) 0.6797(3) 0.0307(11) Uani 1 1 d . . . H16 H 0.6308 -0.1381 0.7118 0.037 Uiso 1 1 calc R . . C17 C 0.6715(2) 0.0021(4) 0.7752(3) 0.0341(12) Uani 1 1 d . . . H17A H 0.6772 0.0562 0.7633 0.041 Uiso 1 1 calc R . . H17B H 0.7081 -0.0283 0.7769 0.041 Uiso 1 1 calc R . . C18 C 0.6788(2) -0.0027(3) 0.8650(3) 0.0315(11) Uani 1 1 d . . . C19 C 0.6315(2) 0.0323(3) 0.8787(3) 0.0271(10) Uani 1 1 d . . . C20 C 0.6326(2) 0.0213(3) 0.9572(3) 0.0277(10) Uani 1 1 d . . . C21 C 0.6852(3) -0.0220(3) 1.0238(3) 0.0305(11) Uani 1 1 d . . . H21 H 0.6871 -0.0288 1.0778 0.037 Uiso 1 1 calc R . . C22 C 0.7353(3) -0.0560(3) 1.0143(3) 0.0339(12) Uani 1 1 d . . . C23 C 0.7301(2) -0.0467(3) 0.9334(3) 0.0336(11) Uani 1 1 d . . . H23 H 0.7625 -0.0711 0.9244 0.040 Uiso 1 1 calc R . . C24 C 0.5217(3) -0.2190(3) 0.5915(4) 0.0327(11) Uani 1 1 d . . . C25 C 0.4484(3) -0.2390(4) 0.5162(5) 0.0570(18) Uani 1 1 d . . . H25A H 0.4449 -0.2944 0.5051 0.086 Uiso 1 1 calc R . . H25B H 0.4374 -0.2114 0.4624 0.086 Uiso 1 1 calc R . . H25C H 0.4166 -0.2239 0.5337 0.086 Uiso 1 1 calc R . . C26 C 0.5672(4) -0.2442(4) 0.5576(6) 0.067(2) Uani 1 1 d . . . H26A H 0.5609 -0.2992 0.5441 0.101 Uiso 1 1 calc R . . H26B H 0.6147 -0.2341 0.6031 0.101 Uiso 1 1 calc R . . H26C H 0.5549 -0.2153 0.5041 0.101 Uiso 1 1 calc R . . C27 C 0.5361(5) -0.2640(5) 0.6720(5) 0.080(3) Uani 1 1 d . . . H27A H 0.5299 -0.3189 0.6579 0.120 Uiso 1 1 calc R . . H27B H 0.5048 -0.2477 0.6899 0.120 Uiso 1 1 calc R . . H27C H 0.5829 -0.2545 0.7205 0.120 Uiso 1 1 calc R . . C28 C 0.7927(3) -0.1020(4) 1.0895(4) 0.0415(13) Uani 1 1 d . . . C29 C 0.8360(5) -0.1437(7) 1.0639(7) 0.094(3) Uiso 1 1 d . . . H29A H 0.8078 -0.1787 1.0149 0.141 Uiso 1 1 calc R . . H29B H 0.8709 -0.1730 1.1146 0.141 Uiso 1 1 calc R . . H29C H 0.8577 -0.1065 1.0455 0.141 Uiso 1 1 calc R . . C30 C 0.7625(6) -0.1645(7) 1.1187(8) 0.109(4) Uiso 1 1 d . . . H30A H 0.7325 -0.1974 1.0682 0.164 Uiso 1 1 calc R . . H30B H 0.7365 -0.1406 1.1412 0.164 Uiso 1 1 calc R . . H30C H 0.7991 -0.1955 1.1654 0.164 Uiso 1 1 calc R . . C31 C 0.8352(7) -0.0522(10) 1.1679(10) 0.139(5) Uiso 1 1 d . . . H31A H 0.8561 -0.0116 1.1522 0.209 Uiso 1 1 calc R . . H31B H 0.8707 -0.0832 1.2160 0.209 Uiso 1 1 calc R . . H31C H 0.8067 -0.0290 1.1869 0.209 Uiso 1 1 calc R . . C32 C 0.5746(2) 0.0500(3) 0.9652(3) 0.0279(10) Uani 1 1 d . . . H32A H 0.5888 0.0513 1.0282 0.034 Uiso 1 1 calc R . . H32B H 0.5620 0.1027 0.9413 0.034 Uiso 1 1 calc R . . O1 O 0.55726(17) 0.1019(2) 0.6712(2) 0.0300(8) Uani 1 1 d . . . O2 O 0.57934(17) 0.0763(2) 0.8151(2) 0.0321(8) Uani 1 1 d . . . Fe1 Fe 0.66628(4) 0.28014(4) 0.81549(5) 0.0319(3) Uani 1 1 d . . . B1 B 0.5747(3) 0.1275(4) 0.7530(3) 0.0283(12) 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 C1 0.036(3) 0.049(4) 0.081(5) -0.019(3) 0.039(3) -0.010(3) C2 0.025(3) 0.063(4) 0.058(4) -0.002(3) 0.017(3) -0.008(3) C3 0.033(3) 0.068(5) 0.057(4) -0.024(3) 0.024(3) -0.022(3) C4 0.052(4) 0.049(4) 0.080(5) -0.011(3) 0.049(4) -0.016(3) C5 0.049(4) 0.093(6) 0.057(4) -0.015(4) 0.040(3) -0.017(4) C6 0.026(2) 0.045(3) 0.028(2) -0.011(2) 0.014(2) -0.007(2) C7 0.021(2) 0.043(3) 0.027(2) -0.005(2) 0.011(2) -0.005(2) C8 0.032(3) 0.038(3) 0.031(3) -0.004(2) 0.010(2) -0.003(2) C9 0.034(3) 0.052(4) 0.042(3) -0.017(3) 0.019(3) -0.007(3) C10 0.036(3) 0.040(3) 0.050(3) -0.004(3) 0.019(3) -0.001(2) C11 0.034(3) 0.030(3) 0.019(2) -0.0020(18) 0.017(2) -0.004(2) C12 0.031(2) 0.032(3) 0.018(2) 0.0009(18) 0.0155(19) -0.0013(19) C13 0.027(2) 0.041(3) 0.020(2) -0.001(2) 0.0140(19) 0.000(2) C14 0.026(2) 0.029(3) 0.022(2) -0.0002(18) 0.0133(19) -0.0015(18) C15 0.031(2) 0.033(3) 0.026(2) 0.001(2) 0.020(2) -0.002(2) C16 0.029(2) 0.040(3) 0.026(2) 0.004(2) 0.017(2) 0.004(2) C17 0.024(2) 0.056(4) 0.023(2) -0.003(2) 0.012(2) -0.005(2) C18 0.024(2) 0.044(3) 0.023(2) -0.007(2) 0.010(2) -0.007(2) C19 0.024(2) 0.032(3) 0.020(2) -0.0022(19) 0.0083(19) -0.0037(19) C20 0.033(3) 0.026(3) 0.025(2) -0.0069(19) 0.015(2) -0.0067(19) C21 0.034(3) 0.032(3) 0.023(2) -0.006(2) 0.014(2) -0.007(2) C22 0.026(2) 0.038(3) 0.027(2) -0.004(2) 0.007(2) -0.006(2) C23 0.023(2) 0.043(3) 0.031(3) -0.002(2) 0.012(2) 0.001(2) C24 0.031(3) 0.030(3) 0.037(3) 0.004(2) 0.018(2) 0.003(2) C25 0.048(4) 0.032(3) 0.077(5) -0.009(3) 0.023(4) -0.002(3) C26 0.076(5) 0.041(4) 0.117(7) -0.030(4) 0.073(5) -0.014(3) C27 0.121(8) 0.050(5) 0.055(4) 0.018(4) 0.038(5) -0.010(5) C28 0.037(3) 0.044(3) 0.032(3) 0.002(2) 0.011(2) 0.004(2) C32 0.036(3) 0.026(3) 0.024(2) -0.0020(19) 0.018(2) 0.000(2) O1 0.0378(19) 0.031(2) 0.0237(16) -0.0033(14) 0.0179(15) -0.0059(15) O2 0.0324(19) 0.042(2) 0.0269(17) 0.0044(15) 0.0194(15) 0.0039(15) Fe1 0.0277(4) 0.0362(5) 0.0319(5) -0.0097(3) 0.0161(3) -0.0082(3) B1 0.022(2) 0.041(3) 0.021(2) -0.003(2) 0.011(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.419(11) . ? C1 C2 1.421(10) . ? C1 Fe1 2.052(6) . ? C2 C3 1.404(11) . ? C2 Fe1 2.047(6) . ? C3 C4 1.364(10) . ? C3 Fe1 2.044(6) . ? C4 C5 1.400(10) . ? C4 Fe1 2.042(6) . ? C5 Fe1 2.037(6) . ? C6 C9 1.406(9) . ? C6 C7 1.437(7) . ? C6 Fe1 2.048(5) . ? C7 C8 1.417(8) . ? C7 B1 1.549(8) . ? C7 Fe1 2.058(5) . ? C8 C10 1.422(8) . ? C8 Fe1 2.047(5) . ? C9 C10 1.433(9) . ? C9 Fe1 2.052(6) . ? C10 Fe1 2.060(6) . ? C11 C12 1.393(7) . ? C11 O1 1.396(6) . ? C11 C13 1.400(7) . ? C12 C14 1.388(7) . ? C12 C32 1.517(7) 2_656 ? C13 C16 1.376(8) . ? C13 C17 1.513(7) . ? C14 C15 1.388(7) . ? C15 C16 1.407(7) . ? C15 C24 1.520(7) . ? C17 C18 1.524(7) . ? C18 C19 1.390(7) . ? C18 C23 1.398(7) . ? C19 O2 1.373(6) . ? C19 C20 1.404(7) . ? C20 C21 1.392(7) . ? C20 C32 1.517(7) . ? C21 C22 1.396(8) . ? C22 C23 1.395(7) . ? C22 C28 1.525(7) . ? C24 C27 1.512(9) . ? C24 C26 1.537(8) . ? C24 C25 1.551(9) . ? C28 C31 1.490(16) . ? C28 C29 1.498(12) . ? C28 C30 1.531(13) . ? C32 C12 1.517(7) 2_656 ? O1 B1 1.367(6) . ? O2 B1 1.384(7) . ? 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 C5 C1 C2 106.2(6) . . ? C5 C1 Fe1 69.1(4) . . ? C2 C1 Fe1 69.5(4) . . ? C3 C2 C1 107.9(6) . . ? C3 C2 Fe1 69.8(4) . . ? C1 C2 Fe1 69.9(4) . . ? C4 C3 C2 108.8(6) . . ? C4 C3 Fe1 70.4(4) . . ? C2 C3 Fe1 70.0(3) . . ? C3 C4 C5 108.9(7) . . ? C3 C4 Fe1 70.6(3) . . ? C5 C4 Fe1 69.8(4) . . ? C4 C5 C1 108.1(7) . . ? C4 C5 Fe1 70.1(3) . . ? C1 C5 Fe1 70.3(4) . . ? C9 C6 C7 108.9(5) . . ? C9 C6 Fe1 70.1(3) . . ? C7 C6 Fe1 69.9(3) . . ? C8 C7 C6 106.7(5) . . ? C8 C7 B1 129.2(5) . . ? C6 C7 B1 124.1(5) . . ? C8 C7 Fe1 69.4(3) . . ? C6 C7 Fe1 69.2(3) . . ? B1 C7 Fe1 125.5(3) . . ? C7 C8 C10 109.1(5) . . ? C7 C8 Fe1 70.2(3) . . ? C10 C8 Fe1 70.2(3) . . ? C6 C9 C10 107.9(5) . . ? C6 C9 Fe1 69.8(3) . . ? C10 C9 Fe1 69.9(3) . . ? C8 C10 C9 107.3(6) . . ? C8 C10 Fe1 69.3(3) . . ? C9 C10 Fe1 69.3(3) . . ? C12 C11 O1 118.3(4) . . ? C12 C11 C13 121.4(5) . . ? O1 C11 C13 120.4(4) . . ? C14 C12 C11 117.6(4) . . ? C14 C12 C32 120.0(4) . 2_656 ? C11 C12 C32 122.4(5) . 2_656 ? C16 C13 C11 118.5(5) . . ? C16 C13 C17 120.7(5) . . ? C11 C13 C17 120.7(5) . . ? C12 C14 C15 123.6(4) . . ? C14 C15 C16 116.3(5) . . ? C14 C15 C24 122.4(5) . . ? C16 C15 C24 121.3(5) . . ? C13 C16 C15 122.6(5) . . ? C13 C17 C18 113.0(4) . . ? C19 C18 C23 118.4(4) . . ? C19 C18 C17 120.4(5) . . ? C23 C18 C17 121.1(5) . . ? O2 C19 C18 122.4(4) . . ? O2 C19 C20 116.1(4) . . ? C18 C19 C20 121.4(5) . . ? C21 C20 C19 118.0(4) . . ? C21 C20 C32 121.4(4) . . ? C19 C20 C32 120.4(4) . . ? C20 C21 C22 122.6(5) . . ? C23 C22 C21 117.3(5) . . ? C23 C22 C28 121.8(5) . . ? C21 C22 C28 120.9(5) . . ? C22 C23 C18 122.2(5) . . ? C27 C24 C15 109.9(5) . . ? C27 C24 C26 112.1(6) . . ? C15 C24 C26 109.9(5) . . ? C27 C24 C25 107.1(6) . . ? C15 C24 C25 112.5(4) . . ? C26 C24 C25 105.4(5) . . ? C31 C28 C29 110.5(8) . . ? C31 C28 C22 110.8(8) . . ? C29 C28 C22 113.8(6) . . ? C31 C28 C30 106.8(9) . . ? C29 C28 C30 105.4(8) . . ? C22 C28 C30 109.1(6) . . ? C12 C32 C20 109.5(4) 2_656 . ? B1 O1 C11 119.8(4) . . ? C19 O2 B1 132.9(4) . . ? C5 Fe1 C4 40.2(3) . . ? C5 Fe1 C3 66.9(3) . . ? C4 Fe1 C3 39.0(3) . . ? C5 Fe1 C2 67.6(3) . . ? C4 Fe1 C2 66.8(3) . . ? C3 Fe1 C2 40.1(3) . . ? C5 Fe1 C8 109.1(3) . . ? C4 Fe1 C8 125.7(3) . . ? C3 Fe1 C8 160.6(3) . . ? C2 Fe1 C8 157.9(3) . . ? C5 Fe1 C6 165.3(3) . . ? C4 Fe1 C6 153.4(2) . . ? C3 Fe1 C6 120.8(2) . . ? C2 Fe1 C6 109.4(3) . . ? C8 Fe1 C6 68.0(2) . . ? C5 Fe1 C9 153.7(3) . . ? C4 Fe1 C9 118.6(3) . . ? C3 Fe1 C9 106.5(2) . . ? C2 Fe1 C9 124.8(3) . . ? C8 Fe1 C9 68.3(2) . . ? C6 Fe1 C9 40.1(3) . . ? C5 Fe1 C1 40.6(3) . . ? C4 Fe1 C1 67.8(3) . . ? C3 Fe1 C1 67.8(3) . . ? C2 Fe1 C1 40.6(3) . . ? C8 Fe1 C1 122.5(3) . . ? C6 Fe1 C1 127.8(3) . . ? C9 Fe1 C1 162.9(3) . . ? C5 Fe1 C7 127.5(3) . . ? C4 Fe1 C7 163.4(3) . . ? C3 Fe1 C7 156.9(3) . . ? C2 Fe1 C7 123.1(3) . . ? C8 Fe1 C7 40.4(2) . . ? C6 Fe1 C7 41.0(2) . . ? C9 Fe1 C7 68.5(2) . . ? C1 Fe1 C7 110.1(2) . . ? C5 Fe1 C10 119.9(3) . . ? C4 Fe1 C10 106.5(3) . . ? C3 Fe1 C10 123.5(3) . . ? C2 Fe1 C10 160.7(3) . . ? C8 Fe1 C10 40.5(2) . . ? C6 Fe1 C10 67.9(2) . . ? C9 Fe1 C10 40.8(2) . . ? C1 Fe1 C10 155.8(3) . . ? C7 Fe1 C10 68.3(2) . . ? O1 B1 O2 120.0(5) . . ? O1 B1 C7 120.1(5) . . ? O2 B1 C7 119.5(4) . . ? 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 C5 C1 C2 C3 0.0(6) . . . . ? Fe1 C1 C2 C3 -59.7(4) . . . . ? C5 C1 C2 Fe1 59.7(4) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? Fe1 C2 C3 C4 -59.9(4) . . . . ? C1 C2 C3 Fe1 59.8(4) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? Fe1 C3 C4 C5 -59.4(5) . . . . ? C2 C3 C4 Fe1 59.7(4) . . . . ? C3 C4 C5 C1 -0.3(7) . . . . ? Fe1 C4 C5 C1 -60.2(4) . . . . ? C3 C4 C5 Fe1 60.0(4) . . . . ? C2 C1 C5 C4 0.2(7) . . . . ? Fe1 C1 C5 C4 60.1(4) . . . . ? C2 C1 C5 Fe1 -59.9(4) . . . . ? C9 C6 C7 C8 -0.1(6) . . . . ? Fe1 C6 C7 C8 -59.5(4) . . . . ? C9 C6 C7 B1 178.8(5) . . . . ? Fe1 C6 C7 B1 119.5(5) . . . . ? C9 C6 C7 Fe1 59.4(4) . . . . ? C6 C7 C8 C10 -0.3(6) . . . . ? B1 C7 C8 C10 -179.2(5) . . . . ? Fe1 C7 C8 C10 -59.7(4) . . . . ? C6 C7 C8 Fe1 59.4(3) . . . . ? B1 C7 C8 Fe1 -119.5(5) . . . . ? C7 C6 C9 C10 0.5(6) . . . . ? Fe1 C6 C9 C10 59.8(4) . . . . ? C7 C6 C9 Fe1 -59.3(3) . . . . ? C7 C8 C10 C9 0.6(6) . . . . ? Fe1 C8 C10 C9 -59.0(4) . . . . ? C7 C8 C10 Fe1 59.7(4) . . . . ? C6 C9 C10 C8 -0.7(6) . . . . ? Fe1 C9 C10 C8 59.0(4) . . . . ? C6 C9 C10 Fe1 -59.7(4) . . . . ? O1 C11 C12 C14 178.9(4) . . . . ? C13 C11 C12 C14 -0.5(6) . . . . ? O1 C11 C12 C32 -2.5(6) . . . 2_656 ? C13 C11 C12 C32 178.2(4) . . . 2_656 ? C12 C11 C13 C16 0.1(7) . . . . ? O1 C11 C13 C16 -179.3(4) . . . . ? C12 C11 C13 C17 -178.0(4) . . . . ? O1 C11 C13 C17 2.6(6) . . . . ? C11 C12 C14 C15 1.2(7) . . . . ? C32 C12 C14 C15 -177.5(4) 2_656 . . . ? C12 C14 C15 C16 -1.3(7) . . . . ? C12 C14 C15 C24 179.3(4) . . . . ? C11 C13 C16 C15 -0.2(7) . . . . ? C17 C13 C16 C15 177.9(4) . . . . ? C14 C15 C16 C13 0.8(7) . . . . ? C24 C15 C16 C13 -179.8(4) . . . . ? C16 C13 C17 C18 -85.7(6) . . . . ? C11 C13 C17 C18 92.4(6) . . . . ? C13 C17 C18 C19 -55.7(7) . . . . ? C13 C17 C18 C23 119.8(6) . . . . ? C23 C18 C19 O2 -179.7(5) . . . . ? C17 C18 C19 O2 -4.2(7) . . . . ? C23 C18 C19 C20 -3.1(7) . . . . ? C17 C18 C19 C20 172.5(5) . . . . ? O2 C19 C20 C21 -179.2(4) . . . . ? C18 C19 C20 C21 4.0(7) . . . . ? O2 C19 C20 C32 6.2(7) . . . . ? C18 C19 C20 C32 -170.6(5) . . . . ? C19 C20 C21 C22 -1.6(7) . . . . ? C32 C20 C21 C22 173.0(5) . . . . ? C20 C21 C22 C23 -1.6(8) . . . . ? C20 C21 C22 C28 179.0(5) . . . . ? C21 C22 C23 C18 2.6(8) . . . . ? C28 C22 C23 C18 -178.0(5) . . . . ? C19 C18 C23 C22 -0.4(8) . . . . ? C17 C18 C23 C22 -175.9(5) . . . . ? C14 C15 C24 C27 -120.5(6) . . . . ? C16 C15 C24 C27 60.2(7) . . . . ? C14 C15 C24 C26 115.7(6) . . . . ? C16 C15 C24 C26 -63.6(7) . . . . ? C14 C15 C24 C25 -1.3(7) . . . . ? C16 C15 C24 C25 179.4(5) . . . . ? C23 C22 C28 C31 117.6(8) . . . . ? C21 C22 C28 C31 -63.1(9) . . . . ? C23 C22 C28 C29 -7.7(9) . . . . ? C21 C22 C28 C29 171.7(6) . . . . ? C23 C22 C28 C30 -125.0(7) . . . . ? C21 C22 C28 C30 54.3(8) . . . . ? C21 C20 C32 C12 -98.8(5) . . . 2_656 ? C19 C20 C32 C12 75.6(6) . . . 2_656 ? C12 C11 O1 B1 119.0(5) . . . . ? C13 C11 O1 B1 -61.6(6) . . . . ? C18 C19 O2 B1 -37.5(8) . . . . ? C20 C19 O2 B1 145.7(5) . . . . ? C1 C5 Fe1 C4 118.8(7) . . . . ? C4 C5 Fe1 C3 -36.5(5) . . . . ? C1 C5 Fe1 C3 82.3(5) . . . . ? C4 C5 Fe1 C2 -80.1(5) . . . . ? C1 C5 Fe1 C2 38.6(4) . . . . ? C4 C5 Fe1 C8 123.2(5) . . . . ? C1 C5 Fe1 C8 -118.0(4) . . . . ? C4 C5 Fe1 C6 -161.1(9) . . . . ? C1 C5 Fe1 C6 -42.3(12) . . . . ? C4 C5 Fe1 C9 43.9(8) . . . . ? C1 C5 Fe1 C9 162.7(5) . . . . ? C4 C5 Fe1 C1 -118.8(7) . . . . ? C4 C5 Fe1 C7 164.5(4) . . . . ? C1 C5 Fe1 C7 -76.7(5) . . . . ? C4 C5 Fe1 C10 80.0(5) . . . . ? C1 C5 Fe1 C10 -161.2(4) . . . . ? C3 C4 Fe1 C5 -119.8(7) . . . . ? C5 C4 Fe1 C3 119.8(7) . . . . ? C3 C4 Fe1 C2 -37.6(4) . . . . ? C5 C4 Fe1 C2 82.2(5) . . . . ? C3 C4 Fe1 C8 163.4(4) . . . . ? C5 C4 Fe1 C8 -76.8(5) . . . . ? C3 C4 Fe1 C6 49.6(8) . . . . ? C5 C4 Fe1 C6 169.4(6) . . . . ? C3 C4 Fe1 C9 80.7(5) . . . . ? C5 C4 Fe1 C9 -159.5(4) . . . . ? C3 C4 Fe1 C1 -81.7(5) . . . . ? C5 C4 Fe1 C1 38.0(5) . . . . ? C3 C4 Fe1 C7 -167.5(8) . . . . ? C5 C4 Fe1 C7 -47.8(11) . . . . ? C3 C4 Fe1 C10 123.2(4) . . . . ? C5 C4 Fe1 C10 -117.1(5) . . . . ? C4 C3 Fe1 C5 37.5(4) . . . . ? C2 C3 Fe1 C5 -82.1(5) . . . . ? C2 C3 Fe1 C4 -119.6(6) . . . . ? C4 C3 Fe1 C2 119.6(6) . . . . ? C4 C3 Fe1 C8 -44.3(9) . . . . ? C2 C3 Fe1 C8 -163.9(7) . . . . ? C4 C3 Fe1 C6 -156.6(4) . . . . ? C2 C3 Fe1 C6 83.8(4) . . . . ? C4 C3 Fe1 C9 -115.4(4) . . . . ? C2 C3 Fe1 C9 125.0(4) . . . . ? C4 C3 Fe1 C1 81.6(5) . . . . ? C2 C3 Fe1 C1 -38.0(4) . . . . ? C4 C3 Fe1 C7 170.9(5) . . . . ? C2 C3 Fe1 C7 51.3(8) . . . . ? C4 C3 Fe1 C10 -74.1(5) . . . . ? C2 C3 Fe1 C10 166.3(4) . . . . ? C3 C2 Fe1 C5 80.3(4) . . . . ? C1 C2 Fe1 C5 -38.6(4) . . . . ? C3 C2 Fe1 C4 36.5(4) . . . . ? C1 C2 Fe1 C4 -82.4(4) . . . . ? C1 C2 Fe1 C3 -118.9(6) . . . . ? C3 C2 Fe1 C8 165.8(6) . . . . ? C1 C2 Fe1 C8 46.9(8) . . . . ? C3 C2 Fe1 C6 -115.2(4) . . . . ? C1 C2 Fe1 C6 125.9(4) . . . . ? C3 C2 Fe1 C9 -73.1(5) . . . . ? C1 C2 Fe1 C9 167.9(4) . . . . ? C3 C2 Fe1 C1 118.9(6) . . . . ? C3 C2 Fe1 C7 -158.6(4) . . . . ? C1 C2 Fe1 C7 82.5(4) . . . . ? C3 C2 Fe1 C10 -36.7(10) . . . . ? C1 C2 Fe1 C10 -155.6(7) . . . . ? C7 C8 Fe1 C5 126.0(4) . . . . ? C10 C8 Fe1 C5 -114.0(4) . . . . ? C7 C8 Fe1 C4 167.6(3) . . . . ? C10 C8 Fe1 C4 -72.4(5) . . . . ? C7 C8 Fe1 C3 -159.6(7) . . . . ? C10 C8 Fe1 C3 -39.7(9) . . . . ? C7 C8 Fe1 C2 48.8(8) . . . . ? C10 C8 Fe1 C2 168.8(6) . . . . ? C7 C8 Fe1 C6 -38.6(3) . . . . ? C10 C8 Fe1 C6 81.3(4) . . . . ? C7 C8 Fe1 C9 -82.0(4) . . . . ? C10 C8 Fe1 C9 38.0(4) . . . . ? C7 C8 Fe1 C1 83.1(4) . . . . ? C10 C8 Fe1 C1 -157.0(4) . . . . ? C10 C8 Fe1 C7 119.9(5) . . . . ? C7 C8 Fe1 C10 -119.9(5) . . . . ? C9 C6 Fe1 C5 -163.1(10) . . . . ? C7 C6 Fe1 C5 -43.1(12) . . . . ? C9 C6 Fe1 C4 44.7(7) . . . . ? C7 C6 Fe1 C4 164.7(6) . . . . ? C9 C6 Fe1 C3 78.7(4) . . . . ? C7 C6 Fe1 C3 -161.3(4) . . . . ? C9 C6 Fe1 C2 121.5(4) . . . . ? C7 C6 Fe1 C2 -118.5(4) . . . . ? C9 C6 Fe1 C8 -82.0(3) . . . . ? C7 C6 Fe1 C8 38.0(3) . . . . ? C7 C6 Fe1 C9 120.0(5) . . . . ? C9 C6 Fe1 C1 163.3(4) . . . . ? C7 C6 Fe1 C1 -76.7(4) . . . . ? C9 C6 Fe1 C7 -120.0(5) . . . . ? C9 C6 Fe1 C10 -38.1(3) . . . . ? C7 C6 Fe1 C10 81.9(4) . . . . ? C6 C9 Fe1 C5 170.4(6) . . . . ? C10 C9 Fe1 C5 51.5(7) . . . . ? C6 C9 Fe1 C4 -159.0(4) . . . . ? C10 C9 Fe1 C4 82.1(4) . . . . ? C6 C9 Fe1 C3 -118.6(4) . . . . ? C10 C9 Fe1 C3 122.5(4) . . . . ? C6 C9 Fe1 C2 -78.5(4) . . . . ? C10 C9 Fe1 C2 162.5(4) . . . . ? C6 C9 Fe1 C8 81.2(3) . . . . ? C10 C9 Fe1 C8 -37.7(3) . . . . ? C10 C9 Fe1 C6 -118.9(5) . . . . ? C6 C9 Fe1 C1 -51.0(9) . . . . ? C10 C9 Fe1 C1 -169.9(8) . . . . ? C6 C9 Fe1 C7 37.6(3) . . . . ? C10 C9 Fe1 C7 -81.3(4) . . . . ? C6 C9 Fe1 C10 118.9(5) . . . . ? C2 C1 Fe1 C5 117.5(6) . . . . ? C5 C1 Fe1 C4 -37.6(4) . . . . ? C2 C1 Fe1 C4 79.8(4) . . . . ? C5 C1 Fe1 C3 -79.9(4) . . . . ? C2 C1 Fe1 C3 37.6(4) . . . . ? C5 C1 Fe1 C2 -117.5(6) . . . . ? C5 C1 Fe1 C8 81.5(5) . . . . ? C2 C1 Fe1 C8 -161.0(4) . . . . ? C5 C1 Fe1 C6 167.5(4) . . . . ? C2 C1 Fe1 C6 -75.0(4) . . . . ? C5 C1 Fe1 C9 -153.2(8) . . . . ? C2 C1 Fe1 C9 -35.8(10) . . . . ? C5 C1 Fe1 C7 124.7(4) . . . . ? C2 C1 Fe1 C7 -117.8(4) . . . . ? C5 C1 Fe1 C10 43.1(8) . . . . ? C2 C1 Fe1 C10 160.6(6) . . . . ? C8 C7 Fe1 C5 -74.5(5) . . . . ? C6 C7 Fe1 C5 167.4(4) . . . . ? B1 C7 Fe1 C5 49.6(6) . . . . ? C8 C7 Fe1 C4 -37.5(10) . . . . ? C6 C7 Fe1 C4 -155.6(8) . . . . ? B1 C7 Fe1 C4 86.6(10) . . . . ? C8 C7 Fe1 C3 162.8(6) . . . . ? C6 C7 Fe1 C3 44.7(7) . . . . ? B1 C7 Fe1 C3 -73.1(8) . . . . ? C8 C7 Fe1 C2 -160.3(4) . . . . ? C6 C7 Fe1 C2 81.6(4) . . . . ? B1 C7 Fe1 C2 -36.1(5) . . . . ? C6 C7 Fe1 C8 -118.1(5) . . . . ? B1 C7 Fe1 C8 124.1(6) . . . . ? C8 C7 Fe1 C6 118.1(5) . . . . ? B1 C7 Fe1 C6 -117.7(6) . . . . ? C8 C7 Fe1 C9 81.3(4) . . . . ? C6 C7 Fe1 C9 -36.8(3) . . . . ? B1 C7 Fe1 C9 -154.6(5) . . . . ? C8 C7 Fe1 C1 -116.9(4) . . . . ? C6 C7 Fe1 C1 125.0(4) . . . . ? B1 C7 Fe1 C1 7.2(5) . . . . ? C8 C7 Fe1 C10 37.3(3) . . . . ? C6 C7 Fe1 C10 -80.8(4) . . . . ? B1 C7 Fe1 C10 161.4(5) . . . . ? C8 C10 Fe1 C5 84.7(4) . . . . ? C9 C10 Fe1 C5 -156.4(4) . . . . ? C8 C10 Fe1 C4 126.1(4) . . . . ? C9 C10 Fe1 C4 -114.9(4) . . . . ? C8 C10 Fe1 C3 165.3(4) . . . . ? C9 C10 Fe1 C3 -75.8(4) . . . . ? C8 C10 Fe1 C2 -167.2(7) . . . . ? C9 C10 Fe1 C2 -48.3(9) . . . . ? C9 C10 Fe1 C8 118.9(5) . . . . ? C8 C10 Fe1 C6 -81.5(4) . . . . ? C9 C10 Fe1 C6 37.5(3) . . . . ? C8 C10 Fe1 C9 -118.9(5) . . . . ? C8 C10 Fe1 C1 53.8(7) . . . . ? C9 C10 Fe1 C1 172.7(5) . . . . ? C8 C10 Fe1 C7 -37.2(3) . . . . ? C9 C10 Fe1 C7 81.8(4) . . . . ? C11 O1 B1 O2 -4.9(7) . . . . ? C11 O1 B1 C7 -177.3(4) . . . . ? C19 O2 B1 O1 89.3(6) . . . . ? C19 O2 B1 C7 -98.3(6) . . . . ? C8 C7 B1 O1 4.0(8) . . . . ? C6 C7 B1 O1 -174.7(4) . . . . ? Fe1 C7 B1 O1 -87.3(5) . . . . ? C8 C7 B1 O2 -168.4(5) . . . . ? C6 C7 B1 O2 12.8(7) . . . . ? Fe1 C7 B1 O2 100.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.875 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.149 # Attachment '7.cif' data_sa0524 _database_code_depnum_ccdc_archive 'CCDC 604019' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0524 _chemical_melting_point ? _chemical_formula_moiety 'C57 H67 B2 Fe O4' _chemical_formula_sum 'C57 H67 B2 Fe O4' _chemical_formula_weight 893.58 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' Fe Fe 0.3463 0.8444 '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' _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 10.7685(3) _cell_length_b 12.7505(4) _cell_length_c 19.0095(6) _cell_angle_alpha 89.514(2) _cell_angle_beta 73.968(2) _cell_angle_gamma 76.0250(10) _cell_volume 2429.57(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50564 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'irregular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8764 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37381 _diffrn_reflns_av_R_equivalents 0.3243 _diffrn_reflns_av_sigmaI/netI 0.2431 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.21 _reflns_number_total 10716 _reflns_number_gt 5877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1999' _computing_structure_solution 'Sir-92 (A.Altomare et al. 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1847P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.017(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10716 _refine_ls_number_parameters 587 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1874 _refine_ls_R_factor_gt 0.1237 _refine_ls_wR_factor_ref 0.3554 _refine_ls_wR_factor_gt 0.3054 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.027 _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 C1 C 0.3312(6) 0.4363(6) -0.0320(3) 0.0393(15) Uani 1 1 d . . . H1 H 0.3069 0.4349 -0.0791 0.047 Uiso 1 1 calc R . . C2 C 0.2900(6) 0.5259(5) 0.0197(3) 0.0329(13) Uani 1 1 d . . . H2 H 0.2329 0.5988 0.0153 0.039 Uiso 1 1 calc R . . C3 C 0.4088(6) 0.3479(5) -0.0051(3) 0.0332(14) Uani 1 1 d . . . H3 H 0.4501 0.2739 -0.0299 0.040 Uiso 1 1 calc R . . C4 C 0.4198(5) 0.3849(5) 0.0645(3) 0.0268(12) Uani 1 1 d . . . C5 C 0.3448(6) 0.4949(5) 0.0783(3) 0.0328(13) Uani 1 1 d . . . H5 H 0.3320 0.5422 0.1227 0.039 Uiso 1 1 calc R . . C6 C 0.0524(7) 0.3716(6) 0.0557(4) 0.0458(18) Uani 1 1 d . . . H6 H 0.0253 0.3784 0.0093 0.055 Uiso 1 1 calc R . . C7 C 0.0207(6) 0.4563(6) 0.1102(4) 0.0470(17) Uani 1 1 d . . . H7 H -0.0325 0.5322 0.1097 0.056 Uiso 1 1 calc R . . C8 C 0.1302(6) 0.2760(6) 0.0760(3) 0.0406(16) Uani 1 1 d . . . H8 H 0.1660 0.2049 0.0468 0.049 Uiso 1 1 calc R . . C9 C 0.1495(6) 0.2991(5) 0.1449(3) 0.0326(13) Uani 1 1 d . . . C10 C 0.0794(6) 0.4132(5) 0.1651(3) 0.0361(14) Uani 1 1 d . . . H10 H 0.0758 0.4545 0.2104 0.043 Uiso 1 1 calc R . . C11 C 0.3170(5) 0.4144(4) 0.3310(3) 0.0236(11) Uani 1 1 d . . . H11A H 0.2867 0.4369 0.2873 0.028 Uiso 1 1 calc R . . H11B H 0.2865 0.4781 0.3665 0.028 Uiso 1 1 calc R . . C12 C 0.1449(5) 0.0857(4) 0.3037(3) 0.0290(12) Uani 1 1 d . . . H12A H 0.0966 0.1240 0.2699 0.035 Uiso 1 1 calc R . . H12B H 0.0874 0.0437 0.3352 0.035 Uiso 1 1 calc R . . C13 C 0.7616(6) 0.2867(5) 0.1361(3) 0.0295(13) Uani 1 1 d . . . H13A H 0.7200 0.3305 0.1016 0.035 Uiso 1 1 calc R . . H13B H 0.8530 0.2963 0.1276 0.035 Uiso 1 1 calc R . . C14 C 0.5551(6) -0.0093(5) 0.0827(3) 0.0300(13) Uani 1 1 d . . . H14A H 0.5019 0.0496 0.0610 0.036 Uiso 1 1 calc R . . H14B H 0.5909 -0.0728 0.0470 0.036 Uiso 1 1 calc R . . C15 C 0.5434(5) 0.3527(4) 0.2354(3) 0.0239(11) Uani 1 1 d . . . C16 C 0.4679(5) 0.3812(4) 0.3083(3) 0.0223(11) Uani 1 1 d . . . C17 C 0.6803(5) 0.3244(4) 0.2147(3) 0.0252(12) Uani 1 1 d . . . C18 C 0.5376(5) 0.3776(4) 0.3609(3) 0.0221(11) Uani 1 1 d . . . H18 H 0.4884 0.3942 0.4109 0.026 Uiso 1 1 calc R . . C19 C 0.6763(5) 0.3507(4) 0.3424(3) 0.0233(11) Uani 1 1 d . . . C20 C 0.7453(5) 0.3232(4) 0.2678(3) 0.0254(12) Uani 1 1 d . . . H20 H 0.8401 0.3032 0.2537 0.030 Uiso 1 1 calc R . . C21 C 0.7534(5) 0.3477(5) 0.3997(3) 0.0269(12) Uani 1 1 d . . . C22 C 0.7870(6) 0.2312(5) 0.4227(3) 0.0371(14) Uani 1 1 d . . . H22A H 0.8402 0.1829 0.3795 0.056 Uiso 1 1 calc R . . H22B H 0.7043 0.2092 0.4447 0.056 Uiso 1 1 calc R . . H22C H 0.8380 0.2269 0.4585 0.056 Uiso 1 1 calc R . . C23 C 0.8817(6) 0.3854(5) 0.3687(3) 0.0383(15) Uani 1 1 d . . . H23A H 0.9381 0.3389 0.3252 0.057 Uiso 1 1 calc R . . H23B H 0.9299 0.3809 0.4058 0.057 Uiso 1 1 calc R . . H23C H 0.8589 0.4605 0.3551 0.057 Uiso 1 1 calc R . . C24 C 0.6706(6) 0.4234(6) 0.4671(3) 0.0473(18) Uani 1 1 d . . . H24A H 0.6492 0.4979 0.4523 0.071 Uiso 1 1 calc R . . H24B H 0.7217 0.4192 0.5029 0.071 Uiso 1 1 calc R . . H24C H 0.5878 0.4016 0.4893 0.071 Uiso 1 1 calc R . . C25 C 0.6646(5) 0.1361(5) 0.1060(3) 0.0272(12) Uani 1 1 d . . . C26 C 0.7675(6) 0.1706(5) 0.1231(3) 0.0269(12) Uani 1 1 d . . . C27 C 0.6696(5) 0.0273(4) 0.0975(3) 0.0254(12) Uani 1 1 d . . . C28 C 0.8777(5) 0.0901(5) 0.1299(3) 0.0271(12) Uani 1 1 d . . . H28 H 0.9489 0.1116 0.1411 0.033 Uiso 1 1 calc R . . C29 C 0.8868(5) -0.0197(4) 0.1210(3) 0.0267(12) Uani 1 1 d . . . C30 C 0.7810(5) -0.0477(4) 0.1043(3) 0.0264(12) Uani 1 1 d . . . H30 H 0.7855 -0.1223 0.0973 0.032 Uiso 1 1 calc R . . C31 C 1.0083(6) -0.1039(5) 0.1318(3) 0.0320(13) Uani 1 1 d . . . C32 C 0.9999(8) -0.1027(7) 0.2123(4) 0.061(2) Uani 1 1 d . . . H32A H 0.9940 -0.0292 0.2301 0.092 Uiso 1 1 calc R . . H32B H 1.0796 -0.1524 0.2196 0.092 Uiso 1 1 calc R . . H32C H 0.9204 -0.1256 0.2396 0.092 Uiso 1 1 calc R . . C33 C 1.1384(7) -0.0757(8) 0.0889(4) 0.075(3) Uani 1 1 d . . . H33A H 1.1380 -0.0029 0.1053 0.112 Uiso 1 1 calc R . . H33B H 1.1456 -0.0779 0.0364 0.112 Uiso 1 1 calc R . . H33C H 1.2147 -0.1284 0.0977 0.112 Uiso 1 1 calc R . . C34 C 1.0182(9) -0.2166(8) 0.1044(5) 0.081(3) Uani 1 1 d U . . H34A H 1.0038 -0.2146 0.0556 0.121 Uiso 1 1 calc R . . H34B H 0.9502 -0.2461 0.1382 0.121 Uiso 1 1 calc R . . H34C H 1.1070 -0.2626 0.1014 0.121 Uiso 1 1 calc R . . C35 C 0.3459(5) 0.0307(4) 0.1914(3) 0.0241(11) Uani 1 1 d . . . C36 C 0.2732(6) 0.0082(4) 0.2592(3) 0.0279(12) Uani 1 1 d . . . C37 C 0.4663(5) -0.0391(4) 0.1523(3) 0.0244(11) Uani 1 1 d . . . C38 C 0.3181(5) -0.0897(4) 0.2877(3) 0.0260(12) Uani 1 1 d . . . H38 H 0.2688 -0.1054 0.3346 0.031 Uiso 1 1 calc R . . C39 C 0.5062(5) -0.1372(4) 0.1823(3) 0.0260(12) Uani 1 1 d . . . H39 H 0.5864 -0.1871 0.1559 0.031 Uiso 1 1 calc R . . C40 C 0.4338(5) -0.1657(4) 0.2495(3) 0.0257(12) Uani 1 1 d . . . C41 C 0.4737(6) -0.2812(5) 0.2745(3) 0.0316(13) Uani 1 1 d . . . C42 C 0.4127(8) -0.2908(5) 0.3564(3) 0.0534(19) Uani 1 1 d . . . H42A H 0.3152 -0.2712 0.3678 0.080 Uiso 1 1 calc R . . H42B H 0.4408 -0.2420 0.3849 0.080 Uiso 1 1 calc R . . H42C H 0.4431 -0.3656 0.3689 0.080 Uiso 1 1 calc R . . C43 C 0.4244(7) -0.3553(5) 0.2307(3) 0.0461(17) Uani 1 1 d . . . H43A H 0.4606 -0.3481 0.1781 0.069 Uiso 1 1 calc R . . H43B H 0.3267 -0.3344 0.2440 0.069 Uiso 1 1 calc R . . H43C H 0.4546 -0.4306 0.2421 0.069 Uiso 1 1 calc R . . C44 C 0.6254(7) -0.3230(6) 0.2574(4) 0.0524(19) Uani 1 1 d . . . H44A H 0.6655 -0.3308 0.2042 0.079 Uiso 1 1 calc R . . H44B H 0.6468 -0.3935 0.2781 0.079 Uiso 1 1 calc R . . H44C H 0.6611 -0.2715 0.2790 0.079 Uiso 1 1 calc R . . C45 C 0.2270(5) 0.2507(4) 0.3216(3) 0.0244(11) Uani 1 1 d . . . C46 C 0.1698(5) 0.1685(4) 0.3516(3) 0.0266(12) Uani 1 1 d . . . C47 C 0.2511(5) 0.3266(4) 0.3654(3) 0.0269(12) Uani 1 1 d . . . C48 C 0.2098(5) 0.3203(5) 0.4411(3) 0.0270(12) Uani 1 1 d . . . H48 H 0.2238 0.3725 0.4716 0.032 Uiso 1 1 calc R . . C49 C 0.1328(5) 0.1646(4) 0.4279(3) 0.0247(11) Uani 1 1 d . . . H49 H 0.0951 0.1075 0.4488 0.030 Uiso 1 1 calc R . . C50 C 0.1487(5) 0.2401(5) 0.4741(3) 0.0265(12) Uani 1 1 d . . . C51 C 0.0941(6) 0.2434(5) 0.5585(3) 0.0333(14) Uani 1 1 d . . . C52 C 0.0411(7) 0.1447(6) 0.5830(3) 0.0456(17) Uani 1 1 d . . . H52A H 0.1135 0.0789 0.5673 0.068 Uiso 1 1 calc R . . H52B H -0.0304 0.1420 0.5609 0.068 Uiso 1 1 calc R . . H52C H 0.0060 0.1496 0.6365 0.068 Uiso 1 1 calc R . . C53 C -0.0211(6) 0.3453(6) 0.5829(3) 0.0424(16) Uani 1 1 d . . . H53A H 0.0118 0.4096 0.5679 0.064 Uiso 1 1 calc R . . H53B H -0.0575 0.3495 0.6364 0.064 Uiso 1 1 calc R . . H53C H -0.0913 0.3418 0.5601 0.064 Uiso 1 1 calc R . . C54 C 0.2019(6) 0.2491(6) 0.5944(3) 0.0438(16) Uani 1 1 d . . . H54A H 0.2328 0.3146 0.5808 0.066 Uiso 1 1 calc R . . H54B H 0.2768 0.1852 0.5778 0.066 Uiso 1 1 calc R . . H54C H 0.1657 0.2510 0.6478 0.066 Uiso 1 1 calc R . . B1 B 0.2354(7) 0.2224(6) 0.1870(3) 0.0298(14) Uani 1 1 d . . . B2 B 0.4925(6) 0.3162(6) 0.1166(3) 0.0279(14) Uani 1 1 d . . . Fe1 Fe 0.22370(7) 0.39857(6) 0.06762(4) 0.0255(3) Uani 1 1 d . . . O1 O 0.2546(5) 0.2666(4) 0.24762(19) 0.0417(11) Uani 1 1 d . . . O2 O 0.5594(4) 0.2118(3) 0.09142(19) 0.0300(9) Uani 1 1 d . . . O3 O 0.2933(4) 0.1205(3) 0.15680(19) 0.0285(9) Uani 1 1 d . . . O4 O 0.4745(4) 0.3700(3) 0.18226(19) 0.0274(9) Uani 1 1 d . . . C55 C 0.5785(9) 0.0608(7) 0.3311(4) 0.067(2) Uani 1 1 d . . . H55A H 0.5521 0.1396 0.3409 0.101 Uiso 1 1 calc R . . H55B H 0.5552 0.0423 0.2873 0.101 Uiso 1 1 calc R . . H55C H 0.6751 0.0347 0.3231 0.101 Uiso 1 1 calc R . . C56 C 0.5328(7) 0.0303(6) 0.4683(4) 0.0469(17) Uani 1 1 d . . . H56A H 0.5004 0.1090 0.4817 0.056 Uiso 1 1 calc R . . H56B H 0.6304 0.0102 0.4612 0.056 Uiso 1 1 calc R . . C57 C 0.5060(7) 0.0078(6) 0.3964(4) 0.0537(19) Uani 1 1 d . . . H57A H 0.4089 0.0329 0.4027 0.064 Uiso 1 1 calc R . . H57B H 0.5319 -0.0715 0.3852 0.064 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 C1 0.037(3) 0.051(4) 0.033(3) 0.011(3) -0.014(3) -0.010(3) C2 0.032(3) 0.032(3) 0.038(3) 0.018(3) -0.013(3) -0.010(3) C3 0.026(3) 0.042(4) 0.030(3) 0.005(2) -0.005(2) -0.009(3) C4 0.023(3) 0.025(3) 0.034(3) 0.009(2) -0.009(2) -0.010(2) C5 0.030(3) 0.028(3) 0.048(3) 0.013(3) -0.013(3) -0.017(3) C6 0.044(4) 0.050(5) 0.062(4) 0.036(4) -0.028(3) -0.032(4) C7 0.018(3) 0.042(4) 0.074(5) 0.026(4) -0.007(3) -0.002(3) C8 0.035(3) 0.046(4) 0.057(4) 0.022(3) -0.027(3) -0.022(3) C9 0.027(3) 0.026(3) 0.051(4) 0.012(3) -0.015(3) -0.013(3) C10 0.026(3) 0.026(3) 0.050(4) 0.005(3) -0.002(3) -0.003(3) C11 0.017(3) 0.018(3) 0.038(3) 0.006(2) -0.009(2) -0.007(2) C12 0.028(3) 0.022(3) 0.038(3) 0.006(2) -0.011(2) -0.006(3) C13 0.033(3) 0.024(3) 0.032(3) 0.003(2) -0.007(2) -0.009(3) C14 0.030(3) 0.028(3) 0.034(3) 0.008(2) -0.009(2) -0.011(3) C15 0.028(3) 0.015(3) 0.037(3) 0.008(2) -0.017(2) -0.011(2) C16 0.015(2) 0.016(3) 0.041(3) 0.009(2) -0.008(2) -0.012(2) C17 0.026(3) 0.017(3) 0.034(3) 0.004(2) -0.009(2) -0.008(2) C18 0.020(3) 0.019(3) 0.025(3) 0.004(2) -0.003(2) -0.006(2) C19 0.020(3) 0.018(3) 0.037(3) 0.011(2) -0.012(2) -0.011(2) C20 0.017(3) 0.022(3) 0.039(3) 0.008(2) -0.008(2) -0.006(2) C21 0.023(3) 0.027(3) 0.035(3) 0.008(2) -0.014(2) -0.007(2) C22 0.030(3) 0.034(4) 0.055(4) 0.019(3) -0.022(3) -0.010(3) C23 0.028(3) 0.044(4) 0.053(4) 0.011(3) -0.022(3) -0.017(3) C24 0.036(4) 0.061(5) 0.041(4) -0.012(3) -0.019(3) 0.005(3) C25 0.025(3) 0.029(3) 0.022(3) 0.009(2) -0.003(2) -0.002(3) C26 0.028(3) 0.025(3) 0.026(3) 0.002(2) 0.000(2) -0.011(3) C27 0.025(3) 0.027(3) 0.024(3) 0.005(2) -0.003(2) -0.012(3) C28 0.023(3) 0.029(3) 0.029(3) -0.002(2) -0.006(2) -0.010(3) C29 0.025(3) 0.025(3) 0.026(3) 0.001(2) -0.004(2) -0.003(2) C30 0.026(3) 0.016(3) 0.035(3) 0.002(2) -0.006(2) -0.005(2) C31 0.025(3) 0.026(3) 0.041(3) -0.001(2) -0.008(2) -0.001(3) C32 0.059(5) 0.063(5) 0.053(4) 0.013(4) -0.023(4) 0.006(4) C33 0.029(4) 0.104(8) 0.073(5) 0.025(5) -0.003(4) 0.005(4) C34 0.073(4) 0.072(4) 0.096(4) -0.008(3) -0.033(4) -0.005(4) C35 0.029(3) 0.009(3) 0.038(3) 0.008(2) -0.014(2) -0.006(2) C36 0.028(3) 0.017(3) 0.042(3) 0.003(2) -0.011(2) -0.010(2) C37 0.026(3) 0.019(3) 0.036(3) 0.008(2) -0.014(2) -0.013(2) C38 0.029(3) 0.018(3) 0.036(3) 0.007(2) -0.011(2) -0.013(2) C39 0.024(3) 0.016(3) 0.037(3) 0.005(2) -0.007(2) -0.006(2) C40 0.022(3) 0.018(3) 0.043(3) 0.007(2) -0.014(2) -0.008(2) C41 0.040(3) 0.019(3) 0.037(3) 0.009(2) -0.013(3) -0.006(3) C42 0.080(6) 0.029(4) 0.048(4) 0.014(3) -0.012(4) -0.015(4) C43 0.067(5) 0.020(3) 0.056(4) 0.007(3) -0.014(3) -0.022(3) C44 0.048(4) 0.035(4) 0.075(5) 0.027(3) -0.027(4) -0.001(3) C45 0.016(2) 0.024(3) 0.031(3) 0.007(2) -0.005(2) -0.003(2) C46 0.015(2) 0.025(3) 0.036(3) -0.001(2) -0.006(2) 0.001(2) C47 0.015(2) 0.021(3) 0.048(3) 0.007(2) -0.013(2) -0.006(2) C48 0.021(3) 0.029(3) 0.034(3) 0.002(2) -0.011(2) -0.008(3) C49 0.019(3) 0.018(3) 0.035(3) 0.011(2) -0.004(2) -0.004(2) C50 0.017(3) 0.031(3) 0.031(3) 0.008(2) -0.008(2) -0.003(2) C51 0.026(3) 0.041(4) 0.030(3) 0.010(2) -0.006(2) -0.006(3) C52 0.051(4) 0.058(5) 0.034(3) 0.014(3) -0.009(3) -0.030(4) C53 0.031(3) 0.051(4) 0.033(3) 0.000(3) 0.003(3) 0.000(3) C54 0.035(4) 0.055(5) 0.044(4) 0.009(3) -0.017(3) -0.010(3) B1 0.033(4) 0.028(4) 0.031(3) 0.009(3) -0.008(3) -0.013(3) B2 0.021(3) 0.030(4) 0.031(3) 0.009(3) -0.002(2) -0.011(3) Fe1 0.0218(5) 0.0216(5) 0.0360(5) 0.0098(3) -0.0108(3) -0.0080(3) O1 0.066(3) 0.047(3) 0.027(2) 0.0165(18) -0.019(2) -0.036(3) O2 0.026(2) 0.027(2) 0.038(2) 0.0078(16) -0.0112(17) -0.0055(18) O3 0.032(2) 0.015(2) 0.040(2) 0.0103(15) -0.0164(17) -0.0038(17) O4 0.027(2) 0.024(2) 0.036(2) 0.0090(16) -0.0169(16) -0.0061(18) C55 0.084(6) 0.049(5) 0.076(5) 0.007(4) -0.031(5) -0.021(5) C56 0.038(4) 0.033(4) 0.076(5) 0.004(3) -0.027(3) -0.006(3) C57 0.040(4) 0.046(5) 0.077(5) 0.003(4) -0.029(4) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.415(8) . ? C1 C2 1.416(9) . ? C1 Fe1 2.050(6) . ? C1 H1 1.0000 . ? C2 C5 1.409(7) . ? C2 Fe1 2.037(6) . ? C2 H2 1.0000 . ? C3 C4 1.453(7) . ? C3 Fe1 2.043(6) . ? C3 H3 1.0000 . ? C4 C5 1.425(8) . ? C4 B2 1.563(8) . ? C4 Fe1 2.061(5) . ? C5 Fe1 2.044(5) . ? C5 H5 1.0000 . ? C6 C7 1.416(10) . ? C6 C8 1.419(9) . ? C6 Fe1 2.028(6) . ? C6 H6 1.0000 . ? C7 C10 1.405(8) . ? C7 Fe1 2.057(6) . ? C7 H7 1.0000 . ? C8 C9 1.426(8) . ? C8 Fe1 2.036(6) . ? C8 H8 1.0000 . ? C9 C10 1.467(8) . ? C9 B1 1.553(8) . ? C9 Fe1 2.054(6) . ? C10 Fe1 2.039(6) . ? C10 H10 1.0000 . ? C11 C16 1.514(7) . ? C11 C47 1.517(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C46 1.517(7) . ? C12 C36 1.520(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C26 1.485(8) . ? C13 C17 1.521(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C37 1.509(7) . ? C14 C27 1.513(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.373(7) . ? C15 O4 1.396(5) . ? C15 C16 1.399(7) . ? C16 C18 1.399(7) . ? C17 C20 1.377(7) . ? C18 C19 1.392(7) . ? C18 H18 0.9500 . ? C19 C20 1.409(7) . ? C19 C21 1.538(7) . ? C20 H20 0.9500 . ? C21 C24 1.530(8) . ? C21 C22 1.531(8) . ? C21 C23 1.534(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.384(8) . ? C25 O2 1.391(6) . ? C25 C26 1.402(7) . ? C26 C28 1.404(8) . ? C27 C30 1.378(7) . ? C28 C29 1.388(8) . ? C28 H28 0.9500 . ? C29 C30 1.387(7) . ? C29 C31 1.541(7) . ? C30 H30 0.9500 . ? C31 C34 1.503(10) . ? C31 C32 1.508(8) . ? C31 C33 1.537(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.377(7) . ? C35 O3 1.394(6) . ? C35 C37 1.396(7) . ? C36 C38 1.389(7) . ? C37 C39 1.393(7) . ? C38 C40 1.396(8) . ? C38 H38 0.9500 . ? C39 C40 1.395(7) . ? C39 H39 0.9500 . ? C40 C41 1.540(7) . ? C41 C42 1.530(8) . ? C41 C44 1.533(9) . ? C41 C43 1.538(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 O1 1.378(6) . ? C45 C46 1.382(7) . ? C45 C47 1.397(7) . ? C46 C49 1.398(7) . ? C47 C48 1.393(7) . ? C48 C50 1.400(7) . ? C48 H48 0.9500 . ? C49 C50 1.381(7) . ? C49 H49 0.9500 . ? C50 C51 1.546(7) . ? C51 C54 1.516(8) . ? C51 C52 1.523(8) . ? C51 C53 1.535(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? B1 O3 1.353(8) . ? B1 O1 1.373(7) . ? B2 O2 1.370(8) . ? B2 O4 1.372(7) . ? C55 C57 1.521(10) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.516(9) . ? C56 C56 1.525(13) 2_656 ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? 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 C3 C1 C2 108.7(5) . . ? C3 C1 Fe1 69.5(3) . . ? C2 C1 Fe1 69.2(3) . . ? C3 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? Fe1 C1 H1 125.6 . . ? C5 C2 C1 108.1(5) . . ? C5 C2 Fe1 70.1(3) . . ? C1 C2 Fe1 70.2(4) . . ? C5 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.0 . . ? C1 C3 C4 107.5(5) . . ? C1 C3 Fe1 70.0(4) . . ? C4 C3 Fe1 69.9(3) . . ? C1 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Fe1 C3 H3 126.2 . . ? C5 C4 C3 106.6(5) . . ? C5 C4 B2 126.3(5) . . ? C3 C4 B2 127.0(5) . . ? C5 C4 Fe1 69.0(3) . . ? C3 C4 Fe1 68.6(3) . . ? B2 C4 Fe1 124.7(4) . . ? C2 C5 C4 109.1(5) . . ? C2 C5 Fe1 69.5(3) . . ? C4 C5 Fe1 70.3(3) . . ? C2 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Fe1 C5 H5 125.5 . . ? C7 C6 C8 110.0(6) . . ? C7 C6 Fe1 70.8(4) . . ? C8 C6 Fe1 69.9(3) . . ? C7 C6 H6 125.0 . . ? C8 C6 H6 125.0 . . ? Fe1 C6 H6 125.0 . . ? C10 C7 C6 106.6(6) . . ? C10 C7 Fe1 69.3(3) . . ? C6 C7 Fe1 68.6(4) . . ? C10 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? Fe1 C7 H7 126.7 . . ? C6 C8 C9 108.2(6) . . ? C6 C8 Fe1 69.2(4) . . ? C9 C8 Fe1 70.2(3) . . ? C6 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 125.9 . . ? C8 C9 C10 105.5(5) . . ? C8 C9 B1 127.3(6) . . ? C10 C9 B1 127.1(5) . . ? C8 C9 Fe1 68.9(3) . . ? C10 C9 Fe1 68.5(3) . . ? B1 C9 Fe1 123.5(4) . . ? C7 C10 C9 109.7(6) . . ? C7 C10 Fe1 70.6(3) . . ? C9 C10 Fe1 69.5(3) . . ? C7 C10 H10 125.1 . . ? C9 C10 H10 125.1 . . ? Fe1 C10 H10 125.1 . . ? C16 C11 C47 114.4(4) . . ? C16 C11 H11A 108.7 . . ? C47 C11 H11A 108.7 . . ? C16 C11 H11B 108.7 . . ? C47 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C46 C12 C36 112.6(4) . . ? C46 C12 H12A 109.1 . . ? C36 C12 H12A 109.1 . . ? C46 C12 H12B 109.1 . . ? C36 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C26 C13 C17 109.4(4) . . ? C26 C13 H13A 109.8 . . ? C17 C13 H13A 109.8 . . ? C26 C13 H13B 109.8 . . ? C17 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? C37 C14 C27 111.2(4) . . ? C37 C14 H14A 109.4 . . ? C27 C14 H14A 109.4 . . ? C37 C14 H14B 109.4 . . ? C27 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C17 C15 O4 120.1(5) . . ? C17 C15 C16 122.3(4) . . ? O4 C15 C16 116.9(5) . . ? C15 C16 C18 117.3(4) . . ? C15 C16 C11 122.4(4) . . ? C18 C16 C11 120.3(5) . . ? C15 C17 C20 118.7(5) . . ? C15 C17 C13 122.1(5) . . ? C20 C17 C13 119.1(5) . . ? C19 C18 C16 122.4(5) . . ? C19 C18 H18 118.8 . . ? C16 C18 H18 118.8 . . ? C18 C19 C20 117.0(4) . . ? C18 C19 C21 122.6(5) . . ? C20 C19 C21 120.4(5) . . ? C17 C20 C19 122.3(5) . . ? C17 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C24 C21 C22 109.6(5) . . ? C24 C21 C23 106.6(5) . . ? C22 C21 C23 110.2(5) . . ? C24 C21 C19 111.3(4) . . ? C22 C21 C19 108.0(4) . . ? C23 C21 C19 111.2(4) . . ? 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 . . ? 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 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 O2 118.4(5) . . ? C27 C25 C26 121.7(5) . . ? O2 C25 C26 119.8(5) . . ? C25 C26 C28 117.2(5) . . ? C25 C26 C13 122.7(5) . . ? C28 C26 C13 120.1(5) . . ? C30 C27 C25 118.3(5) . . ? C30 C27 C14 120.4(5) . . ? C25 C27 C14 121.3(5) . . ? C29 C28 C26 122.8(5) . . ? C29 C28 H28 118.6 . . ? C26 C28 H28 118.6 . . ? C30 C29 C28 116.8(5) . . ? C30 C29 C31 123.2(5) . . ? C28 C29 C31 120.1(5) . . ? C27 C30 C29 123.3(5) . . ? C27 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C34 C31 C32 109.6(6) . . ? C34 C31 C33 106.0(6) . . ? C32 C31 C33 109.0(6) . . ? C34 C31 C29 113.2(5) . . ? C32 C31 C29 108.6(5) . . ? C33 C31 C29 110.4(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 O3 119.8(5) . . ? C36 C35 C37 122.2(5) . . ? O3 C35 C37 117.7(5) . . ? C35 C36 C38 118.8(5) . . ? C35 C36 C12 122.7(5) . . ? C38 C36 C12 118.5(5) . . ? C39 C37 C35 117.0(5) . . ? C39 C37 C14 120.3(5) . . ? C35 C37 C14 122.6(5) . . ? C36 C38 C40 121.8(5) . . ? C36 C38 H38 119.1 . . ? C40 C38 H38 119.1 . . ? C37 C39 C40 123.0(5) . . ? C37 C39 H39 118.5 . . ? C40 C39 H39 118.5 . . ? C39 C40 C38 117.1(5) . . ? C39 C40 C41 120.1(5) . . ? C38 C40 C41 122.5(5) . . ? C42 C41 C44 107.9(5) . . ? C42 C41 C43 108.7(5) . . ? C44 C41 C43 107.8(5) . . ? C42 C41 C40 113.5(5) . . ? C44 C41 C40 111.7(5) . . ? C43 C41 C40 107.1(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O1 C45 C46 121.8(5) . . ? O1 C45 C47 116.5(5) . . ? C46 C45 C47 121.6(5) . . ? C45 C46 C49 118.1(5) . . ? C45 C46 C12 121.4(5) . . ? C49 C46 C12 120.5(5) . . ? C48 C47 C45 117.9(5) . . ? C48 C47 C11 121.4(5) . . ? C45 C47 C11 120.6(5) . . ? C47 C48 C50 122.5(5) . . ? C47 C48 H48 118.7 . . ? C50 C48 H48 118.7 . . ? C50 C49 C46 122.9(5) . . ? C50 C49 H49 118.5 . . ? C46 C49 H49 118.5 . . ? C49 C50 C48 116.9(5) . . ? C49 C50 C51 123.0(5) . . ? C48 C50 C51 120.0(5) . . ? C54 C51 C52 109.3(5) . . ? C54 C51 C53 109.2(5) . . ? C52 C51 C53 108.6(5) . . ? C54 C51 C50 110.5(5) . . ? C52 C51 C50 111.3(5) . . ? C53 C51 C50 107.8(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O3 B1 O1 126.1(6) . . ? O3 B1 C9 116.5(5) . . ? O1 B1 C9 117.1(6) . . ? O2 B2 O4 130.1(5) . . ? O2 B2 C4 116.0(5) . . ? O4 B2 C4 113.9(5) . . ? C6 Fe1 C8 40.9(2) . . ? C6 Fe1 C2 119.5(2) . . ? C8 Fe1 C2 155.2(2) . . ? C6 Fe1 C10 67.6(3) . . ? C8 Fe1 C10 68.8(3) . . ? C2 Fe1 C10 123.5(2) . . ? C6 Fe1 C3 126.0(3) . . ? C8 Fe1 C3 108.5(3) . . ? C2 Fe1 C3 68.7(2) . . ? C10 Fe1 C3 157.4(2) . . ? C6 Fe1 C5 153.8(3) . . ? C8 Fe1 C5 163.6(2) . . ? C2 Fe1 C5 40.4(2) . . ? C10 Fe1 C5 107.1(2) . . ? C3 Fe1 C5 68.7(2) . . ? C6 Fe1 C1 108.0(2) . . ? C8 Fe1 C1 121.3(3) . . ? C2 Fe1 C1 40.5(2) . . ? C10 Fe1 C1 160.4(3) . . ? C3 Fe1 C1 40.5(2) . . ? C5 Fe1 C1 67.9(2) . . ? C6 Fe1 C9 68.8(2) . . ? C8 Fe1 C9 40.8(2) . . ? C2 Fe1 C9 162.0(2) . . ? C10 Fe1 C9 42.0(2) . . ? C3 Fe1 C9 121.2(2) . . ? C5 Fe1 C9 125.6(2) . . ? C1 Fe1 C9 156.2(3) . . ? C6 Fe1 C7 40.5(3) . . ? C8 Fe1 C7 69.1(3) . . ? C2 Fe1 C7 105.5(3) . . ? C10 Fe1 C7 40.1(2) . . ? C3 Fe1 C7 161.7(3) . . ? C5 Fe1 C7 118.7(3) . . ? C1 Fe1 C7 124.1(2) . . ? C9 Fe1 C7 69.7(2) . . ? C6 Fe1 C4 164.2(3) . . ? C8 Fe1 C4 126.7(2) . . ? C2 Fe1 C4 68.6(2) . . ? C10 Fe1 C4 120.9(2) . . ? C3 Fe1 C4 41.5(2) . . ? C5 Fe1 C4 40.6(2) . . ? C1 Fe1 C4 68.5(2) . . ? C9 Fe1 C4 107.9(2) . . ? C7 Fe1 C4 154.3(3) . . ? B1 O1 C45 137.0(5) . . ? B2 O2 C25 134.8(5) . . ? B1 O3 C35 126.9(4) . . ? B2 O4 C15 132.9(4) . . ? C57 C55 H55A 109.5 . . ? C57 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C57 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C56 114.0(7) . 2_656 ? C57 C56 H56A 108.8 . . ? C56 C56 H56A 108.8 2_656 . ? C57 C56 H56B 108.8 . . ? C56 C56 H56B 108.8 2_656 . ? H56A C56 H56B 107.6 . . ? C56 C57 C55 115.0(6) . . ? C56 C57 H57A 108.5 . . ? C55 C57 H57A 108.5 . . ? C56 C57 H57B 108.5 . . ? C55 C57 H57B 108.5 . . ? H57A C57 H57B 107.5 . . ? 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 C3 C1 C2 C5 1.7(7) . . . . ? Fe1 C1 C2 C5 60.1(4) . . . . ? C3 C1 C2 Fe1 -58.4(4) . . . . ? C2 C1 C3 C4 -1.9(7) . . . . ? Fe1 C1 C3 C4 -60.1(4) . . . . ? C2 C1 C3 Fe1 58.2(4) . . . . ? C1 C3 C4 C5 1.4(6) . . . . ? Fe1 C3 C4 C5 -58.8(4) . . . . ? C1 C3 C4 B2 178.3(5) . . . . ? Fe1 C3 C4 B2 118.0(5) . . . . ? C1 C3 C4 Fe1 60.2(4) . . . . ? C1 C2 C5 C4 -0.8(6) . . . . ? Fe1 C2 C5 C4 59.4(4) . . . . ? C1 C2 C5 Fe1 -60.2(4) . . . . ? C3 C4 C5 C2 -0.3(6) . . . . ? B2 C4 C5 C2 -177.2(5) . . . . ? Fe1 C4 C5 C2 -58.9(4) . . . . ? C3 C4 C5 Fe1 58.6(4) . . . . ? B2 C4 C5 Fe1 -118.3(5) . . . . ? C8 C6 C7 C10 0.0(7) . . . . ? Fe1 C6 C7 C10 -59.1(4) . . . . ? C8 C6 C7 Fe1 59.1(4) . . . . ? C7 C6 C8 C9 0.0(7) . . . . ? Fe1 C6 C8 C9 59.7(4) . . . . ? C7 C6 C8 Fe1 -59.7(4) . . . . ? C6 C8 C9 C10 0.0(6) . . . . ? Fe1 C8 C9 C10 59.0(4) . . . . ? C6 C8 C9 B1 -175.8(5) . . . . ? Fe1 C8 C9 B1 -116.8(6) . . . . ? C6 C8 C9 Fe1 -59.0(4) . . . . ? C6 C7 C10 C9 0.0(7) . . . . ? Fe1 C7 C10 C9 -58.7(4) . . . . ? C6 C7 C10 Fe1 58.7(4) . . . . ? C8 C9 C10 C7 0.0(7) . . . . ? B1 C9 C10 C7 175.8(5) . . . . ? Fe1 C9 C10 C7 59.3(4) . . . . ? C8 C9 C10 Fe1 -59.3(4) . . . . ? B1 C9 C10 Fe1 116.5(6) . . . . ? C17 C15 C16 C18 -1.4(8) . . . . ? O4 C15 C16 C18 -171.9(4) . . . . ? C17 C15 C16 C11 178.9(5) . . . . ? O4 C15 C16 C11 8.5(7) . . . . ? C47 C11 C16 C15 101.7(6) . . . . ? C47 C11 C16 C18 -77.9(6) . . . . ? O4 C15 C17 C20 170.7(5) . . . . ? C16 C15 C17 C20 0.5(8) . . . . ? O4 C15 C17 C13 -13.7(8) . . . . ? C16 C15 C17 C13 176.1(5) . . . . ? C26 C13 C17 C15 -80.5(6) . . . . ? C26 C13 C17 C20 95.0(6) . . . . ? C15 C16 C18 C19 2.2(8) . . . . ? C11 C16 C18 C19 -178.1(5) . . . . ? C16 C18 C19 C20 -2.1(8) . . . . ? C16 C18 C19 C21 179.4(5) . . . . ? C15 C17 C20 C19 -0.4(8) . . . . ? C13 C17 C20 C19 -176.1(5) . . . . ? C18 C19 C20 C17 1.1(8) . . . . ? C21 C19 C20 C17 179.7(5) . . . . ? C18 C19 C21 C24 -26.2(7) . . . . ? C20 C19 C21 C24 155.3(5) . . . . ? C18 C19 C21 C22 94.2(6) . . . . ? C20 C19 C21 C22 -84.3(6) . . . . ? C18 C19 C21 C23 -144.9(5) . . . . ? C20 C19 C21 C23 36.7(7) . . . . ? C27 C25 C26 C28 1.2(7) . . . . ? O2 C25 C26 C28 -173.6(4) . . . . ? C27 C25 C26 C13 -177.0(5) . . . . ? O2 C25 C26 C13 8.3(8) . . . . ? C17 C13 C26 C25 82.0(6) . . . . ? C17 C13 C26 C28 -96.1(6) . . . . ? O2 C25 C27 C30 173.1(4) . . . . ? C26 C25 C27 C30 -1.7(8) . . . . ? O2 C25 C27 C14 -8.2(7) . . . . ? C26 C25 C27 C14 177.0(5) . . . . ? C37 C14 C27 C30 80.6(6) . . . . ? C37 C14 C27 C25 -98.0(6) . . . . ? C25 C26 C28 C29 -0.5(8) . . . . ? C13 C26 C28 C29 177.7(5) . . . . ? C26 C28 C29 C30 0.3(8) . . . . ? C26 C28 C29 C31 -177.9(5) . . . . ? C25 C27 C30 C29 1.5(8) . . . . ? C14 C27 C30 C29 -177.1(5) . . . . ? C28 C29 C30 C27 -0.9(8) . . . . ? C31 C29 C30 C27 177.3(5) . . . . ? C30 C29 C31 C34 14.6(8) . . . . ? C28 C29 C31 C34 -167.4(6) . . . . ? C30 C29 C31 C32 -107.4(6) . . . . ? C28 C29 C31 C32 70.7(7) . . . . ? C30 C29 C31 C33 133.2(6) . . . . ? C28 C29 C31 C33 -48.7(7) . . . . ? O3 C35 C36 C38 170.6(4) . . . . ? C37 C35 C36 C38 -3.2(8) . . . . ? O3 C35 C36 C12 -8.8(7) . . . . ? C37 C35 C36 C12 177.4(5) . . . . ? C46 C12 C36 C35 -87.0(6) . . . . ? C46 C12 C36 C38 93.6(6) . . . . ? C36 C35 C37 C39 4.4(7) . . . . ? O3 C35 C37 C39 -169.5(4) . . . . ? C36 C35 C37 C14 -172.3(5) . . . . ? O3 C35 C37 C14 13.8(7) . . . . ? C27 C14 C37 C39 -76.6(6) . . . . ? C27 C14 C37 C35 99.9(6) . . . . ? C35 C36 C38 C40 -0.5(8) . . . . ? C12 C36 C38 C40 178.9(5) . . . . ? C35 C37 C39 C40 -2.0(7) . . . . ? C14 C37 C39 C40 174.7(5) . . . . ? C37 C39 C40 C38 -1.5(7) . . . . ? C37 C39 C40 C41 171.9(5) . . . . ? C36 C38 C40 C39 2.8(7) . . . . ? C36 C38 C40 C41 -170.5(5) . . . . ? C39 C40 C41 C42 163.5(5) . . . . ? C38 C40 C41 C42 -23.5(7) . . . . ? C39 C40 C41 C44 41.2(7) . . . . ? C38 C40 C41 C44 -145.8(5) . . . . ? C39 C40 C41 C43 -76.6(6) . . . . ? C38 C40 C41 C43 96.5(6) . . . . ? O1 C45 C46 C49 -173.7(5) . . . . ? C47 C45 C46 C49 1.7(8) . . . . ? O1 C45 C46 C12 5.2(8) . . . . ? C47 C45 C46 C12 -179.5(5) . . . . ? C36 C12 C46 C45 70.3(6) . . . . ? C36 C12 C46 C49 -110.8(5) . . . . ? O1 C45 C47 C48 172.6(5) . . . . ? C46 C45 C47 C48 -3.0(8) . . . . ? O1 C45 C47 C11 -5.9(7) . . . . ? C46 C45 C47 C11 178.5(5) . . . . ? C16 C11 C47 C48 95.1(6) . . . . ? C16 C11 C47 C45 -86.4(6) . . . . ? C45 C47 C48 C50 1.4(8) . . . . ? C11 C47 C48 C50 179.9(5) . . . . ? C45 C46 C49 C50 1.3(8) . . . . ? C12 C46 C49 C50 -177.6(5) . . . . ? C46 C49 C50 C48 -2.7(8) . . . . ? C46 C49 C50 C51 173.1(5) . . . . ? C47 C48 C50 C49 1.3(8) . . . . ? C47 C48 C50 C51 -174.7(5) . . . . ? C49 C50 C51 C54 130.2(6) . . . . ? C48 C50 C51 C54 -54.1(7) . . . . ? C49 C50 C51 C52 8.5(7) . . . . ? C48 C50 C51 C52 -175.8(5) . . . . ? C49 C50 C51 C53 -110.5(6) . . . . ? C48 C50 C51 C53 65.2(6) . . . . ? C8 C9 B1 O3 -3.6(9) . . . . ? C10 C9 B1 O3 -178.5(5) . . . . ? Fe1 C9 B1 O3 -91.4(6) . . . . ? C8 C9 B1 O1 171.1(6) . . . . ? C10 C9 B1 O1 -3.8(9) . . . . ? Fe1 C9 B1 O1 83.3(6) . . . . ? C5 C4 B2 O2 -179.6(5) . . . . ? C3 C4 B2 O2 4.1(8) . . . . ? Fe1 C4 B2 O2 92.2(6) . . . . ? C5 C4 B2 O4 2.7(8) . . . . ? C3 C4 B2 O4 -173.5(5) . . . . ? Fe1 C4 B2 O4 -85.5(6) . . . . ? C7 C6 Fe1 C8 120.8(5) . . . . ? C7 C6 Fe1 C2 -79.1(4) . . . . ? C8 C6 Fe1 C2 160.1(4) . . . . ? C7 C6 Fe1 C10 37.8(4) . . . . ? C8 C6 Fe1 C10 -83.0(4) . . . . ? C7 C6 Fe1 C3 -163.0(4) . . . . ? C8 C6 Fe1 C3 76.2(5) . . . . ? C7 C6 Fe1 C5 -45.5(7) . . . . ? C8 C6 Fe1 C5 -166.3(5) . . . . ? C7 C6 Fe1 C1 -121.8(4) . . . . ? C8 C6 Fe1 C1 117.3(4) . . . . ? C7 C6 Fe1 C9 83.2(4) . . . . ? C8 C6 Fe1 C9 -37.7(4) . . . . ? C8 C6 Fe1 C7 -120.8(5) . . . . ? C7 C6 Fe1 C4 163.7(7) . . . . ? C8 C6 Fe1 C4 42.8(10) . . . . ? C9 C8 Fe1 C6 -119.4(6) . . . . ? C6 C8 Fe1 C2 -45.0(8) . . . . ? C9 C8 Fe1 C2 -164.4(5) . . . . ? C6 C8 Fe1 C10 79.8(4) . . . . ? C9 C8 Fe1 C10 -39.6(4) . . . . ? C6 C8 Fe1 C3 -124.1(4) . . . . ? C9 C8 Fe1 C3 116.5(4) . . . . ? C6 C8 Fe1 C5 158.3(8) . . . . ? C9 C8 Fe1 C5 38.9(11) . . . . ? C6 C8 Fe1 C1 -81.4(5) . . . . ? C9 C8 Fe1 C1 159.2(3) . . . . ? C6 C8 Fe1 C9 119.4(6) . . . . ? C6 C8 Fe1 C7 36.7(4) . . . . ? C9 C8 Fe1 C7 -82.7(4) . . . . ? C6 C8 Fe1 C4 -166.7(4) . . . . ? C9 C8 Fe1 C4 73.9(4) . . . . ? C5 C2 Fe1 C6 157.8(4) . . . . ? C1 C2 Fe1 C6 -83.4(4) . . . . ? C5 C2 Fe1 C8 -170.1(6) . . . . ? C1 C2 Fe1 C8 -51.3(8) . . . . ? C5 C2 Fe1 C10 76.6(4) . . . . ? C1 C2 Fe1 C10 -164.7(3) . . . . ? C5 C2 Fe1 C3 -81.9(4) . . . . ? C1 C2 Fe1 C3 36.9(3) . . . . ? C1 C2 Fe1 C5 118.7(5) . . . . ? C5 C2 Fe1 C1 -118.7(5) . . . . ? C5 C2 Fe1 C9 44.7(9) . . . . ? C1 C2 Fe1 C9 163.4(7) . . . . ? C5 C2 Fe1 C7 116.4(4) . . . . ? C1 C2 Fe1 C7 -124.9(4) . . . . ? C5 C2 Fe1 C4 -37.2(3) . . . . ? C1 C2 Fe1 C4 81.6(4) . . . . ? C7 C10 Fe1 C6 -38.2(4) . . . . ? C9 C10 Fe1 C6 82.7(4) . . . . ? C7 C10 Fe1 C8 -82.3(4) . . . . ? C9 C10 Fe1 C8 38.5(3) . . . . ? C7 C10 Fe1 C2 73.3(5) . . . . ? C9 C10 Fe1 C2 -165.9(3) . . . . ? C7 C10 Fe1 C3 -169.8(6) . . . . ? C9 C10 Fe1 C3 -49.0(8) . . . . ? C7 C10 Fe1 C5 114.5(4) . . . . ? C9 C10 Fe1 C5 -124.6(3) . . . . ? C7 C10 Fe1 C1 42.5(9) . . . . ? C9 C10 Fe1 C1 163.4(6) . . . . ? C7 C10 Fe1 C9 -120.9(5) . . . . ? C9 C10 Fe1 C7 120.9(5) . . . . ? C7 C10 Fe1 C4 156.7(4) . . . . ? C9 C10 Fe1 C4 -82.5(4) . . . . ? C1 C3 Fe1 C6 74.7(4) . . . . ? C4 C3 Fe1 C6 -167.0(3) . . . . ? C1 C3 Fe1 C8 116.8(4) . . . . ? C4 C3 Fe1 C8 -124.9(3) . . . . ? C1 C3 Fe1 C2 -36.9(4) . . . . ? C4 C3 Fe1 C2 81.4(3) . . . . ? C1 C3 Fe1 C10 -163.9(6) . . . . ? C4 C3 Fe1 C10 -45.6(8) . . . . ? C1 C3 Fe1 C5 -80.4(4) . . . . ? C4 C3 Fe1 C5 37.9(3) . . . . ? C4 C3 Fe1 C1 118.3(5) . . . . ? C1 C3 Fe1 C9 159.9(3) . . . . ? C4 C3 Fe1 C9 -81.8(4) . . . . ? C1 C3 Fe1 C7 37.4(10) . . . . ? C4 C3 Fe1 C7 155.7(8) . . . . ? C1 C3 Fe1 C4 -118.3(5) . . . . ? C2 C5 Fe1 C6 -48.0(7) . . . . ? C4 C5 Fe1 C6 -168.3(5) . . . . ? C2 C5 Fe1 C8 165.2(9) . . . . ? C4 C5 Fe1 C8 44.9(10) . . . . ? C4 C5 Fe1 C2 -120.2(5) . . . . ? C2 C5 Fe1 C10 -121.9(4) . . . . ? C4 C5 Fe1 C10 117.9(3) . . . . ? C2 C5 Fe1 C3 81.6(4) . . . . ? C4 C5 Fe1 C3 -38.6(3) . . . . ? C2 C5 Fe1 C1 38.0(4) . . . . ? C4 C5 Fe1 C1 -82.3(4) . . . . ? C2 C5 Fe1 C9 -164.5(4) . . . . ? C4 C5 Fe1 C9 75.3(4) . . . . ? C2 C5 Fe1 C7 -79.9(4) . . . . ? C4 C5 Fe1 C7 159.8(3) . . . . ? C2 C5 Fe1 C4 120.2(5) . . . . ? C3 C1 Fe1 C6 -124.9(4) . . . . ? C2 C1 Fe1 C6 114.6(4) . . . . ? C3 C1 Fe1 C8 -82.0(4) . . . . ? C2 C1 Fe1 C8 157.5(3) . . . . ? C3 C1 Fe1 C2 120.6(5) . . . . ? C3 C1 Fe1 C10 161.5(6) . . . . ? C2 C1 Fe1 C10 41.0(8) . . . . ? C2 C1 Fe1 C3 -120.6(5) . . . . ? C3 C1 Fe1 C5 82.7(4) . . . . ? C2 C1 Fe1 C5 -37.8(3) . . . . ? C3 C1 Fe1 C9 -46.8(7) . . . . ? C2 C1 Fe1 C9 -167.4(5) . . . . ? C3 C1 Fe1 C7 -166.7(4) . . . . ? C2 C1 Fe1 C7 72.7(4) . . . . ? C3 C1 Fe1 C4 38.8(3) . . . . ? C2 C1 Fe1 C4 -81.8(4) . . . . ? C8 C9 Fe1 C6 37.7(4) . . . . ? C10 C9 Fe1 C6 -79.6(4) . . . . ? B1 C9 Fe1 C6 159.3(6) . . . . ? C10 C9 Fe1 C8 -117.3(5) . . . . ? B1 C9 Fe1 C8 121.6(7) . . . . ? C8 C9 Fe1 C2 158.5(7) . . . . ? C10 C9 Fe1 C2 41.2(9) . . . . ? B1 C9 Fe1 C2 -79.9(9) . . . . ? C8 C9 Fe1 C10 117.3(5) . . . . ? B1 C9 Fe1 C10 -121.1(6) . . . . ? C8 C9 Fe1 C3 -82.4(4) . . . . ? C10 C9 Fe1 C3 160.2(3) . . . . ? B1 C9 Fe1 C3 39.1(6) . . . . ? C8 C9 Fe1 C5 -167.4(4) . . . . ? C10 C9 Fe1 C5 75.3(4) . . . . ? B1 C9 Fe1 C5 -45.8(6) . . . . ? C8 C9 Fe1 C1 -48.9(7) . . . . ? C10 C9 Fe1 C1 -166.2(5) . . . . ? B1 C9 Fe1 C1 72.7(7) . . . . ? C8 C9 Fe1 C7 81.2(4) . . . . ? C10 C9 Fe1 C7 -36.2(4) . . . . ? B1 C9 Fe1 C7 -157.3(6) . . . . ? C8 C9 Fe1 C4 -126.0(4) . . . . ? C10 C9 Fe1 C4 116.7(4) . . . . ? B1 C9 Fe1 C4 -4.4(5) . . . . ? C10 C7 Fe1 C6 118.5(5) . . . . ? C10 C7 Fe1 C8 81.5(4) . . . . ? C6 C7 Fe1 C8 -37.0(3) . . . . ? C10 C7 Fe1 C2 -124.0(4) . . . . ? C6 C7 Fe1 C2 117.5(4) . . . . ? C6 C7 Fe1 C10 -118.5(5) . . . . ? C10 C7 Fe1 C3 167.5(7) . . . . ? C6 C7 Fe1 C3 49.0(10) . . . . ? C10 C7 Fe1 C5 -82.6(4) . . . . ? C6 C7 Fe1 C5 159.0(3) . . . . ? C10 C7 Fe1 C1 -164.1(4) . . . . ? C6 C7 Fe1 C1 77.4(4) . . . . ? C10 C7 Fe1 C9 37.8(4) . . . . ? C6 C7 Fe1 C9 -80.7(4) . . . . ? C10 C7 Fe1 C4 -51.4(7) . . . . ? C6 C7 Fe1 C4 -169.9(4) . . . . ? C5 C4 Fe1 C6 160.7(7) . . . . ? C3 C4 Fe1 C6 42.2(9) . . . . ? B2 C4 Fe1 C6 -78.8(9) . . . . ? C5 C4 Fe1 C8 -165.6(3) . . . . ? C3 C4 Fe1 C8 75.9(4) . . . . ? B2 C4 Fe1 C8 -45.1(6) . . . . ? C5 C4 Fe1 C2 37.0(3) . . . . ? C3 C4 Fe1 C2 -81.6(4) . . . . ? B2 C4 Fe1 C2 157.4(5) . . . . ? C5 C4 Fe1 C10 -80.1(4) . . . . ? C3 C4 Fe1 C10 161.3(3) . . . . ? B2 C4 Fe1 C10 40.3(6) . . . . ? C5 C4 Fe1 C3 118.6(5) . . . . ? B2 C4 Fe1 C3 -121.0(6) . . . . ? C3 C4 Fe1 C5 -118.6(5) . . . . ? B2 C4 Fe1 C5 120.4(6) . . . . ? C5 C4 Fe1 C1 80.7(4) . . . . ? C3 C4 Fe1 C1 -37.9(4) . . . . ? B2 C4 Fe1 C1 -158.9(5) . . . . ? C5 C4 Fe1 C9 -124.3(3) . . . . ? C3 C4 Fe1 C9 117.2(4) . . . . ? B2 C4 Fe1 C9 -3.8(5) . . . . ? C5 C4 Fe1 C7 -44.1(6) . . . . ? C3 C4 Fe1 C7 -162.7(5) . . . . ? B2 C4 Fe1 C7 76.3(7) . . . . ? O3 B1 O1 C45 -66.4(10) . . . . ? C9 B1 O1 C45 119.5(7) . . . . ? C46 C45 O1 B1 3.6(10) . . . . ? C47 C45 O1 B1 -172.0(7) . . . . ? O4 B2 O2 C25 -26.0(10) . . . . ? C4 B2 O2 C25 156.9(5) . . . . ? C27 C25 O2 B2 151.2(6) . . . . ? C26 C25 O2 B2 -33.9(8) . . . . ? O1 B1 O3 C35 23.0(9) . . . . ? C9 B1 O3 C35 -162.9(5) . . . . ? C36 C35 O3 B1 47.3(7) . . . . ? C37 C35 O3 B1 -138.6(5) . . . . ? O2 B2 O4 C15 21.3(10) . . . . ? C4 B2 O4 C15 -161.4(5) . . . . ? C17 C15 O4 B2 42.3(8) . . . . ? C16 C15 O4 B2 -147.1(5) . . . . ? C56 C56 C57 C55 -175.7(7) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.21 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.075 _refine_diff_density_min -2.014 _refine_diff_density_rms 0.136