Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ' ALDRIDGES@CARDIFF.AC.UK ' _publ_contact_author_name 'Dr S Aldridge' loop_ _publ_author_name S.Aldridge J.K.Day D.L.Kays 'Li-ling Ooi' A.Rossin # Attachment '7a.cif' data_sa0435 _database_code_depnum_ccdc_archive 'CCDC 277456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0435 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 B Cl Fe N O2' _chemical_formula_weight 323.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7410(4) _cell_length_b 13.9170(4) _cell_length_c 19.0830(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3118.15(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15241 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7647 _exptl_absorpt_correction_T_max 0.8950 _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 22231 _diffrn_reflns_av_R_equivalents 0.1524 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3175 _reflns_number_gt 2030 _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^)+(0.0533P)^2^+0.8412P] 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 3175 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.1053(4) 0.1989(3) 0.0413(2) 0.0359(10) Uani 1 1 d . . . C2 C 0.1126(3) 0.0428(3) 0.1039(2) 0.0286(9) Uani 1 1 d . . . C3 C 0.1868(4) -0.0116(3) -0.0393(2) 0.0326(10) Uani 1 1 d . . . H3 H 0.1318 -0.0616 -0.0419 0.039 Uiso 1 1 calc R . . C4 C 0.2912(3) -0.0153(3) -0.0020(2) 0.0291(10) Uani 1 1 d . . . H4 H 0.3182 -0.0680 0.0249 0.035 Uiso 1 1 calc R . . C5 C 0.3482(4) 0.0735(3) -0.0119(2) 0.0364(11) Uani 1 1 d . . . H5 H 0.4202 0.0910 0.0069 0.044 Uiso 1 1 calc R . . C6 C 0.2784(4) 0.1311(3) -0.0548(2) 0.0401(12) Uani 1 1 d . . . H6 H 0.2953 0.1945 -0.0700 0.048 Uiso 1 1 calc R . . C7 C 0.1789(4) 0.0784(3) -0.0715(2) 0.0393(11) Uani 1 1 d . . . H7 H 0.1175 0.1003 -0.0996 0.047 Uiso 1 1 calc R . . C8 C 0.3459(3) 0.0055(2) 0.1785(2) 0.0277(9) Uani 1 1 d . . . H8 H 0.2911 -0.0192 0.1426 0.033 Uiso 1 1 calc R . . C9 C 0.2932(4) -0.0144(3) 0.2497(2) 0.0478(13) Uani 1 1 d . . . H9A H 0.3456 0.0066 0.2866 0.072 Uiso 1 1 calc R . . H9B H 0.2787 -0.0834 0.2546 0.072 Uiso 1 1 calc R . . H9C H 0.2212 0.0208 0.2539 0.072 Uiso 1 1 calc R . . C10 C 0.4568(4) -0.0491(3) 0.1677(2) 0.0490(13) Uani 1 1 d . . . H10A H 0.4902 -0.0310 0.1225 0.073 Uiso 1 1 calc R . . H10B H 0.4415 -0.1183 0.1681 0.073 Uiso 1 1 calc R . . H10C H 0.5100 -0.0331 0.2054 0.073 Uiso 1 1 calc R . . C11 C 0.4423(4) 0.1559(3) 0.2149(2) 0.0357(11) Uani 1 1 d . . . H11 H 0.4701 0.1027 0.2456 0.043 Uiso 1 1 calc R . . C12 C 0.3850(5) 0.2287(3) 0.2640(3) 0.0621(16) Uani 1 1 d . . . H12A H 0.3637 0.2861 0.2373 0.093 Uiso 1 1 calc R . . H12B H 0.4381 0.2466 0.3014 0.093 Uiso 1 1 calc R . . H12C H 0.3166 0.1999 0.2846 0.093 Uiso 1 1 calc R . . C13 C 0.5470(4) 0.1955(3) 0.1785(3) 0.0627(16) Uani 1 1 d . . . H13A H 0.5794 0.1461 0.1478 0.094 Uiso 1 1 calc R . . H13B H 0.6037 0.2142 0.2136 0.094 Uiso 1 1 calc R . . H13C H 0.5258 0.2518 0.1505 0.094 Uiso 1 1 calc R . . B1 B 0.2980(4) 0.1552(3) 0.1119(2) 0.0255(10) Uani 1 1 d . . . Cl1 Cl 0.32376(11) 0.28467(7) 0.10003(7) 0.0538(4) Uani 1 1 d . . . Fe1 Fe 0.19114(5) 0.09751(4) 0.03783(3) 0.02341(19) Uani 1 1 d . . . N1 N 0.3586(3) 0.11093(19) 0.16547(15) 0.0221(7) Uani 1 1 d . . . O1 O 0.0461(3) 0.2652(2) 0.04329(18) 0.0599(10) Uani 1 1 d . . . O2 O 0.0576(2) 0.0081(2) 0.14757(15) 0.0432(8) 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 0.032(3) 0.035(2) 0.041(2) 0.000(2) -0.013(2) 0.005(2) C2 0.020(2) 0.036(2) 0.030(2) -0.0054(18) -0.0041(19) -0.0002(18) C3 0.041(3) 0.028(2) 0.030(2) -0.0079(17) 0.001(2) -0.0051(19) C4 0.033(3) 0.029(2) 0.026(2) -0.0042(17) 0.0068(19) 0.0051(18) C5 0.035(3) 0.045(3) 0.029(2) -0.0029(19) 0.011(2) -0.006(2) C6 0.055(3) 0.036(2) 0.030(2) 0.0059(19) 0.010(2) -0.006(2) C7 0.045(3) 0.047(3) 0.026(2) -0.0011(19) -0.005(2) 0.002(2) C8 0.031(2) 0.023(2) 0.029(2) 0.0046(16) -0.0076(18) -0.0028(18) C9 0.053(3) 0.058(3) 0.033(2) 0.008(2) -0.011(2) -0.022(2) C10 0.054(3) 0.033(2) 0.060(3) -0.009(2) -0.021(3) 0.018(2) C11 0.029(3) 0.029(2) 0.050(3) -0.001(2) -0.019(2) -0.0041(19) C12 0.059(4) 0.052(3) 0.075(4) -0.032(3) -0.027(3) 0.005(3) C13 0.033(3) 0.058(3) 0.098(4) 0.027(3) -0.021(3) -0.020(2) B1 0.024(3) 0.018(2) 0.035(3) -0.0041(18) 0.002(2) 0.0004(19) Cl1 0.0615(9) 0.0198(5) 0.0800(9) 0.0090(5) -0.0350(7) -0.0066(5) Fe1 0.0220(3) 0.0220(3) 0.0262(3) 0.0011(2) -0.0023(3) 0.0016(2) N1 0.0158(18) 0.0212(15) 0.0294(17) -0.0028(13) -0.0065(14) -0.0015(13) O1 0.049(2) 0.0444(19) 0.086(3) -0.0099(17) -0.024(2) 0.0231(17) O2 0.0288(18) 0.0561(19) 0.0447(18) -0.0023(15) 0.0108(15) -0.0034(15) _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 O1 1.155(5) . ? C1 Fe1 1.735(4) . ? C2 O2 1.160(4) . ? C2 Fe1 1.738(4) . ? C3 C7 1.398(5) . ? C3 C4 1.418(5) . ? C3 Fe1 2.115(4) . ? C3 H3 0.9500 . ? C4 C5 1.418(5) . ? C4 Fe1 2.103(4) . ? C4 H4 0.9500 . ? C5 C6 1.407(6) . ? C5 Fe1 2.100(4) . ? C5 H5 0.9500 . ? C6 C7 1.416(6) . ? C6 Fe1 2.096(4) . ? C6 H6 0.9500 . ? C7 Fe1 2.107(4) . ? C7 H7 0.9500 . ? C8 N1 1.496(4) . ? C8 C9 1.519(6) . ? C8 C10 1.521(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.499(5) . ? C11 C13 1.516(6) . ? C11 C12 1.535(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? B1 N1 1.389(5) . ? B1 Cl1 1.841(4) . ? B1 Fe1 2.054(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 O1 C1 Fe1 178.5(4) . . ? O2 C2 Fe1 178.0(4) . . ? C7 C3 C4 108.0(4) . . ? C7 C3 Fe1 70.4(2) . . ? C4 C3 Fe1 69.9(2) . . ? C7 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe1 C3 H3 125.4 . . ? C3 C4 C5 108.0(4) . . ? C3 C4 Fe1 70.8(2) . . ? C5 C4 Fe1 70.2(2) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 124.6 . . ? C6 C5 C4 107.4(4) . . ? C6 C5 Fe1 70.2(3) . . ? C4 C5 Fe1 70.4(2) . . ? C6 C5 H5 126.3 . . ? C4 C5 H5 126.3 . . ? Fe1 C5 H5 124.7 . . ? C5 C6 C7 108.4(4) . . ? C5 C6 Fe1 70.6(2) . . ? C7 C6 Fe1 70.7(2) . . ? C5 C6 H6 125.8 . . ? C7 C6 H6 125.8 . . ? Fe1 C6 H6 124.5 . . ? C3 C7 C6 108.1(4) . . ? C3 C7 Fe1 71.0(2) . . ? C6 C7 Fe1 69.9(2) . . ? C3 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe1 C7 H7 124.8 . . ? N1 C8 C9 111.6(3) . . ? N1 C8 C10 112.4(3) . . ? C9 C8 C10 112.3(3) . . ? N1 C8 H8 106.7 . . ? C9 C8 H8 106.7 . . ? C10 C8 H8 106.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C13 113.3(4) . . ? N1 C11 C12 111.9(4) . . ? C13 C11 C12 113.3(4) . . ? N1 C11 H11 105.9 . . ? C13 C11 H11 105.9 . . ? C12 C11 H11 105.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 B1 Cl1 116.1(3) . . ? N1 B1 Fe1 130.2(3) . . ? Cl1 B1 Fe1 113.5(2) . . ? C1 Fe1 C2 91.18(19) . . ? C1 Fe1 B1 90.60(18) . . ? C2 Fe1 B1 89.77(17) . . ? C1 Fe1 C6 97.75(19) . . ? C2 Fe1 C6 165.68(17) . . ? B1 Fe1 C6 101.24(18) . . ? C1 Fe1 C5 131.01(18) . . ? C2 Fe1 C5 136.40(17) . . ? B1 Fe1 C5 80.64(17) . . ? C6 Fe1 C5 39.19(17) . . ? C1 Fe1 C4 160.96(17) . . ? C2 Fe1 C4 103.37(16) . . ? B1 Fe1 C4 101.51(17) . . ? C6 Fe1 C4 65.70(16) . . ? C5 Fe1 C4 39.44(15) . . ? C1 Fe1 C7 95.80(18) . . ? C2 Fe1 C7 128.78(17) . . ? B1 Fe1 C7 140.57(18) . . ? C6 Fe1 C7 39.36(16) . . ? C5 Fe1 C7 65.93(17) . . ? C4 Fe1 C7 65.54(16) . . ? C1 Fe1 C3 126.62(18) . . ? C2 Fe1 C3 100.19(17) . . ? B1 Fe1 C3 140.75(17) . . ? C6 Fe1 C3 65.50(16) . . ? C5 Fe1 C3 65.96(16) . . ? C4 Fe1 C3 39.29(14) . . ? C7 Fe1 C3 38.67(15) . . ? B1 N1 C8 120.4(3) . . ? B1 N1 C11 127.8(3) . . ? C8 N1 C11 111.8(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 C7 C3 C4 C5 -0.4(4) . . . . ? Fe1 C3 C4 C5 -60.6(3) . . . . ? C7 C3 C4 Fe1 60.3(3) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? Fe1 C4 C5 C6 -60.8(3) . . . . ? C3 C4 C5 Fe1 61.0(3) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? Fe1 C5 C6 C7 -60.9(3) . . . . ? C4 C5 C6 Fe1 60.9(3) . . . . ? C4 C3 C7 C6 0.3(5) . . . . ? Fe1 C3 C7 C6 60.3(3) . . . . ? C4 C3 C7 Fe1 -60.0(3) . . . . ? C5 C6 C7 C3 -0.1(5) . . . . ? Fe1 C6 C7 C3 -61.0(3) . . . . ? C5 C6 C7 Fe1 60.8(3) . . . . ? O1 C1 Fe1 C2 -58(16) . . . . ? O1 C1 Fe1 B1 -148(16) . . . . ? O1 C1 Fe1 C6 110(16) . . . . ? O1 C1 Fe1 C5 134(16) . . . . ? O1 C1 Fe1 C4 82(16) . . . . ? O1 C1 Fe1 C7 71(16) . . . . ? O1 C1 Fe1 C3 45(16) . . . . ? O2 C2 Fe1 C1 18(10) . . . . ? O2 C2 Fe1 B1 109(10) . . . . ? O2 C2 Fe1 C6 -110(10) . . . . ? O2 C2 Fe1 C5 -175(100) . . . . ? O2 C2 Fe1 C4 -149(10) . . . . ? O2 C2 Fe1 C7 -80(10) . . . . ? O2 C2 Fe1 C3 -109(10) . . . . ? N1 B1 Fe1 C1 144.8(4) . . . . ? Cl1 B1 Fe1 C1 -40.3(3) . . . . ? N1 B1 Fe1 C2 53.6(4) . . . . ? Cl1 B1 Fe1 C2 -131.5(2) . . . . ? N1 B1 Fe1 C6 -117.2(4) . . . . ? Cl1 B1 Fe1 C6 57.7(3) . . . . ? N1 B1 Fe1 C5 -83.7(4) . . . . ? Cl1 B1 Fe1 C5 91.3(2) . . . . ? N1 B1 Fe1 C4 -50.0(4) . . . . ? Cl1 B1 Fe1 C4 124.9(2) . . . . ? N1 B1 Fe1 C7 -115.3(4) . . . . ? Cl1 B1 Fe1 C7 59.6(4) . . . . ? N1 B1 Fe1 C3 -52.3(5) . . . . ? Cl1 B1 Fe1 C3 122.6(2) . . . . ? C5 C6 Fe1 C1 151.8(3) . . . . ? C7 C6 Fe1 C1 -89.7(3) . . . . ? C5 C6 Fe1 C2 -80.1(8) . . . . ? C7 C6 Fe1 C2 38.4(9) . . . . ? C5 C6 Fe1 B1 59.6(3) . . . . ? C7 C6 Fe1 B1 178.1(3) . . . . ? C7 C6 Fe1 C5 118.5(4) . . . . ? C5 C6 Fe1 C4 -38.1(2) . . . . ? C7 C6 Fe1 C4 80.4(3) . . . . ? C5 C6 Fe1 C7 -118.5(4) . . . . ? C5 C6 Fe1 C3 -81.4(3) . . . . ? C7 C6 Fe1 C3 37.1(3) . . . . ? C6 C5 Fe1 C1 -38.4(4) . . . . ? C4 C5 Fe1 C1 -156.2(3) . . . . ? C6 C5 Fe1 C2 159.3(3) . . . . ? C4 C5 Fe1 C2 41.5(4) . . . . ? C6 C5 Fe1 B1 -121.0(3) . . . . ? C4 C5 Fe1 B1 121.2(3) . . . . ? C4 C5 Fe1 C6 -117.8(4) . . . . ? C6 C5 Fe1 C4 117.8(4) . . . . ? C6 C5 Fe1 C7 37.6(3) . . . . ? C4 C5 Fe1 C7 -80.2(3) . . . . ? C6 C5 Fe1 C3 80.1(3) . . . . ? C4 C5 Fe1 C3 -37.6(2) . . . . ? C3 C4 Fe1 C1 -49.1(6) . . . . ? C5 C4 Fe1 C1 69.1(6) . . . . ? C3 C4 Fe1 C2 89.8(3) . . . . ? C5 C4 Fe1 C2 -152.0(3) . . . . ? C3 C4 Fe1 B1 -177.7(2) . . . . ? C5 C4 Fe1 B1 -59.4(3) . . . . ? C3 C4 Fe1 C6 -80.4(3) . . . . ? C5 C4 Fe1 C6 37.8(3) . . . . ? C3 C4 Fe1 C5 -118.2(3) . . . . ? C3 C4 Fe1 C7 -37.0(2) . . . . ? C5 C4 Fe1 C7 81.2(3) . . . . ? C5 C4 Fe1 C3 118.2(3) . . . . ? C3 C7 Fe1 C1 -146.4(3) . . . . ? C6 C7 Fe1 C1 95.2(3) . . . . ? C3 C7 Fe1 C2 -50.1(3) . . . . ? C6 C7 Fe1 C2 -168.6(3) . . . . ? C3 C7 Fe1 B1 115.6(3) . . . . ? C6 C7 Fe1 B1 -2.9(4) . . . . ? C3 C7 Fe1 C6 118.5(4) . . . . ? C3 C7 Fe1 C5 81.0(3) . . . . ? C6 C7 Fe1 C5 -37.4(3) . . . . ? C3 C7 Fe1 C4 37.6(2) . . . . ? C6 C7 Fe1 C4 -80.9(3) . . . . ? C6 C7 Fe1 C3 -118.5(4) . . . . ? C7 C3 Fe1 C1 43.4(4) . . . . ? C4 C3 Fe1 C1 162.1(3) . . . . ? C7 C3 Fe1 C2 142.6(3) . . . . ? C4 C3 Fe1 C2 -98.7(2) . . . . ? C7 C3 Fe1 B1 -115.1(3) . . . . ? C4 C3 Fe1 B1 3.6(4) . . . . ? C7 C3 Fe1 C6 -37.8(3) . . . . ? C4 C3 Fe1 C6 81.0(3) . . . . ? C7 C3 Fe1 C5 -80.9(3) . . . . ? C4 C3 Fe1 C5 37.8(2) . . . . ? C7 C3 Fe1 C4 -118.7(4) . . . . ? C4 C3 Fe1 C7 118.7(4) . . . . ? Cl1 B1 N1 C8 -178.6(3) . . . . ? Fe1 B1 N1 C8 -3.8(6) . . . . ? Cl1 B1 N1 C11 0.2(6) . . . . ? Fe1 B1 N1 C11 175.1(3) . . . . ? C9 C8 N1 B1 -115.4(4) . . . . ? C10 C8 N1 B1 117.5(4) . . . . ? C9 C8 N1 C11 65.6(4) . . . . ? C10 C8 N1 C11 -61.6(4) . . . . ? C13 C11 N1 B1 -63.4(5) . . . . ? C12 C11 N1 B1 66.1(5) . . . . ? C13 C11 N1 C8 115.5(4) . . . . ? C12 C11 N1 C8 -115.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.505 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.092 # Attachment '13.cif' data_sa0526 _database_code_depnum_ccdc_archive 'CCDC 277457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H46 B2 F24 Fe N O3 P' _chemical_formula_weight 1429.45 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' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 '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 13.0324(2) _cell_length_b 13.9949(2) _cell_length_c 19.1002(3) _cell_angle_alpha 68.7080(10) _cell_angle_beta 83.7430(10) _cell_angle_gamma 87.4800(10) _cell_volume 3226.47(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details 'Soratv (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 'Nonius CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51247 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.54 _reflns_number_total 14704 _reflns_number_gt 8994 _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. During the course of refinement, four of the CF3 groups of the BArf anion were found to be disordered. The disorder in each was modelled over two sites, with the occupancy of each site refined using a free variable. Only the higher occupancy sites were refined anisotropically. ; _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^)+(0.0916P)^2^+0.2013P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14704 _refine_ls_number_parameters 913 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1992 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.222 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.07617(4) -0.06273(4) -0.26656(3) 0.02616(17) Uani 1 1 d . . . P1 P -0.14228(7) -0.22223(7) -0.30690(5) 0.0240(2) Uani 1 1 d . . . F1 F 0.3615(4) 0.2004(3) -0.4879(2) 0.0535(12) Uani 0.820(9) 1 d PU A 1 F1A F 0.3224(18) 0.176(2) -0.4707(14) 0.067(7) Uiso 0.180(9) 1 d P A 2 F2 F 0.2913(4) 0.0562(4) -0.43722(19) 0.093(2) Uani 0.820(9) 1 d PU A 1 F2A F 0.3726(13) 0.0200(10) -0.4455(8) 0.037(5) Uiso 0.180(9) 1 d P A 2 F3 F 0.4526(5) 0.0705(5) -0.4773(2) 0.110(2) Uani 0.820(9) 1 d PU A 1 F3A F 0.4579(19) 0.144(2) -0.4849(13) 0.093(8) Uiso 0.180(9) 1 d P A 2 F4 F 0.3688(2) -0.1318(2) -0.12658(16) 0.0776(10) Uani 1 1 d U . . F5 F 0.4564(3) -0.18472(19) -0.20398(17) 0.0771(9) Uani 1 1 d U . . F6 F 0.5293(2) -0.1147(2) -0.14246(18) 0.0833(11) Uani 1 1 d U . . F7 F 0.1360(2) 0.0573(2) -0.03624(15) 0.0636(8) Uani 1 1 d U . . F8 F -0.0116(2) 0.1272(2) -0.05244(16) 0.0742(9) Uani 1 1 d U . . F9 F 0.1029(3) 0.1887(3) -0.00816(15) 0.0808(10) Uani 1 1 d U . . F10 F 0.0429(4) 0.4949(3) -0.3358(3) 0.0684(16) Uani 0.740(8) 1 d PU B 1 F10A F -0.0170(12) 0.4600(12) -0.3080(8) 0.071(4) Uiso 0.260(8) 1 d PD B 2 F11 F 0.0478(5) 0.3756(5) -0.3795(3) 0.094(2) Uani 0.740(8) 1 d PU B 1 F11A F 0.0809(8) 0.4325(9) -0.3918(6) 0.049(3) Uiso 0.260(8) 1 d PD B 2 F12 F -0.0662(3) 0.3814(4) -0.2927(3) 0.094(2) Uani 0.740(8) 1 d PU B 1 F12A F -0.0349(9) 0.3327(8) -0.3320(6) 0.052(3) Uiso 0.260(8) 1 d P B 2 F13 F 0.3053(3) 0.6658(2) -0.3552(2) 0.0870(10) Uani 1 1 d U . . F14 F 0.4564(3) 0.7259(2) -0.3544(2) 0.0909(11) Uani 1 1 d U . . F15 F 0.3989(3) 0.7342(2) -0.4549(2) 0.0935(11) Uani 1 1 d U . . F16 F 0.6949(3) 0.3886(3) -0.4778(2) 0.0820(17) Uani 0.842(8) 1 d PU C 1 F16A F 0.7478(17) 0.3866(19) -0.4213(13) 0.077(8) Uiso 0.158(8) 1 d P C 2 F17 F 0.7683(3) 0.4652(5) -0.4199(2) 0.0820(17) Uani 0.842(8) 1 d PU C 1 F17A F 0.7573(14) 0.5295(14) -0.4495(11) 0.043(5) Uiso 0.158(8) 1 d P C 2 F18 F 0.7006(3) 0.5489(4) -0.5216(2) 0.0893(17) Uani 0.842(8) 1 d PU C 1 F18A F 0.6886(15) 0.4908(18) -0.5232(12) 0.057(6) Uiso 0.158(8) 1 d P C 2 F19 F 0.4028(3) 0.4480(2) -0.03677(16) 0.0754(9) Uani 1 1 d U . . F20 F 0.3524(2) 0.2977(2) 0.03527(16) 0.0699(8) Uani 1 1 d U . . F21 F 0.4973(2) 0.3507(2) 0.04545(14) 0.0618(8) Uani 1 1 d U . . F22 F 0.7624(5) 0.1480(8) -0.1566(5) 0.117(3) Uani 0.680(8) 1 d PDU D 1 F22A F 0.7254(8) 0.0842(7) -0.1101(6) 0.063(3) Uiso 0.320(8) 1 d PD D 2 F23 F 0.8000(3) 0.2728(5) -0.1280(3) 0.106(3) Uani 0.680(8) 1 d PDU D 1 F23A F 0.7861(8) 0.2201(9) -0.1761(6) 0.066(4) Uiso 0.320(8) 1 d PD D 2 F24 F 0.7538(4) 0.1383(5) -0.0390(3) 0.0616(15) Uani 0.680(8) 1 d PDU D 1 F24A F 0.7829(12) 0.1772(13) -0.0593(9) 0.101(6) Uiso 0.320(8) 1 d PD D 2 O1 O 0.2571(2) -0.1629(2) -0.3092(2) 0.0556(9) Uani 1 1 d . . . O2 O 0.0219(2) -0.0055(2) -0.41991(16) 0.0489(8) Uani 1 1 d . . . O3 O -0.07431(18) -0.23715(17) -0.24258(13) 0.0275(6) Uani 1 1 d . . . N1 N 0.0559(2) -0.2932(2) -0.16001(17) 0.0295(7) Uani 1 1 d . . . C1 C 0.1009(5) -0.0372(4) -0.1683(3) 0.0598(15) Uani 1 1 d . . . H1 H 0.1361 -0.0836 -0.1285 0.072 Uiso 1 1 calc R . . C2 C -0.0029(4) -0.0370(4) -0.1746(3) 0.0599(15) Uani 1 1 d . . . H2 H -0.0520 -0.0835 -0.1398 0.072 Uiso 1 1 calc R . . C3 C -0.0237(3) 0.0410(4) -0.2389(3) 0.0518(13) Uani 1 1 d . . . H3 H -0.0899 0.0585 -0.2566 0.062 Uiso 1 1 calc R . . C4 C 0.1463(3) 0.0428(4) -0.2309(3) 0.0482(12) Uani 1 1 d . . . H4 H 0.2174 0.0603 -0.2410 0.058 Uiso 1 1 calc R . . C5 C 0.0689(4) 0.0915(3) -0.2750(2) 0.0489(12) Uani 1 1 d . . . H5 H 0.0767 0.1485 -0.3212 0.059 Uiso 1 1 calc R . . C6 C 0.1862(3) -0.1234(3) -0.2906(2) 0.0356(9) Uani 1 1 d . . . C7 C 0.0397(3) -0.0335(3) -0.3578(2) 0.0345(9) Uani 1 1 d . . . C8 C 0.0015(3) -0.3941(3) -0.1207(2) 0.0383(10) Uani 1 1 d . . . H8 H 0.0420 -0.4336 -0.0776 0.046 Uiso 1 1 calc R . . C9 C -0.1069(3) -0.3811(3) -0.0855(2) 0.0488(12) Uani 1 1 d . . . H9A H -0.1041 -0.3355 -0.0571 0.073 Uiso 1 1 calc R . . H9B H -0.1335 -0.4481 -0.0514 0.073 Uiso 1 1 calc R . . H9C H -0.1527 -0.3512 -0.1256 0.073 Uiso 1 1 calc R . . C10 C 0.0036(4) -0.4582(3) -0.1701(3) 0.0482(11) Uani 1 1 d . . . H10A H -0.0356 -0.4231 -0.2134 0.072 Uiso 1 1 calc R . . H10B H -0.0274 -0.5252 -0.1407 0.072 Uiso 1 1 calc R . . H10C H 0.0752 -0.4677 -0.1882 0.072 Uiso 1 1 calc R . . C11 C 0.1546(3) -0.2906(3) -0.1281(2) 0.0419(11) Uani 1 1 d . . . H11 H 0.1857 -0.2217 -0.1572 0.050 Uiso 1 1 calc R . . C12 C 0.2320(4) -0.3691(4) -0.1386(3) 0.0592(13) Uani 1 1 d . . . H12A H 0.2047 -0.4382 -0.1107 0.089 Uiso 1 1 calc R . . H12B H 0.2968 -0.3614 -0.1196 0.089 Uiso 1 1 calc R . . H12C H 0.2448 -0.3587 -0.1924 0.089 Uiso 1 1 calc R . . C13 C 0.1385(4) -0.3002(4) -0.0456(3) 0.0574(14) Uani 1 1 d . . . H13A H 0.0859 -0.2508 -0.0396 0.086 Uiso 1 1 calc R . . H13B H 0.2036 -0.2861 -0.0299 0.086 Uiso 1 1 calc R . . H13C H 0.1157 -0.3699 -0.0141 0.086 Uiso 1 1 calc R . . C14 C -0.2040(3) -0.0996(3) -0.3319(2) 0.0300(8) Uani 1 1 d . . . C15 C -0.2192(3) -0.0404(3) -0.4052(2) 0.0414(10) Uani 1 1 d . . . H15 H -0.1929 -0.0632 -0.4449 0.050 Uiso 1 1 calc R . . C16 C -0.2424(3) -0.0650(3) -0.2736(2) 0.0365(9) Uani 1 1 d . . . H16 H -0.2323 -0.1053 -0.2227 0.044 Uiso 1 1 calc R . . C17 C -0.2724(4) 0.0519(3) -0.4220(3) 0.0558(13) Uani 1 1 d . . . H17 H -0.2831 0.0919 -0.4728 0.067 Uiso 1 1 calc R . . C18 C -0.2949(3) 0.0274(4) -0.2899(3) 0.0489(12) Uani 1 1 d . . . H18 H -0.3206 0.0510 -0.2506 0.059 Uiso 1 1 calc R . . C19 C -0.3097(3) 0.0855(3) -0.3645(3) 0.0581(14) Uani 1 1 d . . . H19 H -0.3459 0.1489 -0.3759 0.070 Uiso 1 1 calc R . . C20 C -0.0692(3) -0.2406(3) -0.3853(2) 0.0272(8) Uani 1 1 d . . . C21 C -0.1215(3) -0.2479(3) -0.4435(2) 0.0363(9) Uani 1 1 d . . . H21 H -0.1944 -0.2395 -0.4418 0.044 Uiso 1 1 calc R . . C22 C 0.0377(3) -0.2528(3) -0.3887(2) 0.0334(9) Uani 1 1 d . . . H22 H 0.0741 -0.2487 -0.3494 0.040 Uiso 1 1 calc R . . C23 C 0.0909(3) -0.2708(3) -0.4498(3) 0.0451(11) Uani 1 1 d . . . H23 H 0.1639 -0.2782 -0.4526 0.054 Uiso 1 1 calc R . . C24 C -0.0678(4) -0.2672(3) -0.5028(2) 0.0467(11) Uani 1 1 d . . . H24 H -0.1038 -0.2734 -0.5416 0.056 Uiso 1 1 calc R . . C25 C 0.0383(4) -0.2778(3) -0.5065(2) 0.0484(11) Uani 1 1 d . . . H25 H 0.0750 -0.2901 -0.5482 0.058 Uiso 1 1 calc R . . C26 C -0.2385(3) -0.3199(3) -0.27315(19) 0.0285(8) Uani 1 1 d . . . C27 C -0.2183(3) -0.4133(3) -0.2836(2) 0.0338(9) Uani 1 1 d . . . H27 H -0.1550 -0.4235 -0.3098 0.041 Uiso 1 1 calc R . . C28 C -0.3322(3) -0.3061(3) -0.2353(2) 0.0377(10) Uani 1 1 d . . . H28 H -0.3470 -0.2427 -0.2286 0.045 Uiso 1 1 calc R . . C29 C -0.4040(3) -0.3849(3) -0.2075(3) 0.0442(11) Uani 1 1 d . . . H29 H -0.4674 -0.3757 -0.1810 0.053 Uiso 1 1 calc R . . C30 C -0.2916(3) -0.4911(3) -0.2553(2) 0.0414(10) Uani 1 1 d . . . H30 H -0.2778 -0.5548 -0.2617 0.050 Uiso 1 1 calc R . . C31 C -0.3834(3) -0.4762(3) -0.2182(2) 0.0418(11) Uani 1 1 d . . . H31 H -0.4333 -0.5294 -0.1997 0.050 Uiso 1 1 calc R . . C32 C 0.4191(2) 0.1793(3) -0.27227(19) 0.0235(8) Uani 1 1 d . . . C33 C 0.4022(3) 0.1844(3) -0.3446(2) 0.0277(8) Uani 1 1 d . . . H33 H 0.3907 0.2496 -0.3821 0.033 Uiso 1 1 calc R . . C34 C 0.4016(3) 0.0977(3) -0.3637(2) 0.0268(8) Uani 1 1 d . A . C35 C 0.4203(3) 0.0010(3) -0.3108(2) 0.0300(8) Uani 1 1 d . . . H35 H 0.4221 -0.0583 -0.3240 0.036 Uiso 1 1 calc R . . C36 C 0.4361(3) -0.0062(3) -0.2385(2) 0.0271(8) Uani 1 1 d . . . C37 C 0.4356(3) 0.0816(3) -0.2198(2) 0.0266(8) Uani 1 1 d . . . H37 H 0.4469 0.0745 -0.1699 0.032 Uiso 1 1 calc R . . C38 C 0.3775(4) 0.1047(3) -0.4398(2) 0.0449(11) Uani 1 1 d . . . C39 C 0.4485(3) -0.1085(3) -0.1790(2) 0.0364(9) Uani 1 1 d . . . C40 C 0.2779(3) 0.2840(2) -0.22769(19) 0.0228(7) Uani 1 1 d . . . C41 C 0.2329(3) 0.2204(3) -0.1569(2) 0.0268(8) Uani 1 1 d . . . H41 H 0.2767 0.1795 -0.1206 0.032 Uiso 1 1 calc R . . C42 C 0.1273(3) 0.2149(3) -0.1377(2) 0.0295(8) Uani 1 1 d . . . C43 C 0.0608(3) 0.2722(3) -0.1894(2) 0.0322(9) Uani 1 1 d . . . H43 H -0.0117 0.2693 -0.1764 0.039 Uiso 1 1 calc R . . C44 C 0.1026(3) 0.3335(3) -0.2604(2) 0.0283(8) Uani 1 1 d . B . C45 C 0.2090(3) 0.3386(3) -0.2792(2) 0.0255(8) Uani 1 1 d . . . H45 H 0.2355 0.3805 -0.3288 0.031 Uiso 1 1 calc R . . C46 C 0.0876(3) 0.1480(3) -0.0598(2) 0.0408(10) Uani 1 1 d . . . C47 C 0.0331(3) 0.3933(3) -0.3178(3) 0.0399(10) Uani 1 1 d . . . C48 C 0.4506(3) 0.3853(3) -0.31502(19) 0.0236(8) Uani 1 1 d . . . C49 C 0.4090(3) 0.4818(3) -0.3228(2) 0.0285(8) Uani 1 1 d . . . H49 H 0.3484 0.4863 -0.2917 0.034 Uiso 1 1 calc R . . C50 C 0.4537(3) 0.5715(3) -0.3750(2) 0.0383(10) Uani 1 1 d . . . C51 C 0.5430(3) 0.5682(3) -0.4194(2) 0.0385(10) Uani 1 1 d . . . H51 H 0.5738 0.6295 -0.4547 0.046 Uiso 1 1 calc R . . C52 C 0.5868(3) 0.4740(3) -0.4117(2) 0.0315(9) Uani 1 1 d . C . C53 C 0.5403(3) 0.3845(3) -0.36090(19) 0.0252(8) Uani 1 1 d . . . H53 H 0.5713 0.3204 -0.3575 0.030 Uiso 1 1 calc R . . C54 C 0.4037(4) 0.6730(4) -0.3833(3) 0.0562(13) Uani 1 1 d . . . C55 C 0.6878(3) 0.4690(4) -0.4562(2) 0.0444(11) Uani 1 1 d . . . C56 C 0.4658(3) 0.2720(3) -0.17605(19) 0.0240(8) Uani 1 1 d . . . C57 C 0.5669(3) 0.2340(3) -0.1703(2) 0.0318(9) Uani 1 1 d . . . H57 H 0.5977 0.2086 -0.2075 0.038 Uiso 1 1 calc R . . C58 C 0.6237(3) 0.2319(3) -0.1132(2) 0.0408(10) Uani 1 1 d . D . C59 C 0.5812(3) 0.2698(3) -0.0578(2) 0.0389(10) Uani 1 1 d . . . H59 H 0.6198 0.2681 -0.0179 0.047 Uiso 1 1 calc R . . C60 C 0.4829(3) 0.3094(3) -0.0620(2) 0.0287(8) Uani 1 1 d . . . C61 C 0.4269(3) 0.3108(3) -0.12046(19) 0.0248(8) Uani 1 1 d . . . H61 H 0.3593 0.3393 -0.1227 0.030 Uiso 1 1 calc R . . C62 C 0.7320(4) 0.1905(5) -0.1094(3) 0.0792(18) Uani 1 1 d DU . . C63 C 0.4356(3) 0.3507(3) -0.0046(2) 0.0400(10) Uani 1 1 d . . . B1 B 0.0202(3) -0.2099(3) -0.2188(2) 0.0248(9) Uani 1 1 d . . . B2 B 0.4025(3) 0.2808(3) -0.2479(2) 0.0222(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0296(3) 0.0219(3) 0.0280(3) -0.0098(2) -0.0029(2) -0.0032(2) P1 0.0259(5) 0.0219(5) 0.0249(5) -0.0088(4) -0.0042(4) -0.0012(4) F1 0.085(3) 0.039(2) 0.0318(19) -0.0022(15) -0.0176(19) -0.020(2) F2 0.116(4) 0.108(3) 0.044(2) 0.0007(19) -0.034(2) -0.076(3) F3 0.152(4) 0.138(5) 0.059(3) -0.062(3) -0.030(3) 0.089(4) F4 0.079(2) 0.0476(16) 0.0624(18) 0.0225(14) 0.0215(16) 0.0139(14) F5 0.136(3) 0.0274(14) 0.0686(19) -0.0166(14) -0.0221(18) 0.0163(15) F6 0.073(2) 0.0485(17) 0.099(2) 0.0208(16) -0.0541(18) -0.0077(15) F7 0.0611(17) 0.0513(16) 0.0529(16) 0.0074(13) 0.0101(13) -0.0043(14) F8 0.0371(15) 0.087(2) 0.0698(19) 0.0038(16) 0.0100(13) -0.0225(15) F9 0.113(2) 0.089(2) 0.0418(16) -0.0298(16) 0.0212(16) -0.0388(19) F10 0.086(3) 0.033(2) 0.077(3) 0.0019(19) -0.050(2) 0.003(2) F11 0.123(4) 0.123(4) 0.077(3) -0.076(3) -0.071(3) 0.080(4) F12 0.024(2) 0.109(4) 0.094(4) 0.026(3) -0.011(2) 0.010(2) F13 0.073(2) 0.0479(17) 0.136(3) -0.0327(19) -0.003(2) 0.0175(15) F14 0.121(3) 0.0501(18) 0.126(3) -0.0504(19) -0.064(2) 0.0302(17) F15 0.114(3) 0.0386(16) 0.112(3) -0.0010(18) -0.045(2) 0.0163(17) F16 0.066(2) 0.084(3) 0.112(3) -0.069(2) 0.051(2) -0.0227(19) F17 0.040(2) 0.154(5) 0.062(3) -0.051(3) -0.0051(18) 0.007(2) F18 0.088(3) 0.074(3) 0.062(2) 0.012(2) 0.045(2) -0.005(2) F19 0.128(3) 0.0558(17) 0.0569(17) -0.0345(15) -0.0355(17) 0.0411(17) F20 0.0666(18) 0.093(2) 0.0605(18) -0.0447(17) 0.0134(15) -0.0082(17) F21 0.0763(18) 0.0783(19) 0.0479(15) -0.0391(14) -0.0262(14) 0.0131(15) F22 0.081(4) 0.183(7) 0.130(5) -0.105(5) -0.041(4) 0.063(4) F23 0.022(2) 0.145(5) 0.118(4) -0.007(4) -0.004(2) -0.003(3) F24 0.040(3) 0.069(3) 0.068(3) -0.011(3) -0.033(2) 0.024(2) O1 0.0383(18) 0.0404(18) 0.092(3) -0.0342(18) 0.0116(17) -0.0011(14) O2 0.070(2) 0.0443(18) 0.0289(16) -0.0062(14) -0.0101(15) -0.0172(15) O3 0.0327(14) 0.0230(13) 0.0250(13) -0.0051(10) -0.0066(11) -0.0052(11) N1 0.0318(17) 0.0238(16) 0.0348(18) -0.0110(14) -0.0096(14) -0.0028(13) C1 0.105(5) 0.041(3) 0.051(3) -0.031(2) -0.042(3) 0.022(3) C2 0.080(4) 0.055(3) 0.052(3) -0.035(3) 0.030(3) -0.028(3) C3 0.032(2) 0.056(3) 0.090(4) -0.051(3) -0.018(2) 0.011(2) C4 0.033(2) 0.049(3) 0.085(4) -0.051(3) -0.005(2) -0.004(2) C5 0.085(4) 0.023(2) 0.039(2) -0.0116(19) -0.005(2) -0.001(2) C6 0.033(2) 0.028(2) 0.050(3) -0.0208(19) 0.0005(19) -0.0075(18) C7 0.039(2) 0.026(2) 0.038(2) -0.0115(18) 0.0006(18) -0.0099(17) C8 0.051(3) 0.024(2) 0.036(2) -0.0023(17) -0.0150(19) -0.0009(18) C9 0.058(3) 0.045(3) 0.036(2) -0.004(2) -0.001(2) -0.017(2) C10 0.069(3) 0.025(2) 0.052(3) -0.013(2) -0.018(2) 0.006(2) C11 0.043(2) 0.033(2) 0.050(3) -0.011(2) -0.025(2) 0.0009(19) C12 0.044(3) 0.048(3) 0.083(4) -0.018(3) -0.018(3) 0.014(2) C13 0.076(4) 0.052(3) 0.046(3) -0.011(2) -0.032(3) -0.002(3) C14 0.0251(19) 0.0246(19) 0.041(2) -0.0116(17) -0.0068(16) -0.0018(15) C15 0.048(3) 0.032(2) 0.042(2) -0.0100(19) -0.011(2) 0.0062(19) C16 0.028(2) 0.037(2) 0.051(3) -0.024(2) -0.0005(18) -0.0019(17) C17 0.059(3) 0.031(2) 0.072(3) -0.008(2) -0.024(3) 0.012(2) C18 0.032(2) 0.047(3) 0.081(4) -0.040(3) -0.005(2) 0.003(2) C19 0.038(3) 0.032(2) 0.114(5) -0.035(3) -0.024(3) 0.010(2) C20 0.033(2) 0.0200(18) 0.0275(19) -0.0076(15) -0.0012(16) -0.0016(15) C21 0.042(2) 0.038(2) 0.028(2) -0.0105(18) -0.0074(18) -0.0004(18) C22 0.034(2) 0.033(2) 0.037(2) -0.0167(18) -0.0022(17) -0.0003(17) C23 0.038(2) 0.048(3) 0.055(3) -0.028(2) 0.009(2) -0.004(2) C24 0.062(3) 0.051(3) 0.030(2) -0.017(2) -0.008(2) 0.003(2) C25 0.057(3) 0.052(3) 0.039(3) -0.023(2) 0.004(2) 0.001(2) C26 0.031(2) 0.029(2) 0.0234(18) -0.0067(16) -0.0035(15) -0.0035(16) C27 0.038(2) 0.030(2) 0.034(2) -0.0130(17) 0.0016(17) -0.0076(17) C28 0.036(2) 0.035(2) 0.046(2) -0.020(2) -0.0004(19) -0.0079(18) C29 0.034(2) 0.045(3) 0.055(3) -0.021(2) 0.007(2) -0.010(2) C30 0.051(3) 0.029(2) 0.046(3) -0.0155(19) -0.002(2) -0.0122(19) C31 0.044(3) 0.038(2) 0.042(2) -0.013(2) 0.002(2) -0.020(2) C32 0.0170(17) 0.0249(18) 0.0253(18) -0.0056(15) -0.0005(14) -0.0016(14) C33 0.027(2) 0.0237(19) 0.029(2) -0.0056(16) -0.0042(15) -0.0026(15) C34 0.0248(19) 0.030(2) 0.0279(19) -0.0129(16) -0.0018(15) -0.0023(15) C35 0.027(2) 0.0244(19) 0.040(2) -0.0131(17) -0.0008(16) -0.0024(15) C36 0.0197(18) 0.0217(18) 0.036(2) -0.0055(16) -0.0047(15) 0.0028(14) C37 0.0206(18) 0.0252(19) 0.032(2) -0.0066(16) -0.0060(15) 0.0004(14) C38 0.069(3) 0.030(2) 0.038(2) -0.013(2) -0.009(2) -0.007(2) C39 0.035(2) 0.028(2) 0.041(2) -0.0050(18) -0.0082(19) -0.0003(17) C40 0.0268(19) 0.0184(17) 0.0238(18) -0.0079(14) -0.0036(15) -0.0037(14) C41 0.0264(19) 0.0249(19) 0.030(2) -0.0112(16) -0.0027(15) -0.0007(15) C42 0.027(2) 0.028(2) 0.035(2) -0.0143(17) 0.0036(16) -0.0085(16) C43 0.0202(19) 0.033(2) 0.049(2) -0.0217(19) -0.0009(17) -0.0036(16) C44 0.0248(19) 0.029(2) 0.035(2) -0.0155(17) -0.0065(16) 0.0026(15) C45 0.0253(19) 0.0230(18) 0.0284(19) -0.0092(15) -0.0042(15) 0.0005(15) C46 0.035(2) 0.043(3) 0.040(2) -0.011(2) 0.0037(19) -0.011(2) C47 0.030(2) 0.041(2) 0.054(3) -0.024(2) -0.0110(19) 0.0126(19) C48 0.0229(18) 0.0219(18) 0.0255(18) -0.0074(15) -0.0049(15) 0.0004(14) C49 0.0265(19) 0.0248(19) 0.033(2) -0.0094(16) 0.0001(16) -0.0017(15) C50 0.043(2) 0.0208(19) 0.050(3) -0.0101(18) -0.007(2) -0.0006(17) C51 0.042(2) 0.029(2) 0.035(2) -0.0015(18) 0.0021(19) -0.0083(18) C52 0.034(2) 0.034(2) 0.0245(19) -0.0088(17) 0.0007(16) -0.0033(17) C53 0.0275(19) 0.0253(19) 0.0226(18) -0.0083(15) -0.0019(15) 0.0000(15) C54 0.057(3) 0.034(3) 0.074(4) -0.016(3) 0.003(3) -0.011(2) C55 0.042(3) 0.056(3) 0.028(2) -0.009(2) 0.0063(19) -0.014(2) C56 0.0217(18) 0.0223(18) 0.0244(18) -0.0044(15) 0.0001(14) -0.0050(14) C57 0.028(2) 0.038(2) 0.031(2) -0.0142(18) -0.0063(16) 0.0025(17) C58 0.029(2) 0.057(3) 0.039(2) -0.018(2) -0.0127(18) 0.0064(19) C59 0.034(2) 0.050(3) 0.036(2) -0.016(2) -0.0186(18) 0.0003(19) C60 0.034(2) 0.027(2) 0.0257(19) -0.0093(16) -0.0049(16) -0.0049(16) C61 0.0234(18) 0.0219(18) 0.0265(19) -0.0052(15) -0.0017(15) -0.0032(14) C62 0.063(3) 0.130(5) 0.071(4) -0.063(4) -0.031(3) 0.032(3) C63 0.054(3) 0.037(2) 0.034(2) -0.0162(19) -0.014(2) 0.006(2) B1 0.024(2) 0.028(2) 0.027(2) -0.0142(18) -0.0030(17) -0.0005(17) B2 0.023(2) 0.0199(19) 0.022(2) -0.0054(16) -0.0026(16) -0.0006(16) _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 C6 1.738(4) . ? Fe1 C7 1.754(4) . ? Fe1 B1 2.057(4) . ? Fe1 C2 2.077(4) . ? Fe1 C3 2.079(4) . ? Fe1 C1 2.093(4) . ? Fe1 C5 2.104(4) . ? Fe1 C4 2.114(4) . ? P1 O3 1.540(2) . ? P1 C20 1.778(4) . ? P1 C14 1.785(4) . ? P1 C26 1.787(3) . ? F1 C38 1.343(6) . ? F1A C38 1.21(2) . ? F2 C38 1.324(5) . ? F2A C38 1.234(14) . ? F3 C38 1.325(6) . ? F3A C38 1.28(2) . ? F4 C39 1.324(5) . ? F5 C39 1.313(5) . ? F6 C39 1.309(4) . ? F7 C46 1.337(5) . ? F8 C46 1.319(5) . ? F9 C46 1.342(5) . ? F10 C47 1.345(6) . ? F10A C47 1.174(13) . ? F11 C47 1.284(6) . ? F11A C47 1.402(12) . ? F12 C47 1.325(6) . ? F12A C47 1.365(11) . ? F13 C54 1.329(6) . ? F14 C54 1.322(5) . ? F15 C54 1.330(6) . ? F16 C55 1.328(6) . ? F16A C55 1.36(2) . ? F17 C55 1.308(6) . ? F17A C55 1.312(17) . ? F18 C55 1.338(5) . ? F18A C55 1.20(2) . ? F19 C63 1.346(5) . ? F20 C63 1.337(5) . ? F21 C63 1.315(4) . ? F22 C62 1.271(7) . ? F22A C62 1.499(10) . ? F23 C62 1.400(8) . ? F23A C62 1.319(11) . ? F24 C62 1.331(7) . ? F24A C62 1.178(14) . ? O1 C6 1.145(5) . ? O2 C7 1.152(4) . ? O3 B1 1.469(4) . ? N1 B1 1.397(5) . ? N1 C11 1.490(5) . ? N1 C8 1.503(5) . ? C1 C2 1.371(7) . ? C1 C4 1.401(7) . ? C2 C3 1.360(7) . ? C3 C5 1.403(6) . ? C4 C5 1.378(6) . ? C8 C10 1.517(6) . ? C8 C9 1.530(6) . ? C11 C12 1.512(6) . ? C11 C13 1.524(6) . ? C14 C15 1.374(5) . ? C14 C16 1.406(5) . ? C15 C17 1.387(6) . ? C16 C18 1.384(6) . ? C17 C19 1.380(7) . ? C18 C19 1.389(7) . ? C20 C22 1.393(5) . ? C20 C21 1.402(5) . ? C21 C24 1.371(6) . ? C22 C23 1.389(5) . ? C23 C25 1.377(6) . ? C24 C25 1.381(6) . ? C26 C28 1.392(5) . ? C26 C27 1.402(5) . ? C27 C30 1.394(5) . ? C28 C29 1.390(5) . ? C29 C31 1.376(6) . ? C30 C31 1.371(6) . ? C32 C37 1.395(5) . ? C32 C33 1.399(5) . ? C32 B2 1.646(5) . ? C33 C34 1.388(5) . ? C34 C35 1.394(5) . ? C34 C38 1.489(5) . ? C35 C36 1.384(5) . ? C36 C37 1.398(5) . ? C36 C39 1.485(5) . ? C40 C45 1.394(5) . ? C40 C41 1.402(5) . ? C40 B2 1.630(5) . ? C41 C42 1.383(5) . ? C42 C43 1.386(5) . ? C42 C46 1.489(5) . ? C43 C44 1.381(5) . ? C44 C45 1.393(5) . ? C44 C47 1.485(5) . ? C48 C53 1.385(5) . ? C48 C49 1.395(5) . ? C48 B2 1.650(5) . ? C49 C50 1.392(5) . ? C50 C51 1.373(6) . ? C50 C54 1.498(6) . ? C51 C52 1.378(6) . ? C52 C53 1.391(5) . ? C52 C55 1.500(6) . ? C56 C61 1.399(5) . ? C56 C57 1.399(5) . ? C56 B2 1.642(5) . ? C57 C58 1.375(5) . ? C58 C59 1.400(6) . ? C58 C62 1.501(7) . ? C59 C60 1.372(5) . ? C60 C61 1.393(5) . ? C60 C63 1.483(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 C6 Fe1 C7 89.37(19) . . ? C6 Fe1 B1 83.22(17) . . ? C7 Fe1 B1 98.40(16) . . ? C6 Fe1 C2 141.0(2) . . ? C7 Fe1 C2 129.4(2) . . ? B1 Fe1 C2 86.53(17) . . ? C6 Fe1 C3 163.17(17) . . ? C7 Fe1 C3 96.0(2) . . ? B1 Fe1 C3 111.60(18) . . ? C2 Fe1 C3 38.2(2) . . ? C6 Fe1 C1 106.8(2) . . ? C7 Fe1 C1 157.19(19) . . ? B1 Fe1 C1 99.38(18) . . ? C2 Fe1 C1 38.4(2) . . ? C3 Fe1 C1 64.12(19) . . ? C6 Fe1 C5 124.77(18) . . ? C7 Fe1 C5 93.11(17) . . ? B1 Fe1 C5 149.95(18) . . ? C2 Fe1 C5 64.97(18) . . ? C3 Fe1 C5 39.20(18) . . ? C1 Fe1 C5 64.55(18) . . ? C6 Fe1 C4 99.27(17) . . ? C7 Fe1 C4 124.02(18) . . ? B1 Fe1 C4 137.43(18) . . ? C2 Fe1 C4 64.86(18) . . ? C3 Fe1 C4 64.56(16) . . ? C1 Fe1 C4 38.92(19) . . ? C5 Fe1 C4 38.15(17) . . ? O3 P1 C20 110.94(16) . . ? O3 P1 C14 109.89(15) . . ? C20 P1 C14 112.56(18) . . ? O3 P1 C26 107.77(15) . . ? C20 P1 C26 106.39(17) . . ? C14 P1 C26 109.11(17) . . ? B1 O3 P1 148.0(2) . . ? B1 N1 C11 122.5(3) . . ? B1 N1 C8 125.7(3) . . ? C11 N1 C8 111.8(3) . . ? C2 C1 C4 108.3(4) . . ? C2 C1 Fe1 70.2(3) . . ? C4 C1 Fe1 71.3(2) . . ? C3 C2 C1 108.3(4) . . ? C3 C2 Fe1 71.0(3) . . ? C1 C2 Fe1 71.4(3) . . ? C2 C3 C5 108.7(4) . . ? C2 C3 Fe1 70.8(3) . . ? C5 C3 Fe1 71.4(3) . . ? C5 C4 C1 107.5(4) . . ? C5 C4 Fe1 70.5(2) . . ? C1 C4 Fe1 69.8(2) . . ? C4 C5 C3 107.2(4) . . ? C4 C5 Fe1 71.3(2) . . ? C3 C5 Fe1 69.4(2) . . ? O1 C6 Fe1 177.1(4) . . ? O2 C7 Fe1 173.0(3) . . ? N1 C8 C10 112.7(3) . . ? N1 C8 C9 112.2(3) . . ? C10 C8 C9 113.2(4) . . ? N1 C11 C12 112.7(3) . . ? N1 C11 C13 112.7(4) . . ? C12 C11 C13 110.8(4) . . ? C15 C14 C16 119.2(4) . . ? C15 C14 P1 122.6(3) . . ? C16 C14 P1 118.2(3) . . ? C14 C15 C17 121.0(4) . . ? C18 C16 C14 120.2(4) . . ? C19 C17 C15 119.6(5) . . ? C16 C18 C19 119.4(4) . . ? C17 C19 C18 120.7(4) . . ? C22 C20 C21 119.2(3) . . ? C22 C20 P1 122.0(3) . . ? C21 C20 P1 118.7(3) . . ? C24 C21 C20 120.1(4) . . ? C23 C22 C20 119.8(4) . . ? C25 C23 C22 120.2(4) . . ? C21 C24 C25 120.4(4) . . ? C23 C25 C24 120.2(4) . . ? C28 C26 C27 119.4(3) . . ? C28 C26 P1 121.4(3) . . ? C27 C26 P1 119.2(3) . . ? C30 C27 C26 119.6(4) . . ? C29 C28 C26 120.0(4) . . ? C31 C29 C28 120.2(4) . . ? C31 C30 C27 120.3(4) . . ? C30 C31 C29 120.6(4) . . ? C37 C32 C33 116.1(3) . . ? C37 C32 B2 122.2(3) . . ? C33 C32 B2 121.0(3) . . ? C34 C33 C32 122.4(3) . . ? C33 C34 C35 120.5(3) . . ? C33 C34 C38 121.2(3) . . ? C35 C34 C38 118.2(3) . . ? C36 C35 C34 118.2(3) . . ? C35 C36 C37 120.7(3) . . ? C35 C36 C39 119.8(3) . . ? C37 C36 C39 119.4(3) . . ? C32 C37 C36 122.0(3) . . ? F1A C38 F2A 122.9(13) . . ? F1A C38 F3A 93.7(15) . . ? F2A C38 F3A 102.3(14) . . ? F1A C38 F3 122.7(12) . . ? F2A C38 F3 58.5(7) . . ? F3A C38 F3 44.5(12) . . ? F1A C38 F2 79.0(12) . . ? F2A C38 F2 54.5(7) . . ? F3A C38 F2 140.8(11) . . ? F3 C38 F2 108.5(5) . . ? F1A C38 F1 27.5(11) . . ? F2A C38 F1 132.4(7) . . ? F3A C38 F1 66.9(12) . . ? F3 C38 F1 102.9(4) . . ? F2 C38 F1 103.6(4) . . ? F1A C38 C34 114.7(12) . . ? F2A C38 C34 112.9(7) . . ? F3A C38 C34 105.6(11) . . ? F3 C38 C34 113.7(4) . . ? F2 C38 C34 112.5(4) . . ? F1 C38 C34 114.7(3) . . ? F6 C39 F5 106.3(4) . . ? F6 C39 F4 105.2(4) . . ? F5 C39 F4 105.2(3) . . ? F6 C39 C36 113.2(3) . . ? F5 C39 C36 114.2(3) . . ? F4 C39 C36 111.9(3) . . ? C45 C40 C41 115.6(3) . . ? C45 C40 B2 124.4(3) . . ? C41 C40 B2 119.6(3) . . ? C42 C41 C40 122.6(3) . . ? C41 C42 C43 120.4(3) . . ? C41 C42 C46 118.4(3) . . ? C43 C42 C46 121.2(3) . . ? C44 C43 C42 118.4(3) . . ? C43 C44 C45 120.8(3) . . ? C43 C44 C47 119.6(3) . . ? C45 C44 C47 119.6(3) . . ? C44 C45 C40 122.1(3) . . ? F8 C46 F7 106.0(3) . . ? F8 C46 F9 107.4(4) . . ? F7 C46 F9 104.0(4) . . ? F8 C46 C42 113.7(4) . . ? F7 C46 C42 112.8(4) . . ? F9 C46 C42 112.3(3) . . ? F10A C47 F11 126.2(7) . . ? F10A C47 F12 58.1(8) . . ? F11 C47 F12 109.0(5) . . ? F10A C47 F10 43.2(8) . . ? F11 C47 F10 107.3(5) . . ? F12 C47 F10 100.5(4) . . ? F10A C47 F12A 105.3(9) . . ? F11 C47 F12A 60.6(6) . . ? F12 C47 F12A 53.6(5) . . ? F10 C47 F12A 134.7(6) . . ? F10A C47 F11A 106.9(9) . . ? F11 C47 F11A 37.2(4) . . ? F12 C47 F11A 130.1(6) . . ? F10 C47 F11A 73.1(6) . . ? F12A C47 F11A 95.3(7) . . ? F10A C47 C44 119.2(7) . . ? F11 C47 C44 113.6(4) . . ? F12 C47 C44 113.6(4) . . ? F10 C47 C44 111.9(3) . . ? F12A C47 C44 112.7(6) . . ? F11A C47 C44 114.5(6) . . ? C53 C48 C49 116.0(3) . . ? C53 C48 B2 122.6(3) . . ? C49 C48 B2 121.0(3) . . ? C50 C49 C48 121.9(4) . . ? C51 C50 C49 120.8(4) . . ? C51 C50 C54 119.4(4) . . ? C49 C50 C54 119.9(4) . . ? C50 C51 C52 118.5(3) . . ? C51 C52 C53 120.4(3) . . ? C51 C52 C55 119.3(3) . . ? C53 C52 C55 120.2(4) . . ? C48 C53 C52 122.4(3) . . ? F14 C54 F15 104.5(4) . . ? F14 C54 F13 110.6(4) . . ? F15 C54 F13 102.5(4) . . ? F14 C54 C50 111.6(4) . . ? F15 C54 C50 113.4(4) . . ? F13 C54 C50 113.6(4) . . ? F18A C55 F17 126.0(10) . . ? F18A C55 F17A 104.3(12) . . ? F17 C55 F17A 39.6(8) . . ? F18A C55 F16 66.0(11) . . ? F17 C55 F16 106.6(5) . . ? F17A C55 F16 132.6(9) . . ? F18A C55 F18 38.5(10) . . ? F17 C55 F18 107.4(4) . . ? F17A C55 F18 72.3(9) . . ? F16 C55 F18 103.4(4) . . ? F18A C55 F16A 114.8(15) . . ? F17 C55 F16A 51.1(10) . . ? F17A C55 F16A 89.1(13) . . ? F16 C55 F16A 59.4(11) . . ? F18 C55 F16A 133.7(10) . . ? F18A C55 C52 118.2(10) . . ? F17 C55 C52 113.7(4) . . ? F17A C55 C52 112.1(8) . . ? F16 C55 C52 112.9(3) . . ? F18 C55 C52 112.2(4) . . ? F16A C55 C52 114.0(10) . . ? C61 C56 C57 115.2(3) . . ? C61 C56 B2 122.6(3) . . ? C57 C56 B2 121.9(3) . . ? C58 C57 C56 123.0(4) . . ? C57 C58 C59 120.1(4) . . ? C57 C58 C62 121.1(4) . . ? C59 C58 C62 118.9(4) . . ? C60 C59 C58 118.9(3) . . ? C59 C60 C61 120.0(4) . . ? C59 C60 C63 120.4(3) . . ? C61 C60 C63 119.6(3) . . ? C60 C61 C56 122.9(3) . . ? F24A C62 F22 117.0(10) . . ? F24A C62 F23A 113.2(11) . . ? F22 C62 F23A 44.9(5) . . ? F24A C62 F24 29.2(8) . . ? F22 C62 F24 114.7(7) . . ? F23A C62 F24 134.4(7) . . ? F24A C62 F23 70.5(9) . . ? F22 C62 F23 103.6(7) . . ? F23A C62 F23 61.9(6) . . ? F24 C62 F23 99.5(5) . . ? F24A C62 F22A 101.8(10) . . ? F22 C62 F22A 45.4(5) . . ? F23A C62 F22A 90.3(7) . . ? F24 C62 F22A 81.5(6) . . ? F23 C62 F22A 142.2(6) . . ? F24A C62 C58 125.6(10) . . ? F22 C62 C58 115.8(5) . . ? F23A C62 C58 112.5(7) . . ? F24 C62 C58 112.8(5) . . ? F23 C62 C58 108.4(5) . . ? F22A C62 C58 105.7(6) . . ? F21 C63 F20 105.6(3) . . ? F21 C63 F19 106.7(3) . . ? F20 C63 F19 105.7(4) . . ? F21 C63 C60 114.4(4) . . ? F20 C63 C60 112.3(3) . . ? F19 C63 C60 111.5(3) . . ? N1 B1 O3 110.5(3) . . ? N1 B1 Fe1 129.1(3) . . ? O3 B1 Fe1 120.2(3) . . ? C40 B2 C56 112.1(3) . . ? C40 B2 C32 103.1(3) . . ? C56 B2 C32 112.5(3) . . ? C40 B2 C48 114.4(3) . . ? C56 B2 C48 102.9(2) . . ? C32 B2 C48 112.1(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.086 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.078 data_sa0416 _database_code_depnum_ccdc_archive 'CCDC 282084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0416 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C152 H112 B4 F96 N4' _chemical_formula_weight 3861.70 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 22.3190(4) _cell_length_b 16.0297(5) _cell_length_c 15.4055(5) _cell_angle_alpha 90.00 _cell_angle_beta 133.2110(10) _cell_angle_gamma 90.00 _cell_volume 4017.04(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13444 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9585 _exptl_absorpt_correction_T_max 0.9617 _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 15523 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4562 _reflns_number_gt 3386 _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^)+(0.0780P)^2^+9.4259P] 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 4562 _refine_ls_number_parameters 292 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1917 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.066 _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 N1 N 1.0000 0.3552(3) 0.2500 0.0517(10) Uani 1 2 d S . . H1A H 1.0266 0.3209 0.2377 0.062 Uiso 0.50 1 calc PR . . H1B H 0.9734 0.3209 0.2623 0.062 Uiso 0.50 1 calc PR . . C17 C 1.0638(2) 0.3981(2) 0.3623(4) 0.0583(10) Uani 1 1 d . . . H17 H 1.0374 0.4439 0.3702 0.070 Uiso 1 1 calc R . . C19 C 1.1058(3) 0.3395(3) 0.4668(4) 0.0710(12) Uani 1 1 d . . . H19A H 1.0642 0.3111 0.4609 0.107 Uiso 1 1 calc R . . H19B H 1.1426 0.3714 0.5411 0.107 Uiso 1 1 calc R . . H19C H 1.1376 0.2980 0.4659 0.107 Uiso 1 1 calc R . . C18 C 1.1230(3) 0.4370(4) 0.3570(5) 0.0932(17) Uani 1 1 d . . . H18A H 1.1491 0.3930 0.3484 0.140 Uiso 1 1 calc R . . H18B H 1.1652 0.4683 0.4305 0.140 Uiso 1 1 calc R . . H18C H 1.0930 0.4749 0.2887 0.140 Uiso 1 1 calc R . . C1 C 0.93166(14) 0.17797(16) 0.6311(2) 0.0236(5) Uani 1 1 d . . . C2 C 0.84992(15) 0.15250(16) 0.5398(2) 0.0243(5) Uani 1 1 d . . . H2 H 0.8323 0.1025 0.5498 0.029 Uiso 1 1 calc R . . C3 C 0.79343(15) 0.19784(17) 0.4347(2) 0.0273(6) Uani 1 1 d . . . C4 C 0.81582(16) 0.27126(18) 0.4164(2) 0.0312(6) Uani 1 1 d . . . H4 H 0.7773 0.3021 0.3448 0.037 Uiso 1 1 calc R . . C5 C 0.89649(16) 0.29873(17) 0.5059(2) 0.0302(6) Uani 1 1 d . . . C6 C 0.95247(15) 0.25346(17) 0.6104(2) 0.0268(5) Uani 1 1 d . . . H6 H 1.0069 0.2741 0.6703 0.032 Uiso 1 1 calc R . . C7 C 0.70774(16) 0.16471(18) 0.3393(2) 0.0316(6) Uani 1 1 d . . . C8 C 0.9214(2) 0.3773(2) 0.4856(3) 0.0449(8) Uani 1 1 d . . . C9 C 1.04849(14) 0.06308(16) 0.7256(2) 0.0232(5) Uani 1 1 d . . . C10 C 1.06621(15) 0.09376(16) 0.6597(2) 0.0248(5) Uani 1 1 d . . . H10 H 1.0466 0.1475 0.6244 0.030 Uiso 1 1 calc R . . C11 C 1.11156(15) 0.04814(17) 0.6441(2) 0.0271(6) Uani 1 1 d . . . C12 C 1.13861(16) -0.03193(18) 0.6897(2) 0.0321(6) Uani 1 1 d . . . H12 H 1.1679 -0.0638 0.6770 0.039 Uiso 1 1 calc R . . C13 C 1.12163(16) -0.06399(18) 0.7541(2) 0.0304(6) Uani 1 1 d . . . C14 C 1.07951(15) -0.01648(17) 0.7740(2) 0.0270(5) Uani 1 1 d . . . H14 H 1.0716 -0.0392 0.8224 0.032 Uiso 1 1 calc R . . C15 C 1.13157(16) 0.08741(18) 0.5783(2) 0.0312(6) Uani 1 1 d . . . C16 C 1.14576(19) -0.1511(2) 0.8008(3) 0.0401(7) Uani 1 1 d . . . B1 B 1.0000 0.1204(3) 0.7500 0.0232(8) Uani 1 2 d S . . F1 F 0.70404(11) 0.09843(15) 0.28389(19) 0.0645(7) Uani 1 1 d . . . F2 F 0.67434(11) 0.14020(15) 0.38028(17) 0.0567(6) Uani 1 1 d . . . F3 F 0.65595(11) 0.22044(15) 0.2545(2) 0.0735(8) Uani 1 1 d . . . F4 F 0.99176(14) 0.40834(15) 0.5814(2) 0.0832(9) Uani 1 1 d U . . F5 F 0.9292(2) 0.36676(18) 0.4073(3) 0.0944(9) Uani 1 1 d U . . F6 F 0.86684(15) 0.43796(14) 0.4386(3) 0.0817(8) Uani 1 1 d . . . F7 F 1.18662(14) 0.14795(16) 0.63919(18) 0.0700(7) Uani 1 1 d . . . F8 F 1.16078(16) 0.03347(14) 0.5496(2) 0.0648(7) Uani 1 1 d . . . F9 F 1.06652(12) 0.12222(15) 0.47567(17) 0.0563(6) Uani 1 1 d . . . F10 F 1.19258(15) -0.18792(14) 0.7886(2) 0.0668(7) Uani 1 1 d . . . F11 F 1.18618(15) -0.15681(13) 0.91609(18) 0.0623(6) Uani 1 1 d . . . F12 F 1.07967(14) -0.20105(13) 0.7462(2) 0.0813(8) Uani 1 1 d U . . 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 N1 0.0294(18) 0.070(3) 0.049(2) 0.000 0.0246(18) 0.000 C17 0.062(2) 0.042(2) 0.064(2) -0.0051(17) 0.040(2) 0.0018(17) C19 0.067(3) 0.076(3) 0.060(3) 0.011(2) 0.040(2) 0.010(2) C18 0.077(3) 0.092(4) 0.075(3) -0.001(3) 0.038(3) -0.039(3) C1 0.0228(11) 0.0298(13) 0.0224(11) -0.0012(10) 0.0171(10) 0.0024(10) C2 0.0233(11) 0.0282(13) 0.0238(12) 0.0002(10) 0.0170(10) 0.0011(10) C3 0.0223(12) 0.0356(15) 0.0219(12) -0.0004(10) 0.0143(10) 0.0043(11) C4 0.0292(13) 0.0357(15) 0.0253(13) 0.0069(11) 0.0173(11) 0.0085(11) C5 0.0307(13) 0.0314(14) 0.0301(13) 0.0005(11) 0.0215(12) 0.0013(11) C6 0.0234(11) 0.0305(13) 0.0261(12) -0.0001(10) 0.0168(11) 0.0010(10) C7 0.0238(12) 0.0381(16) 0.0268(13) 0.0007(11) 0.0149(11) 0.0048(11) C8 0.0434(17) 0.0397(17) 0.0436(17) 0.0092(14) 0.0267(15) 0.0010(14) C9 0.0197(11) 0.0287(13) 0.0194(11) -0.0016(9) 0.0127(10) -0.0015(10) C10 0.0244(12) 0.0256(12) 0.0244(12) -0.0014(10) 0.0167(10) -0.0009(10) C11 0.0244(12) 0.0365(15) 0.0232(12) -0.0037(11) 0.0174(11) -0.0025(11) C12 0.0293(13) 0.0399(16) 0.0324(14) -0.0006(12) 0.0231(12) 0.0043(12) C13 0.0281(13) 0.0326(14) 0.0287(13) 0.0016(11) 0.0187(11) 0.0031(11) C14 0.0262(12) 0.0335(14) 0.0230(12) 0.0010(10) 0.0174(10) 0.0000(11) C15 0.0318(13) 0.0385(15) 0.0288(13) -0.0043(12) 0.0229(12) -0.0022(12) C16 0.0420(16) 0.0386(17) 0.0434(17) 0.0058(13) 0.0307(15) 0.0079(14) B1 0.0217(17) 0.027(2) 0.0206(18) 0.000 0.0145(16) 0.000 F1 0.0302(9) 0.0872(16) 0.0573(12) -0.0441(12) 0.0227(9) -0.0098(10) F2 0.0386(10) 0.0904(16) 0.0458(11) -0.0173(11) 0.0307(9) -0.0222(10) F3 0.0252(9) 0.0718(15) 0.0610(14) 0.0273(11) 0.0053(9) 0.0035(10) F4 0.0618(14) 0.0595(14) 0.0665(15) 0.0192(11) 0.0199(12) -0.0247(11) F5 0.153(3) 0.0807(17) 0.115(2) -0.0010(16) 0.117(2) -0.0261(18) F6 0.0699(15) 0.0441(13) 0.111(2) 0.0333(13) 0.0539(16) 0.0136(11) F7 0.0796(15) 0.0985(18) 0.0499(12) -0.0324(12) 0.0513(12) -0.0574(14) F8 0.1097(18) 0.0573(13) 0.0876(16) 0.0167(11) 0.0909(16) 0.0247(12) F9 0.0484(11) 0.0828(15) 0.0450(11) 0.0248(10) 0.0348(10) 0.0119(10) F10 0.0949(17) 0.0526(13) 0.0914(17) 0.0275(12) 0.0787(16) 0.0381(12) F11 0.0873(16) 0.0536(13) 0.0497(12) 0.0208(10) 0.0484(12) 0.0282(11) F12 0.0576(13) 0.0412(12) 0.1021(19) 0.0189(12) 0.0380(14) -0.0017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C17 1.455(4) 2_755 ? N1 C17 1.455(4) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? C17 C19 1.512(6) . ? C17 C18 1.513(6) . ? C17 H17 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C1 C2 1.400(3) . ? C1 C6 1.409(4) . ? C1 B1 1.645(3) . ? C2 C3 1.395(3) . ? C2 H2 0.9500 . ? C3 C4 1.381(4) . ? C3 C7 1.500(4) . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 C8 1.494(4) . ? C6 H6 0.9500 . ? C7 F2 1.324(3) . ? C7 F1 1.329(3) . ? C7 F3 1.331(3) . ? C8 F4 1.311(4) . ? C8 F6 1.321(4) . ? C8 F5 1.341(4) . ? C9 C14 1.398(4) . ? C9 C10 1.407(3) . ? C9 B1 1.647(3) . ? C10 C11 1.396(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 C15 1.498(4) . ? C12 C13 1.382(4) . ? C12 H12 0.9500 . ? C13 C14 1.396(4) . ? C13 C16 1.493(4) . ? C14 H14 0.9500 . ? C15 F7 1.324(3) . ? C15 F8 1.327(3) . ? C15 F9 1.332(3) . ? C16 F10 1.321(4) . ? C16 F11 1.334(4) . ? C16 F12 1.351(4) . ? B1 C1 1.645(3) 2_756 ? B1 C9 1.647(3) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 N1 C17 123.7(4) 2_755 . ? C17 N1 H1A 106.4 2_755 . ? C17 N1 H1A 106.4 . . ? C17 N1 H1B 106.4 2_755 . ? C17 N1 H1B 106.4 . . ? H1A N1 H1B 106.5 . . ? N1 C17 C19 111.2(3) . . ? N1 C17 C18 108.1(3) . . ? C19 C17 C18 112.7(4) . . ? N1 C17 H17 108.2 . . ? C19 C17 H17 108.2 . . ? C18 C17 H17 108.2 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C1 C6 115.3(2) . . ? C2 C1 B1 122.2(2) . . ? C6 C1 B1 122.4(2) . . ? C3 C2 C1 122.4(2) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C4 C3 C2 121.0(2) . . ? C4 C3 C7 119.9(2) . . ? C2 C3 C7 119.0(2) . . ? C3 C4 C5 118.1(2) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 C8 121.0(3) . . ? C4 C5 C8 118.3(3) . . ? C5 C6 C1 122.5(2) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? F2 C7 F1 105.1(3) . . ? F2 C7 F3 105.8(2) . . ? F1 C7 F3 106.0(2) . . ? F2 C7 C3 113.2(2) . . ? F1 C7 C3 112.9(2) . . ? F3 C7 C3 113.0(2) . . ? F4 C8 F6 106.4(3) . . ? F4 C8 F5 105.6(3) . . ? F6 C8 F5 103.8(3) . . ? F4 C8 C5 114.5(3) . . ? F6 C8 C5 113.5(3) . . ? F5 C8 C5 112.2(3) . . ? C14 C9 C10 114.9(2) . . ? C14 C9 B1 123.4(2) . . ? C10 C9 B1 121.5(2) . . ? C11 C10 C9 122.4(2) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C12 C11 C10 120.9(2) . . ? C12 C11 C15 120.2(2) . . ? C10 C11 C15 118.9(2) . . ? C13 C12 C11 118.0(2) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 C16 120.6(2) . . ? C14 C13 C16 118.7(2) . . ? C13 C14 C9 122.9(2) . . ? C13 C14 H14 118.5 . . ? C9 C14 H14 118.5 . . ? F7 C15 F8 106.5(2) . . ? F7 C15 F9 105.2(3) . . ? F8 C15 F9 105.2(2) . . ? F7 C15 C11 113.0(2) . . ? F8 C15 C11 113.2(2) . . ? F9 C15 C11 113.0(2) . . ? F10 C16 F11 106.2(3) . . ? F10 C16 F12 106.3(3) . . ? F11 C16 F12 104.1(3) . . ? F10 C16 C13 114.1(3) . . ? F11 C16 C13 113.4(3) . . ? F12 C16 C13 112.0(2) . . ? C1 B1 C1 111.8(3) 2_756 . ? C1 B1 C9 108.27(12) 2_756 . ? C1 B1 C9 108.20(11) . . ? C1 B1 C9 108.20(11) 2_756 2_756 ? C1 B1 C9 108.27(12) . 2_756 ? C9 B1 C9 112.2(3) . 2_756 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B F12 0.92 2.21 3.069(4) 154.5 5_756 N1 H1A F12 0.92 2.21 3.069(4) 154.5 6 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.569 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.064 # Attachment '3a.cif' data_sa0406 _database_code_depnum_ccdc_archive 'CCDC 282085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0406 _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 B1 Cl1 Fe1 O3' _chemical_formula_sum 'C21 H26 B1 Cl1 Fe1 O3' _chemical_formula_weight 428.53 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3300(3) _cell_length_b 8.7470(3) _cell_length_c 14.5400(5) _cell_angle_alpha 75.677(2) _cell_angle_beta 89.5730(10) _cell_angle_gamma 88.4810(10) _cell_volume 1026.13(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10013 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 0.9572 _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 15859 _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_sigmaI/netI 0.1109 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.40 _reflns_number_total 4575 _reflns_number_gt 2951 _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 'Dirdif-99 (Beurskens et al., 1999)' _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^)+(0.0370P)^2^+0.6726P] 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 4575 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.3002(4) 0.0659(4) -0.1143(2) 0.0282(8) Uani 1 1 d . . . C2 C 0.0274(5) 0.2174(4) -0.1034(2) 0.0296(8) Uani 1 1 d . . . C3 C 0.3938(4) 0.3386(4) -0.2588(2) 0.0238(8) Uani 1 1 d . . . C4 C 0.3875(4) 0.3920(4) -0.1731(2) 0.0276(8) Uani 1 1 d . . . C5 C 0.2379(4) 0.4728(4) -0.1718(2) 0.0255(8) Uani 1 1 d . . . C6 C 0.1509(4) 0.4702(4) -0.2561(2) 0.0244(8) Uani 1 1 d . . . C7 C 0.2500(4) 0.3887(4) -0.3107(2) 0.0236(8) Uani 1 1 d . . . C8 C 0.5343(4) 0.2548(4) -0.2924(3) 0.0389(10) Uani 1 1 d . . . H8A H 0.4948 0.1767 -0.3244 0.058 Uiso 1 1 calc R . . H8B H 0.6005 0.2014 -0.2379 0.058 Uiso 1 1 calc R . . H8C H 0.5989 0.3318 -0.3370 0.058 Uiso 1 1 calc R . . C9 C 0.5196(5) 0.3710(4) -0.1014(3) 0.0424(10) Uani 1 1 d . . . H9A H 0.5986 0.4534 -0.1227 0.064 Uiso 1 1 calc R . . H9B H 0.5719 0.2671 -0.0943 0.064 Uiso 1 1 calc R . . H9C H 0.4747 0.3789 -0.0402 0.064 Uiso 1 1 calc R . . C10 C 0.1834(5) 0.5560(4) -0.0968(3) 0.0386(10) Uani 1 1 d . . . H10A H 0.2286 0.5004 -0.0352 0.058 Uiso 1 1 calc R . . H10B H 0.0659 0.5566 -0.0929 0.058 Uiso 1 1 calc R . . H10C H 0.2204 0.6649 -0.1138 0.058 Uiso 1 1 calc R . . C11 C -0.0107(4) 0.5473(4) -0.2850(3) 0.0371(9) Uani 1 1 d . . . H11A H -0.0762 0.5436 -0.2283 0.056 Uiso 1 1 calc R . . H11B H -0.0646 0.4909 -0.3260 0.056 Uiso 1 1 calc R . . H11C H 0.0034 0.6574 -0.3196 0.056 Uiso 1 1 calc R . . C12 C 0.2210(5) 0.3826(4) -0.4110(2) 0.0342(9) Uani 1 1 d . . . H12A H 0.2796 0.4669 -0.4541 0.051 Uiso 1 1 calc R . . H12B H 0.1058 0.3967 -0.4249 0.051 Uiso 1 1 calc R . . H12C H 0.2586 0.2801 -0.4199 0.051 Uiso 1 1 calc R . . C13 C -0.1652(4) 0.0089(4) -0.3010(2) 0.0242(8) Uani 1 1 d . . . C14 C -0.1927(4) 0.0340(4) -0.3975(2) 0.0254(8) Uani 1 1 d . . . C15 C -0.2992(4) -0.0632(4) -0.4270(2) 0.0261(8) Uani 1 1 d . . . H15 H -0.3174 -0.0488 -0.4930 0.031 Uiso 1 1 calc R . . C16 C -0.3806(4) -0.1812(4) -0.3633(2) 0.0260(8) Uani 1 1 d . . . C17 C -0.3500(4) -0.1996(4) -0.2670(2) 0.0288(8) Uani 1 1 d . . . H17 H -0.4050 -0.2789 -0.2223 0.035 Uiso 1 1 calc R . . C18 C -0.2437(4) -0.1079(4) -0.2338(2) 0.0278(8) Uani 1 1 d . . . C19 C -0.1111(4) 0.1647(4) -0.4681(2) 0.0338(9) Uani 1 1 d . . . H19A H -0.1502 0.1689 -0.5321 0.051 Uiso 1 1 calc R . . H19B H 0.0053 0.1444 -0.4656 0.051 Uiso 1 1 calc R . . H19C H -0.1353 0.2657 -0.4526 0.051 Uiso 1 1 calc R . . C20 C -0.4952(4) -0.2845(4) -0.3967(3) 0.0359(9) Uani 1 1 d . . . H20A H -0.5250 -0.2362 -0.4628 0.054 Uiso 1 1 calc R . . H20B H -0.5917 -0.2969 -0.3569 0.054 Uiso 1 1 calc R . . H20C H -0.4440 -0.3883 -0.3924 0.054 Uiso 1 1 calc R . . C21 C -0.2143(5) -0.1292(4) -0.1293(2) 0.0380(9) Uani 1 1 d . . . H21A H -0.2770 -0.2175 -0.0933 0.057 Uiso 1 1 calc R . . H21B H -0.2470 -0.0325 -0.1109 0.057 Uiso 1 1 calc R . . H21C H -0.0998 -0.1516 -0.1158 0.057 Uiso 1 1 calc R . . O1 O 0.3731(3) -0.0446(3) -0.07491(18) 0.0419(7) Uani 1 1 d . . . O2 O -0.0847(3) 0.2109(3) -0.05671(18) 0.0448(7) Uani 1 1 d . . . O3 O -0.0717(3) 0.1139(3) -0.26686(15) 0.0259(5) Uani 1 1 d . . . B1 B 0.0891(5) 0.1034(4) -0.2477(3) 0.0229(8) Uani 1 1 d . . . Cl1 Cl 0.19822(10) -0.04688(10) -0.29332(6) 0.0321(2) Uani 1 1 d . . . Fe1 Fe 0.19767(6) 0.23727(5) -0.17705(3) 0.02159(15) 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 0.027(2) 0.033(2) 0.0245(19) -0.0071(16) 0.0007(16) -0.0066(17) C2 0.033(2) 0.034(2) 0.0237(19) -0.0093(15) -0.0043(17) -0.0024(17) C3 0.0221(18) 0.0162(17) 0.0297(19) 0.0003(14) 0.0038(15) 0.0029(13) C4 0.0257(19) 0.0235(19) 0.031(2) -0.0007(15) -0.0034(16) -0.0054(15) C5 0.030(2) 0.0213(18) 0.0246(19) -0.0048(14) 0.0019(16) -0.0006(15) C6 0.0233(18) 0.0232(19) 0.0256(18) -0.0045(14) 0.0000(15) 0.0037(14) C7 0.0260(19) 0.0216(18) 0.0220(18) -0.0026(14) 0.0049(15) -0.0048(14) C8 0.031(2) 0.030(2) 0.053(2) -0.0058(18) 0.0105(19) 0.0038(17) C9 0.037(2) 0.038(2) 0.047(2) 0.0004(18) -0.015(2) -0.0085(18) C10 0.054(3) 0.032(2) 0.033(2) -0.0142(17) 0.0056(19) 0.0005(19) C11 0.027(2) 0.037(2) 0.044(2) -0.0048(18) -0.0035(18) 0.0061(17) C12 0.047(2) 0.031(2) 0.0228(19) -0.0035(15) 0.0039(18) -0.0055(17) C13 0.0171(17) 0.0252(19) 0.031(2) -0.0079(15) -0.0033(15) 0.0006(14) C14 0.0205(18) 0.029(2) 0.0270(19) -0.0076(15) -0.0002(15) -0.0007(15) C15 0.0227(19) 0.033(2) 0.0235(18) -0.0093(15) -0.0016(15) 0.0025(15) C16 0.0223(18) 0.0229(19) 0.033(2) -0.0077(15) -0.0003(16) 0.0013(14) C17 0.028(2) 0.0222(19) 0.032(2) -0.0005(15) 0.0043(17) 0.0008(15) C18 0.0244(19) 0.027(2) 0.030(2) -0.0041(15) 0.0025(16) 0.0074(15) C19 0.032(2) 0.039(2) 0.031(2) -0.0077(16) -0.0016(17) -0.0072(17) C20 0.030(2) 0.036(2) 0.043(2) -0.0105(17) 0.0021(18) -0.0057(17) C21 0.042(2) 0.039(2) 0.029(2) -0.0021(17) -0.0030(18) 0.0025(18) O1 0.0443(17) 0.0335(16) 0.0413(16) 0.0031(12) -0.0086(14) 0.0050(13) O2 0.0320(16) 0.0657(19) 0.0413(16) -0.0218(14) 0.0160(14) -0.0072(14) O3 0.0234(13) 0.0281(13) 0.0287(13) -0.0121(10) -0.0041(11) 0.0018(10) B1 0.024(2) 0.022(2) 0.020(2) -0.0017(15) 0.0029(17) 0.0029(16) Cl1 0.0273(5) 0.0345(5) 0.0383(5) -0.0171(4) -0.0016(4) 0.0060(4) Fe1 0.0202(3) 0.0230(3) 0.0210(3) -0.00436(19) 0.0003(2) 0.00008(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 C1 O1 1.154(4) . ? C1 Fe1 1.754(4) . ? C2 O2 1.145(4) . ? C2 Fe1 1.757(4) . ? C3 C7 1.421(5) . ? C3 C4 1.435(5) . ? C3 C8 1.506(5) . ? C3 Fe1 2.096(3) . ? C4 C5 1.419(5) . ? C4 C9 1.498(5) . ? C4 Fe1 2.118(3) . ? C5 C6 1.433(5) . ? C5 C10 1.514(4) . ? C5 Fe1 2.116(3) . ? C6 C7 1.435(4) . ? C6 C11 1.505(5) . ? C6 Fe1 2.105(3) . ? C7 C12 1.495(5) . ? C7 Fe1 2.113(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.385(4) . ? C13 C18 1.399(5) . ? C13 O3 1.402(4) . ? C14 C15 1.386(4) . ? C14 C19 1.508(5) . ? C15 C16 1.391(5) . ? C15 H15 0.9500 . ? C16 C17 1.395(5) . ? C16 C20 1.494(5) . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C21 1.505(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O3 B1 1.366(4) . ? B1 Cl1 1.831(4) . ? B1 Fe1 1.977(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 O1 C1 Fe1 177.3(3) . . ? O2 C2 Fe1 177.3(3) . . ? C7 C3 C4 108.6(3) . . ? C7 C3 C8 125.2(3) . . ? C4 C3 C8 126.0(3) . . ? C7 C3 Fe1 70.93(18) . . ? C4 C3 Fe1 70.94(18) . . ? C8 C3 Fe1 127.7(2) . . ? C5 C4 C3 107.5(3) . . ? C5 C4 C9 127.1(3) . . ? C3 C4 C9 125.3(3) . . ? C5 C4 Fe1 70.32(19) . . ? C3 C4 Fe1 69.26(19) . . ? C9 C4 Fe1 127.7(2) . . ? C4 C5 C6 108.6(3) . . ? C4 C5 C10 125.6(3) . . ? C6 C5 C10 125.7(3) . . ? C4 C5 Fe1 70.53(19) . . ? C6 C5 Fe1 69.74(19) . . ? C10 C5 Fe1 128.3(2) . . ? C5 C6 C7 107.6(3) . . ? C5 C6 C11 126.3(3) . . ? C7 C6 C11 126.0(3) . . ? C5 C6 Fe1 70.56(18) . . ? C7 C6 Fe1 70.43(18) . . ? C11 C6 Fe1 127.1(2) . . ? C3 C7 C6 107.7(3) . . ? C3 C7 C12 125.5(3) . . ? C6 C7 C12 126.0(3) . . ? C3 C7 Fe1 69.63(18) . . ? C6 C7 Fe1 69.79(18) . . ? C12 C7 Fe1 134.0(2) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 122.1(3) . . ? C14 C13 O3 120.1(3) . . ? C18 C13 O3 117.3(3) . . ? C13 C14 C15 117.9(3) . . ? C13 C14 C19 121.0(3) . . ? C15 C14 C19 121.1(3) . . ? C14 C15 C16 122.4(3) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C17 117.1(3) . . ? C15 C16 C20 121.5(3) . . ? C17 C16 C20 121.4(3) . . ? C18 C17 C16 122.9(3) . . ? C18 C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? C17 C18 C13 117.5(3) . . ? C17 C18 C21 121.7(3) . . ? C13 C18 C21 120.8(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? B1 O3 C13 128.3(3) . . ? O3 B1 Cl1 114.2(3) . . ? O3 B1 Fe1 123.7(3) . . ? Cl1 B1 Fe1 122.1(2) . . ? C1 Fe1 C2 96.73(16) . . ? C1 Fe1 B1 87.38(15) . . ? C2 Fe1 B1 87.17(15) . . ? C1 Fe1 C3 96.52(14) . . ? C2 Fe1 C3 160.58(14) . . ? B1 Fe1 C3 107.58(14) . . ? C1 Fe1 C6 161.35(14) . . ? C2 Fe1 C6 97.91(14) . . ? B1 Fe1 C6 104.80(14) . . ? C3 Fe1 C6 66.59(12) . . ? C1 Fe1 C7 129.61(14) . . ? C2 Fe1 C7 132.81(14) . . ? B1 Fe1 C7 86.68(14) . . ? C3 Fe1 C7 39.45(12) . . ? C6 Fe1 C7 39.78(12) . . ? C1 Fe1 C5 127.52(15) . . ? C2 Fe1 C5 94.41(14) . . ? B1 Fe1 C5 144.38(14) . . ? C3 Fe1 C5 66.22(12) . . ? C6 Fe1 C5 39.70(13) . . ? C7 Fe1 C5 66.35(12) . . ? C1 Fe1 C4 95.60(14) . . ? C2 Fe1 C4 124.47(15) . . ? B1 Fe1 C4 147.37(15) . . ? C3 Fe1 C4 39.80(13) . . ? C6 Fe1 C4 66.51(13) . . ? C7 Fe1 C4 66.47(13) . . ? C5 Fe1 C4 39.15(13) . . ? 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 C7 C3 C4 C5 1.0(4) . . . . ? C8 C3 C4 C5 176.5(3) . . . . ? Fe1 C3 C4 C5 -60.2(2) . . . . ? C7 C3 C4 C9 -176.5(3) . . . . ? C8 C3 C4 C9 -1.0(5) . . . . ? Fe1 C3 C4 C9 122.3(3) . . . . ? C7 C3 C4 Fe1 61.2(2) . . . . ? C8 C3 C4 Fe1 -123.3(3) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C9 C4 C5 C6 177.4(3) . . . . ? Fe1 C4 C5 C6 -59.6(2) . . . . ? C3 C4 C5 C10 -176.8(3) . . . . ? C9 C4 C5 C10 0.7(6) . . . . ? Fe1 C4 C5 C10 123.7(3) . . . . ? C3 C4 C5 Fe1 59.6(2) . . . . ? C9 C4 C5 Fe1 -123.0(3) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C10 C5 C6 C7 175.8(3) . . . . ? Fe1 C5 C6 C7 -61.0(2) . . . . ? C4 C5 C6 C11 -177.6(3) . . . . ? C10 C5 C6 C11 -0.9(6) . . . . ? Fe1 C5 C6 C11 122.3(3) . . . . ? C4 C5 C6 Fe1 60.1(2) . . . . ? C10 C5 C6 Fe1 -123.2(3) . . . . ? C4 C3 C7 C6 -1.6(4) . . . . ? C8 C3 C7 C6 -177.1(3) . . . . ? Fe1 C3 C7 C6 59.6(2) . . . . ? C4 C3 C7 C12 168.5(3) . . . . ? C8 C3 C7 C12 -7.0(5) . . . . ? Fe1 C3 C7 C12 -130.2(3) . . . . ? C4 C3 C7 Fe1 -61.2(2) . . . . ? C8 C3 C7 Fe1 123.2(3) . . . . ? C5 C6 C7 C3 1.6(4) . . . . ? C11 C6 C7 C3 178.2(3) . . . . ? Fe1 C6 C7 C3 -59.5(2) . . . . ? C5 C6 C7 C12 -168.5(3) . . . . ? C11 C6 C7 C12 8.2(5) . . . . ? Fe1 C6 C7 C12 130.4(3) . . . . ? C5 C6 C7 Fe1 61.1(2) . . . . ? C11 C6 C7 Fe1 -122.2(3) . . . . ? C18 C13 C14 C15 -1.4(5) . . . . ? O3 C13 C14 C15 -173.4(3) . . . . ? C18 C13 C14 C19 177.7(3) . . . . ? O3 C13 C14 C19 5.7(5) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C19 C14 C15 C16 -177.7(3) . . . . ? C14 C15 C16 C17 -0.4(5) . . . . ? C14 C15 C16 C20 179.9(3) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C20 C16 C17 C18 179.1(3) . . . . ? C16 C17 C18 C13 0.5(5) . . . . ? C16 C17 C18 C21 179.4(3) . . . . ? C14 C13 C18 C17 0.5(5) . . . . ? O3 C13 C18 C17 172.7(3) . . . . ? C14 C13 C18 C21 -178.4(3) . . . . ? O3 C13 C18 C21 -6.2(5) . . . . ? C14 C13 O3 B1 -94.0(4) . . . . ? C18 C13 O3 B1 93.7(4) . . . . ? C13 O3 B1 Cl1 12.2(4) . . . . ? C13 O3 B1 Fe1 -167.8(2) . . . . ? O1 C1 Fe1 C2 -164(7) . . . . ? O1 C1 Fe1 B1 109(7) . . . . ? O1 C1 Fe1 C3 2(7) . . . . ? O1 C1 Fe1 C6 -23(7) . . . . ? O1 C1 Fe1 C7 25(7) . . . . ? O1 C1 Fe1 C5 -63(7) . . . . ? O1 C1 Fe1 C4 -38(7) . . . . ? O2 C2 Fe1 C1 158(6) . . . . ? O2 C2 Fe1 B1 -115(6) . . . . ? O2 C2 Fe1 C3 25(7) . . . . ? O2 C2 Fe1 C6 -11(6) . . . . ? O2 C2 Fe1 C7 -33(7) . . . . ? O2 C2 Fe1 C5 29(6) . . . . ? O2 C2 Fe1 C4 56(7) . . . . ? O3 B1 Fe1 C1 135.8(3) . . . . ? Cl1 B1 Fe1 C1 -44.1(2) . . . . ? O3 B1 Fe1 C2 38.9(3) . . . . ? Cl1 B1 Fe1 C2 -141.0(2) . . . . ? O3 B1 Fe1 C3 -128.2(3) . . . . ? Cl1 B1 Fe1 C3 51.9(2) . . . . ? O3 B1 Fe1 C6 -58.5(3) . . . . ? Cl1 B1 Fe1 C6 121.5(2) . . . . ? O3 B1 Fe1 C7 -94.2(3) . . . . ? Cl1 B1 Fe1 C7 85.8(2) . . . . ? O3 B1 Fe1 C5 -54.7(4) . . . . ? Cl1 B1 Fe1 C5 125.4(2) . . . . ? O3 B1 Fe1 C4 -127.9(3) . . . . ? Cl1 B1 Fe1 C4 52.2(4) . . . . ? C7 C3 Fe1 C1 150.6(2) . . . . ? C4 C3 Fe1 C1 -90.9(2) . . . . ? C8 C3 Fe1 C1 30.3(3) . . . . ? C7 C3 Fe1 C2 -76.7(5) . . . . ? C4 C3 Fe1 C2 41.8(5) . . . . ? C8 C3 Fe1 C2 163.0(4) . . . . ? C7 C3 Fe1 B1 61.3(2) . . . . ? C4 C3 Fe1 B1 179.76(19) . . . . ? C8 C3 Fe1 B1 -59.0(3) . . . . ? C7 C3 Fe1 C6 -37.64(18) . . . . ? C4 C3 Fe1 C6 80.8(2) . . . . ? C8 C3 Fe1 C6 -157.9(4) . . . . ? C4 C3 Fe1 C7 118.5(3) . . . . ? C8 C3 Fe1 C7 -120.3(4) . . . . ? C7 C3 Fe1 C5 -81.1(2) . . . . ? C4 C3 Fe1 C5 37.35(18) . . . . ? C8 C3 Fe1 C5 158.6(4) . . . . ? C7 C3 Fe1 C4 -118.5(3) . . . . ? C8 C3 Fe1 C4 121.2(4) . . . . ? C5 C6 Fe1 C1 -54.0(5) . . . . ? C7 C6 Fe1 C1 63.7(5) . . . . ? C11 C6 Fe1 C1 -175.4(4) . . . . ? C5 C6 Fe1 C2 87.4(2) . . . . ? C7 C6 Fe1 C2 -154.9(2) . . . . ? C11 C6 Fe1 C2 -33.9(3) . . . . ? C5 C6 Fe1 B1 176.5(2) . . . . ? C7 C6 Fe1 B1 -65.7(2) . . . . ? C11 C6 Fe1 B1 55.2(3) . . . . ? C5 C6 Fe1 C3 -80.4(2) . . . . ? C7 C6 Fe1 C3 37.33(19) . . . . ? C11 C6 Fe1 C3 158.3(3) . . . . ? C5 C6 Fe1 C7 -117.7(3) . . . . ? C11 C6 Fe1 C7 120.9(4) . . . . ? C7 C6 Fe1 C5 117.7(3) . . . . ? C11 C6 Fe1 C5 -121.3(4) . . . . ? C5 C6 Fe1 C4 -36.85(19) . . . . ? C7 C6 Fe1 C4 80.9(2) . . . . ? C11 C6 Fe1 C4 -158.2(3) . . . . ? C3 C7 Fe1 C1 -39.3(3) . . . . ? C6 C7 Fe1 C1 -158.2(2) . . . . ? C12 C7 Fe1 C1 80.8(4) . . . . ? C3 C7 Fe1 C2 153.8(2) . . . . ? C6 C7 Fe1 C2 35.0(3) . . . . ? C12 C7 Fe1 C2 -86.0(4) . . . . ? C3 C7 Fe1 B1 -123.1(2) . . . . ? C6 C7 Fe1 B1 118.0(2) . . . . ? C12 C7 Fe1 B1 -3.0(3) . . . . ? C6 C7 Fe1 C3 -118.9(3) . . . . ? C12 C7 Fe1 C3 120.1(4) . . . . ? C3 C7 Fe1 C6 118.9(3) . . . . ? C12 C7 Fe1 C6 -121.0(4) . . . . ? C3 C7 Fe1 C5 80.7(2) . . . . ? C6 C7 Fe1 C5 -38.11(19) . . . . ? C12 C7 Fe1 C5 -159.1(4) . . . . ? C3 C7 Fe1 C4 37.86(19) . . . . ? C6 C7 Fe1 C4 -81.0(2) . . . . ? C12 C7 Fe1 C4 158.0(4) . . . . ? C4 C5 Fe1 C1 41.6(3) . . . . ? C6 C5 Fe1 C1 161.0(2) . . . . ? C10 C5 Fe1 C1 -79.0(4) . . . . ? C4 C5 Fe1 C2 143.5(2) . . . . ? C6 C5 Fe1 C2 -97.1(2) . . . . ? C10 C5 Fe1 C2 23.0(3) . . . . ? C4 C5 Fe1 B1 -125.2(3) . . . . ? C6 C5 Fe1 B1 -5.8(3) . . . . ? C10 C5 Fe1 B1 114.3(3) . . . . ? C4 C5 Fe1 C3 -37.96(19) . . . . ? C6 C5 Fe1 C3 81.4(2) . . . . ? C10 C5 Fe1 C3 -158.5(4) . . . . ? C4 C5 Fe1 C6 -119.4(3) . . . . ? C10 C5 Fe1 C6 120.0(4) . . . . ? C4 C5 Fe1 C7 -81.2(2) . . . . ? C6 C5 Fe1 C7 38.19(19) . . . . ? C10 C5 Fe1 C7 158.2(4) . . . . ? C6 C5 Fe1 C4 119.4(3) . . . . ? C10 C5 Fe1 C4 -120.5(4) . . . . ? C5 C4 Fe1 C1 -148.1(2) . . . . ? C3 C4 Fe1 C1 93.5(2) . . . . ? C9 C4 Fe1 C1 -25.8(4) . . . . ? C5 C4 Fe1 C2 -46.0(3) . . . . ? C3 C4 Fe1 C2 -164.4(2) . . . . ? C9 C4 Fe1 C2 76.3(4) . . . . ? C5 C4 Fe1 B1 118.0(3) . . . . ? C3 C4 Fe1 B1 -0.4(3) . . . . ? C9 C4 Fe1 B1 -119.7(4) . . . . ? C5 C4 Fe1 C3 118.4(3) . . . . ? C9 C4 Fe1 C3 -119.3(4) . . . . ? C5 C4 Fe1 C6 37.35(19) . . . . ? C3 C4 Fe1 C6 -81.08(19) . . . . ? C9 C4 Fe1 C6 159.6(4) . . . . ? C5 C4 Fe1 C7 80.9(2) . . . . ? C3 C4 Fe1 C7 -37.53(18) . . . . ? C9 C4 Fe1 C7 -156.8(4) . . . . ? C3 C4 Fe1 C5 -118.4(3) . . . . ? C9 C4 Fe1 C5 122.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.392 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.101 # Attachment '2a.cif' data_sa0405 _database_code_depnum_ccdc_archive 'CCDC 282086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0405 _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 B1 Cl1 Fe O3' _chemical_formula_sum 'C16 H16 B1 Cl1 Fe O3' _chemical_formula_weight 358.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 7.8325(3) _cell_length_b 8.0671(3) _cell_length_c 13.6886(6) _cell_angle_alpha 81.631(2) _cell_angle_beta 81.424(2) _cell_angle_gamma 75.958(2) _cell_volume 824.29(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13545 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7887 _exptl_absorpt_correction_T_max 0.9478 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 13020 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3685 _reflns_number_gt 2614 _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 'Dirdif-99 (Beurskens et al., 1999)' _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^)+(0.0588P)^2^+0.0432P] 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 3685 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.008 _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 0.0496(5) -0.4373(4) 0.1178(2) 0.0357(8) Uani 1 1 d . . . C2 C 0.3403(5) -0.6728(5) 0.0885(3) 0.0408(9) Uani 1 1 d . . . C3 C 0.4293(5) -0.5755(5) 0.2762(3) 0.0430(9) Uani 1 1 d . . . H3 H 0.5005 -0.6854 0.2954 0.052 Uiso 1 1 calc R . . C4 C 0.2618(5) -0.5010(5) 0.3238(3) 0.0416(9) Uani 1 1 d . . . H4 H 0.2005 -0.5508 0.3814 0.050 Uiso 1 1 calc R . . C5 C 0.2013(5) -0.3384(4) 0.2703(3) 0.0416(9) Uani 1 1 d . . . H5 H 0.0912 -0.2604 0.2850 0.050 Uiso 1 1 calc R . . C6 C 0.3343(6) -0.3126(5) 0.1905(3) 0.0490(10) Uani 1 1 d . . . H6 H 0.3298 -0.2139 0.1428 0.059 Uiso 1 1 calc R . . C7 C 0.4722(5) -0.4584(5) 0.1950(3) 0.0495(10) Uani 1 1 d . . . H7 H 0.5785 -0.4760 0.1504 0.059 Uiso 1 1 calc R . . C8 C -0.1401(4) -0.8425(4) 0.2861(2) 0.0307(7) Uani 1 1 d . . . C9 C -0.1813(4) -0.9340(4) 0.2181(2) 0.0347(8) Uani 1 1 d . . . C10 C -0.2646(4) -1.0672(4) 0.2549(3) 0.0376(8) Uani 1 1 d . . . H10 H -0.2941 -1.1314 0.2095 0.045 Uiso 1 1 calc R . . C11 C -0.3066(4) -1.1098(4) 0.3567(3) 0.0363(8) Uani 1 1 d . . . C12 C -0.2673(4) -1.0101(4) 0.4215(3) 0.0360(8) Uani 1 1 d . . . H12 H -0.2981 -1.0352 0.4909 0.043 Uiso 1 1 calc R . . C13 C -0.1842(4) -0.8747(4) 0.3878(2) 0.0330(8) Uani 1 1 d . . . C14 C -0.1332(5) -0.8911(5) 0.1081(3) 0.0513(10) Uani 1 1 d . . . H14A H -0.1897 -0.7710 0.0880 0.077 Uiso 1 1 calc R . . H14B H -0.1744 -0.9667 0.0714 0.077 Uiso 1 1 calc R . . H14C H -0.0042 -0.9076 0.0933 0.077 Uiso 1 1 calc R . . C15 C -0.3920(5) -1.2598(5) 0.3944(3) 0.0506(10) Uani 1 1 d . . . H15A H -0.4089 -1.2729 0.4673 0.076 Uiso 1 1 calc R . . H15B H -0.3152 -1.3651 0.3710 0.076 Uiso 1 1 calc R . . H15C H -0.5071 -1.2385 0.3694 0.076 Uiso 1 1 calc R . . C16 C -0.1431(5) -0.7690(5) 0.4603(3) 0.0427(9) Uani 1 1 d . . . H16A H -0.0146 -0.7812 0.4553 0.064 Uiso 1 1 calc R . . H16B H -0.1874 -0.8096 0.5281 0.064 Uiso 1 1 calc R . . H16C H -0.2007 -0.6477 0.4445 0.064 Uiso 1 1 calc R . . B1 B 0.1193(5) -0.7177(5) 0.2386(3) 0.0291(8) Uani 1 1 d . . . Cl1 Cl 0.25061(11) -0.92238(10) 0.28790(7) 0.0420(3) Uani 1 1 d . . . Fe1 Fe 0.23920(6) -0.53192(6) 0.17766(3) 0.03072(18) Uani 1 1 d . . . O1 O -0.0771(4) -0.3746(3) 0.08167(19) 0.0491(7) Uani 1 1 d . . . O2 O 0.4086(4) -0.7678(4) 0.0328(2) 0.0612(8) Uani 1 1 d . . . O3 O -0.0574(3) -0.7053(3) 0.24893(16) 0.0341(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(2) 0.0286(18) 0.0323(18) -0.0033(14) -0.0043(17) -0.0094(17) C2 0.038(2) 0.043(2) 0.041(2) -0.0021(18) -0.0089(17) -0.0081(18) C3 0.034(2) 0.041(2) 0.058(2) -0.0139(19) -0.0205(18) -0.0029(17) C4 0.043(2) 0.048(2) 0.038(2) -0.0096(17) -0.0132(17) -0.0118(19) C5 0.042(2) 0.035(2) 0.052(2) -0.0171(17) -0.0145(18) -0.0027(17) C6 0.058(3) 0.039(2) 0.058(2) -0.0068(18) -0.009(2) -0.024(2) C7 0.034(2) 0.056(3) 0.065(3) -0.020(2) -0.0018(19) -0.018(2) C8 0.0199(16) 0.0307(17) 0.0384(19) 0.0008(15) -0.0046(14) -0.0021(14) C9 0.0243(17) 0.042(2) 0.0366(18) -0.0080(16) -0.0039(14) -0.0037(16) C10 0.0313(19) 0.041(2) 0.043(2) -0.0127(16) -0.0096(16) -0.0049(16) C11 0.0238(18) 0.0317(18) 0.052(2) -0.0027(16) -0.0070(16) -0.0027(15) C12 0.0294(19) 0.041(2) 0.0340(18) 0.0038(16) -0.0070(15) -0.0042(16) C13 0.0263(18) 0.0325(18) 0.0390(19) -0.0031(15) -0.0073(15) -0.0027(15) C14 0.052(2) 0.067(3) 0.035(2) -0.0095(18) 0.0028(18) -0.015(2) C15 0.050(2) 0.036(2) 0.066(3) 0.0030(19) -0.013(2) -0.0124(19) C16 0.045(2) 0.045(2) 0.039(2) -0.0046(16) -0.0067(17) -0.0111(19) B1 0.030(2) 0.029(2) 0.0269(19) -0.0066(15) -0.0054(15) -0.0017(16) Cl1 0.0322(5) 0.0295(5) 0.0601(6) 0.0037(4) -0.0094(4) -0.0019(4) Fe1 0.0309(3) 0.0293(3) 0.0328(3) -0.0049(2) -0.0049(2) -0.0068(2) O1 0.0493(17) 0.0486(16) 0.0487(15) -0.0047(12) -0.0232(13) 0.0004(14) O2 0.0613(19) 0.0676(19) 0.0503(17) -0.0277(15) 0.0023(15) 0.0006(16) O3 0.0273(12) 0.0321(13) 0.0410(13) 0.0025(10) -0.0050(10) -0.0067(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.147(4) . ? C1 Fe1 1.758(4) . ? C2 O2 1.141(4) . ? C2 Fe1 1.757(4) . ? C3 C7 1.406(5) . ? C3 C4 1.409(5) . ? C3 Fe1 2.089(3) . ? C3 H3 0.9500 . ? C4 C5 1.415(5) . ? C4 Fe1 2.089(3) . ? C4 H4 0.9500 . ? C5 C6 1.421(5) . ? C5 Fe1 2.090(3) . ? C5 H5 0.9500 . ? C6 C7 1.392(5) . ? C6 Fe1 2.118(3) . ? C6 H6 0.9500 . ? C7 Fe1 2.106(4) . ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C8 C13 1.386(5) . ? C8 O3 1.410(4) . ? C9 C10 1.385(5) . ? C9 C14 1.507(5) . ? C10 C11 1.396(5) . ? C10 H10 0.9500 . ? C11 C12 1.392(5) . ? C11 C15 1.512(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C16 1.514(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? B1 O3 1.350(4) . ? B1 Cl1 1.816(4) . ? B1 Fe1 1.977(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 O1 C1 Fe1 177.8(3) . . ? O2 C2 Fe1 177.8(3) . . ? C7 C3 C4 107.8(3) . . ? C7 C3 Fe1 71.1(2) . . ? C4 C3 Fe1 70.31(19) . . ? C7 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe1 C3 H3 124.2 . . ? C3 C4 C5 107.6(3) . . ? C3 C4 Fe1 70.3(2) . . ? C5 C4 Fe1 70.25(19) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? Fe1 C4 H4 124.9 . . ? C4 C5 C6 107.9(3) . . ? C4 C5 Fe1 70.17(19) . . ? C6 C5 Fe1 71.3(2) . . ? C4 C5 H5 126.0 . . ? C6 C5 H5 126.0 . . ? Fe1 C5 H5 124.1 . . ? C7 C6 C5 107.4(3) . . ? C7 C6 Fe1 70.3(2) . . ? C5 C6 Fe1 69.23(19) . . ? C7 C6 H6 126.3 . . ? C5 C6 H6 126.3 . . ? Fe1 C6 H6 125.8 . . ? C6 C7 C3 109.2(3) . . ? C6 C7 Fe1 71.2(2) . . ? C3 C7 Fe1 69.8(2) . . ? C6 C7 H7 125.4 . . ? C3 C7 H7 125.4 . . ? Fe1 C7 H7 125.2 . . ? C9 C8 C13 122.9(3) . . ? C9 C8 O3 118.0(3) . . ? C13 C8 O3 119.0(3) . . ? C10 C9 C8 117.8(3) . . ? C10 C9 C14 121.6(3) . . ? C8 C9 C14 120.6(3) . . ? C9 C10 C11 121.9(3) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 117.8(3) . . ? C12 C11 C15 121.6(3) . . ? C10 C11 C15 120.5(3) . . ? C11 C12 C13 122.1(3) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C8 C13 C12 117.4(3) . . ? C8 C13 C16 121.9(3) . . ? C12 C13 C16 120.7(3) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 B1 Cl1 115.5(3) . . ? O3 B1 Fe1 125.2(3) . . ? Cl1 B1 Fe1 119.4(2) . . ? C2 Fe1 C1 95.82(16) . . ? C2 Fe1 B1 84.87(16) . . ? C1 Fe1 B1 87.76(15) . . ? C2 Fe1 C4 138.69(16) . . ? C1 Fe1 C4 123.73(15) . . ? B1 Fe1 C4 85.25(14) . . ? C2 Fe1 C3 102.88(15) . . ? C1 Fe1 C3 160.90(15) . . ? B1 Fe1 C3 97.63(15) . . ? C4 Fe1 C3 39.40(14) . . ? C2 Fe1 C5 160.29(16) . . ? C1 Fe1 C5 94.88(15) . . ? B1 Fe1 C5 112.08(15) . . ? C4 Fe1 C5 39.58(13) . . ? C3 Fe1 C5 66.10(14) . . ? C2 Fe1 C7 95.55(16) . . ? C1 Fe1 C7 135.68(16) . . ? B1 Fe1 C7 135.89(16) . . ? C4 Fe1 C7 65.65(15) . . ? C3 Fe1 C7 39.16(15) . . ? C5 Fe1 C7 65.42(15) . . ? C2 Fe1 C6 121.77(17) . . ? C1 Fe1 C6 101.16(16) . . ? B1 Fe1 C6 150.23(16) . . ? C4 Fe1 C6 66.08(15) . . ? C3 Fe1 C6 65.64(15) . . ? C5 Fe1 C6 39.47(15) . . ? C7 Fe1 C6 38.48(15) . . ? B1 O3 C8 124.6(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 C7 C3 C4 C5 0.9(4) . . . . ? Fe1 C3 C4 C5 -60.6(2) . . . . ? C7 C3 C4 Fe1 61.5(2) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? Fe1 C4 C5 C6 -61.6(2) . . . . ? C3 C4 C5 Fe1 60.6(2) . . . . ? C4 C5 C6 C7 0.7(4) . . . . ? Fe1 C5 C6 C7 -60.2(2) . . . . ? C4 C5 C6 Fe1 60.9(2) . . . . ? C5 C6 C7 C3 -0.2(4) . . . . ? Fe1 C6 C7 C3 -59.7(2) . . . . ? C5 C6 C7 Fe1 59.5(2) . . . . ? C4 C3 C7 C6 -0.5(4) . . . . ? Fe1 C3 C7 C6 60.6(3) . . . . ? C4 C3 C7 Fe1 -61.0(2) . . . . ? C13 C8 C9 C10 -2.4(5) . . . . ? O3 C8 C9 C10 -179.2(3) . . . . ? C13 C8 C9 C14 178.8(3) . . . . ? O3 C8 C9 C14 2.0(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C14 C9 C10 C11 178.8(3) . . . . ? C9 C10 C11 C12 2.1(5) . . . . ? C9 C10 C11 C15 -177.9(3) . . . . ? C10 C11 C12 C13 -1.8(5) . . . . ? C15 C11 C12 C13 178.2(3) . . . . ? C9 C8 C13 C12 2.6(5) . . . . ? O3 C8 C13 C12 179.4(3) . . . . ? C9 C8 C13 C16 -177.9(3) . . . . ? O3 C8 C13 C16 -1.2(5) . . . . ? C11 C12 C13 C8 -0.5(5) . . . . ? C11 C12 C13 C16 -179.9(3) . . . . ? O2 C2 Fe1 C1 -152(9) . . . . ? O2 C2 Fe1 B1 -65(9) . . . . ? O2 C2 Fe1 C4 12(9) . . . . ? O2 C2 Fe1 C3 31(9) . . . . ? O2 C2 Fe1 C5 85(9) . . . . ? O2 C2 Fe1 C7 70(9) . . . . ? O2 C2 Fe1 C6 101(9) . . . . ? O1 C1 Fe1 C2 152(8) . . . . ? O1 C1 Fe1 B1 67(8) . . . . ? O1 C1 Fe1 C4 -15(8) . . . . ? O1 C1 Fe1 C3 -40(8) . . . . ? O1 C1 Fe1 C5 -45(8) . . . . ? O1 C1 Fe1 C7 -104(8) . . . . ? O1 C1 Fe1 C6 -84(8) . . . . ? O3 B1 Fe1 C2 -117.0(3) . . . . ? Cl1 B1 Fe1 C2 64.4(2) . . . . ? O3 B1 Fe1 C1 -20.9(3) . . . . ? Cl1 B1 Fe1 C1 160.4(2) . . . . ? O3 B1 Fe1 C4 103.2(3) . . . . ? Cl1 B1 Fe1 C4 -75.5(2) . . . . ? O3 B1 Fe1 C3 140.7(3) . . . . ? Cl1 B1 Fe1 C3 -38.0(2) . . . . ? O3 B1 Fe1 C5 73.4(3) . . . . ? Cl1 B1 Fe1 C5 -105.2(2) . . . . ? O3 B1 Fe1 C7 150.3(3) . . . . ? Cl1 B1 Fe1 C7 -28.3(3) . . . . ? O3 B1 Fe1 C6 87.8(4) . . . . ? Cl1 B1 Fe1 C6 -90.8(4) . . . . ? C3 C4 Fe1 C2 31.4(3) . . . . ? C5 C4 Fe1 C2 149.5(3) . . . . ? C3 C4 Fe1 C1 -167.8(2) . . . . ? C5 C4 Fe1 C1 -49.7(3) . . . . ? C3 C4 Fe1 B1 108.1(2) . . . . ? C5 C4 Fe1 B1 -133.8(2) . . . . ? C5 C4 Fe1 C3 118.1(3) . . . . ? C3 C4 Fe1 C5 -118.1(3) . . . . ? C3 C4 Fe1 C7 -37.8(2) . . . . ? C5 C4 Fe1 C7 80.3(2) . . . . ? C3 C4 Fe1 C6 -80.1(2) . . . . ? C5 C4 Fe1 C6 37.9(2) . . . . ? C7 C3 Fe1 C2 82.9(2) . . . . ? C4 C3 Fe1 C2 -159.3(2) . . . . ? C7 C3 Fe1 C1 -85.2(5) . . . . ? C4 C3 Fe1 C1 32.6(6) . . . . ? C7 C3 Fe1 B1 169.3(2) . . . . ? C4 C3 Fe1 B1 -72.9(2) . . . . ? C7 C3 Fe1 C4 -117.8(3) . . . . ? C7 C3 Fe1 C5 -79.8(2) . . . . ? C4 C3 Fe1 C5 37.9(2) . . . . ? C4 C3 Fe1 C7 117.8(3) . . . . ? C7 C3 Fe1 C6 -36.4(2) . . . . ? C4 C3 Fe1 C6 81.4(2) . . . . ? C4 C5 Fe1 C2 -96.8(5) . . . . ? C6 C5 Fe1 C2 21.0(5) . . . . ? C4 C5 Fe1 C1 140.5(2) . . . . ? C6 C5 Fe1 C1 -101.6(2) . . . . ? C4 C5 Fe1 B1 50.9(2) . . . . ? C6 C5 Fe1 B1 168.8(2) . . . . ? C6 C5 Fe1 C4 117.9(3) . . . . ? C4 C5 Fe1 C3 -37.8(2) . . . . ? C6 C5 Fe1 C3 80.1(2) . . . . ? C4 C5 Fe1 C7 -80.9(2) . . . . ? C6 C5 Fe1 C7 37.0(2) . . . . ? C4 C5 Fe1 C6 -117.9(3) . . . . ? C6 C7 Fe1 C2 136.7(3) . . . . ? C3 C7 Fe1 C2 -103.6(2) . . . . ? C6 C7 Fe1 C1 32.5(3) . . . . ? C3 C7 Fe1 C1 152.2(2) . . . . ? C6 C7 Fe1 B1 -134.9(3) . . . . ? C3 C7 Fe1 B1 -15.3(3) . . . . ? C6 C7 Fe1 C4 -81.6(2) . . . . ? C3 C7 Fe1 C4 38.1(2) . . . . ? C6 C7 Fe1 C3 -119.7(3) . . . . ? C6 C7 Fe1 C5 -37.9(2) . . . . ? C3 C7 Fe1 C5 81.7(2) . . . . ? C3 C7 Fe1 C6 119.7(3) . . . . ? C7 C6 Fe1 C2 -53.4(3) . . . . ? C5 C6 Fe1 C2 -171.8(2) . . . . ? C7 C6 Fe1 C1 -157.5(2) . . . . ? C5 C6 Fe1 C1 84.1(2) . . . . ? C7 C6 Fe1 B1 97.2(4) . . . . ? C5 C6 Fe1 B1 -21.3(4) . . . . ? C7 C6 Fe1 C4 80.4(2) . . . . ? C5 C6 Fe1 C4 -38.0(2) . . . . ? C7 C6 Fe1 C3 37.0(2) . . . . ? C5 C6 Fe1 C3 -81.4(2) . . . . ? C7 C6 Fe1 C5 118.4(3) . . . . ? C5 C6 Fe1 C7 -118.4(3) . . . . ? Cl1 B1 O3 C8 -6.0(4) . . . . ? Fe1 B1 O3 C8 175.3(2) . . . . ? C9 C8 O3 B1 -95.9(4) . . . . ? C13 C8 O3 B1 87.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.518 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.194 # Attachment '2d.cif' data_sa0404 _database_code_depnum_ccdc_archive 'CCDC 282087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0404 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 B Fe O3 S' _chemical_formula_weight 432.11 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4401(4) _cell_length_b 9.7496(3) _cell_length_c 14.5657(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.901(1) _cell_angle_gamma 90.00 _cell_volume 2049.51(12) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6714 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Rod _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7535 _exptl_absorpt_correction_T_max 0.9192 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12489 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.43 _reflns_number_total 4272 _reflns_number_gt 2833 _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 'Dirdif-99 (Beurskens et al., 1999)' _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^)+(0.0453P)^2^+1.7529P] 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 4272 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.0033(2) 0.1272(4) 0.3843(3) 0.0325(9) Uani 1 1 d . . . C2 C 0.1126(3) 0.1664(4) 0.2554(2) 0.0312(8) Uani 1 1 d . . . C3 C -0.0441(3) -0.1300(4) 0.3106(3) 0.0400(10) Uani 1 1 d . . . H3 H -0.0916 -0.1353 0.3541 0.048 Uiso 1 1 calc R . . C4 C 0.0526(3) -0.1481(3) 0.3295(3) 0.0338(9) Uani 1 1 d . . . H4 H 0.0809 -0.1687 0.3877 0.041 Uiso 1 1 calc R . . C5 C 0.0982(3) -0.1302(4) 0.2474(3) 0.0340(9) Uani 1 1 d . . . H5 H 0.1632 -0.1364 0.2401 0.041 Uiso 1 1 calc R . . C6 C 0.0312(3) -0.1012(4) 0.1767(3) 0.0359(9) Uani 1 1 d . . . H6 H 0.0433 -0.0838 0.1140 0.043 Uiso 1 1 calc R . . C7 C -0.0567(3) -0.1030(4) 0.2163(3) 0.0391(10) Uani 1 1 d . . . H7 H -0.1144 -0.0884 0.1846 0.047 Uiso 1 1 calc R . . C8 C -0.1417(2) 0.3199(4) 0.3150(2) 0.0278(8) Uani 1 1 d . . . C9 C -0.2156(2) 0.2533(4) 0.3539(3) 0.0338(9) Uani 1 1 d . . . C10 C -0.2438(3) 0.3017(4) 0.4387(3) 0.0400(10) Uani 1 1 d . . . H10 H -0.2939 0.2571 0.4671 0.048 Uiso 1 1 calc R . . C11 C -0.2018(3) 0.4122(4) 0.4830(3) 0.0395(10) Uani 1 1 d . . . C12 C -0.1283(3) 0.4748(4) 0.4408(3) 0.0365(9) Uani 1 1 d . . . H12 H -0.0984 0.5504 0.4703 0.044 Uiso 1 1 calc R . . C13 C -0.0970(2) 0.4303(4) 0.3565(3) 0.0315(8) Uani 1 1 d . . . C14 C -0.2634(3) 0.1340(4) 0.3067(3) 0.0487(11) Uani 1 1 d . . . H14A H -0.2339 0.1154 0.2484 0.073 Uiso 1 1 calc R . . H14B H -0.3289 0.1564 0.2949 0.073 Uiso 1 1 calc R . . H14C H -0.2585 0.0527 0.3462 0.073 Uiso 1 1 calc R . . C15 C -0.2352(3) 0.4629(5) 0.5742(3) 0.0613(13) Uani 1 1 d . . . H15A H -0.1972 0.5409 0.5950 0.092 Uiso 1 1 calc R . . H15B H -0.2302 0.3889 0.6196 0.092 Uiso 1 1 calc R . . H15C H -0.3001 0.4919 0.5671 0.092 Uiso 1 1 calc R . . C16 C -0.0160(3) 0.4986(4) 0.3122(3) 0.0430(10) Uani 1 1 d . . . H16A H 0.0069 0.5740 0.3512 0.064 Uiso 1 1 calc R . . H16B H -0.0358 0.5347 0.2519 0.064 Uiso 1 1 calc R . . H16C H 0.0337 0.4314 0.3047 0.064 Uiso 1 1 calc R . . C17 C -0.1123(3) 0.2959(4) 0.0225(2) 0.0332(9) Uani 1 1 d . . . C18 C -0.2068(3) 0.3022(5) 0.0358(3) 0.0482(11) Uani 1 1 d . . . H18 H -0.2349 0.2419 0.0778 0.058 Uiso 1 1 calc R . . C19 C -0.2598(3) 0.3979(6) -0.0131(3) 0.0619(14) Uani 1 1 d . . . H19 H -0.3244 0.4036 -0.0034 0.074 Uiso 1 1 calc R . . C20 C -0.2208(3) 0.4841(5) -0.0751(3) 0.0558(12) Uani 1 1 d . . . H20 H -0.2581 0.5492 -0.1078 0.067 Uiso 1 1 calc R . . C21 C -0.1279(3) 0.4762(4) -0.0898(3) 0.0503(11) Uani 1 1 d . . . H21 H -0.1005 0.5353 -0.1331 0.060 Uiso 1 1 calc R . . C22 C -0.0741(3) 0.3822(4) -0.0415(3) 0.0401(10) Uani 1 1 d . . . H22 H -0.0097 0.3765 -0.0524 0.048 Uiso 1 1 calc R . . B1 B -0.0551(3) 0.1850(4) 0.2025(3) 0.0279(9) Uani 1 1 d . . . Fe1 Fe 0.02450(3) 0.05167(5) 0.27799(3) 0.02514(17) Uani 1 1 d . . . O1 O -0.0044(2) 0.1684(3) 0.45774(18) 0.0490(8) Uani 1 1 d . . . O2 O 0.17106(19) 0.2457(3) 0.2424(2) 0.0498(7) Uani 1 1 d . . . O3 O -0.11629(17) 0.2819(3) 0.22682(16) 0.0348(6) Uani 1 1 d . . . S1 S -0.03871(8) 0.17246(11) 0.07751(7) 0.0435(3) 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 0.037(2) 0.033(2) 0.028(2) 0.0057(17) -0.0028(17) 0.0091(17) C2 0.034(2) 0.033(2) 0.027(2) -0.0026(16) -0.0011(16) 0.0065(18) C3 0.041(2) 0.029(2) 0.051(3) -0.0031(19) 0.007(2) -0.0065(18) C4 0.044(2) 0.0253(19) 0.033(2) 0.0031(16) 0.0015(18) 0.0022(17) C5 0.040(2) 0.028(2) 0.034(2) -0.0019(17) 0.0004(18) 0.0076(17) C6 0.049(2) 0.029(2) 0.030(2) -0.0078(17) -0.0005(18) 0.0036(18) C7 0.042(2) 0.028(2) 0.046(3) -0.0046(18) -0.0099(19) -0.0018(17) C8 0.0308(19) 0.0306(19) 0.0219(19) 0.0007(16) -0.0036(15) 0.0109(16) C9 0.029(2) 0.038(2) 0.033(2) 0.0042(18) -0.0075(17) 0.0050(17) C10 0.030(2) 0.049(3) 0.041(2) 0.010(2) 0.0056(18) 0.0056(19) C11 0.037(2) 0.051(3) 0.030(2) 0.0023(19) 0.0056(18) 0.0158(19) C12 0.039(2) 0.036(2) 0.034(2) -0.0085(18) -0.0032(18) 0.0105(18) C13 0.0319(19) 0.031(2) 0.032(2) 0.0065(17) -0.0013(16) 0.0094(17) C14 0.040(2) 0.046(3) 0.060(3) -0.006(2) -0.004(2) 0.000(2) C15 0.067(3) 0.078(4) 0.040(3) -0.006(2) 0.014(2) 0.018(3) C16 0.046(2) 0.036(2) 0.048(3) 0.003(2) 0.007(2) 0.0035(19) C17 0.042(2) 0.038(2) 0.0190(19) -0.0025(17) -0.0057(16) 0.0059(18) C18 0.046(2) 0.069(3) 0.029(2) 0.007(2) -0.0069(19) -0.005(2) C19 0.038(2) 0.108(4) 0.039(3) 0.005(3) -0.011(2) 0.012(3) C20 0.068(3) 0.065(3) 0.033(3) 0.008(2) -0.015(2) 0.023(3) C21 0.062(3) 0.047(3) 0.042(3) 0.016(2) -0.001(2) 0.005(2) C22 0.042(2) 0.047(2) 0.032(2) 0.0029(19) 0.0029(18) 0.003(2) B1 0.029(2) 0.029(2) 0.025(2) 0.0018(18) -0.0036(18) 0.0007(18) Fe1 0.0293(3) 0.0251(3) 0.0210(3) -0.0003(2) 0.0003(2) 0.0017(2) O1 0.0661(19) 0.0582(19) 0.0224(16) -0.0042(13) -0.0001(14) 0.0233(16) O2 0.0428(17) 0.0462(17) 0.060(2) 0.0049(15) 0.0046(14) -0.0079(15) O3 0.0414(14) 0.0406(15) 0.0220(14) -0.0001(12) -0.0027(11) 0.0132(12) S1 0.0624(7) 0.0461(6) 0.0219(5) 0.0022(4) 0.0010(5) 0.0200(5) _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 O1 1.151(4) . ? C1 Fe1 1.751(4) . ? C2 O2 1.165(4) . ? C2 Fe1 1.734(4) . ? C3 C7 1.406(6) . ? C3 C4 1.424(5) . ? C3 Fe1 2.092(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 Fe1 2.122(4) . ? C4 H4 0.9500 . ? C5 C6 1.418(5) . ? C5 Fe1 2.123(3) . ? C5 H5 0.9500 . ? C6 C7 1.411(5) . ? C6 Fe1 2.102(4) . ? C6 H6 0.9500 . ? C7 Fe1 2.094(4) . ? C7 H7 0.9500 . ? C8 C13 1.383(5) . ? C8 C9 1.386(5) . ? C8 O3 1.398(4) . ? C9 C10 1.395(5) . ? C9 C14 1.507(5) . ? C10 C11 1.385(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(5) . ? C11 C15 1.511(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C16 1.510(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.384(5) . ? C17 C18 1.385(5) . ? C17 S1 1.779(4) . ? C18 C19 1.389(6) . ? C18 H18 0.9500 . ? C19 C20 1.368(6) . ? C19 H19 0.9500 . ? C20 C21 1.368(6) . ? C20 H20 0.9500 . ? C21 C22 1.379(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? B1 O3 1.349(5) . ? B1 S1 1.848(4) . ? B1 Fe1 2.034(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 O1 C1 Fe1 173.4(3) . . ? O2 C2 Fe1 178.1(3) . . ? C7 C3 C4 107.9(3) . . ? C7 C3 Fe1 70.5(2) . . ? C4 C3 Fe1 71.4(2) . . ? C7 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe1 C3 H3 123.7 . . ? C5 C4 C3 107.8(4) . . ? C5 C4 Fe1 70.9(2) . . ? C3 C4 Fe1 69.1(2) . . ? C5 C4 H4 126.1 . . ? C3 C4 H4 126.1 . . ? Fe1 C4 H4 125.5 . . ? C4 C5 C6 108.5(3) . . ? C4 C5 Fe1 70.7(2) . . ? C6 C5 Fe1 69.6(2) . . ? C4 C5 H5 125.8 . . ? C6 C5 H5 125.8 . . ? Fe1 C5 H5 125.5 . . ? C7 C6 C5 107.6(3) . . ? C7 C6 Fe1 70.1(2) . . ? C5 C6 Fe1 71.2(2) . . ? C7 C6 H6 126.2 . . ? C5 C6 H6 126.2 . . ? Fe1 C6 H6 124.2 . . ? C3 C7 C6 108.2(4) . . ? C3 C7 Fe1 70.3(2) . . ? C6 C7 Fe1 70.6(2) . . ? C3 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe1 C7 H7 124.8 . . ? C13 C8 C9 122.7(3) . . ? C13 C8 O3 118.4(3) . . ? C9 C8 O3 118.7(3) . . ? C8 C9 C10 117.1(3) . . ? C8 C9 C14 121.5(3) . . ? C10 C9 C14 121.5(3) . . ? C11 C10 C9 122.6(3) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 117.8(3) . . ? C10 C11 C15 121.1(4) . . ? C12 C11 C15 121.1(4) . . ? C11 C12 C13 122.0(4) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C8 C13 C12 117.8(3) . . ? C8 C13 C16 120.9(3) . . ? C12 C13 C16 121.2(3) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 118.9(4) . . ? C22 C17 S1 118.0(3) . . ? C18 C17 S1 122.9(3) . . ? C17 C18 C19 119.2(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C17 121.2(4) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? O3 B1 S1 114.3(3) . . ? O3 B1 Fe1 132.0(3) . . ? S1 B1 Fe1 113.7(2) . . ? C2 Fe1 C1 92.70(17) . . ? C2 Fe1 B1 83.70(16) . . ? C1 Fe1 B1 95.56(16) . . ? C2 Fe1 C3 160.98(16) . . ? C1 Fe1 C3 93.27(16) . . ? B1 Fe1 C3 113.63(16) . . ? C2 Fe1 C7 141.92(16) . . ? C1 Fe1 C7 124.79(16) . . ? B1 Fe1 C7 85.97(16) . . ? C3 Fe1 C7 39.24(15) . . ? C2 Fe1 C6 105.88(16) . . ? C1 Fe1 C6 158.84(16) . . ? B1 Fe1 C6 96.45(16) . . ? C3 Fe1 C6 65.93(16) . . ? C7 Fe1 C6 39.31(14) . . ? C2 Fe1 C4 121.78(15) . . ? C1 Fe1 C4 96.32(15) . . ? B1 Fe1 C4 151.17(16) . . ? C3 Fe1 C4 39.51(15) . . ? C7 Fe1 C4 65.72(15) . . ? C6 Fe1 C4 65.46(15) . . ? C2 Fe1 C5 97.07(15) . . ? C1 Fe1 C5 129.84(15) . . ? B1 Fe1 C5 134.33(15) . . ? C3 Fe1 C5 65.48(15) . . ? C7 Fe1 C5 65.56(15) . . ? C6 Fe1 C5 39.22(14) . . ? C4 Fe1 C5 38.40(13) . . ? B1 O3 C8 128.4(3) . . ? C17 S1 B1 107.76(18) . . ? 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 C7 C3 C4 C5 0.8(4) . . . . ? Fe1 C3 C4 C5 -60.6(2) . . . . ? C7 C3 C4 Fe1 61.4(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? Fe1 C4 C5 C6 -59.6(3) . . . . ? C3 C4 C5 Fe1 59.4(3) . . . . ? C4 C5 C6 C7 -0.6(4) . . . . ? Fe1 C5 C6 C7 -60.9(3) . . . . ? C4 C5 C6 Fe1 60.3(2) . . . . ? C4 C3 C7 C6 -1.2(4) . . . . ? Fe1 C3 C7 C6 60.8(3) . . . . ? C4 C3 C7 Fe1 -62.0(3) . . . . ? C5 C6 C7 C3 1.1(4) . . . . ? Fe1 C6 C7 C3 -60.5(3) . . . . ? C5 C6 C7 Fe1 61.7(3) . . . . ? C13 C8 C9 C10 -0.3(5) . . . . ? O3 C8 C9 C10 -174.8(3) . . . . ? C13 C8 C9 C14 179.5(3) . . . . ? O3 C8 C9 C14 5.1(5) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C14 C9 C10 C11 -179.2(4) . . . . ? C9 C10 C11 C12 -0.7(6) . . . . ? C9 C10 C11 C15 179.1(4) . . . . ? C10 C11 C12 C13 0.4(6) . . . . ? C15 C11 C12 C13 -179.5(4) . . . . ? C9 C8 C13 C12 0.0(5) . . . . ? O3 C8 C13 C12 174.5(3) . . . . ? C9 C8 C13 C16 179.2(3) . . . . ? O3 C8 C13 C16 -6.3(5) . . . . ? C11 C12 C13 C8 0.0(5) . . . . ? C11 C12 C13 C16 -179.2(3) . . . . ? C22 C17 C18 C19 -2.1(6) . . . . ? S1 C17 C18 C19 -177.1(3) . . . . ? C17 C18 C19 C20 1.1(7) . . . . ? C18 C19 C20 C21 0.3(7) . . . . ? C19 C20 C21 C22 -0.5(7) . . . . ? C20 C21 C22 C17 -0.6(6) . . . . ? C18 C17 C22 C21 1.9(6) . . . . ? S1 C17 C22 C21 177.1(3) . . . . ? O2 C2 Fe1 C1 -10(10) . . . . ? O2 C2 Fe1 B1 85(10) . . . . ? O2 C2 Fe1 C3 -119(10) . . . . ? O2 C2 Fe1 C7 160(10) . . . . ? O2 C2 Fe1 C6 180(100) . . . . ? O2 C2 Fe1 C4 -110(10) . . . . ? O2 C2 Fe1 C5 -141(10) . . . . ? O1 C1 Fe1 C2 -89(3) . . . . ? O1 C1 Fe1 B1 -173(3) . . . . ? O1 C1 Fe1 C3 73(3) . . . . ? O1 C1 Fe1 C7 98(3) . . . . ? O1 C1 Fe1 C6 63(3) . . . . ? O1 C1 Fe1 C4 33(3) . . . . ? O1 C1 Fe1 C5 13(3) . . . . ? O3 B1 Fe1 C2 -102.7(4) . . . . ? S1 B1 Fe1 C2 76.1(2) . . . . ? O3 B1 Fe1 C1 -10.6(4) . . . . ? S1 B1 Fe1 C1 168.2(2) . . . . ? O3 B1 Fe1 C3 85.4(4) . . . . ? S1 B1 Fe1 C3 -95.7(2) . . . . ? O3 B1 Fe1 C7 114.0(4) . . . . ? S1 B1 Fe1 C7 -67.2(2) . . . . ? O3 B1 Fe1 C6 151.9(4) . . . . ? S1 B1 Fe1 C6 -29.2(2) . . . . ? O3 B1 Fe1 C4 103.4(4) . . . . ? S1 B1 Fe1 C4 -77.8(4) . . . . ? O3 B1 Fe1 C5 163.5(3) . . . . ? S1 B1 Fe1 C5 -17.6(3) . . . . ? C7 C3 Fe1 C2 -105.5(5) . . . . ? C4 C3 Fe1 C2 12.1(6) . . . . ? C7 C3 Fe1 C1 146.5(2) . . . . ? C4 C3 Fe1 C1 -96.0(2) . . . . ? C7 C3 Fe1 B1 48.9(3) . . . . ? C4 C3 Fe1 B1 166.5(2) . . . . ? C4 C3 Fe1 C7 117.6(3) . . . . ? C7 C3 Fe1 C6 -37.6(2) . . . . ? C4 C3 Fe1 C6 80.0(2) . . . . ? C7 C3 Fe1 C4 -117.6(3) . . . . ? C7 C3 Fe1 C5 -80.8(2) . . . . ? C4 C3 Fe1 C5 36.8(2) . . . . ? C3 C7 Fe1 C2 149.4(3) . . . . ? C6 C7 Fe1 C2 30.9(4) . . . . ? C3 C7 Fe1 C1 -42.2(3) . . . . ? C6 C7 Fe1 C1 -160.7(2) . . . . ? C3 C7 Fe1 B1 -136.2(2) . . . . ? C6 C7 Fe1 B1 105.3(2) . . . . ? C6 C7 Fe1 C3 -118.5(3) . . . . ? C3 C7 Fe1 C6 118.5(3) . . . . ? C3 C7 Fe1 C4 38.2(2) . . . . ? C6 C7 Fe1 C4 -80.3(2) . . . . ? C3 C7 Fe1 C5 80.5(2) . . . . ? C6 C7 Fe1 C5 -38.0(2) . . . . ? C7 C6 Fe1 C2 -160.8(2) . . . . ? C5 C6 Fe1 C2 81.6(2) . . . . ? C7 C6 Fe1 C1 48.7(5) . . . . ? C5 C6 Fe1 C1 -69.0(5) . . . . ? C7 C6 Fe1 B1 -75.5(3) . . . . ? C5 C6 Fe1 B1 166.8(2) . . . . ? C7 C6 Fe1 C3 37.5(2) . . . . ? C5 C6 Fe1 C3 -80.1(2) . . . . ? C5 C6 Fe1 C7 -117.6(3) . . . . ? C7 C6 Fe1 C4 81.0(2) . . . . ? C5 C6 Fe1 C4 -36.6(2) . . . . ? C7 C6 Fe1 C5 117.6(3) . . . . ? C5 C4 Fe1 C2 -56.7(3) . . . . ? C3 C4 Fe1 C2 -175.4(2) . . . . ? C5 C4 Fe1 C1 -153.9(2) . . . . ? C3 C4 Fe1 C1 87.5(2) . . . . ? C5 C4 Fe1 B1 92.3(4) . . . . ? C3 C4 Fe1 B1 -26.3(4) . . . . ? C5 C4 Fe1 C3 118.7(3) . . . . ? C5 C4 Fe1 C7 80.7(2) . . . . ? C3 C4 Fe1 C7 -38.0(2) . . . . ? C5 C4 Fe1 C6 37.3(2) . . . . ? C3 C4 Fe1 C6 -81.3(3) . . . . ? C3 C4 Fe1 C5 -118.7(3) . . . . ? C4 C5 Fe1 C2 134.3(2) . . . . ? C6 C5 Fe1 C2 -106.5(2) . . . . ? C4 C5 Fe1 C1 34.8(3) . . . . ? C6 C5 Fe1 C1 154.0(2) . . . . ? C4 C5 Fe1 B1 -137.7(3) . . . . ? C6 C5 Fe1 B1 -18.4(3) . . . . ? C4 C5 Fe1 C3 -37.8(2) . . . . ? C6 C5 Fe1 C3 81.4(2) . . . . ? C4 C5 Fe1 C7 -81.2(2) . . . . ? C6 C5 Fe1 C7 38.1(2) . . . . ? C4 C5 Fe1 C6 -119.2(3) . . . . ? C6 C5 Fe1 C4 119.2(3) . . . . ? S1 B1 O3 C8 -177.7(3) . . . . ? Fe1 B1 O3 C8 1.1(6) . . . . ? C13 C8 O3 B1 95.3(4) . . . . ? C9 C8 O3 B1 -90.0(4) . . . . ? C22 C17 S1 B1 130.6(3) . . . . ? C18 C17 S1 B1 -54.4(4) . . . . ? O3 B1 S1 C17 -0.6(3) . . . . ? Fe1 B1 S1 C17 -179.63(19) . . . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.398 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.090