# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gerhard Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; 1,2-Olefin Addition of a Frustrated Amine/Borane Lewis Pair ; loop_ _publ_author_name 'G Erker' 'Roland Frohlich' 'Gerald Kehr' 'Jean-Baptiste Sortais' 'Tanja Voss' # Attachment '2.cif' data_erk5158 _database_code_depnum_ccdc_archive 'CCDC 743168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H21 Fe N O' _chemical_formula_weight 311.20 _chemical_absolute_configuration ad 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3447(2) _cell_length_b 14.1452(3) _cell_length_c 14.2521(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1480.68(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1671 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7858 _exptl_absorpt_correction_T_max 0.9702 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6229 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 28.07 _reflns_number_total 3435 _reflns_number_gt 3302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0311P)^2^+1.4273P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 3435 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Fe Fe 0.09934(5) 0.35091(3) 0.85523(2) 0.03038(10) Uani 1 1 d . . . O1 O 0.0223(4) 0.4790(2) 0.61953(16) 0.0596(7) Uani 1 1 d . . . N1 N 0.2183(4) 0.6476(2) 0.87042(18) 0.0476(6) Uani 1 1 d . . . C1 C -0.0999(4) 0.3790(2) 0.9485(2) 0.0403(6) Uani 1 1 d . . . C2 C 0.0075(4) 0.3001(2) 0.9796(2) 0.0431(7) Uani 1 1 d . . . H2 H 0.0729 0.2969 1.0362 0.052 Uiso 1 1 calc R . . C3 C -0.0016(5) 0.2283(2) 0.9109(2) 0.0463(7) Uani 1 1 d . . . H3 H 0.0578 0.1696 0.9137 0.056 Uiso 1 1 calc R . . C4 C -0.1156(4) 0.2599(2) 0.8370(2) 0.0453(7) Uani 1 1 d . . . H4 H -0.1455 0.2259 0.7825 0.054 Uiso 1 1 calc R . . C5 C -0.1764(3) 0.3525(2) 0.8604(2) 0.0415(6) Uani 1 1 d . . . H5 H -0.2544 0.3901 0.8237 0.050 Uiso 1 1 calc R . . C6 C -0.1192(5) 0.4747(2) 0.9952(2) 0.0449(7) Uani 1 1 d . . . H6 H -0.2517 0.4856 1.0022 0.054 Uiso 1 1 calc R . . C7 C -0.0415(6) 0.4751(3) 1.0943(2) 0.0604(10) Uani 1 1 d . . . H7A H -0.1056 0.4289 1.1323 0.091 Uiso 1 1 calc R . . H7B H -0.0563 0.5374 1.1217 0.091 Uiso 1 1 calc R . . H7C H 0.0869 0.4591 1.0921 0.091 Uiso 1 1 calc R . . C8 C -0.0476(4) 0.5569(2) 0.9358(2) 0.0457(7) Uani 1 1 d . . . H8A H -0.0808 0.6162 0.9670 0.055 Uiso 1 1 calc R . . H8B H -0.1106 0.5557 0.8752 0.055 Uiso 1 1 calc R . . C9 C 0.1609(4) 0.5585(2) 0.9168(2) 0.0374(6) Uani 1 1 d . . . H9 H 0.2238 0.5548 0.9781 0.045 Uiso 1 1 calc R . . C10 C 0.2248(3) 0.47598(18) 0.8577(2) 0.0321(5) Uani 1 1 d . . . C11 C 0.3478(4) 0.4051(2) 0.8894(2) 0.0376(6) Uani 1 1 d . . . H11 H 0.4060 0.4039 0.9481 0.045 Uiso 1 1 calc R . . C12 C 0.3679(4) 0.3366(2) 0.8173(2) 0.0422(7) Uani 1 1 d . . . H12 H 0.4402 0.2819 0.8210 0.051 Uiso 1 1 calc R . . C13 C 0.2618(4) 0.3640(2) 0.7390(2) 0.0375(6) Uani 1 1 d . . . H13 H 0.2504 0.3308 0.6822 0.045 Uiso 1 1 calc R . . C14 C 0.1744(4) 0.4520(2) 0.76263(18) 0.0328(5) Uani 1 1 d . . . C15 C 0.0493(4) 0.5012(2) 0.7004(2) 0.0435(7) Uani 1 1 d . . . H15 H -0.0146 0.5534 0.7245 0.052 Uiso 1 1 calc R . . C16 C 0.1663(7) 0.7312(3) 0.9238(3) 0.0678(12) Uani 1 1 d . . . H16A H 0.2124 0.7259 0.9873 0.102 Uiso 1 1 calc R . . H16B H 0.0347 0.7364 0.9253 0.102 Uiso 1 1 calc R . . H16C H 0.2174 0.7870 0.8943 0.102 Uiso 1 1 calc R . . C17 C 0.4147(5) 0.6474(3) 0.8569(3) 0.0627(9) Uani 1 1 d . . . H17A H 0.4523 0.7071 0.8297 0.094 Uiso 1 1 calc R . . H17B H 0.4481 0.5961 0.8151 0.094 Uiso 1 1 calc R . . H17C H 0.4746 0.6387 0.9170 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.02939(16) 0.03274(17) 0.02901(16) 0.00254(16) 0.00130(15) -0.00164(15) O1 0.0689(16) 0.0717(17) 0.0382(12) 0.0049(11) -0.0136(11) 0.0099(13) N1 0.0643(16) 0.0365(12) 0.0420(14) 0.0012(12) -0.0053(12) -0.0079(13) C1 0.0334(12) 0.0496(16) 0.0378(13) -0.0028(11) 0.0115(13) -0.0100(13) C2 0.0477(17) 0.0467(17) 0.0350(14) 0.0100(13) 0.0059(12) -0.0098(14) C3 0.0573(19) 0.0366(15) 0.0450(16) 0.0067(13) 0.0070(14) -0.0110(13) C4 0.0446(15) 0.0462(15) 0.0451(16) -0.0057(12) 0.0018(14) -0.0160(14) C5 0.0265(11) 0.0547(16) 0.0433(14) 0.0009(18) 0.0011(12) -0.0066(12) C6 0.0378(15) 0.0560(18) 0.0410(15) -0.0147(13) 0.0077(13) -0.0040(14) C7 0.069(2) 0.074(2) 0.0380(16) -0.0127(16) 0.0090(16) -0.016(2) C8 0.0422(16) 0.0454(16) 0.0495(16) -0.0088(14) 0.0018(13) 0.0044(13) C9 0.0423(15) 0.0359(14) 0.0339(13) 0.0003(12) -0.0029(11) -0.0050(12) C10 0.0301(11) 0.0337(12) 0.0324(12) 0.0049(12) -0.0021(11) -0.0046(9) C11 0.0285(13) 0.0465(16) 0.0379(14) 0.0067(12) -0.0030(11) -0.0023(12) C12 0.0287(13) 0.0476(18) 0.0502(15) 0.0068(13) 0.0040(11) 0.0052(12) C13 0.0361(13) 0.0411(16) 0.0353(13) 0.0034(12) 0.0077(11) 0.0012(12) C14 0.0343(12) 0.0344(13) 0.0296(12) 0.0046(11) 0.0020(10) -0.0017(11) C15 0.0463(17) 0.0457(16) 0.0385(14) 0.0085(13) -0.0013(13) 0.0040(13) C16 0.099(3) 0.0387(18) 0.066(2) -0.0068(17) 0.000(2) -0.0122(19) C17 0.073(2) 0.0540(17) 0.0617(18) 0.0021(19) 0.004(2) -0.0281(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 Fe C10 1.995(2) . ? Fe C1 2.016(3) . ? Fe C14 2.022(3) . ? Fe C5 2.027(3) . ? Fe C2 2.028(3) . ? Fe C11 2.039(3) . ? Fe C3 2.046(3) . ? Fe C13 2.049(3) . ? Fe C4 2.053(3) . ? Fe C12 2.055(3) . ? O1 C15 1.211(4) . ? N1 C17 1.456(5) . ? N1 C16 1.457(5) . ? N1 C9 1.483(4) . ? C1 C5 1.426(4) . ? C1 C2 1.437(5) . ? C1 C6 1.515(4) . ? C2 C3 1.412(4) . ? C2 H2 0.9400 . ? C3 C4 1.418(5) . ? C3 H3 0.9400 . ? C4 C5 1.424(4) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.524(4) . ? C6 C8 1.532(5) . ? C6 H6 0.9900 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.555(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.514(4) . ? C9 H9 0.9900 . ? C10 C11 1.423(4) . ? C10 C14 1.445(4) . ? C11 C12 1.419(4) . ? C11 H11 0.9400 . ? C12 C13 1.415(4) . ? C12 H12 0.9400 . ? C13 C14 1.440(4) . ? C13 H13 0.9400 . ? C14 C15 1.454(4) . ? C15 H15 0.9400 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? 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 C10 Fe C1 98.55(12) . . ? C10 Fe C14 42.16(11) . . ? C1 Fe C14 119.25(12) . . ? C10 Fe C5 116.80(12) . . ? C1 Fe C5 41.29(12) . . ? C14 Fe C5 106.74(12) . . ? C10 Fe C2 116.89(13) . . ? C1 Fe C2 41.63(13) . . ? C14 Fe C2 155.72(12) . . ? C5 Fe C2 68.90(13) . . ? C10 Fe C11 41.30(11) . . ? C1 Fe C11 114.72(12) . . ? C14 Fe C11 69.26(11) . . ? C5 Fe C11 151.84(13) . . ? C2 Fe C11 102.84(13) . . ? C10 Fe C3 155.79(12) . . ? C1 Fe C3 69.41(13) . . ? C14 Fe C3 162.00(12) . . ? C5 Fe C3 68.49(14) . . ? C2 Fe C3 40.55(12) . . ? C11 Fe C3 123.41(13) . . ? C10 Fe C13 70.45(12) . . ? C1 Fe C13 159.61(12) . . ? C14 Fe C13 41.43(11) . . ? C5 Fe C13 127.60(12) . . ? C2 Fe C13 158.71(13) . . ? C11 Fe C13 68.76(12) . . ? C3 Fe C13 126.93(13) . . ? C10 Fe C4 155.95(12) . . ? C1 Fe C4 69.46(12) . . ? C14 Fe C4 124.75(12) . . ? C5 Fe C4 40.84(13) . . ? C2 Fe C4 68.47(13) . . ? C11 Fe C4 162.62(13) . . ? C3 Fe C4 40.47(13) . . ? C13 Fe C4 113.69(12) . . ? C10 Fe C12 69.41(12) . . ? C1 Fe C12 152.77(13) . . ? C14 Fe C12 68.66(12) . . ? C5 Fe C12 165.88(13) . . ? C2 Fe C12 120.94(13) . . ? C11 Fe C12 40.57(12) . . ? C3 Fe C12 111.51(14) . . ? C13 Fe C12 40.32(12) . . ? C4 Fe C12 130.02(13) . . ? C17 N1 C16 109.3(3) . . ? C17 N1 C9 109.8(3) . . ? C16 N1 C9 112.5(3) . . ? C5 C1 C2 106.5(3) . . ? C5 C1 C6 125.8(3) . . ? C2 C1 C6 127.5(3) . . ? C5 C1 Fe 69.76(15) . . ? C2 C1 Fe 69.62(17) . . ? C6 C1 Fe 122.3(2) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe 70.41(17) . . ? C1 C2 Fe 68.76(16) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe C2 H2 126.7 . . ? C2 C3 C4 108.5(3) . . ? C2 C3 Fe 69.04(17) . . ? C4 C3 Fe 70.04(17) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Fe C3 H3 126.7 . . ? C3 C4 C5 107.5(3) . . ? C3 C4 Fe 69.48(18) . . ? C5 C4 Fe 68.59(15) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? Fe C4 H4 127.2 . . ? C4 C5 C1 108.9(3) . . ? C4 C5 Fe 70.57(17) . . ? C1 C5 Fe 68.95(16) . . ? C4 C5 H5 125.5 . . ? C1 C5 H5 125.5 . . ? Fe C5 H5 126.5 . . ? C1 C6 C7 112.1(3) . . ? C1 C6 C8 113.8(2) . . ? C7 C6 C8 112.4(3) . . ? C1 C6 H6 106.0 . . ? C7 C6 H6 106.0 . . ? C8 C6 H6 106.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C9 116.4(3) . . ? C6 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? C6 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? N1 C9 C10 108.6(2) . . ? N1 C9 C8 111.7(3) . . ? C10 C9 C8 113.0(2) . . ? N1 C9 H9 107.8 . . ? C10 C9 H9 107.8 . . ? C8 C9 H9 107.8 . . ? C11 C10 C14 107.1(2) . . ? C11 C10 C9 124.3(3) . . ? C14 C10 C9 128.6(2) . . ? C11 C10 Fe 70.99(15) . . ? C14 C10 Fe 69.92(15) . . ? C9 C10 Fe 123.39(19) . . ? C12 C11 C10 108.5(3) . . ? C12 C11 Fe 70.35(16) . . ? C10 C11 Fe 67.71(14) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe C11 H11 127.8 . . ? C13 C12 C11 109.1(3) . . ? C13 C12 Fe 69.61(15) . . ? C11 C12 Fe 69.08(15) . . ? C13 C12 H12 125.5 . . ? C11 C12 H12 125.5 . . ? Fe C12 H12 127.4 . . ? C12 C13 C14 107.3(3) . . ? C12 C13 Fe 70.07(16) . . ? C14 C13 Fe 68.27(15) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? Fe C13 H13 126.9 . . ? C13 C14 C10 107.9(2) . . ? C13 C14 C15 123.6(3) . . ? C10 C14 C15 128.4(3) . . ? C13 C14 Fe 70.30(15) . . ? C10 C14 Fe 67.92(14) . . ? C15 C14 Fe 124.3(2) . . ? O1 C15 C14 124.0(3) . . ? O1 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Fe C1 C5 121.31(19) . . . . ? C14 Fe C1 C5 82.1(2) . . . . ? C2 Fe C1 C5 -117.4(3) . . . . ? C11 Fe C1 C5 161.21(18) . . . . ? C3 Fe C1 C5 -80.5(2) . . . . ? C13 Fe C1 C5 65.8(4) . . . . ? C4 Fe C1 C5 -37.09(18) . . . . ? C12 Fe C1 C5 -177.7(3) . . . . ? C10 Fe C1 C2 -121.29(18) . . . . ? C14 Fe C1 C2 -160.49(17) . . . . ? C5 Fe C1 C2 117.4(3) . . . . ? C11 Fe C1 C2 -81.4(2) . . . . ? C3 Fe C1 C2 36.95(18) . . . . ? C13 Fe C1 C2 -176.8(3) . . . . ? C4 Fe C1 C2 80.3(2) . . . . ? C12 Fe C1 C2 -60.3(3) . . . . ? C10 Fe C1 C6 1.0(3) . . . . ? C14 Fe C1 C6 -38.2(3) . . . . ? C5 Fe C1 C6 -120.3(3) . . . . ? C2 Fe C1 C6 122.3(3) . . . . ? C11 Fe C1 C6 40.9(3) . . . . ? C3 Fe C1 C6 159.2(3) . . . . ? C13 Fe C1 C6 -54.5(5) . . . . ? C4 Fe C1 C6 -157.4(3) . . . . ? C12 Fe C1 C6 62.0(4) . . . . ? C5 C1 C2 C3 1.0(3) . . . . ? C6 C1 C2 C3 -175.0(3) . . . . ? Fe C1 C2 C3 -59.3(2) . . . . ? C5 C1 C2 Fe 60.33(18) . . . . ? C6 C1 C2 Fe -115.6(3) . . . . ? C10 Fe C2 C3 -168.58(19) . . . . ? C1 Fe C2 C3 120.1(3) . . . . ? C14 Fe C2 C3 165.2(3) . . . . ? C5 Fe C2 C3 81.2(2) . . . . ? C11 Fe C2 C3 -127.0(2) . . . . ? C13 Fe C2 C3 -63.0(4) . . . . ? C4 Fe C2 C3 37.2(2) . . . . ? C12 Fe C2 C3 -87.5(2) . . . . ? C10 Fe C2 C1 71.4(2) . . . . ? C14 Fe C2 C1 45.1(4) . . . . ? C5 Fe C2 C1 -38.90(18) . . . . ? C11 Fe C2 C1 112.90(19) . . . . ? C3 Fe C2 C1 -120.1(3) . . . . ? C13 Fe C2 C1 176.9(3) . . . . ? C4 Fe C2 C1 -82.9(2) . . . . ? C12 Fe C2 C1 152.40(18) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? Fe C2 C3 C4 -59.1(2) . . . . ? C1 C2 C3 Fe 58.3(2) . . . . ? C10 Fe C3 C2 25.5(4) . . . . ? C1 Fe C3 C2 -37.9(2) . . . . ? C14 Fe C3 C2 -160.1(4) . . . . ? C5 Fe C3 C2 -82.3(2) . . . . ? C11 Fe C3 C2 68.8(2) . . . . ? C13 Fe C3 C2 156.12(19) . . . . ? C4 Fe C3 C2 -120.0(3) . . . . ? C12 Fe C3 C2 112.9(2) . . . . ? C10 Fe C3 C4 145.5(3) . . . . ? C1 Fe C3 C4 82.1(2) . . . . ? C14 Fe C3 C4 -40.1(5) . . . . ? C5 Fe C3 C4 37.74(18) . . . . ? C2 Fe C3 C4 120.0(3) . . . . ? C11 Fe C3 C4 -171.18(18) . . . . ? C13 Fe C3 C4 -83.9(2) . . . . ? C12 Fe C3 C4 -127.08(19) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? Fe C3 C4 C5 -58.2(2) . . . . ? C2 C3 C4 Fe 58.5(2) . . . . ? C10 Fe C4 C3 -145.3(3) . . . . ? C1 Fe C4 C3 -82.0(2) . . . . ? C14 Fe C4 C3 165.99(18) . . . . ? C5 Fe C4 C3 -119.5(3) . . . . ? C2 Fe C4 C3 -37.25(19) . . . . ? C11 Fe C4 C3 25.4(5) . . . . ? C13 Fe C4 C3 119.78(19) . . . . ? C12 Fe C4 C3 75.7(2) . . . . ? C10 Fe C4 C5 -25.8(4) . . . . ? C1 Fe C4 C5 37.48(18) . . . . ? C14 Fe C4 C5 -74.6(2) . . . . ? C2 Fe C4 C5 82.2(2) . . . . ? C11 Fe C4 C5 144.8(4) . . . . ? C3 Fe C4 C5 119.5(3) . . . . ? C13 Fe C4 C5 -120.75(19) . . . . ? C12 Fe C4 C5 -164.80(18) . . . . ? C3 C4 C5 C1 0.3(3) . . . . ? Fe C4 C5 C1 -58.43(18) . . . . ? C3 C4 C5 Fe 58.8(2) . . . . ? C2 C1 C5 C4 -0.8(3) . . . . ? C6 C1 C5 C4 175.2(3) . . . . ? Fe C1 C5 C4 59.42(19) . . . . ? C2 C1 C5 Fe -60.2(2) . . . . ? C6 C1 C5 Fe 115.8(3) . . . . ? C10 Fe C5 C4 168.54(17) . . . . ? C1 Fe C5 C4 -120.3(3) . . . . ? C14 Fe C5 C4 124.21(18) . . . . ? C2 Fe C5 C4 -81.1(2) . . . . ? C11 Fe C5 C4 -158.6(2) . . . . ? C3 Fe C5 C4 -37.41(18) . . . . ? C13 Fe C5 C4 83.4(2) . . . . ? C12 Fe C5 C4 55.4(6) . . . . ? C10 Fe C5 C1 -71.2(2) . . . . ? C14 Fe C5 C1 -115.51(18) . . . . ? C2 Fe C5 C1 39.21(18) . . . . ? C11 Fe C5 C1 -38.3(3) . . . . ? C3 Fe C5 C1 82.88(19) . . . . ? C13 Fe C5 C1 -156.35(17) . . . . ? C4 Fe C5 C1 120.3(3) . . . . ? C12 Fe C5 C1 175.7(5) . . . . ? C5 C1 C6 C7 172.6(3) . . . . ? C2 C1 C6 C7 -12.2(4) . . . . ? Fe C1 C6 C7 -100.2(3) . . . . ? C5 C1 C6 C8 -58.5(4) . . . . ? C2 C1 C6 C8 116.7(3) . . . . ? Fe C1 C6 C8 28.7(4) . . . . ? C1 C6 C8 C9 -65.8(4) . . . . ? C7 C6 C8 C9 62.9(4) . . . . ? C17 N1 C9 C10 -56.6(3) . . . . ? C16 N1 C9 C10 -178.5(3) . . . . ? C17 N1 C9 C8 178.1(3) . . . . ? C16 N1 C9 C8 56.1(3) . . . . ? C6 C8 C9 N1 -172.0(2) . . . . ? C6 C8 C9 C10 65.2(3) . . . . ? N1 C9 C10 C11 119.0(3) . . . . ? C8 C9 C10 C11 -116.5(3) . . . . ? N1 C9 C10 C14 -62.3(3) . . . . ? C8 C9 C10 C14 62.2(4) . . . . ? N1 C9 C10 Fe -152.3(2) . . . . ? C8 C9 C10 Fe -27.8(3) . . . . ? C1 Fe C10 C11 118.01(18) . . . . ? C14 Fe C10 C11 -117.2(2) . . . . ? C5 Fe C10 C11 157.17(17) . . . . ? C2 Fe C10 C11 78.5(2) . . . . ? C3 Fe C10 C11 60.2(4) . . . . ? C13 Fe C10 C11 -79.73(18) . . . . ? C4 Fe C10 C11 175.8(3) . . . . ? C12 Fe C10 C11 -36.69(18) . . . . ? C1 Fe C10 C14 -124.75(17) . . . . ? C5 Fe C10 C14 -85.59(19) . . . . ? C2 Fe C10 C14 -164.28(17) . . . . ? C11 Fe C10 C14 117.2(2) . . . . ? C3 Fe C10 C14 177.4(3) . . . . ? C13 Fe C10 C14 37.51(16) . . . . ? C4 Fe C10 C14 -67.0(3) . . . . ? C12 Fe C10 C14 80.55(17) . . . . ? C1 Fe C10 C9 -1.1(3) . . . . ? C14 Fe C10 C9 123.6(3) . . . . ? C5 Fe C10 C9 38.0(3) . . . . ? C2 Fe C10 C9 -40.6(3) . . . . ? C11 Fe C10 C9 -119.1(3) . . . . ? C3 Fe C10 C9 -58.9(4) . . . . ? C13 Fe C10 C9 161.1(3) . . . . ? C4 Fe C10 C9 56.6(4) . . . . ? C12 Fe C10 C9 -155.8(3) . . . . ? C14 C10 C11 C12 -2.3(3) . . . . ? C9 C10 C11 C12 176.7(2) . . . . ? Fe C10 C11 C12 58.6(2) . . . . ? C14 C10 C11 Fe -60.91(17) . . . . ? C9 C10 C11 Fe 118.0(3) . . . . ? C10 Fe C11 C12 -120.7(3) . . . . ? C1 Fe C11 C12 165.34(18) . . . . ? C14 Fe C11 C12 -81.04(18) . . . . ? C5 Fe C11 C12 -167.9(2) . . . . ? C2 Fe C11 C12 122.99(19) . . . . ? C3 Fe C11 C12 84.5(2) . . . . ? C13 Fe C11 C12 -36.51(18) . . . . ? C4 Fe C11 C12 65.1(5) . . . . ? C1 Fe C11 C10 -74.0(2) . . . . ? C14 Fe C11 C10 39.65(17) . . . . ? C5 Fe C11 C10 -47.2(3) . . . . ? C2 Fe C11 C10 -116.32(19) . . . . ? C3 Fe C11 C10 -154.77(18) . . . . ? C13 Fe C11 C10 84.18(19) . . . . ? C4 Fe C11 C10 -174.2(4) . . . . ? C12 Fe C11 C10 120.7(3) . . . . ? C10 C11 C12 C13 1.2(3) . . . . ? Fe C11 C12 C13 58.2(2) . . . . ? C10 C11 C12 Fe -57.04(19) . . . . ? C10 Fe C12 C13 -83.7(2) . . . . ? C1 Fe C12 C13 -151.2(2) . . . . ? C14 Fe C12 C13 -38.40(18) . . . . ? C5 Fe C12 C13 35.0(6) . . . . ? C2 Fe C12 C13 166.53(18) . . . . ? C11 Fe C12 C13 -121.0(3) . . . . ? C3 Fe C12 C13 122.25(19) . . . . ? C4 Fe C12 C13 79.7(2) . . . . ? C10 Fe C12 C11 37.32(17) . . . . ? C1 Fe C12 C11 -30.2(3) . . . . ? C14 Fe C12 C11 82.62(18) . . . . ? C5 Fe C12 C11 156.1(5) . . . . ? C2 Fe C12 C11 -72.4(2) . . . . ? C3 Fe C12 C11 -116.73(18) . . . . ? C13 Fe C12 C11 121.0(3) . . . . ? C4 Fe C12 C11 -159.28(18) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? Fe C12 C13 C14 58.30(19) . . . . ? C11 C12 C13 Fe -57.9(2) . . . . ? C10 Fe C13 C12 80.89(19) . . . . ? C1 Fe C13 C12 140.7(3) . . . . ? C14 Fe C13 C12 119.0(3) . . . . ? C5 Fe C13 C12 -169.82(19) . . . . ? C2 Fe C13 C12 -33.4(4) . . . . ? C11 Fe C13 C12 36.73(18) . . . . ? C3 Fe C13 C12 -79.8(2) . . . . ? C4 Fe C13 C12 -124.6(2) . . . . ? C10 Fe C13 C14 -38.14(16) . . . . ? C1 Fe C13 C14 21.7(4) . . . . ? C5 Fe C13 C14 71.2(2) . . . . ? C2 Fe C13 C14 -152.4(3) . . . . ? C11 Fe C13 C14 -82.30(18) . . . . ? C3 Fe C13 C14 161.15(18) . . . . ? C4 Fe C13 C14 116.34(18) . . . . ? C12 Fe C13 C14 -119.0(3) . . . . ? C12 C13 C14 C10 -1.8(3) . . . . ? Fe C13 C14 C10 57.62(17) . . . . ? C12 C13 C14 C15 -178.2(3) . . . . ? Fe C13 C14 C15 -118.8(3) . . . . ? C12 C13 C14 Fe -59.43(19) . . . . ? C11 C10 C14 C13 2.5(3) . . . . ? C9 C10 C14 C13 -176.4(3) . . . . ? Fe C10 C14 C13 -59.09(18) . . . . ? C11 C10 C14 C15 178.7(3) . . . . ? C9 C10 C14 C15 -0.2(5) . . . . ? Fe C10 C14 C15 117.1(3) . . . . ? C11 C10 C14 Fe 61.60(18) . . . . ? C9 C10 C14 Fe -117.3(3) . . . . ? C10 Fe C14 C13 119.9(2) . . . . ? C1 Fe C14 C13 -171.50(17) . . . . ? C5 Fe C14 C13 -128.46(18) . . . . ? C2 Fe C14 C13 155.9(3) . . . . ? C11 Fe C14 C13 81.01(18) . . . . ? C3 Fe C14 C13 -56.7(5) . . . . ? C4 Fe C14 C13 -87.3(2) . . . . ? C12 Fe C14 C13 37.41(17) . . . . ? C1 Fe C14 C10 68.62(19) . . . . ? C5 Fe C14 C10 111.66(17) . . . . ? C2 Fe C14 C10 36.0(4) . . . . ? C11 Fe C14 C10 -38.86(16) . . . . ? C3 Fe C14 C10 -176.6(4) . . . . ? C13 Fe C14 C10 -119.9(2) . . . . ? C4 Fe C14 C10 152.83(17) . . . . ? C12 Fe C14 C10 -82.47(17) . . . . ? C10 Fe C14 C15 -122.3(3) . . . . ? C1 Fe C14 C15 -53.7(3) . . . . ? C5 Fe C14 C15 -10.6(3) . . . . ? C2 Fe C14 C15 -86.3(4) . . . . ? C11 Fe C14 C15 -161.2(3) . . . . ? C3 Fe C14 C15 61.1(5) . . . . ? C13 Fe C14 C15 117.8(3) . . . . ? C4 Fe C14 C15 30.5(3) . . . . ? C12 Fe C14 C15 155.2(3) . . . . ? C13 C14 C15 O1 -8.6(5) . . . . ? C10 C14 C15 O1 175.7(3) . . . . ? Fe C14 C15 O1 -96.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.211 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.047 # Attachment '3.cif' data_erk5080 _database_code_depnum_ccdc_archive 'CCDC 743169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H21 B F15 Fe N O' _chemical_formula_weight 823.19 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' 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' 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' _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 9.6199(2) _cell_length_b 11.9463(3) _cell_length_c 14.9994(5) _cell_angle_alpha 105.859(1) _cell_angle_beta 96.052(1) _cell_angle_gamma 103.077(1) _cell_volume 1589.21(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3967 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9651 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13635 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.30 _reflns_number_total 6413 _reflns_number_gt 4014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0198P)^2^+1.2431P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6413 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Fe Fe 0.32978(6) 1.23292(4) 0.27188(4) 0.03578(16) Uani 1 1 d . . . O1 O 0.3349(2) 0.89962(17) 0.20482(16) 0.0281(5) Uani 1 1 d . . . N1 N 0.7026(3) 1.1487(2) 0.1792(2) 0.0370(7) Uani 1 1 d . . . B1 B 0.3707(4) 0.7843(3) 0.2215(3) 0.0279(9) Uani 1 1 d . . . C1 C 0.4668(4) 1.3507(3) 0.3885(3) 0.0421(10) Uani 1 1 d . . . C2 C 0.3560(4) 1.4019(3) 0.3607(3) 0.0506(11) Uani 1 1 d . . . H2 H 0.3713 1.4738 0.3444 0.061 Uiso 1 1 calc R . . C3 C 0.2197(5) 1.3280(4) 0.3613(3) 0.0634(14) Uani 1 1 d . . . H3 H 0.1290 1.3410 0.3446 0.076 Uiso 1 1 calc R . . C4 C 0.2437(5) 1.2304(4) 0.3917(3) 0.0621(13) Uani 1 1 d . . . H4 H 0.1721 1.1673 0.3991 0.074 Uiso 1 1 calc R . . C5 C 0.3952(5) 1.2455(3) 0.4088(3) 0.0485(11) Uani 1 1 d . . . H5 H 0.4412 1.1938 0.4302 0.058 Uiso 1 1 calc R . . C6 C 0.6272(4) 1.3927(3) 0.3880(3) 0.0462(10) Uani 1 1 d . . . H6 H 0.6767 1.4143 0.4540 0.055 Uiso 1 1 calc R . . C7 C 0.6656(5) 1.5073(3) 0.3597(4) 0.0660(14) Uani 1 1 d . . . H7A H 0.6124 1.4930 0.2972 0.099 Uiso 1 1 calc R . . H7B H 0.7689 1.5303 0.3595 0.099 Uiso 1 1 calc R . . H7C H 0.6399 1.5717 0.4043 0.099 Uiso 1 1 calc R . . C8 C 0.6863(4) 1.2916(3) 0.3306(3) 0.0431(10) Uani 1 1 d . . . H8A H 0.6576 1.2216 0.3532 0.052 Uiso 1 1 calc R . . H8B H 0.7924 1.3192 0.3448 0.052 Uiso 1 1 calc R . . C9 C 0.6392(4) 1.2484(3) 0.2227(3) 0.0356(9) Uani 1 1 d . . . H9 H 0.6772 1.3168 0.1990 0.043 Uiso 1 1 calc R . . C10 C 0.4764(4) 1.2053(3) 0.1896(2) 0.0301(8) Uani 1 1 d . . . C11 C 0.3869(4) 1.2673(3) 0.1527(3) 0.0393(9) Uani 1 1 d . . . H11 H 0.4200 1.3428 0.1433 0.047 Uiso 1 1 calc R . . C12 C 0.2414(4) 1.1990(3) 0.1322(3) 0.0428(10) Uani 1 1 d . . . H12 H 0.1618 1.2223 0.1084 0.051 Uiso 1 1 calc R . . C13 C 0.2339(4) 1.0900(3) 0.1529(3) 0.0366(9) Uani 1 1 d . . . H13 H 0.1493 1.0286 0.1464 0.044 Uiso 1 1 calc R . . C14 C 0.3797(4) 1.0903(3) 0.1860(2) 0.0278(8) Uani 1 1 d . . . C15 C 0.4226(4) 1.0006(3) 0.2177(2) 0.0257(8) Uani 1 1 d . . . H15 H 0.5182 1.0164 0.2489 0.031 Uiso 1 1 calc R . . C16 C 0.6721(5) 1.1180(4) 0.0769(3) 0.0520(11) Uani 1 1 d . . . H16A H 0.7227 1.1852 0.0579 0.078 Uiso 1 1 calc R . . H16B H 0.5685 1.1010 0.0556 0.078 Uiso 1 1 calc R . . H16C H 0.7046 1.0473 0.0490 0.078 Uiso 1 1 calc R . . C17 C 0.8601(4) 1.1781(4) 0.2112(3) 0.0553(12) Uani 1 1 d . . . H17A H 0.8994 1.1188 0.1713 0.083 Uiso 1 1 calc R . . H17B H 0.8794 1.1773 0.2758 0.083 Uiso 1 1 calc R . . H17C H 0.9054 1.2577 0.2077 0.083 Uiso 1 1 calc R . . C21 C 0.2954(4) 0.6793(3) 0.1219(2) 0.0276(8) Uani 1 1 d . . . C22 C 0.3453(4) 0.5778(3) 0.0901(3) 0.0317(8) Uani 1 1 d . . . F22 F 0.4513(2) 0.55950(16) 0.14781(15) 0.0455(6) Uani 1 1 d . . . C23 C 0.2939(4) 0.4908(3) 0.0045(3) 0.0387(9) Uani 1 1 d . . . F23 F 0.3491(3) 0.39430(18) -0.01904(16) 0.0584(7) Uani 1 1 d . . . C24 C 0.1840(4) 0.5006(3) -0.0563(3) 0.0423(10) Uani 1 1 d . . . F24 F 0.1328(3) 0.4172(2) -0.14063(16) 0.0652(7) Uani 1 1 d . . . C25 C 0.1262(4) 0.5969(3) -0.0275(3) 0.0389(9) Uani 1 1 d . . . F25 F 0.0155(3) 0.60723(19) -0.08564(17) 0.0592(6) Uani 1 1 d . . . C26 C 0.1793(4) 0.6816(3) 0.0591(3) 0.0309(8) Uani 1 1 d . . . F26 F 0.1102(2) 0.76923(17) 0.08060(15) 0.0460(6) Uani 1 1 d . . . C31 C 0.2892(4) 0.7647(3) 0.3086(2) 0.0293(8) Uani 1 1 d . . . C32 C 0.3006(4) 0.8602(3) 0.3888(3) 0.0369(9) Uani 1 1 d . . . F32 F 0.3915(3) 0.96893(17) 0.39855(15) 0.0565(6) Uani 1 1 d . . . C33 C 0.2258(4) 0.8513(4) 0.4605(3) 0.0444(10) Uani 1 1 d . . . F33 F 0.2411(3) 0.9484(2) 0.53583(17) 0.0763(8) Uani 1 1 d . . . C34 C 0.1348(4) 0.7430(4) 0.4561(3) 0.0420(10) Uani 1 1 d . . . F34 F 0.0582(3) 0.7338(2) 0.52493(17) 0.0631(7) Uani 1 1 d . . . C35 C 0.1237(4) 0.6453(3) 0.3810(3) 0.0380(9) Uani 1 1 d . . . F35 F 0.0375(2) 0.5367(2) 0.37683(18) 0.0620(7) Uani 1 1 d . . . C36 C 0.2000(4) 0.6570(3) 0.3101(3) 0.0321(8) Uani 1 1 d . . . F36 F 0.1842(2) 0.55401(16) 0.23977(15) 0.0490(6) Uani 1 1 d . . . C41 C 0.5460(4) 0.8069(3) 0.2396(2) 0.0274(8) Uani 1 1 d . . . C42 C 0.6307(4) 0.8021(3) 0.3181(2) 0.0315(8) Uani 1 1 d . . . F42 F 0.5689(2) 0.77641(19) 0.38971(15) 0.0485(6) Uani 1 1 d . . . C43 C 0.7785(4) 0.8205(3) 0.3293(3) 0.0420(10) Uani 1 1 d . . . F43 F 0.8545(2) 0.8154(2) 0.40833(17) 0.0642(7) Uani 1 1 d . . . C44 C 0.8512(4) 0.8467(3) 0.2609(3) 0.0422(10) Uani 1 1 d . . . F44 F 0.9953(2) 0.8666(2) 0.27121(18) 0.0680(7) Uani 1 1 d . . . C45 C 0.7728(4) 0.8517(3) 0.1804(3) 0.0384(9) Uani 1 1 d . . . F45 F 0.8421(2) 0.8752(2) 0.11133(17) 0.0556(6) Uani 1 1 d . . . C46 C 0.6262(4) 0.8321(3) 0.1722(2) 0.0315(8) Uani 1 1 d . . . F46 F 0.5547(2) 0.83891(18) 0.09151(14) 0.0412(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 Fe 0.0377(3) 0.0285(3) 0.0424(4) 0.0093(2) 0.0076(3) 0.0129(2) O1 0.0313(13) 0.0185(11) 0.0338(15) 0.0087(10) 0.0040(11) 0.0054(10) N1 0.0311(18) 0.0385(17) 0.042(2) 0.0115(15) 0.0109(15) 0.0083(14) B1 0.035(2) 0.0219(19) 0.030(2) 0.0100(17) 0.0055(19) 0.0119(18) C1 0.048(3) 0.030(2) 0.040(3) -0.0026(18) 0.001(2) 0.0124(18) C2 0.049(3) 0.035(2) 0.062(3) 0.001(2) 0.007(2) 0.018(2) C3 0.047(3) 0.050(3) 0.084(4) -0.003(3) 0.018(3) 0.022(2) C4 0.064(3) 0.056(3) 0.057(3) 0.002(2) 0.029(3) 0.008(2) C5 0.071(3) 0.043(2) 0.031(2) 0.0070(19) 0.012(2) 0.019(2) C6 0.048(3) 0.037(2) 0.044(3) 0.0008(19) -0.004(2) 0.0149(19) C7 0.057(3) 0.034(2) 0.093(4) 0.005(2) 0.008(3) 0.006(2) C8 0.041(2) 0.037(2) 0.045(3) 0.0061(19) -0.005(2) 0.0128(18) C9 0.035(2) 0.0262(18) 0.045(3) 0.0125(17) 0.0067(19) 0.0059(17) C10 0.033(2) 0.0282(18) 0.030(2) 0.0115(16) 0.0012(17) 0.0089(16) C11 0.045(2) 0.0310(19) 0.043(3) 0.0182(18) 0.001(2) 0.0078(18) C12 0.044(3) 0.041(2) 0.048(3) 0.0197(19) -0.004(2) 0.017(2) C13 0.033(2) 0.0299(19) 0.045(3) 0.0110(18) 0.0039(19) 0.0070(17) C14 0.032(2) 0.0226(16) 0.029(2) 0.0062(15) 0.0029(16) 0.0093(15) C15 0.0303(19) 0.0234(17) 0.025(2) 0.0062(15) 0.0062(16) 0.0105(15) C16 0.059(3) 0.052(2) 0.044(3) 0.013(2) 0.017(2) 0.009(2) C17 0.033(2) 0.063(3) 0.069(3) 0.016(2) 0.014(2) 0.013(2) C21 0.031(2) 0.0260(17) 0.025(2) 0.0080(15) 0.0072(17) 0.0053(15) C22 0.036(2) 0.0285(18) 0.030(2) 0.0087(17) 0.0041(17) 0.0076(16) F22 0.0548(14) 0.0303(11) 0.0490(14) 0.0069(10) -0.0049(11) 0.0194(10) C23 0.049(2) 0.0275(19) 0.035(2) 0.0013(17) 0.012(2) 0.0103(18) F23 0.0769(17) 0.0337(12) 0.0565(16) -0.0052(11) 0.0129(13) 0.0218(12) C24 0.056(3) 0.034(2) 0.024(2) -0.0016(17) 0.006(2) -0.0023(19) F24 0.0885(19) 0.0497(13) 0.0339(15) -0.0090(11) -0.0038(13) 0.0056(13) C25 0.040(2) 0.039(2) 0.031(2) 0.0135(18) -0.0026(19) -0.0004(18) F25 0.0583(16) 0.0543(14) 0.0502(16) 0.0139(12) -0.0203(13) 0.0021(12) C26 0.032(2) 0.0265(18) 0.032(2) 0.0074(16) 0.0075(18) 0.0056(16) F26 0.0385(13) 0.0421(12) 0.0524(15) 0.0068(11) -0.0050(11) 0.0167(10) C31 0.030(2) 0.0274(18) 0.033(2) 0.0087(16) 0.0055(17) 0.0117(16) C32 0.046(2) 0.032(2) 0.034(2) 0.0091(17) 0.0075(19) 0.0131(18) F32 0.0858(18) 0.0287(11) 0.0411(15) -0.0004(10) 0.0140(13) 0.0004(12) C33 0.058(3) 0.051(2) 0.030(2) 0.0059(19) 0.016(2) 0.029(2) F33 0.118(2) 0.0652(16) 0.0452(17) 0.0013(13) 0.0336(16) 0.0331(16) C34 0.033(2) 0.068(3) 0.040(3) 0.029(2) 0.017(2) 0.025(2) F34 0.0559(16) 0.1055(19) 0.0506(16) 0.0391(15) 0.0305(13) 0.0378(14) C35 0.029(2) 0.045(2) 0.044(3) 0.022(2) 0.0076(19) 0.0077(18) F35 0.0550(15) 0.0632(15) 0.0703(19) 0.0346(14) 0.0205(14) -0.0011(12) C36 0.033(2) 0.033(2) 0.029(2) 0.0078(17) 0.0017(17) 0.0095(17) F36 0.0683(16) 0.0287(11) 0.0412(14) 0.0075(10) 0.0120(12) -0.0013(11) C41 0.032(2) 0.0213(16) 0.027(2) 0.0033(15) 0.0038(17) 0.0111(15) C42 0.035(2) 0.0322(19) 0.027(2) 0.0066(16) 0.0051(17) 0.0121(16) F42 0.0518(14) 0.0695(15) 0.0364(14) 0.0282(12) 0.0085(11) 0.0254(12) C43 0.043(3) 0.048(2) 0.034(2) 0.0066(19) -0.005(2) 0.023(2) F43 0.0505(15) 0.0978(19) 0.0493(16) 0.0247(14) -0.0058(12) 0.0341(14) C44 0.026(2) 0.046(2) 0.051(3) 0.005(2) 0.006(2) 0.0144(18) F44 0.0317(14) 0.0977(19) 0.0722(19) 0.0179(15) 0.0064(13) 0.0240(13) C45 0.038(2) 0.039(2) 0.041(3) 0.0087(18) 0.017(2) 0.0157(18) F45 0.0435(14) 0.0741(16) 0.0546(16) 0.0217(13) 0.0234(12) 0.0174(12) C46 0.035(2) 0.0310(19) 0.029(2) 0.0070(16) 0.0057(18) 0.0122(17) F46 0.0429(13) 0.0532(13) 0.0321(13) 0.0180(10) 0.0083(10) 0.0153(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 Fe C10 1.994(3) . ? Fe C14 2.024(3) . ? Fe C1 2.026(4) . ? Fe C2 2.035(4) . ? Fe C5 2.037(4) . ? Fe C11 2.043(4) . ? Fe C13 2.055(4) . ? Fe C3 2.055(4) . ? Fe C4 2.061(4) . ? Fe C12 2.069(4) . ? O1 C15 1.258(4) . ? O1 B1 1.570(4) . ? N1 C16 1.457(5) . ? N1 C17 1.471(5) . ? N1 C9 1.485(4) . ? B1 C41 1.628(5) . ? B1 C21 1.633(5) . ? B1 C31 1.636(5) . ? C1 C5 1.418(5) . ? C1 C2 1.424(5) . ? C1 C6 1.511(5) . ? C2 C3 1.408(6) . ? C2 H2 0.9400 . ? C3 C4 1.418(6) . ? C3 H3 0.9400 . ? C4 C5 1.414(6) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.520(5) . ? C6 C8 1.540(5) . ? C6 H6 0.9900 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.540(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.516(5) . ? C9 H9 0.9900 . ? C10 C11 1.418(4) . ? C10 C14 1.458(4) . ? C11 C12 1.406(5) . ? C11 H11 0.9400 . ? C12 C13 1.407(5) . ? C12 H12 0.9400 . ? C13 C14 1.437(5) . ? C13 H13 0.9400 . ? C14 C15 1.408(4) . ? C15 H15 0.9400 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C21 C22 1.387(4) . ? C21 C26 1.394(5) . ? C22 F22 1.362(4) . ? C22 C23 1.370(5) . ? C23 F23 1.353(4) . ? C23 C24 1.369(5) . ? C24 F24 1.339(4) . ? C24 C25 1.375(5) . ? C25 F25 1.353(4) . ? C25 C26 1.371(5) . ? C26 F26 1.348(3) . ? C31 C36 1.383(5) . ? C31 C32 1.388(5) . ? C32 F32 1.352(4) . ? C32 C33 1.370(5) . ? C33 F33 1.348(4) . ? C33 C34 1.369(5) . ? C34 F34 1.343(4) . ? C34 C35 1.358(5) . ? C35 F35 1.353(4) . ? C35 C36 1.375(5) . ? C36 F36 1.349(4) . ? C41 C42 1.382(5) . ? C41 C46 1.391(5) . ? C42 F42 1.353(4) . ? C42 C43 1.373(5) . ? C43 F43 1.350(4) . ? C43 C44 1.366(5) . ? C44 F44 1.337(4) . ? C44 C45 1.377(5) . ? C45 F45 1.348(4) . ? C45 C46 1.363(5) . ? C46 F46 1.360(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 C10 Fe C14 42.54(13) . . ? C10 Fe C1 98.11(15) . . ? C14 Fe C1 123.47(14) . . ? C10 Fe C2 118.64(15) . . ? C14 Fe C2 159.57(15) . . ? C1 Fe C2 41.04(15) . . ? C10 Fe C5 114.48(16) . . ? C14 Fe C5 109.57(14) . . ? C1 Fe C5 40.83(15) . . ? C2 Fe C5 67.77(16) . . ? C10 Fe C11 41.10(13) . . ? C14 Fe C11 68.56(13) . . ? C1 Fe C11 110.99(16) . . ? C2 Fe C11 102.22(16) . . ? C5 Fe C11 147.19(17) . . ? C10 Fe C13 70.78(14) . . ? C14 Fe C13 41.25(13) . . ? C1 Fe C13 164.63(13) . . ? C2 Fe C13 153.80(15) . . ? C5 Fe C13 133.39(14) . . ? C11 Fe C13 67.97(14) . . ? C10 Fe C3 158.01(16) . . ? C14 Fe C3 159.35(16) . . ? C1 Fe C3 68.94(17) . . ? C2 Fe C3 40.26(16) . . ? C5 Fe C3 67.82(18) . . ? C11 Fe C3 125.36(17) . . ? C13 Fe C3 124.90(16) . . ? C10 Fe C4 152.65(17) . . ? C14 Fe C4 124.37(16) . . ? C1 Fe C4 68.84(17) . . ? C2 Fe C4 67.69(17) . . ? C5 Fe C4 40.36(17) . . ? C11 Fe C4 165.48(16) . . ? C13 Fe C4 116.27(17) . . ? C3 Fe C4 40.29(17) . . ? C10 Fe C12 69.27(14) . . ? C14 Fe C12 67.99(13) . . ? C1 Fe C12 147.01(15) . . ? C2 Fe C12 117.32(15) . . ? C5 Fe C12 172.03(16) . . ? C11 Fe C12 39.97(14) . . ? C13 Fe C12 39.89(13) . . ? C3 Fe C12 111.58(17) . . ? C4 Fe C12 134.16(18) . . ? C15 O1 B1 127.1(3) . . ? C16 N1 C17 109.3(3) . . ? C16 N1 C9 110.2(3) . . ? C17 N1 C9 112.7(3) . . ? O1 B1 C41 108.5(3) . . ? O1 B1 C21 102.9(3) . . ? C41 B1 C21 111.0(3) . . ? O1 B1 C31 104.3(2) . . ? C41 B1 C31 116.3(3) . . ? C21 B1 C31 112.5(3) . . ? C5 C1 C2 106.1(4) . . ? C5 C1 C6 126.5(3) . . ? C2 C1 C6 127.2(3) . . ? C5 C1 Fe 70.0(2) . . ? C2 C1 Fe 69.8(2) . . ? C6 C1 Fe 120.7(3) . . ? C3 C2 C1 109.3(4) . . ? C3 C2 Fe 70.6(2) . . ? C1 C2 Fe 69.1(2) . . ? C3 C2 H2 125.3 . . ? C1 C2 H2 125.3 . . ? Fe C2 H2 126.5 . . ? C2 C3 C4 107.7(4) . . ? C2 C3 Fe 69.1(2) . . ? C4 C3 Fe 70.1(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Fe C3 H3 126.2 . . ? C5 C4 C3 107.5(4) . . ? C5 C4 Fe 68.9(2) . . ? C3 C4 Fe 69.6(3) . . ? C5 C4 H4 126.3 . . ? C3 C4 H4 126.3 . . ? Fe C4 H4 126.8 . . ? C4 C5 C1 109.4(4) . . ? C4 C5 Fe 70.7(3) . . ? C1 C5 Fe 69.2(2) . . ? C4 C5 H5 125.3 . . ? C1 C5 H5 125.3 . . ? Fe C5 H5 126.4 . . ? C1 C6 C7 112.3(3) . . ? C1 C6 C8 112.5(3) . . ? C7 C6 C8 113.0(3) . . ? C1 C6 H6 106.2 . . ? C7 C6 H6 106.2 . . ? C8 C6 H6 106.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C9 117.7(3) . . ? C6 C8 H8A 107.9 . . ? C9 C8 H8A 107.9 . . ? C6 C8 H8B 107.9 . . ? C9 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? N1 C9 C10 108.1(3) . . ? N1 C9 C8 110.4(3) . . ? C10 C9 C8 114.1(3) . . ? N1 C9 H9 108.0 . . ? C10 C9 H9 108.0 . . ? C8 C9 H9 108.0 . . ? C11 C10 C14 105.6(3) . . ? C11 C10 C9 126.9(3) . . ? C14 C10 C9 127.5(3) . . ? C11 C10 Fe 71.3(2) . . ? C14 C10 Fe 69.83(18) . . ? C9 C10 Fe 124.9(2) . . ? C12 C11 C10 109.8(3) . . ? C12 C11 Fe 71.0(2) . . ? C10 C11 Fe 67.57(19) . . ? C12 C11 H11 125.1 . . ? C10 C11 H11 125.1 . . ? Fe C11 H11 127.9 . . ? C11 C12 C13 109.1(3) . . ? C11 C12 Fe 69.0(2) . . ? C13 C12 Fe 69.5(2) . . ? C11 C12 H12 125.5 . . ? C13 C12 H12 125.5 . . ? Fe C12 H12 127.6 . . ? C12 C13 C14 107.2(3) . . ? C12 C13 Fe 70.6(2) . . ? C14 C13 Fe 68.2(2) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? Fe C13 H13 126.3 . . ? C15 C14 C13 126.5(3) . . ? C15 C14 C10 125.0(3) . . ? C13 C14 C10 108.2(3) . . ? C15 C14 Fe 123.3(2) . . ? C13 C14 Fe 70.56(19) . . ? C10 C14 Fe 67.62(17) . . ? O1 C15 C14 121.0(3) . . ? O1 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C21 C26 112.7(3) . . ? C22 C21 B1 122.1(3) . . ? C26 C21 B1 125.1(3) . . ? F22 C22 C23 116.1(3) . . ? F22 C22 C21 118.8(3) . . ? C23 C22 C21 125.1(3) . . ? F23 C23 C24 120.1(3) . . ? F23 C23 C22 120.3(3) . . ? C24 C23 C22 119.7(3) . . ? F24 C24 C23 120.8(3) . . ? F24 C24 C25 121.1(4) . . ? C23 C24 C25 118.1(3) . . ? F25 C25 C26 120.2(3) . . ? F25 C25 C24 119.2(3) . . ? C26 C25 C24 120.6(4) . . ? F26 C26 C25 115.0(3) . . ? F26 C26 C21 121.3(3) . . ? C25 C26 C21 123.7(3) . . ? C36 C31 C32 113.3(3) . . ? C36 C31 B1 125.4(3) . . ? C32 C31 B1 121.3(3) . . ? F32 C32 C33 117.1(3) . . ? F32 C32 C31 119.1(3) . . ? C33 C32 C31 123.9(3) . . ? F33 C33 C32 120.6(4) . . ? F33 C33 C34 119.3(3) . . ? C32 C33 C34 120.1(4) . . ? F34 C34 C35 120.8(4) . . ? F34 C34 C33 120.6(4) . . ? C35 C34 C33 118.6(3) . . ? F35 C35 C34 119.5(3) . . ? F35 C35 C36 120.5(3) . . ? C34 C35 C36 120.0(3) . . ? F36 C36 C35 115.4(3) . . ? F36 C36 C31 120.6(3) . . ? C35 C36 C31 124.1(3) . . ? C42 C41 C46 112.9(3) . . ? C42 C41 B1 126.4(3) . . ? C46 C41 B1 120.7(3) . . ? F42 C42 C43 115.7(3) . . ? F42 C42 C41 120.3(3) . . ? C43 C42 C41 124.0(3) . . ? F43 C43 C44 119.0(3) . . ? F43 C43 C42 120.8(4) . . ? C44 C43 C42 120.2(4) . . ? F44 C44 C43 121.0(4) . . ? F44 C44 C45 120.4(4) . . ? C43 C44 C45 118.6(3) . . ? F45 C45 C46 121.3(4) . . ? F45 C45 C44 119.6(3) . . ? C46 C45 C44 119.1(3) . . ? F46 C46 C45 116.5(3) . . ? F46 C46 C41 118.3(3) . . ? C45 C46 C41 125.2(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 C15 O1 B1 C41 -10.7(4) . . . . ? C15 O1 B1 C21 -128.4(3) . . . . ? C15 O1 B1 C31 113.9(3) . . . . ? C10 Fe C1 C5 -118.4(2) . . . . ? C14 Fe C1 C5 -81.3(3) . . . . ? C2 Fe C1 C5 116.6(3) . . . . ? C11 Fe C1 C5 -158.9(2) . . . . ? C13 Fe C1 C5 -75.8(6) . . . . ? C3 Fe C1 C5 80.0(3) . . . . ? C4 Fe C1 C5 36.7(2) . . . . ? C12 Fe C1 C5 177.5(3) . . . . ? C10 Fe C1 C2 125.0(2) . . . . ? C14 Fe C1 C2 162.1(2) . . . . ? C5 Fe C1 C2 -116.6(3) . . . . ? C11 Fe C1 C2 84.5(3) . . . . ? C13 Fe C1 C2 167.6(5) . . . . ? C3 Fe C1 C2 -36.6(2) . . . . ? C4 Fe C1 C2 -79.9(3) . . . . ? C12 Fe C1 C2 60.9(4) . . . . ? C10 Fe C1 C6 2.9(3) . . . . ? C14 Fe C1 C6 40.0(3) . . . . ? C2 Fe C1 C6 -122.1(4) . . . . ? C5 Fe C1 C6 121.3(4) . . . . ? C11 Fe C1 C6 -37.6(3) . . . . ? C13 Fe C1 C6 45.5(7) . . . . ? C3 Fe C1 C6 -158.7(3) . . . . ? C4 Fe C1 C6 158.0(3) . . . . ? C12 Fe C1 C6 -61.2(4) . . . . ? C5 C1 C2 C3 -1.6(4) . . . . ? C6 C1 C2 C3 173.2(4) . . . . ? Fe C1 C2 C3 59.3(3) . . . . ? C5 C1 C2 Fe -61.0(3) . . . . ? C6 C1 C2 Fe 113.9(4) . . . . ? C10 Fe C2 C3 171.9(3) . . . . ? C14 Fe C2 C3 -168.0(4) . . . . ? C1 Fe C2 C3 -120.6(4) . . . . ? C5 Fe C2 C3 -81.5(3) . . . . ? C11 Fe C2 C3 131.3(3) . . . . ? C13 Fe C2 C3 66.8(5) . . . . ? C4 Fe C2 C3 -37.7(3) . . . . ? C12 Fe C2 C3 91.8(3) . . . . ? C10 Fe C2 C1 -67.5(3) . . . . ? C14 Fe C2 C1 -47.3(5) . . . . ? C5 Fe C2 C1 39.2(2) . . . . ? C11 Fe C2 C1 -108.0(2) . . . . ? C13 Fe C2 C1 -172.6(3) . . . . ? C3 Fe C2 C1 120.6(4) . . . . ? C4 Fe C2 C1 82.9(3) . . . . ? C12 Fe C2 C1 -147.6(2) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? Fe C2 C3 C4 59.7(3) . . . . ? C1 C2 C3 Fe -58.4(3) . . . . ? C10 Fe C3 C2 -19.4(6) . . . . ? C14 Fe C3 C2 168.1(4) . . . . ? C1 Fe C3 C2 37.3(3) . . . . ? C5 Fe C3 C2 81.3(3) . . . . ? C11 Fe C3 C2 -64.1(3) . . . . ? C13 Fe C3 C2 -150.4(2) . . . . ? C4 Fe C3 C2 119.0(4) . . . . ? C12 Fe C3 C2 -107.3(3) . . . . ? C10 Fe C3 C4 -138.4(4) . . . . ? C14 Fe C3 C4 49.1(6) . . . . ? C1 Fe C3 C4 -81.7(3) . . . . ? C2 Fe C3 C4 -119.0(4) . . . . ? C5 Fe C3 C4 -37.6(3) . . . . ? C11 Fe C3 C4 176.9(3) . . . . ? C13 Fe C3 C4 90.7(3) . . . . ? C12 Fe C3 C4 133.8(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? Fe C3 C4 C5 58.7(3) . . . . ? C2 C3 C4 Fe -59.1(3) . . . . ? C10 Fe C4 C5 28.1(5) . . . . ? C14 Fe C4 C5 79.7(3) . . . . ? C1 Fe C4 C5 -37.1(2) . . . . ? C2 Fe C4 C5 -81.4(3) . . . . ? C11 Fe C4 C5 -129.3(7) . . . . ? C13 Fe C4 C5 127.0(2) . . . . ? C3 Fe C4 C5 -119.1(4) . . . . ? C12 Fe C4 C5 171.5(2) . . . . ? C10 Fe C4 C3 147.2(3) . . . . ? C14 Fe C4 C3 -161.1(2) . . . . ? C1 Fe C4 C3 82.0(3) . . . . ? C2 Fe C4 C3 37.7(3) . . . . ? C5 Fe C4 C3 119.1(4) . . . . ? C11 Fe C4 C3 -10.1(8) . . . . ? C13 Fe C4 C3 -113.9(3) . . . . ? C12 Fe C4 C3 -69.4(3) . . . . ? C3 C4 C5 C1 -0.7(5) . . . . ? Fe C4 C5 C1 58.5(3) . . . . ? C3 C4 C5 Fe -59.2(3) . . . . ? C2 C1 C5 C4 1.4(4) . . . . ? C6 C1 C5 C4 -173.5(4) . . . . ? Fe C1 C5 C4 -59.5(3) . . . . ? C2 C1 C5 Fe 60.9(3) . . . . ? C6 C1 C5 Fe -114.1(4) . . . . ? C10 Fe C5 C4 -166.3(2) . . . . ? C14 Fe C5 C4 -120.5(2) . . . . ? C1 Fe C5 C4 120.6(3) . . . . ? C2 Fe C5 C4 81.2(3) . . . . ? C11 Fe C5 C4 159.0(3) . . . . ? C13 Fe C5 C4 -80.1(3) . . . . ? C3 Fe C5 C4 37.6(2) . . . . ? C12 Fe C5 C4 -49.7(12) . . . . ? C10 Fe C5 C1 73.1(2) . . . . ? C14 Fe C5 C1 118.9(2) . . . . ? C2 Fe C5 C1 -39.4(2) . . . . ? C11 Fe C5 C1 38.4(4) . . . . ? C13 Fe C5 C1 159.3(2) . . . . ? C3 Fe C5 C1 -83.0(2) . . . . ? C4 Fe C5 C1 -120.6(3) . . . . ? C12 Fe C5 C1 -170.3(10) . . . . ? C5 C1 C6 C7 178.0(4) . . . . ? C2 C1 C6 C7 4.1(6) . . . . ? Fe C1 C6 C7 91.1(4) . . . . ? C5 C1 C6 C8 49.2(5) . . . . ? C2 C1 C6 C8 -124.6(4) . . . . ? Fe C1 C6 C8 -37.6(4) . . . . ? C1 C6 C8 C9 70.2(4) . . . . ? C7 C6 C8 C9 -58.1(5) . . . . ? C16 N1 C9 C10 61.2(4) . . . . ? C17 N1 C9 C10 -176.5(3) . . . . ? C16 N1 C9 C8 -173.3(3) . . . . ? C17 N1 C9 C8 -50.9(4) . . . . ? C6 C8 C9 N1 -178.4(3) . . . . ? C6 C8 C9 C10 -56.4(4) . . . . ? N1 C9 C10 C11 -131.4(4) . . . . ? C8 C9 C10 C11 105.3(4) . . . . ? N1 C9 C10 C14 46.3(5) . . . . ? C8 C9 C10 C14 -77.0(4) . . . . ? N1 C9 C10 Fe 136.6(2) . . . . ? C8 C9 C10 Fe 13.3(4) . . . . ? C14 Fe C10 C11 115.3(3) . . . . ? C1 Fe C10 C11 -112.8(2) . . . . ? C2 Fe C10 C11 -75.0(3) . . . . ? C5 Fe C10 C11 -152.0(2) . . . . ? C13 Fe C10 C11 78.2(2) . . . . ? C3 Fe C10 C11 -60.8(5) . . . . ? C4 Fe C10 C11 -171.5(3) . . . . ? C12 Fe C10 C11 35.6(2) . . . . ? C1 Fe C10 C14 132.0(2) . . . . ? C2 Fe C10 C14 169.7(2) . . . . ? C5 Fe C10 C14 92.8(2) . . . . ? C11 Fe C10 C14 -115.3(3) . . . . ? C13 Fe C10 C14 -37.08(19) . . . . ? C3 Fe C10 C14 -176.1(4) . . . . ? C4 Fe C10 C14 73.2(4) . . . . ? C12 Fe C10 C14 -79.6(2) . . . . ? C14 Fe C10 C9 -122.3(3) . . . . ? C1 Fe C10 C9 9.7(3) . . . . ? C2 Fe C10 C9 47.5(3) . . . . ? C5 Fe C10 C9 -29.5(3) . . . . ? C11 Fe C10 C9 122.5(3) . . . . ? C13 Fe C10 C9 -159.3(3) . . . . ? C3 Fe C10 C9 61.6(6) . . . . ? C4 Fe C10 C9 -49.1(5) . . . . ? C12 Fe C10 C9 158.1(3) . . . . ? C14 C10 C11 C12 3.3(4) . . . . ? C9 C10 C11 C12 -178.6(3) . . . . ? Fe C10 C11 C12 -58.5(3) . . . . ? C14 C10 C11 Fe 61.8(2) . . . . ? C9 C10 C11 Fe -120.1(4) . . . . ? C10 Fe C11 C12 122.0(3) . . . . ? C14 Fe C11 C12 80.9(2) . . . . ? C1 Fe C11 C12 -160.17(19) . . . . ? C2 Fe C11 C12 -118.2(2) . . . . ? C5 Fe C11 C12 174.0(2) . . . . ? C13 Fe C11 C12 36.32(19) . . . . ? C3 Fe C11 C12 -81.7(3) . . . . ? C4 Fe C11 C12 -73.7(7) . . . . ? C14 Fe C11 C10 -41.1(2) . . . . ? C1 Fe C11 C10 77.9(2) . . . . ? C2 Fe C11 C10 119.8(2) . . . . ? C5 Fe C11 C10 52.1(3) . . . . ? C13 Fe C11 C10 -85.6(2) . . . . ? C3 Fe C11 C10 156.4(2) . . . . ? C4 Fe C11 C10 164.4(6) . . . . ? C12 Fe C11 C10 -122.0(3) . . . . ? C10 C11 C12 C13 -1.6(5) . . . . ? Fe C11 C12 C13 -58.1(3) . . . . ? C10 C11 C12 Fe 56.5(3) . . . . ? C10 Fe C12 C11 -36.61(19) . . . . ? C14 Fe C12 C11 -82.5(2) . . . . ? C1 Fe C12 C11 35.6(3) . . . . ? C2 Fe C12 C11 75.8(2) . . . . ? C5 Fe C12 C11 -156.1(10) . . . . ? C13 Fe C12 C11 -121.1(3) . . . . ? C3 Fe C12 C11 119.8(2) . . . . ? C4 Fe C12 C11 160.4(2) . . . . ? C10 Fe C12 C13 84.5(2) . . . . ? C14 Fe C12 C13 38.7(2) . . . . ? C1 Fe C12 C13 156.7(2) . . . . ? C2 Fe C12 C13 -163.1(2) . . . . ? C5 Fe C12 C13 -35.0(12) . . . . ? C11 Fe C12 C13 121.1(3) . . . . ? C3 Fe C12 C13 -119.1(2) . . . . ? C4 Fe C12 C13 -78.5(3) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? Fe C12 C13 C14 -58.6(2) . . . . ? C11 C12 C13 Fe 57.7(3) . . . . ? C10 Fe C13 C12 -80.4(2) . . . . ? C14 Fe C13 C12 -118.5(3) . . . . ? C1 Fe C13 C12 -125.6(6) . . . . ? C2 Fe C13 C12 35.8(5) . . . . ? C5 Fe C13 C12 173.7(2) . . . . ? C11 Fe C13 C12 -36.4(2) . . . . ? C3 Fe C13 C12 82.2(3) . . . . ? C4 Fe C13 C12 128.4(2) . . . . ? C10 Fe C13 C14 38.19(19) . . . . ? C1 Fe C13 C14 -7.0(7) . . . . ? C2 Fe C13 C14 154.4(3) . . . . ? C5 Fe C13 C14 -67.7(3) . . . . ? C11 Fe C13 C14 82.2(2) . . . . ? C3 Fe C13 C14 -159.2(2) . . . . ? C4 Fe C13 C14 -113.1(2) . . . . ? C12 Fe C13 C14 118.5(3) . . . . ? C12 C13 C14 C15 177.7(3) . . . . ? Fe C13 C14 C15 117.6(3) . . . . ? C12 C13 C14 C10 2.9(4) . . . . ? Fe C13 C14 C10 -57.2(2) . . . . ? C12 C13 C14 Fe 60.1(3) . . . . ? C11 C10 C14 C15 -178.7(3) . . . . ? C9 C10 C14 C15 3.2(5) . . . . ? Fe C10 C14 C15 -115.9(3) . . . . ? C11 C10 C14 C13 -3.8(4) . . . . ? C9 C10 C14 C13 178.1(3) . . . . ? Fe C10 C14 C13 59.0(2) . . . . ? C11 C10 C14 Fe -62.8(2) . . . . ? C9 C10 C14 Fe 119.1(4) . . . . ? C10 Fe C14 C15 118.2(4) . . . . ? C1 Fe C14 C15 56.2(3) . . . . ? C2 Fe C14 C15 91.6(5) . . . . ? C5 Fe C14 C15 12.9(3) . . . . ? C11 Fe C14 C15 157.8(3) . . . . ? C13 Fe C14 C15 -121.6(4) . . . . ? C3 Fe C14 C15 -66.0(6) . . . . ? C4 Fe C14 C15 -29.7(4) . . . . ? C12 Fe C14 C15 -159.0(3) . . . . ? C10 Fe C14 C13 -120.3(3) . . . . ? C1 Fe C14 C13 177.8(2) . . . . ? C2 Fe C14 C13 -146.9(4) . . . . ? C5 Fe C14 C13 134.5(2) . . . . ? C11 Fe C14 C13 -80.6(2) . . . . ? C3 Fe C14 C13 55.6(5) . . . . ? C4 Fe C14 C13 91.9(3) . . . . ? C12 Fe C14 C13 -37.4(2) . . . . ? C1 Fe C14 C10 -61.9(2) . . . . ? C2 Fe C14 C10 -26.6(5) . . . . ? C5 Fe C14 C10 -105.3(2) . . . . ? C11 Fe C14 C10 39.7(2) . . . . ? C13 Fe C14 C10 120.3(3) . . . . ? C3 Fe C14 C10 175.9(5) . . . . ? C4 Fe C14 C10 -147.8(2) . . . . ? C12 Fe C14 C10 82.9(2) . . . . ? B1 O1 C15 C14 169.9(3) . . . . ? C13 C14 C15 O1 12.1(5) . . . . ? C10 C14 C15 O1 -173.9(3) . . . . ? Fe C14 C15 O1 101.6(3) . . . . ? O1 B1 C21 C22 153.6(3) . . . . ? C41 B1 C21 C22 37.6(4) . . . . ? C31 B1 C21 C22 -94.7(4) . . . . ? O1 B1 C21 C26 -24.7(4) . . . . ? C41 B1 C21 C26 -140.7(3) . . . . ? C31 B1 C21 C26 87.0(4) . . . . ? C26 C21 C22 F22 -175.1(3) . . . . ? B1 C21 C22 F22 6.4(5) . . . . ? C26 C21 C22 C23 3.4(5) . . . . ? B1 C21 C22 C23 -175.1(3) . . . . ? F22 C22 C23 F23 -0.6(5) . . . . ? C21 C22 C23 F23 -179.1(3) . . . . ? F22 C22 C23 C24 177.9(3) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? F23 C23 C24 F24 -2.0(5) . . . . ? C22 C23 C24 F24 179.5(3) . . . . ? F23 C23 C24 C25 176.7(3) . . . . ? C22 C23 C24 C25 -1.8(5) . . . . ? F24 C24 C25 F25 0.0(5) . . . . ? C23 C24 C25 F25 -178.7(3) . . . . ? F24 C24 C25 C26 179.9(3) . . . . ? C23 C24 C25 C26 1.1(5) . . . . ? F25 C25 C26 F26 2.1(5) . . . . ? C24 C25 C26 F26 -177.7(3) . . . . ? F25 C25 C26 C21 -178.2(3) . . . . ? C24 C25 C26 C21 2.0(5) . . . . ? C22 C21 C26 F26 175.7(3) . . . . ? B1 C21 C26 F26 -5.9(5) . . . . ? C22 C21 C26 C25 -4.0(5) . . . . ? B1 C21 C26 C25 174.4(3) . . . . ? O1 B1 C31 C36 130.8(3) . . . . ? C41 B1 C31 C36 -109.7(4) . . . . ? C21 B1 C31 C36 20.0(4) . . . . ? O1 B1 C31 C32 -46.5(4) . . . . ? C41 B1 C31 C32 73.0(4) . . . . ? C21 B1 C31 C32 -157.4(3) . . . . ? C36 C31 C32 F32 176.1(3) . . . . ? B1 C31 C32 F32 -6.2(5) . . . . ? C36 C31 C32 C33 -3.1(5) . . . . ? B1 C31 C32 C33 174.6(3) . . . . ? F32 C32 C33 F33 1.5(5) . . . . ? C31 C32 C33 F33 -179.3(3) . . . . ? F32 C32 C33 C34 -178.3(3) . . . . ? C31 C32 C33 C34 0.9(6) . . . . ? F33 C33 C34 F34 1.7(6) . . . . ? C32 C33 C34 F34 -178.4(3) . . . . ? F33 C33 C34 C35 -178.2(3) . . . . ? C32 C33 C34 C35 1.7(6) . . . . ? F34 C34 C35 F35 -1.8(5) . . . . ? C33 C34 C35 F35 178.1(3) . . . . ? F34 C34 C35 C36 178.3(3) . . . . ? C33 C34 C35 C36 -1.8(6) . . . . ? F35 C35 C36 F36 -1.4(5) . . . . ? C34 C35 C36 F36 178.5(3) . . . . ? F35 C35 C36 C31 179.4(3) . . . . ? C34 C35 C36 C31 -0.7(6) . . . . ? C32 C31 C36 F36 -176.1(3) . . . . ? B1 C31 C36 F36 6.3(5) . . . . ? C32 C31 C36 C35 3.0(5) . . . . ? B1 C31 C36 C35 -174.5(3) . . . . ? O1 B1 C41 C42 122.3(3) . . . . ? C21 B1 C41 C42 -125.2(3) . . . . ? C31 B1 C41 C42 5.1(5) . . . . ? O1 B1 C41 C46 -58.7(4) . . . . ? C21 B1 C41 C46 53.8(4) . . . . ? C31 B1 C41 C46 -175.9(3) . . . . ? C46 C41 C42 F42 -178.9(3) . . . . ? B1 C41 C42 F42 0.2(5) . . . . ? C46 C41 C42 C43 0.1(5) . . . . ? B1 C41 C42 C43 179.1(3) . . . . ? F42 C42 C43 F43 -1.5(5) . . . . ? C41 C42 C43 F43 179.5(3) . . . . ? F42 C42 C43 C44 179.8(3) . . . . ? C41 C42 C43 C44 0.8(6) . . . . ? F43 C43 C44 F44 0.2(5) . . . . ? C42 C43 C44 F44 178.9(3) . . . . ? F43 C43 C44 C45 -180.0(3) . . . . ? C42 C43 C44 C45 -1.3(6) . . . . ? F44 C44 C45 F45 0.9(5) . . . . ? C43 C44 C45 F45 -178.8(3) . . . . ? F44 C44 C45 C46 -179.3(3) . . . . ? C43 C44 C45 C46 0.9(5) . . . . ? F45 C45 C46 F46 -0.7(5) . . . . ? C44 C45 C46 F46 179.6(3) . . . . ? F45 C45 C46 C41 179.8(3) . . . . ? C44 C45 C46 C41 0.0(5) . . . . ? C42 C41 C46 F46 179.9(3) . . . . ? B1 C41 C46 F46 0.8(4) . . . . ? C42 C41 C46 C45 -0.5(5) . . . . ? B1 C41 C46 C45 -179.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.267 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.066 # Attachment 'rev_5.cif' data_erk5129 _database_code_depnum_ccdc_archive 'CCDC 743170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H23 B F15 Fe N, C H2 Cl2' _chemical_formula_sum 'C37 H25 B Cl2 F15 Fe N' _chemical_formula_weight 906.14 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' N N 0.0061 0.0033 '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' 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 9.9961(2) _cell_length_b 13.2908(3) _cell_length_c 14.8471(3) _cell_angle_alpha 91.398(1) _cell_angle_beta 109.054(1) _cell_angle_gamma 105.386(1) _cell_volume 1784.25(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8372 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29354 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8787 _reflns_number_gt 7250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0785P)^2^+1.6787P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8787 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Fe Fe -0.18717(5) 0.55840(3) 0.63874(3) 0.04805(13) Uani 1 1 d . . . N1 N -0.10622(18) 0.81678(13) 0.78643(12) 0.0273(3) Uani 1 1 d . . . B1 B 0.2684(2) 0.86167(18) 0.71562(16) 0.0266(4) Uani 1 1 d . . . C1 C -0.1640(3) 0.50574(19) 0.7658(2) 0.0470(6) Uani 1 1 d . . . C2 C -0.2898(4) 0.4359(2) 0.6941(3) 0.0605(8) Uani 1 1 d . . . H2 H -0.3879 0.4183 0.6930 0.073 Uiso 1 1 calc R . . C3 C -0.2397(5) 0.3977(2) 0.6247(3) 0.0782(11) Uani 1 1 d . . . H3 H -0.2998 0.3506 0.5692 0.094 Uiso 1 1 calc R . . C4 C -0.0868(5) 0.4412(3) 0.6520(4) 0.0828(13) Uani 1 1 d . . . H4 H -0.0264 0.4295 0.6182 0.099 Uiso 1 1 calc R . . C5 C -0.0394(4) 0.5065(2) 0.7407(3) 0.0596(8) Uani 1 1 d . . . H5 H 0.0589 0.5440 0.7765 0.071 Uiso 1 1 calc R . . C6 C -0.1623(3) 0.5714(2) 0.85009(19) 0.0432(5) Uani 1 1 d . . . H6 H -0.0601 0.6176 0.8818 0.052 Uiso 1 1 calc R . . C7 C -0.2039(5) 0.5020(3) 0.9237(3) 0.0701(10) Uani 1 1 d . . . H7A H -0.3045 0.4568 0.8947 0.105 Uiso 1 1 calc R . . H7B H -0.1966 0.5463 0.9791 0.105 Uiso 1 1 calc R . . H7C H -0.1370 0.4592 0.9438 0.105 Uiso 1 1 calc R . . C8 C -0.2652(3) 0.6418(2) 0.8231(2) 0.0430(5) Uani 1 1 d . . . H8A H -0.3665 0.5949 0.7968 0.052 Uiso 1 1 calc R . . H8B H -0.2566 0.6796 0.8832 0.052 Uiso 1 1 calc R . . C9 C -0.2504(2) 0.72355(17) 0.75330(17) 0.0336(4) Uani 1 1 d . . . H9 H -0.3350 0.7531 0.7406 0.040 Uiso 1 1 calc R . . C10 C -0.2468(3) 0.68608(18) 0.65914(17) 0.0385(5) Uani 1 1 d . . . C11 C -0.3459(4) 0.6273(2) 0.5707(2) 0.0609(8) Uani 1 1 d . . . H11 H -0.4489 0.5989 0.5535 0.073 Uiso 1 1 calc R . . C12 C -0.2594(5) 0.6197(3) 0.5136(2) 0.0761(12) Uani 1 1 d . . . H12 H -0.2962 0.5840 0.4512 0.091 Uiso 1 1 calc R . . C13 C -0.1082(4) 0.6743(2) 0.5649(2) 0.0563(8) Uani 1 1 d . . . H13 H -0.0281 0.6804 0.5432 0.068 Uiso 1 1 calc R . . C14 C -0.1022(3) 0.71750(17) 0.65508(16) 0.0355(5) Uani 1 1 d . . . C15 C 0.0069(2) 0.78527(15) 0.74552(14) 0.0255(4) Uani 1 1 d . . . H15 H 0.0553 0.7400 0.7889 0.031 Uiso 1 1 calc R . . C16 C 0.1256(2) 0.88115(16) 0.73976(15) 0.0290(4) Uani 1 1 d . . . H16A H 0.1643 0.9262 0.8012 0.035 Uiso 1 1 calc R . . H16B H 0.0780 0.9206 0.6904 0.035 Uiso 1 1 calc R . . C17 C -0.1470(3) 0.90968(18) 0.74270(19) 0.0374(5) Uani 1 1 d . . . H17A H -0.2230 0.9240 0.7639 0.056 Uiso 1 1 calc R . . H17B H -0.1841 0.8946 0.6733 0.056 Uiso 1 1 calc R . . H17C H -0.0605 0.9706 0.7627 0.056 Uiso 1 1 calc R . . C18 C -0.0413(3) 0.8457(2) 0.89224(16) 0.0398(5) Uani 1 1 d . . . H18A H 0.0435 0.9075 0.9077 0.060 Uiso 1 1 calc R . . H18B H -0.0104 0.7877 0.9223 0.060 Uiso 1 1 calc R . . H18C H -0.1147 0.8606 0.9157 0.060 Uiso 1 1 calc R . . C21 C 0.2558(2) 0.86223(16) 0.60170(14) 0.0280(4) Uani 1 1 d . . . C22 C 0.3764(2) 0.85674(17) 0.57663(15) 0.0308(4) Uani 1 1 d . . . F22 F 0.49501(14) 0.83950(12) 0.64415(10) 0.0399(3) Uani 1 1 d . . . C23 C 0.3875(3) 0.86810(18) 0.48732(17) 0.0363(5) Uani 1 1 d . . . F23 F 0.50874(18) 0.86154(14) 0.46998(12) 0.0514(4) Uani 1 1 d . . . C24 C 0.2711(3) 0.8849(2) 0.41494(17) 0.0411(5) Uani 1 1 d . . . F24 F 0.2780(2) 0.89640(16) 0.32692(11) 0.0619(5) Uani 1 1 d . . . C25 C 0.1487(3) 0.89056(19) 0.43455(17) 0.0387(5) Uani 1 1 d . . . F25 F 0.03345(19) 0.90628(15) 0.36450(11) 0.0555(4) Uani 1 1 d . . . C26 C 0.1434(2) 0.88051(17) 0.52587(16) 0.0321(4) Uani 1 1 d . . . F26 F 0.01825(15) 0.89040(12) 0.53609(11) 0.0431(3) Uani 1 1 d . . . C31 C 0.4116(2) 0.96791(16) 0.76865(15) 0.0288(4) Uani 1 1 d . . . C32 C 0.3971(2) 1.06743(18) 0.75191(17) 0.0351(5) Uani 1 1 d . . . F32 F 0.26821(16) 1.07764(11) 0.69192(12) 0.0468(4) Uani 1 1 d . . . C33 C 0.5071(3) 1.16026(18) 0.7921(2) 0.0419(5) Uani 1 1 d . . . F33 F 0.4818(2) 1.25288(12) 0.77237(16) 0.0633(5) Uani 1 1 d . . . C34 C 0.6432(3) 1.1578(2) 0.8519(2) 0.0437(6) Uani 1 1 d . . . F34 F 0.75260(19) 1.24634(14) 0.89176(15) 0.0663(5) Uani 1 1 d . . . C35 C 0.6661(2) 1.0622(2) 0.86935(17) 0.0392(5) Uani 1 1 d . . . F35 F 0.79993(17) 1.05636(15) 0.92502(12) 0.0580(4) Uani 1 1 d . . . C36 C 0.5528(2) 0.97101(18) 0.82835(15) 0.0320(4) Uani 1 1 d . . . F36 F 0.59127(14) 0.88165(11) 0.84931(10) 0.0395(3) Uani 1 1 d . . . C41 C 0.3021(2) 0.75506(16) 0.76140(14) 0.0280(4) Uani 1 1 d . . . C42 C 0.2980(2) 0.66310(17) 0.71303(15) 0.0324(4) Uani 1 1 d . . . F42 F 0.25884(18) 0.65078(11) 0.61646(10) 0.0437(3) Uani 1 1 d . . . C43 C 0.3336(3) 0.57860(18) 0.75764(18) 0.0380(5) Uani 1 1 d . . . F43 F 0.3285(2) 0.49224(13) 0.70602(12) 0.0570(4) Uani 1 1 d . . . C44 C 0.3733(3) 0.58171(19) 0.85519(18) 0.0392(5) Uani 1 1 d . . . F44 F 0.4089(2) 0.50049(13) 0.89866(13) 0.0568(4) Uani 1 1 d . . . C45 C 0.3756(3) 0.66948(19) 0.90710(16) 0.0361(5) Uani 1 1 d . . . F45 F 0.41567(19) 0.67483(13) 1.00307(10) 0.0507(4) Uani 1 1 d . . . C46 C 0.3388(2) 0.75161(17) 0.86008(15) 0.0318(4) Uani 1 1 d . . . F46 F 0.34446(17) 0.83500(11) 0.91629(9) 0.0413(3) Uani 1 1 d . . . C100 C -0.2061(4) 0.7622(3) 1.1539(3) 0.0658(8) Uani 1 1 d . . . H10A H -0.1880 0.7932 1.2189 0.079 Uiso 1 1 calc R . . H10B H -0.2928 0.7003 1.1368 0.079 Uiso 1 1 calc R . . Cl1 Cl -0.05402(16) 0.72388(14) 1.15259(13) 0.1215(5) Uani 1 1 d . . . Cl2 Cl -0.24239(13) 0.85385(8) 1.07334(7) 0.0785(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 Fe 0.0607(3) 0.02851(19) 0.0493(2) -0.00536(15) 0.02459(19) -0.00247(16) N1 0.0247(8) 0.0268(8) 0.0313(8) 0.0038(6) 0.0121(6) 0.0058(6) B1 0.0261(10) 0.0264(10) 0.0283(10) 0.0032(8) 0.0120(8) 0.0063(8) C1 0.0479(14) 0.0274(11) 0.0654(17) 0.0073(11) 0.0207(12) 0.0086(10) C2 0.0643(18) 0.0310(13) 0.078(2) 0.0042(13) 0.0285(16) -0.0038(12) C3 0.114(3) 0.0285(14) 0.084(2) -0.0109(14) 0.044(2) -0.0024(16) C4 0.117(3) 0.0380(16) 0.121(3) 0.0021(18) 0.076(3) 0.0242(19) C5 0.0610(18) 0.0400(14) 0.092(2) 0.0145(15) 0.0406(17) 0.0189(13) C6 0.0470(13) 0.0347(12) 0.0487(14) 0.0153(10) 0.0206(11) 0.0071(10) C7 0.100(3) 0.0494(17) 0.068(2) 0.0296(16) 0.041(2) 0.0152(17) C8 0.0414(12) 0.0379(12) 0.0555(14) 0.0112(11) 0.0288(11) 0.0052(10) C9 0.0217(9) 0.0319(10) 0.0448(12) 0.0060(9) 0.0114(8) 0.0039(8) C10 0.0344(11) 0.0322(11) 0.0372(11) 0.0045(9) 0.0045(9) 0.0006(9) C11 0.0564(17) 0.0501(16) 0.0459(15) 0.0005(12) -0.0045(13) -0.0059(13) C12 0.104(3) 0.0563(19) 0.0362(14) -0.0088(13) 0.0132(16) -0.0145(18) C13 0.083(2) 0.0387(14) 0.0398(13) -0.0077(11) 0.0312(14) -0.0058(13) C14 0.0439(12) 0.0292(10) 0.0305(10) 0.0011(8) 0.0152(9) 0.0033(9) C15 0.0268(9) 0.0240(9) 0.0286(9) 0.0031(7) 0.0135(7) 0.0072(7) C16 0.0289(9) 0.0258(9) 0.0348(10) 0.0027(8) 0.0161(8) 0.0057(7) C17 0.0336(11) 0.0313(11) 0.0522(13) 0.0106(9) 0.0178(10) 0.0132(9) C18 0.0466(13) 0.0419(12) 0.0303(10) -0.0010(9) 0.0192(9) 0.0050(10) C21 0.0285(9) 0.0267(9) 0.0293(9) 0.0044(7) 0.0119(8) 0.0064(7) C22 0.0313(10) 0.0313(10) 0.0311(10) 0.0043(8) 0.0125(8) 0.0089(8) F22 0.0314(6) 0.0570(9) 0.0362(7) 0.0065(6) 0.0129(5) 0.0189(6) C23 0.0421(12) 0.0337(11) 0.0388(11) 0.0044(9) 0.0223(10) 0.0100(9) F23 0.0531(9) 0.0643(10) 0.0525(9) 0.0105(7) 0.0357(7) 0.0206(8) C24 0.0570(14) 0.0382(12) 0.0327(11) 0.0111(9) 0.0210(10) 0.0138(11) F24 0.0862(13) 0.0781(12) 0.0366(8) 0.0222(8) 0.0331(8) 0.0324(10) C25 0.0443(12) 0.0368(12) 0.0332(11) 0.0123(9) 0.0099(9) 0.0125(10) F25 0.0583(10) 0.0691(11) 0.0391(8) 0.0220(7) 0.0081(7) 0.0276(8) C26 0.0317(10) 0.0291(10) 0.0358(11) 0.0073(8) 0.0121(8) 0.0085(8) F26 0.0332(7) 0.0557(9) 0.0455(8) 0.0161(7) 0.0138(6) 0.0196(6) C31 0.0285(9) 0.0292(10) 0.0309(9) 0.0020(8) 0.0158(8) 0.0052(7) C32 0.0319(10) 0.0318(11) 0.0450(12) 0.0055(9) 0.0194(9) 0.0070(8) F32 0.0380(7) 0.0335(7) 0.0704(10) 0.0164(7) 0.0185(7) 0.0123(6) C33 0.0439(13) 0.0275(11) 0.0605(15) 0.0020(10) 0.0297(12) 0.0059(9) F33 0.0577(10) 0.0270(7) 0.1104(15) 0.0088(8) 0.0401(10) 0.0069(7) C34 0.0380(12) 0.0362(12) 0.0525(14) -0.0109(10) 0.0234(11) -0.0045(9) F34 0.0474(9) 0.0432(9) 0.0923(14) -0.0251(9) 0.0258(9) -0.0123(7) C35 0.0300(10) 0.0475(13) 0.0334(11) -0.0056(9) 0.0104(9) 0.0017(9) F35 0.0352(8) 0.0655(11) 0.0523(9) -0.0075(8) -0.0021(7) 0.0030(7) C36 0.0319(10) 0.0352(11) 0.0295(10) 0.0024(8) 0.0138(8) 0.0065(8) F36 0.0331(6) 0.0413(7) 0.0422(7) 0.0090(6) 0.0098(5) 0.0111(6) C41 0.0295(9) 0.0273(9) 0.0294(9) 0.0040(7) 0.0135(8) 0.0073(7) C42 0.0361(10) 0.0325(10) 0.0306(10) 0.0033(8) 0.0141(8) 0.0103(8) F42 0.0643(9) 0.0369(7) 0.0310(7) -0.0003(5) 0.0156(6) 0.0177(7) C43 0.0445(12) 0.0308(11) 0.0435(12) 0.0033(9) 0.0184(10) 0.0147(9) F43 0.0874(12) 0.0393(8) 0.0547(9) 0.0025(7) 0.0264(9) 0.0335(8) C44 0.0412(12) 0.0361(12) 0.0436(12) 0.0136(10) 0.0158(10) 0.0144(9) F44 0.0726(11) 0.0448(9) 0.0584(10) 0.0235(8) 0.0201(8) 0.0276(8) C45 0.0379(11) 0.0411(12) 0.0299(10) 0.0111(9) 0.0138(9) 0.0093(9) F45 0.0667(10) 0.0539(9) 0.0320(7) 0.0167(6) 0.0186(7) 0.0153(8) C46 0.0355(10) 0.0314(10) 0.0309(10) 0.0043(8) 0.0160(8) 0.0079(8) F46 0.0591(9) 0.0381(7) 0.0308(6) 0.0019(5) 0.0216(6) 0.0132(6) C100 0.0640(19) 0.066(2) 0.071(2) 0.0086(16) 0.0285(16) 0.0180(16) Cl1 0.0891(8) 0.1363(12) 0.1418(12) -0.0171(10) 0.0212(8) 0.0636(9) Cl2 0.1005(7) 0.0728(6) 0.0728(6) 0.0159(4) 0.0433(5) 0.0249(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 Fe C10 1.989(3) . ? Fe C1 1.992(3) . ? Fe C5 2.020(4) . ? Fe C2 2.027(3) . ? Fe C12 2.036(4) . ? Fe C14 2.034(2) . ? Fe C11 2.036(4) . ? Fe C3 2.048(3) . ? Fe C13 2.050(3) . ? Fe C4 2.046(4) . ? N1 C18 1.486(3) . ? N1 C17 1.499(3) . ? N1 C9 1.554(3) . ? N1 C15 1.584(2) . ? B1 C21 1.655(3) . ? B1 C41 1.653(3) . ? B1 C16 1.662(3) . ? B1 C31 1.673(3) . ? C1 C5 1.410(4) . ? C1 C2 1.426(4) . ? C1 C6 1.501(4) . ? C2 C3 1.420(5) . ? C2 H2 0.9400 . ? C3 C4 1.396(6) . ? C3 H3 0.9400 . ? C4 C5 1.425(6) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.536(4) . ? C6 C8 1.534(4) . ? C6 H6 0.9900 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.532(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.488(3) . ? C9 H9 0.9900 . ? C10 C14 1.415(3) . ? C10 C11 1.416(4) . ? C11 C12 1.413(6) . ? C11 H11 0.9400 . ? C12 C13 1.425(5) . ? C12 H12 0.9400 . ? C13 C14 1.422(3) . ? C13 H13 0.9400 . ? C14 C15 1.506(3) . ? C15 C16 1.519(3) . ? C15 H15 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C21 C26 1.386(3) . ? C21 C22 1.391(3) . ? C22 F22 1.358(2) . ? C22 C23 1.375(3) . ? C23 F23 1.342(3) . ? C23 C24 1.376(4) . ? C24 F24 1.341(3) . ? C24 C25 1.367(4) . ? C25 F25 1.345(3) . ? C25 C26 1.382(3) . ? C26 F26 1.347(3) . ? C31 C32 1.388(3) . ? C31 C36 1.389(3) . ? C32 F32 1.349(3) . ? C32 C33 1.380(3) . ? C33 F33 1.342(3) . ? C33 C34 1.370(4) . ? C34 F34 1.338(3) . ? C34 C35 1.365(4) . ? C35 F35 1.347(3) . ? C35 C36 1.382(3) . ? C36 F36 1.356(3) . ? C41 C42 1.386(3) . ? C41 C46 1.394(3) . ? C42 F42 1.351(2) . ? C42 C43 1.386(3) . ? C43 F43 1.345(3) . ? C43 C44 1.367(3) . ? C44 F44 1.340(3) . ? C44 C45 1.373(4) . ? C45 F45 1.343(3) . ? C45 C46 1.377(3) . ? C46 F46 1.348(3) . ? C100 Cl1 1.732(4) . ? C100 Cl2 1.752(4) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Fe C1 100.15(11) . . ? C10 Fe C5 124.50(12) . . ? C1 Fe C5 41.15(12) . . ? C10 Fe C2 111.23(13) . . ? C1 Fe C2 41.56(12) . . ? C5 Fe C2 68.72(14) . . ? C10 Fe C12 68.49(14) . . ? C1 Fe C12 164.58(16) . . ? C5 Fe C12 154.11(17) . . ? C2 Fe C12 131.24(15) . . ? C10 Fe C14 41.17(10) . . ? C1 Fe C14 110.70(10) . . ? C5 Fe C14 105.82(12) . . ? C2 Fe C14 144.37(12) . . ? C12 Fe C14 68.13(11) . . ? C10 Fe C11 41.18(11) . . ? C1 Fe C11 124.03(13) . . ? C5 Fe C11 162.99(14) . . ? C2 Fe C11 105.45(14) . . ? C12 Fe C11 40.62(16) . . ? C14 Fe C11 69.07(11) . . ? C10 Fe C3 147.66(15) . . ? C1 Fe C3 69.20(14) . . ? C5 Fe C3 67.86(16) . . ? C2 Fe C3 40.78(15) . . ? C12 Fe C3 114.52(16) . . ? C14 Fe C3 170.97(15) . . ? C11 Fe C3 118.87(16) . . ? C10 Fe C13 69.30(12) . . ? C1 Fe C13 146.53(11) . . ? C5 Fe C13 118.11(14) . . ? C2 Fe C13 171.84(13) . . ? C12 Fe C13 40.83(14) . . ? C14 Fe C13 40.74(9) . . ? C11 Fe C13 69.31(15) . . ? C3 Fe C13 135.56(14) . . ? C10 Fe C4 165.32(16) . . ? C1 Fe C4 69.63(15) . . ? C5 Fe C4 41.01(16) . . ? C2 Fe C4 68.58(15) . . ? C12 Fe C4 123.42(18) . . ? C14 Fe C4 131.18(15) . . ? C11 Fe C4 153.44(17) . . ? C3 Fe C4 39.87(18) . . ? C13 Fe C4 113.11(15) . . ? C18 N1 C17 107.67(18) . . ? C18 N1 C9 113.68(17) . . ? C17 N1 C9 106.46(16) . . ? C18 N1 C15 111.27(16) . . ? C17 N1 C15 110.45(15) . . ? C9 N1 C15 107.21(15) . . ? C21 B1 C41 113.60(16) . . ? C21 B1 C16 115.31(17) . . ? C41 B1 C16 108.65(16) . . ? C21 B1 C31 102.02(15) . . ? C41 B1 C31 110.57(16) . . ? C16 B1 C31 106.23(16) . . ? C5 C1 C2 107.3(3) . . ? C5 C1 C6 125.3(3) . . ? C2 C1 C6 127.3(3) . . ? C5 C1 Fe 70.49(19) . . ? C2 C1 Fe 70.55(18) . . ? C6 C1 Fe 121.89(17) . . ? C1 C2 C3 107.4(3) . . ? C1 C2 Fe 67.89(16) . . ? C3 C2 Fe 70.38(19) . . ? C1 C2 H2 126.3 . . ? C3 C2 H2 126.3 . . ? Fe C2 H2 127.0 . . ? C4 C3 C2 109.2(3) . . ? C4 C3 Fe 70.02(19) . . ? C2 C3 Fe 68.84(17) . . ? C4 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? Fe C3 H3 127.3 . . ? C3 C4 C5 107.2(3) . . ? C3 C4 Fe 70.1(2) . . ? C5 C4 Fe 68.49(19) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe C4 H4 126.6 . . ? C1 C5 C4 108.9(3) . . ? C1 C5 Fe 68.36(18) . . ? C4 C5 Fe 70.5(2) . . ? C1 C5 H5 125.6 . . ? C4 C5 H5 125.6 . . ? Fe C5 H5 127.2 . . ? C1 C6 C7 111.0(2) . . ? C1 C6 C8 113.9(2) . . ? C7 C6 C8 108.3(2) . . ? C1 C6 H6 107.8 . . ? C7 C6 H6 107.8 . . ? C8 C6 H6 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 122.0(2) . . ? C9 C8 H8A 106.8 . . ? C6 C8 H8A 106.8 . . ? C9 C8 H8B 106.8 . . ? C6 C8 H8B 106.8 . . ? H8A C8 H8B 106.7 . . ? C10 C9 C8 116.8(2) . . ? C10 C9 N1 99.28(16) . . ? C8 C9 N1 116.66(19) . . ? C10 C9 H9 107.8 . . ? C8 C9 H9 107.8 . . ? N1 C9 H9 107.8 . . ? C14 C10 C11 109.2(3) . . ? C14 C10 C9 112.04(19) . . ? C11 C10 C9 138.8(3) . . ? C14 C10 Fe 71.14(15) . . ? C11 C10 Fe 71.20(18) . . ? C9 C10 Fe 122.73(17) . . ? C10 C11 C12 106.4(3) . . ? C10 C11 Fe 67.62(16) . . ? C12 C11 Fe 69.7(2) . . ? C10 C11 H11 126.8 . . ? C12 C11 H11 126.8 . . ? Fe C11 H11 127.4 . . ? C13 C12 C11 109.9(3) . . ? C13 C12 Fe 70.09(19) . . ? C11 C12 Fe 69.68(19) . . ? C13 C12 H12 125.1 . . ? C11 C12 H12 125.1 . . ? Fe C12 H12 126.8 . . ? C12 C13 C14 106.4(3) . . ? C12 C13 Fe 69.08(18) . . ? C14 C13 Fe 69.06(14) . . ? C12 C13 H13 126.8 . . ? C14 C13 H13 126.8 . . ? Fe C13 H13 126.6 . . ? C10 C14 C13 108.1(2) . . ? C10 C14 C15 111.48(19) . . ? C13 C14 C15 140.4(2) . . ? C10 C14 Fe 67.68(13) . . ? C13 C14 Fe 70.20(14) . . ? C15 C14 Fe 126.18(15) . . ? C14 C15 C16 120.03(17) . . ? C14 C15 N1 98.72(15) . . ? C16 C15 N1 111.81(15) . . ? C14 C15 H15 108.5 . . ? C16 C15 H15 108.5 . . ? N1 C15 H15 108.5 . . ? C15 C16 B1 117.96(16) . . ? C15 C16 H16A 107.8 . . ? B1 C16 H16A 107.8 . . ? C15 C16 H16B 107.8 . . ? B1 C16 H16B 107.8 . . ? H16A C16 H16B 107.2 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C26 C21 C22 112.75(18) . . ? C26 C21 B1 127.66(18) . . ? C22 C21 B1 119.10(18) . . ? F22 C22 C23 115.60(19) . . ? F22 C22 C21 119.10(18) . . ? C23 C22 C21 125.3(2) . . ? F23 C23 C24 120.1(2) . . ? F23 C23 C22 121.0(2) . . ? C24 C23 C22 119.0(2) . . ? F24 C24 C25 120.6(2) . . ? F24 C24 C23 120.6(2) . . ? C25 C24 C23 118.8(2) . . ? F25 C25 C24 119.6(2) . . ? F25 C25 C26 120.2(2) . . ? C24 C25 C26 120.3(2) . . ? F26 C26 C25 114.22(19) . . ? F26 C26 C21 121.83(19) . . ? C25 C26 C21 123.9(2) . . ? C32 C31 C36 112.44(19) . . ? C32 C31 B1 119.77(19) . . ? C36 C31 B1 127.75(19) . . ? F32 C32 C33 115.6(2) . . ? F32 C32 C31 119.7(2) . . ? C33 C32 C31 124.7(2) . . ? F33 C33 C34 119.8(2) . . ? F33 C33 C32 120.3(2) . . ? C34 C33 C32 119.8(2) . . ? F34 C34 C35 120.2(2) . . ? F34 C34 C33 121.4(3) . . ? C35 C34 C33 118.4(2) . . ? F35 C35 C34 120.2(2) . . ? F35 C35 C36 119.7(2) . . ? C34 C35 C36 120.1(2) . . ? F36 C36 C35 114.1(2) . . ? F36 C36 C31 121.41(19) . . ? C35 C36 C31 124.5(2) . . ? C42 C41 C46 112.66(19) . . ? C42 C41 B1 127.85(18) . . ? C46 C41 B1 119.48(18) . . ? F42 C42 C41 120.88(19) . . ? F42 C42 C43 115.00(19) . . ? C41 C42 C43 124.1(2) . . ? F43 C43 C44 119.0(2) . . ? F43 C43 C42 120.8(2) . . ? C44 C43 C42 120.2(2) . . ? F44 C44 C43 120.4(2) . . ? F44 C44 C45 121.1(2) . . ? C43 C44 C45 118.6(2) . . ? F45 C45 C44 119.7(2) . . ? F45 C45 C46 120.8(2) . . ? C44 C45 C46 119.5(2) . . ? F46 C46 C45 115.79(19) . . ? F46 C46 C41 119.30(19) . . ? C45 C46 C41 124.9(2) . . ? Cl1 C100 Cl2 111.5(2) . . ? Cl1 C100 H10A 109.3 . . ? Cl2 C100 H10A 109.3 . . ? Cl1 C100 H10B 109.3 . . ? Cl2 C100 H10B 109.3 . . ? H10A C100 H10B 108.0 . . ? 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 C10 Fe C1 C5 -132.03(18) . . . . ? C2 Fe C1 C5 117.3(3) . . . . ? C12 Fe C1 C5 -173.3(4) . . . . ? C14 Fe C1 C5 -90.60(19) . . . . ? C11 Fe C1 C5 -168.74(18) . . . . ? C3 Fe C1 C5 79.7(2) . . . . ? C13 Fe C1 C5 -64.4(3) . . . . ? C4 Fe C1 C5 37.0(2) . . . . ? C10 Fe C1 C2 110.64(19) . . . . ? C5 Fe C1 C2 -117.3(3) . . . . ? C12 Fe C1 C2 69.4(5) . . . . ? C14 Fe C1 C2 152.07(18) . . . . ? C11 Fe C1 C2 73.9(2) . . . . ? C3 Fe C1 C2 -37.6(2) . . . . ? C13 Fe C1 C2 178.3(2) . . . . ? C4 Fe C1 C2 -80.3(2) . . . . ? C10 Fe C1 C6 -11.9(2) . . . . ? C5 Fe C1 C6 120.1(3) . . . . ? C2 Fe C1 C6 -122.5(3) . . . . ? C12 Fe C1 C6 -53.1(5) . . . . ? C14 Fe C1 C6 29.5(2) . . . . ? C11 Fe C1 C6 -48.6(3) . . . . ? C3 Fe C1 C6 -160.1(3) . . . . ? C13 Fe C1 C6 55.8(3) . . . . ? C4 Fe C1 C6 157.2(3) . . . . ? C5 C1 C2 C3 -1.8(4) . . . . ? C6 C1 C2 C3 175.3(3) . . . . ? Fe C1 C2 C3 59.5(2) . . . . ? C5 C1 C2 Fe -61.3(2) . . . . ? C6 C1 C2 Fe 115.8(3) . . . . ? C10 Fe C2 C1 -81.19(19) . . . . ? C5 Fe C2 C1 38.86(18) . . . . ? C12 Fe C2 C1 -160.7(2) . . . . ? C14 Fe C2 C1 -48.8(3) . . . . ? C11 Fe C2 C1 -124.28(19) . . . . ? C3 Fe C2 C1 119.2(3) . . . . ? C13 Fe C2 C1 -173.3(9) . . . . ? C4 Fe C2 C1 83.0(2) . . . . ? C10 Fe C2 C3 159.6(2) . . . . ? C1 Fe C2 C3 -119.2(3) . . . . ? C5 Fe C2 C3 -80.3(3) . . . . ? C12 Fe C2 C3 80.1(3) . . . . ? C14 Fe C2 C3 -168.0(2) . . . . ? C11 Fe C2 C3 116.5(3) . . . . ? C13 Fe C2 C3 67.5(10) . . . . ? C4 Fe C2 C3 -36.2(3) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? Fe C2 C3 C4 58.5(3) . . . . ? C1 C2 C3 Fe -57.9(2) . . . . ? C10 Fe C3 C4 -158.4(3) . . . . ? C1 Fe C3 C4 -82.8(3) . . . . ? C5 Fe C3 C4 -38.4(2) . . . . ? C2 Fe C3 C4 -121.0(4) . . . . ? C12 Fe C3 C4 113.5(3) . . . . ? C14 Fe C3 C4 8.3(10) . . . . ? C11 Fe C3 C4 158.9(3) . . . . ? C13 Fe C3 C4 69.7(3) . . . . ? C10 Fe C3 C2 -37.4(4) . . . . ? C1 Fe C3 C2 38.3(2) . . . . ? C5 Fe C3 C2 82.6(2) . . . . ? C12 Fe C3 C2 -125.5(3) . . . . ? C14 Fe C3 C2 129.4(8) . . . . ? C11 Fe C3 C2 -80.0(3) . . . . ? C13 Fe C3 C2 -169.2(2) . . . . ? C4 Fe C3 C2 121.0(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? Fe C3 C4 C5 58.7(2) . . . . ? C2 C3 C4 Fe -57.8(3) . . . . ? C10 Fe C4 C3 129.1(5) . . . . ? C1 Fe C4 C3 81.6(2) . . . . ? C5 Fe C4 C3 118.7(3) . . . . ? C2 Fe C4 C3 37.0(2) . . . . ? C12 Fe C4 C3 -89.2(3) . . . . ? C14 Fe C4 C3 -178.3(2) . . . . ? C11 Fe C4 C3 -44.7(5) . . . . ? C13 Fe C4 C3 -134.4(2) . . . . ? C10 Fe C4 C5 10.4(6) . . . . ? C1 Fe C4 C5 -37.15(19) . . . . ? C2 Fe C4 C5 -81.8(2) . . . . ? C12 Fe C4 C5 152.1(2) . . . . ? C14 Fe C4 C5 63.0(3) . . . . ? C11 Fe C4 C5 -163.5(3) . . . . ? C3 Fe C4 C5 -118.7(3) . . . . ? C13 Fe C4 C5 106.8(2) . . . . ? C2 C1 C5 C4 2.3(4) . . . . ? C6 C1 C5 C4 -174.8(3) . . . . ? Fe C1 C5 C4 -59.0(3) . . . . ? C2 C1 C5 Fe 61.3(2) . . . . ? C6 C1 C5 Fe -115.8(3) . . . . ? C3 C4 C5 C1 -2.0(4) . . . . ? Fe C4 C5 C1 57.7(2) . . . . ? C3 C4 C5 Fe -59.7(3) . . . . ? C10 Fe C5 C1 62.5(2) . . . . ? C2 Fe C5 C1 -39.24(17) . . . . ? C12 Fe C5 C1 175.9(3) . . . . ? C14 Fe C5 C1 103.54(17) . . . . ? C11 Fe C5 C1 33.6(5) . . . . ? C3 Fe C5 C1 -83.3(2) . . . . ? C13 Fe C5 C1 145.68(16) . . . . ? C4 Fe C5 C1 -120.7(3) . . . . ? C10 Fe C5 C4 -176.8(2) . . . . ? C1 Fe C5 C4 120.7(3) . . . . ? C2 Fe C5 C4 81.4(2) . . . . ? C12 Fe C5 C4 -63.4(4) . . . . ? C14 Fe C5 C4 -135.8(2) . . . . ? C11 Fe C5 C4 154.2(4) . . . . ? C3 Fe C5 C4 37.4(2) . . . . ? C13 Fe C5 C4 -93.7(2) . . . . ? C5 C1 C6 C7 -114.6(3) . . . . ? C2 C1 C6 C7 68.9(4) . . . . ? Fe C1 C6 C7 157.8(2) . . . . ? C5 C1 C6 C8 122.9(3) . . . . ? C2 C1 C6 C8 -53.7(4) . . . . ? Fe C1 C6 C8 35.2(3) . . . . ? C1 C6 C8 C9 -58.0(3) . . . . ? C7 C6 C8 C9 178.0(3) . . . . ? C6 C8 C9 C10 51.7(3) . . . . ? C6 C8 C9 N1 -65.4(3) . . . . ? C18 N1 C9 C10 -156.23(19) . . . . ? C17 N1 C9 C10 85.4(2) . . . . ? C15 N1 C9 C10 -32.8(2) . . . . ? C18 N1 C9 C8 -29.9(3) . . . . ? C17 N1 C9 C8 -148.3(2) . . . . ? C15 N1 C9 C8 93.5(2) . . . . ? C8 C9 C10 C14 -104.0(2) . . . . ? N1 C9 C10 C14 22.3(2) . . . . ? C8 C9 C10 C11 75.9(4) . . . . ? N1 C9 C10 C11 -157.9(3) . . . . ? C8 C9 C10 Fe -22.9(3) . . . . ? N1 C9 C10 Fe 103.38(18) . . . . ? C1 Fe C10 C14 109.92(15) . . . . ? C5 Fe C10 C14 73.54(18) . . . . ? C2 Fe C10 C14 151.69(16) . . . . ? C12 Fe C10 C14 -80.93(17) . . . . ? C11 Fe C10 C14 -118.9(2) . . . . ? C3 Fe C10 C14 176.9(2) . . . . ? C13 Fe C10 C14 -37.03(15) . . . . ? C4 Fe C10 C14 65.3(6) . . . . ? C1 Fe C10 C11 -131.20(19) . . . . ? C5 Fe C10 C11 -167.58(19) . . . . ? C2 Fe C10 C11 -89.4(2) . . . . ? C12 Fe C10 C11 37.9(2) . . . . ? C14 Fe C10 C11 118.9(2) . . . . ? C3 Fe C10 C11 -64.2(3) . . . . ? C13 Fe C10 C11 81.8(2) . . . . ? C4 Fe C10 C11 -175.8(5) . . . . ? C1 Fe C10 C9 5.3(2) . . . . ? C5 Fe C10 C9 -31.0(2) . . . . ? C2 Fe C10 C9 47.1(2) . . . . ? C12 Fe C10 C9 174.5(2) . . . . ? C14 Fe C10 C9 -104.6(2) . . . . ? C11 Fe C10 C9 136.5(3) . . . . ? C3 Fe C10 C9 72.3(3) . . . . ? C13 Fe C10 C9 -141.6(2) . . . . ? C4 Fe C10 C9 -39.3(6) . . . . ? C14 C10 C11 C12 2.1(3) . . . . ? C9 C10 C11 C12 -177.8(3) . . . . ? Fe C10 C11 C12 -59.2(2) . . . . ? C14 C10 C11 Fe 61.32(18) . . . . ? C9 C10 C11 Fe -118.6(3) . . . . ? C1 Fe C11 C10 63.3(2) . . . . ? C5 Fe C11 C10 37.3(5) . . . . ? C2 Fe C11 C10 104.75(18) . . . . ? C12 Fe C11 C10 -118.5(2) . . . . ? C14 Fe C11 C10 -38.11(15) . . . . ? C3 Fe C11 C10 146.62(18) . . . . ? C13 Fe C11 C10 -81.83(17) . . . . ? C4 Fe C11 C10 177.6(3) . . . . ? C10 Fe C11 C12 118.5(2) . . . . ? C1 Fe C11 C12 -178.16(17) . . . . ? C5 Fe C11 C12 155.8(4) . . . . ? C2 Fe C11 C12 -136.75(19) . . . . ? C14 Fe C11 C12 80.40(18) . . . . ? C3 Fe C11 C12 -94.9(2) . . . . ? C13 Fe C11 C12 36.68(17) . . . . ? C4 Fe C11 C12 -63.9(4) . . . . ? C10 C11 C12 C13 -0.8(4) . . . . ? Fe C11 C12 C13 -58.7(3) . . . . ? C10 C11 C12 Fe 57.9(2) . . . . ? C10 Fe C12 C13 82.8(2) . . . . ? C1 Fe C12 C13 127.0(4) . . . . ? C5 Fe C12 C13 -42.8(4) . . . . ? C2 Fe C12 C13 -177.27(19) . . . . ? C14 Fe C12 C13 38.35(18) . . . . ? C11 Fe C12 C13 121.3(3) . . . . ? C3 Fe C12 C13 -132.3(2) . . . . ? C4 Fe C12 C13 -87.5(2) . . . . ? C10 Fe C12 C11 -38.46(17) . . . . ? C1 Fe C12 C11 5.8(5) . . . . ? C5 Fe C12 C11 -164.1(3) . . . . ? C2 Fe C12 C11 61.4(3) . . . . ? C14 Fe C12 C11 -82.93(18) . . . . ? C3 Fe C12 C11 106.5(2) . . . . ? C13 Fe C12 C11 -121.3(3) . . . . ? C4 Fe C12 C11 151.3(2) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? Fe C12 C13 C14 -59.2(2) . . . . ? C11 C12 C13 Fe 58.4(3) . . . . ? C10 Fe C13 C12 -80.7(2) . . . . ? C1 Fe C13 C12 -157.4(2) . . . . ? C5 Fe C13 C12 160.4(2) . . . . ? C2 Fe C13 C12 14.6(11) . . . . ? C14 Fe C13 C12 -118.1(3) . . . . ? C11 Fe C13 C12 -36.5(2) . . . . ? C3 Fe C13 C12 74.1(3) . . . . ? C4 Fe C13 C12 115.0(3) . . . . ? C10 Fe C13 C14 37.41(16) . . . . ? C1 Fe C13 C14 -39.3(3) . . . . ? C5 Fe C13 C14 -81.6(2) . . . . ? C2 Fe C13 C14 132.7(9) . . . . ? C12 Fe C13 C14 118.1(3) . . . . ? C11 Fe C13 C14 81.58(19) . . . . ? C3 Fe C13 C14 -167.8(2) . . . . ? C4 Fe C13 C14 -127.0(2) . . . . ? C11 C10 C14 C13 -2.6(3) . . . . ? C9 C10 C14 C13 177.3(2) . . . . ? Fe C10 C14 C13 58.71(19) . . . . ? C11 C10 C14 C15 177.0(2) . . . . ? C9 C10 C14 C15 -3.1(3) . . . . ? Fe C10 C14 C15 -121.62(18) . . . . ? C11 C10 C14 Fe -61.4(2) . . . . ? C9 C10 C14 Fe 118.56(19) . . . . ? C12 C13 C14 C10 2.1(3) . . . . ? Fe C13 C14 C10 -57.16(18) . . . . ? C12 C13 C14 C15 -177.4(3) . . . . ? Fe C13 C14 C15 123.3(3) . . . . ? C12 C13 C14 Fe 59.2(2) . . . . ? C1 Fe C14 C10 -81.61(16) . . . . ? C5 Fe C14 C10 -124.77(16) . . . . ? C2 Fe C14 C10 -49.4(3) . . . . ? C12 Fe C14 C10 81.88(19) . . . . ? C11 Fe C14 C10 38.12(16) . . . . ? C3 Fe C14 C10 -169.3(8) . . . . ? C13 Fe C14 C10 120.3(2) . . . . ? C4 Fe C14 C10 -162.2(2) . . . . ? C10 Fe C14 C13 -120.3(2) . . . . ? C1 Fe C14 C13 158.1(2) . . . . ? C5 Fe C14 C13 114.9(2) . . . . ? C2 Fe C14 C13 -169.7(2) . . . . ? C12 Fe C14 C13 -38.4(2) . . . . ? C11 Fe C14 C13 -82.2(2) . . . . ? C3 Fe C14 C13 70.4(9) . . . . ? C4 Fe C14 C13 77.5(3) . . . . ? C10 Fe C14 C15 101.0(2) . . . . ? C1 Fe C14 C15 19.3(2) . . . . ? C5 Fe C14 C15 -23.8(2) . . . . ? C2 Fe C14 C15 51.6(3) . . . . ? C12 Fe C14 C15 -177.2(3) . . . . ? C11 Fe C14 C15 139.1(2) . . . . ? C3 Fe C14 C15 -68.3(9) . . . . ? C13 Fe C14 C15 -138.7(3) . . . . ? C4 Fe C14 C15 -61.2(3) . . . . ? C10 C14 C15 C16 -138.8(2) . . . . ? C13 C14 C15 C16 40.7(4) . . . . ? Fe C14 C15 C16 143.74(17) . . . . ? C10 C14 C15 N1 -17.3(2) . . . . ? C13 C14 C15 N1 162.2(3) . . . . ? Fe C14 C15 N1 -94.73(19) . . . . ? C18 N1 C15 C14 155.96(17) . . . . ? C17 N1 C15 C14 -84.51(19) . . . . ? C9 N1 C15 C14 31.09(19) . . . . ? C18 N1 C15 C16 -76.7(2) . . . . ? C17 N1 C15 C16 42.8(2) . . . . ? C9 N1 C15 C16 158.45(17) . . . . ? C14 C15 C16 B1 -75.1(2) . . . . ? N1 C15 C16 B1 170.09(16) . . . . ? C21 B1 C16 C15 97.0(2) . . . . ? C41 B1 C16 C15 -31.8(2) . . . . ? C31 B1 C16 C15 -150.81(17) . . . . ? C41 B1 C21 C26 128.8(2) . . . . ? C16 B1 C21 C26 2.4(3) . . . . ? C31 B1 C21 C26 -112.2(2) . . . . ? C41 B1 C21 C22 -59.8(2) . . . . ? C16 B1 C21 C22 173.81(18) . . . . ? C31 B1 C21 C22 59.2(2) . . . . ? C26 C21 C22 F22 179.77(19) . . . . ? B1 C21 C22 F22 7.2(3) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? B1 C21 C22 C23 -172.4(2) . . . . ? F22 C22 C23 F23 0.4(3) . . . . ? C21 C22 C23 F23 180.0(2) . . . . ? F22 C22 C23 C24 179.5(2) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? F23 C23 C24 F24 -0.9(4) . . . . ? C22 C23 C24 F24 180.0(2) . . . . ? F23 C23 C24 C25 179.6(2) . . . . ? C22 C23 C24 C25 0.5(4) . . . . ? F24 C24 C25 F25 0.9(4) . . . . ? C23 C24 C25 F25 -179.6(2) . . . . ? F24 C24 C25 C26 -178.8(2) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? F25 C25 C26 F26 -1.5(3) . . . . ? C24 C25 C26 F26 178.3(2) . . . . ? F25 C25 C26 C21 178.7(2) . . . . ? C24 C25 C26 C21 -1.5(4) . . . . ? C22 C21 C26 F26 -178.74(19) . . . . ? B1 C21 C26 F26 -6.9(3) . . . . ? C22 C21 C26 C25 1.0(3) . . . . ? B1 C21 C26 C25 172.9(2) . . . . ? C21 B1 C31 C32 69.1(2) . . . . ? C41 B1 C31 C32 -169.74(18) . . . . ? C16 B1 C31 C32 -52.0(2) . . . . ? C21 B1 C31 C36 -108.6(2) . . . . ? C41 B1 C31 C36 12.5(3) . . . . ? C16 B1 C31 C36 130.2(2) . . . . ? C36 C31 C32 F32 177.18(19) . . . . ? B1 C31 C32 F32 -0.9(3) . . . . ? C36 C31 C32 C33 -2.3(3) . . . . ? B1 C31 C32 C33 179.6(2) . . . . ? F32 C32 C33 F33 1.3(3) . . . . ? C31 C32 C33 F33 -179.2(2) . . . . ? F32 C32 C33 C34 -178.2(2) . . . . ? C31 C32 C33 C34 1.3(4) . . . . ? F33 C33 C34 F34 0.2(4) . . . . ? C32 C33 C34 F34 179.7(2) . . . . ? F33 C33 C34 C35 -179.0(2) . . . . ? C32 C33 C34 C35 0.5(4) . . . . ? F34 C34 C35 F35 -1.6(4) . . . . ? C33 C34 C35 F35 177.7(2) . . . . ? F34 C34 C35 C36 179.7(2) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? F35 C35 C36 F36 -0.5(3) . . . . ? C34 C35 C36 F36 178.2(2) . . . . ? F35 C35 C36 C31 -178.9(2) . . . . ? C34 C35 C36 C31 -0.2(4) . . . . ? C32 C31 C36 F36 -176.56(18) . . . . ? B1 C31 C36 F36 1.3(3) . . . . ? C32 C31 C36 C35 1.8(3) . . . . ? B1 C31 C36 C35 179.7(2) . . . . ? C21 B1 C41 C42 -10.7(3) . . . . ? C16 B1 C41 C42 119.1(2) . . . . ? C31 B1 C41 C42 -124.7(2) . . . . ? C21 B1 C41 C46 169.82(18) . . . . ? C16 B1 C41 C46 -60.4(2) . . . . ? C31 B1 C41 C46 55.8(2) . . . . ? C46 C41 C42 F42 177.45(19) . . . . ? B1 C41 C42 F42 -2.0(3) . . . . ? C46 C41 C42 C43 -3.2(3) . . . . ? B1 C41 C42 C43 177.3(2) . . . . ? F42 C42 C43 F43 0.1(3) . . . . ? C41 C42 C43 F43 -179.3(2) . . . . ? F42 C42 C43 C44 -179.3(2) . . . . ? C41 C42 C43 C44 1.3(4) . . . . ? F43 C43 C44 F44 1.1(4) . . . . ? C42 C43 C44 F44 -179.5(2) . . . . ? F43 C43 C44 C45 -178.9(2) . . . . ? C42 C43 C44 C45 0.5(4) . . . . ? F44 C44 C45 F45 0.8(4) . . . . ? C43 C44 C45 F45 -179.3(2) . . . . ? F44 C44 C45 C46 179.8(2) . . . . ? C43 C44 C45 C46 -0.2(4) . . . . ? F45 C45 C46 F46 -0.6(3) . . . . ? C44 C45 C46 F46 -179.7(2) . . . . ? F45 C45 C46 C41 177.1(2) . . . . ? C44 C45 C46 C41 -2.0(4) . . . . ? C42 C41 C46 F46 -178.83(19) . . . . ? B1 C41 C46 F46 0.7(3) . . . . ? C42 C41 C46 C45 3.5(3) . . . . ? B1 C41 C46 C45 -176.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.664 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.064