# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Martin Albrecht' _publ_contact_author_email MARTIN.ALBRECHT@UNIFR.CH _publ_section_title ; Main-chain organometallic polymers comprising redox-active iron(II) centers connected by ditopic N-heterocyclic carbenes ; loop_ _publ_author_name 'Martin Albrecht' 'Laszlo Mercs' 'Antonia Neels' 'Helen Stoeckli-Evans' #################################################END data_Complex12 _database_code_depnum_ccdc_archive 'CCDC 726548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 B F4 Fe N3 O' _chemical_formula_weight 467.10 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' _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 11.7156(9) _cell_length_b 14.0710(7) _cell_length_c 13.7433(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.542(6) _cell_angle_gamma 90.00 _cell_volume 2182.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15967 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 29.39 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98369 _exptl_absorpt_correction_T_max 1.01637 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30379 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 29.20 _reflns_number_total 5895 _reflns_number_gt 3905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997), MERCURY (Macrea 2006)' _computing_publication_material SHELXL-97 _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^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0064(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5895 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _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 0.42427(15) 0.22195(13) 0.32442(11) 0.0329(4) Uani 1 1 d . . . H1 H 0.3880 0.2813 0.3301 0.039 Uiso 1 1 calc R . . C2 C 0.38904(14) 0.13360(14) 0.35442(11) 0.0329(4) Uani 1 1 d . . . H2 H 0.3244 0.1224 0.3825 0.039 Uiso 1 1 calc R . . C3 C 0.46838(15) 0.06398(13) 0.33488(12) 0.0317(4) Uani 1 1 d . . . H3 H 0.4670 -0.0020 0.3491 0.038 Uiso 1 1 calc R . . C4 C 0.54847(14) 0.10939(12) 0.29119(11) 0.0310(4) Uani 1 1 d . . . H4 H 0.6101 0.0794 0.2696 0.037 Uiso 1 1 calc R . . C5 C 0.52190(14) 0.20827(13) 0.28455(11) 0.0306(4) Uani 1 1 d . . . H5 H 0.5625 0.2561 0.2582 0.037 Uiso 1 1 calc R . . C6 C 0.29292(14) 0.02263(12) 0.17203(12) 0.0269(3) Uani 1 1 d . . . C7 C 0.24657(13) 0.21928(11) 0.14166(10) 0.0212(3) Uani 1 1 d . . . C8 C 0.14913(14) 0.34889(12) 0.06358(12) 0.0310(4) Uani 1 1 d . . . H8 H 0.1342 0.4077 0.0286 0.037 Uiso 1 1 calc R . . C9 C 0.07004(14) 0.29566(13) 0.09334(12) 0.0317(4) Uani 1 1 d . . . H9 H -0.0117 0.3094 0.0832 0.038 Uiso 1 1 calc R . . C10 C 0.07195(13) 0.14202(12) 0.18658(12) 0.0277(3) Uani 1 1 d . . . H10 H 0.1343 0.0961 0.2224 0.033 Uiso 1 1 calc R . . C11 C 0.01559(17) 0.18398(15) 0.26362(14) 0.0428(5) Uani 1 1 d . . . H11A H -0.0468 0.2287 0.2302 0.051 Uiso 1 1 calc R . . H11B H 0.0759 0.2175 0.3155 0.051 Uiso 1 1 calc R . . H11 H -0.0189 0.1330 0.2951 0.051 Uiso 1 1 calc R . . C12 C -0.01574(18) 0.08840(16) 0.10402(16) 0.0522(5) Uani 1 1 d . . . H12C H -0.0499 0.0360 0.1338 0.063 Uiso 1 1 calc R . . H12B H 0.0249 0.0629 0.0559 0.063 Uiso 1 1 calc R . . H12D H -0.0790 0.1316 0.0688 0.063 Uiso 1 1 calc R . . C13 C 0.36691(14) 0.34436(11) 0.07894(11) 0.0265(3) Uani 1 1 d . . . H13 H 0.4321 0.2970 0.1025 0.032 Uiso 1 1 calc R . . C14 C 0.35422(16) 0.36416(14) -0.03216(12) 0.0363(4) Uani 1 1 d . . . H14A H 0.2956 0.4146 -0.0555 0.044 Uiso 1 1 calc R . . H14B H 0.3281 0.3063 -0.0715 0.044 Uiso 1 1 calc R . . H14C H 0.4308 0.3844 -0.0411 0.044 Uiso 1 1 calc R . . C15 C 0.39966(17) 0.43297(13) 0.14306(14) 0.0383(4) Uani 1 1 d . . . H15C H 0.4770 0.4562 0.1387 0.046 Uiso 1 1 calc R . . H15B H 0.4035 0.4179 0.2135 0.046 Uiso 1 1 calc R . . H15A H 0.3396 0.4821 0.1184 0.046 Uiso 1 1 calc R . . C16 C 0.51829(13) 0.13535(11) 0.05018(11) 0.0265(3) Uani 1 1 d . . . H16 H 0.5819 0.1503 0.1073 0.032 Uiso 1 1 calc R . . C17 C 0.54127(15) 0.12805(13) -0.04301(12) 0.0332(4) Uani 1 1 d . . . H17 H 0.6193 0.1378 -0.0492 0.040 Uiso 1 1 calc R . . C18 C 0.45073(18) 0.10657(11) -0.12668(13) 0.0363(4) Uani 1 1 d . . . H18 H 0.4651 0.1005 -0.1912 0.044 Uiso 1 1 calc R . . C19 C 0.33842(17) 0.09396(12) -0.11484(12) 0.0346(4) Uani 1 1 d . . . H19 H 0.2737 0.0797 -0.1713 0.041 Uiso 1 1 calc R . . C20 C 0.32175(15) 0.10242(12) -0.01985(11) 0.0291(4) Uani 1 1 d . . . H20 H 0.2440 0.0938 -0.0125 0.035 Uiso 1 1 calc R . . B1 B 0.23358(16) 0.15445(15) 0.58833(16) 0.0342(5) Uani 1 1 d . . . F1A F 0.3274(9) 0.0957(9) 0.6291(7) 0.0512(18) Uani 0.60 1 d P . . F1B F 0.3329(15) 0.0944(13) 0.6109(12) 0.067(4) Uani 0.40 1 d P . . F2A F 0.1730(4) 0.1270(5) 0.4953(3) 0.0749(14) Uani 0.60 1 d P . . F2B F 0.1377(6) 0.1141(7) 0.5232(7) 0.112(3) Uani 0.40 1 d P . . F3A F 0.2749(7) 0.2392(6) 0.5591(7) 0.069(4) Uani 0.50 1 d P . . F3B F 0.261(2) 0.2187(18) 0.5231(13) 0.078(8) Uani 0.20 1 d P . . F3C F 0.2638(15) 0.2432(12) 0.6122(14) 0.110(7) Uani 0.30 1 d P . . F4A F 0.1667(5) 0.1593(5) 0.6523(5) 0.065(2) Uani 0.50 1 d P . . F4B F 0.2091(10) 0.2008(9) 0.6716(6) 0.080(4) Uani 0.30 1 d P . . F4C F 0.1548(15) 0.1134(12) 0.6382(14) 0.090(6) Uani 0.20 1 d P . . Fe1 Fe 0.374562(18) 0.128026(16) 0.199265(15) 0.02061(6) Uani 1 1 d . . . N1 N 0.25679(11) 0.30219(9) 0.09336(9) 0.0238(3) Uani 1 1 d . . . N2 N 0.13021(11) 0.21654(9) 0.14188(9) 0.0242(3) Uani 1 1 d . . . N3 N 0.40984(11) 0.12226(9) 0.06354(9) 0.0228(3) Uani 1 1 d . . . O1 O 0.24597(11) -0.05037(9) 0.15902(10) 0.0406(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 0.0368(10) 0.0345(10) 0.0231(8) -0.0067(7) 0.0006(7) 0.0066(8) C2 0.0307(8) 0.0467(10) 0.0213(7) -0.0006(8) 0.0071(6) 0.0022(8) C3 0.0325(9) 0.0338(10) 0.0254(8) 0.0072(7) 0.0019(7) 0.0030(7) C4 0.0220(7) 0.0400(11) 0.0278(8) 0.0009(7) 0.0014(6) 0.0070(7) C5 0.0286(9) 0.0345(10) 0.0251(8) 0.0002(7) 0.0008(6) -0.0061(7) C6 0.0257(8) 0.0301(9) 0.0283(8) 0.0000(7) 0.0131(6) 0.0055(7) C7 0.0202(7) 0.0252(8) 0.0188(7) -0.0025(6) 0.0063(6) 0.0019(6) C8 0.0280(8) 0.0328(10) 0.0334(8) 0.0078(7) 0.0103(7) 0.0127(7) C9 0.0215(8) 0.0402(10) 0.0330(8) 0.0065(7) 0.0066(6) 0.0128(7) C10 0.0231(7) 0.0294(9) 0.0338(8) -0.0021(7) 0.0131(6) 0.0003(7) C11 0.0489(12) 0.0472(12) 0.0428(10) 0.0049(9) 0.0304(9) 0.0129(9) C12 0.0432(12) 0.0524(13) 0.0588(13) -0.0134(10) 0.0097(10) -0.0160(10) C13 0.0262(8) 0.0243(9) 0.0309(8) 0.0023(6) 0.0107(6) 0.0030(6) C14 0.0403(9) 0.0381(10) 0.0346(8) 0.0063(8) 0.0173(7) 0.0020(8) C15 0.0429(10) 0.0307(10) 0.0444(10) -0.0047(8) 0.0168(8) -0.0040(8) C16 0.0271(8) 0.0227(8) 0.0318(7) 0.0011(7) 0.0116(6) 0.0030(7) C17 0.0414(9) 0.0255(8) 0.0412(9) 0.0008(8) 0.0259(7) 0.0030(8) C18 0.0620(12) 0.0228(9) 0.0316(8) -0.0008(7) 0.0255(8) 0.0036(8) C19 0.0482(11) 0.0300(9) 0.0246(8) -0.0021(7) 0.0082(7) 0.0043(8) C20 0.0290(8) 0.0308(9) 0.0271(8) -0.0014(6) 0.0065(6) 0.0035(7) B1 0.0201(9) 0.0380(12) 0.0427(11) -0.0032(9) 0.0050(8) 0.0017(8) F1A 0.034(3) 0.059(3) 0.0580(16) 0.0058(16) 0.0078(19) 0.022(2) F1B 0.034(4) 0.047(5) 0.129(10) 0.029(6) 0.037(5) 0.012(3) F2A 0.056(3) 0.117(4) 0.0424(13) -0.0210(16) -0.0016(15) 0.000(3) F2B 0.042(3) 0.082(4) 0.179(10) -0.034(6) -0.029(4) -0.020(3) F3A 0.035(2) 0.042(5) 0.124(11) 0.028(7) 0.013(7) -0.009(3) F3B 0.080(15) 0.117(19) 0.050(7) 0.041(8) 0.041(8) 0.049(12) F3C 0.056(8) 0.044(6) 0.20(2) -0.034(12) -0.022(11) -0.006(5) F4A 0.044(3) 0.114(7) 0.043(3) -0.019(3) 0.019(2) 0.018(4) F4B 0.103(10) 0.104(10) 0.031(3) -0.007(4) 0.014(4) 0.054(7) F4C 0.059(6) 0.145(14) 0.083(9) -0.047(8) 0.047(6) -0.044(8) Fe1 0.01841(10) 0.02290(11) 0.02077(10) 0.00041(10) 0.00569(7) 0.00276(10) N1 0.0208(6) 0.0259(7) 0.0257(6) 0.0027(5) 0.0080(5) 0.0054(5) N2 0.0200(6) 0.0284(7) 0.0245(6) 0.0004(5) 0.0066(5) 0.0039(5) N3 0.0244(6) 0.0205(7) 0.0244(6) 0.0004(5) 0.0081(5) 0.0038(5) O1 0.0418(7) 0.0303(7) 0.0570(8) -0.0080(6) 0.0260(6) -0.0065(6) _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 C2 1.406(3) . ? C1 C5 1.408(2) . ? C1 Fe1 2.1230(16) . ? C1 H1 0.9500 . ? C2 C3 1.425(2) . ? C2 Fe1 2.0947(15) . ? C2 H2 0.9500 . ? C3 C4 1.397(2) . ? C3 Fe1 2.0968(15) . ? C3 H3 0.9500 . ? C4 C5 1.423(2) . ? C4 Fe1 2.1064(15) . ? C4 H4 0.9500 . ? C5 Fe1 2.1317(16) . ? C5 H5 0.9500 . ? C6 O1 1.156(2) . ? C6 Fe1 1.7500(17) . ? C7 N1 1.3632(19) . ? C7 N2 1.3646(19) . ? C7 Fe1 1.9718(15) . ? C8 C9 1.338(2) . ? C8 N1 1.3833(19) . ? C8 H8 0.9500 . ? C9 N2 1.389(2) . ? C9 H9 0.9500 . ? C10 N2 1.472(2) . ? C10 C11 1.510(2) . ? C10 C12 1.512(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11 0.9800 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12D 0.9800 . ? C13 N1 1.481(2) . ? C13 C15 1.516(2) . ? C13 C14 1.520(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 N3 1.3443(19) . ? C16 C17 1.381(2) . ? C16 H16 0.9500 . ? C17 C18 1.373(3) . ? C17 H17 0.9500 . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.376(2) . ? C19 H19 0.9500 . ? C20 N3 1.3500(19) . ? C20 H20 0.9500 . ? B1 F3C 1.315(16) . ? B1 F4A 1.326(6) . ? B1 F2A 1.343(4) . ? B1 F2B 1.359(7) . ? B1 F3B 1.368(19) . ? B1 F1A 1.370(11) . ? B1 F3A 1.386(7) . ? B1 F1B 1.403(18) . ? B1 F4C 1.411(18) . ? B1 F4B 1.412(9) . ? F2A F2B 0.661(9) . ? F2A F3B 1.63(2) . ? F2B F4C 1.54(2) . ? F3A F3B 0.56(2) . ? F3A F3C 0.777(16) . ? F3B F3C 1.26(3) . ? F3C F4B 1.309(17) . ? F4A F4C 0.677(13) . ? F4A F4B 0.766(11) . ? F4B F4C 1.404(18) . ? Fe1 N3 2.0173(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 109.05(15) . . ? C2 C1 Fe1 69.44(9) . . ? C5 C1 Fe1 71.01(9) . . ? C2 C1 H1 125.5 . . ? C5 C1 H1 125.5 . . ? Fe1 C1 H1 125.6 . . ? C1 C2 C3 107.16(15) . . ? C1 C2 Fe1 71.62(9) . . ? C3 C2 Fe1 70.21(9) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 126.4 . . ? Fe1 C2 H2 123.4 . . ? C4 C3 C2 108.29(16) . . ? C4 C3 Fe1 70.96(9) . . ? C2 C3 Fe1 70.05(9) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe1 C3 H3 124.7 . . ? C3 C4 C5 108.31(15) . . ? C3 C4 Fe1 70.22(9) . . ? C5 C4 Fe1 71.34(9) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe1 C4 H4 124.2 . . ? C1 C5 C4 107.17(15) . . ? C1 C5 Fe1 70.35(9) . . ? C4 C5 Fe1 69.42(9) . . ? C1 C5 H5 126.4 . . ? C4 C5 H5 126.4 . . ? Fe1 C5 H5 125.4 . . ? O1 C6 Fe1 174.89(15) . . ? N1 C7 N2 104.09(12) . . ? N1 C7 Fe1 126.60(11) . . ? N2 C7 Fe1 129.30(11) . . ? C9 C8 N1 107.16(14) . . ? C9 C8 H8 126.4 . . ? N1 C8 H8 126.4 . . ? C8 C9 N2 106.95(14) . . ? C8 C9 H9 126.5 . . ? N2 C9 H9 126.5 . . ? N2 C10 C11 110.66(14) . . ? N2 C10 C12 109.87(14) . . ? C11 C10 C12 112.60(15) . . ? N2 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11 109.5 . . ? H11A C11 H11 109.5 . . ? H11B C11 H11 109.5 . . ? C10 C12 H12C 109.5 . . ? C10 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C10 C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? N1 C13 C15 110.22(13) . . ? N1 C13 C14 110.72(13) . . ? C15 C13 C14 112.00(14) . . ? N1 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15C 109.5 . . ? C13 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C13 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? N3 C16 C17 122.87(15) . . ? N3 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C18 C17 C16 119.61(16) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 118.47(15) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C20 C19 C18 118.88(16) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N3 C20 C19 123.56(16) . . ? N3 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? F3C B1 F4A 87.3(7) . . ? F3C B1 F2A 123.3(9) . . ? F4A B1 F2A 113.0(3) . . ? F3C B1 F2B 132.9(9) . . ? F4A B1 F2B 85.8(4) . . ? F2A B1 F2B 28.3(4) . . ? F3C B1 F3B 56.1(12) . . ? F4A B1 F3B 132.9(11) . . ? F2A B1 F3B 73.8(9) . . ? F2B B1 F3B 98.0(10) . . ? F3C B1 F1A 109.8(10) . . ? F4A B1 F1A 108.1(6) . . ? F2A B1 F1A 112.2(5) . . ? F2B B1 F1A 116.6(7) . . ? F3B B1 F1A 111.5(12) . . ? F3C B1 F3A 33.3(7) . . ? F4A B1 F3A 117.5(4) . . ? F2A B1 F3A 96.2(5) . . ? F2B B1 F3A 117.4(6) . . ? F3B B1 F3A 23.4(9) . . ? F1A B1 F3A 109.5(6) . . ? F3C B1 F1B 111.4(11) . . ? F4A B1 F1B 119.1(8) . . ? F2A B1 F1B 103.5(7) . . ? F2B B1 F1B 112.6(8) . . ? F3B B1 F1B 102.7(13) . . ? F1A B1 F1B 11.3(11) . . ? F3A B1 F1B 104.4(8) . . ? F3C B1 F4C 115.8(8) . . ? F4A B1 F4C 28.4(5) . . ? F2A B1 F4C 95.6(7) . . ? F2B B1 F4C 67.4(7) . . ? F3B B1 F4C 152.1(14) . . ? F1A B1 F4C 96.4(9) . . ? F3A B1 F4C 144.8(7) . . ? F1B B1 F4C 104.9(11) . . ? F3C B1 F4B 57.2(7) . . ? F4A B1 F4B 32.3(5) . . ? F2A B1 F4B 137.3(5) . . ? F2B B1 F4B 114.5(6) . . ? F3B B1 F4B 111.0(11) . . ? F1A B1 F4B 105.2(6) . . ? F3A B1 F4B 90.0(6) . . ? F1B B1 F4B 115.8(8) . . ? F4C B1 F4B 59.6(7) . . ? F2B F2A B1 77.2(9) . . ? F2B F2A F3B 122.2(14) . . ? B1 F2A F3B 53.8(7) . . ? F2A F2B B1 74.5(9) . . ? F2A F2B F4C 132.0(13) . . ? B1 F2B F4C 57.9(7) . . ? F3B F3A F3C 142(3) . . ? F3B F3A B1 76(2) . . ? F3C F3A B1 68.3(14) . . ? F3A F3B F3C 22.5(16) . . ? F3A F3B B1 80(2) . . ? F3C F3B B1 59.8(11) . . ? F3A F3B F2A 130(2) . . ? F3C F3B F2A 107.3(14) . . ? B1 F3B F2A 52.4(7) . . ? F3A F3C F3B 16.0(12) . . ? F3A F3C F4B 142(2) . . ? F3B F3C F4B 126.0(19) . . ? F3A F3C B1 78.4(16) . . ? F3B F3C B1 64.1(15) . . ? F4B F3C B1 65.1(8) . . ? F4C F4A F4B 153(2) . . ? F4C F4A B1 82.8(17) . . ? F4B F4A B1 80.0(10) . . ? F4A F4B F3C 120.8(12) . . ? F4A F4B F4C 12.7(10) . . ? F3C F4B F4C 116.7(13) . . ? F4A F4B B1 67.7(8) . . ? F3C F4B B1 57.7(8) . . ? F4C F4B B1 60.2(8) . . ? F4A F4C F4B 14.4(11) . . ? F4A F4C B1 68.8(16) . . ? F4B F4C B1 60.2(9) . . ? F4A F4C F2B 104(2) . . ? F4B F4C F2B 104.7(14) . . ? B1 F4C F2B 54.7(7) . . ? C6 Fe1 C7 98.79(7) . . ? C6 Fe1 N3 90.22(6) . . ? C7 Fe1 N3 88.69(5) . . ? C6 Fe1 C2 98.05(7) . . ? C7 Fe1 C2 103.28(6) . . ? N3 Fe1 C2 164.14(5) . . ? C6 Fe1 C3 87.26(7) . . ? C7 Fe1 C3 142.93(6) . . ? N3 Fe1 C3 128.03(6) . . ? C2 Fe1 C3 39.74(7) . . ? C6 Fe1 C4 114.09(7) . . ? C7 Fe1 C4 146.23(7) . . ? N3 Fe1 C4 98.32(6) . . ? C2 Fe1 C4 65.96(6) . . ? C3 Fe1 C4 38.82(6) . . ? C6 Fe1 C1 135.75(7) . . ? C7 Fe1 C1 86.21(6) . . ? N3 Fe1 C1 133.98(6) . . ? C2 Fe1 C1 38.94(7) . . ? C3 Fe1 C1 65.34(7) . . ? C4 Fe1 C1 65.18(7) . . ? C6 Fe1 C5 151.90(7) . . ? C7 Fe1 C5 107.01(7) . . ? N3 Fe1 C5 101.15(6) . . ? C2 Fe1 C5 65.65(7) . . ? C3 Fe1 C5 65.45(7) . . ? C4 Fe1 C5 39.24(7) . . ? C1 Fe1 C5 38.64(6) . . ? C7 N1 C8 111.00(13) . . ? C7 N1 C13 126.97(12) . . ? C8 N1 C13 121.88(13) . . ? C7 N2 C9 110.79(13) . . ? C7 N2 C10 126.60(13) . . ? C9 N2 C10 122.60(13) . . ? C16 N3 C20 116.60(13) . . ? C16 N3 Fe1 123.79(10) . . ? C20 N3 Fe1 119.60(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 1.37(17) . . . . ? Fe1 C1 C2 C3 61.57(10) . . . . ? C5 C1 C2 Fe1 -60.20(11) . . . . ? C1 C2 C3 C4 -1.53(17) . . . . ? Fe1 C2 C3 C4 60.96(11) . . . . ? C1 C2 C3 Fe1 -62.49(10) . . . . ? C2 C3 C4 C5 1.11(17) . . . . ? Fe1 C3 C4 C5 61.50(11) . . . . ? C2 C3 C4 Fe1 -60.39(11) . . . . ? C2 C1 C5 C4 -0.70(17) . . . . ? Fe1 C1 C5 C4 -59.93(10) . . . . ? C2 C1 C5 Fe1 59.23(11) . . . . ? C3 C4 C5 C1 -0.26(17) . . . . ? Fe1 C4 C5 C1 60.53(11) . . . . ? C3 C4 C5 Fe1 -60.79(11) . . . . ? N1 C8 C9 N2 0.31(18) . . . . ? N3 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C17 C18 C19 C20 -0.6(2) . . . . ? C18 C19 C20 N3 -0.2(3) . . . . ? F3C B1 F2A F2B -119.9(16) . . . . ? F4A B1 F2A F2B -17.2(16) . . . . ? F3B B1 F2A F2B -147.6(19) . . . . ? F1A B1 F2A F2B 105.3(15) . . . . ? F3A B1 F2A F2B -140.7(15) . . . . ? F1B B1 F2A F2B 112.9(16) . . . . ? F4C B1 F2A F2B 6.0(16) . . . . ? F4B B1 F2A F2B -43.9(19) . . . . ? F3C B1 F2A F3B 27.7(18) . . . . ? F4A B1 F2A F3B 130.3(12) . . . . ? F2B B1 F2A F3B 147.6(19) . . . . ? F1A B1 F2A F3B -107.1(13) . . . . ? F3A B1 F2A F3B 6.9(13) . . . . ? F1B B1 F2A F3B -99.5(14) . . . . ? F4C B1 F2A F3B 153.6(14) . . . . ? F4B B1 F2A F3B 103.7(15) . . . . ? F3B F2A F2B B1 -30.8(16) . . . . ? B1 F2A F2B F4C -7.4(19) . . . . ? F3B F2A F2B F4C -38(3) . . . . ? F3C B1 F2B F2A 81.7(18) . . . . ? F4A B1 F2B F2A 164.1(15) . . . . ? F3B B1 F2B F2A 31.3(18) . . . . ? F1A B1 F2B F2A -87.7(15) . . . . ? F3A B1 F2B F2A 45.2(16) . . . . ? F1B B1 F2B F2A -76.1(17) . . . . ? F4C B1 F2B F2A -173.5(17) . . . . ? F4B B1 F2B F2A 148.9(13) . . . . ? F3C B1 F2B F4C -104.8(12) . . . . ? F4A B1 F2B F4C -22.4(8) . . . . ? F2A B1 F2B F4C 173.5(17) . . . . ? F3B B1 F2B F4C -155.2(13) . . . . ? F1A B1 F2B F4C 85.8(10) . . . . ? F3A B1 F2B F4C -141.4(9) . . . . ? F1B B1 F2B F4C 97.4(11) . . . . ? F4B B1 F2B F4C -37.7(10) . . . . ? F3C B1 F3A F3B -164(3) . . . . ? F4A B1 F3A F3B -137(3) . . . . ? F2A B1 F3A F3B -17(3) . . . . ? F2B B1 F3A F3B -37(3) . . . . ? F1A B1 F3A F3B 99(3) . . . . ? F1B B1 F3A F3B 89(3) . . . . ? F4C B1 F3A F3B -126(3) . . . . ? F4B B1 F3A F3B -155(3) . . . . ? F4A B1 F3A F3C 27(2) . . . . ? F2A B1 F3A F3C 147.2(18) . . . . ? F2B B1 F3A F3C 127.4(18) . . . . ? F3B B1 F3A F3C 164(3) . . . . ? F1A B1 F3A F3C -96.6(19) . . . . ? F1B B1 F3A F3C -107.2(19) . . . . ? F4C B1 F3A F3C 38(2) . . . . ? F4B B1 F3A F3C 9.6(19) . . . . ? B1 F3A F3B F3C 24(5) . . . . ? F3C F3A F3B B1 -24(5) . . . . ? F3C F3A F3B F2A -6(8) . . . . ? B1 F3A F3B F2A 18(3) . . . . ? F3C B1 F3B F3A 10(2) . . . . ? F4A B1 F3B F3A 56(3) . . . . ? F2A B1 F3B F3A 163(3) . . . . ? F2B B1 F3B F3A 148(3) . . . . ? F1A B1 F3B F3A -90(3) . . . . ? F1B B1 F3B F3A -97(3) . . . . ? F4C B1 F3B F3A 92(3) . . . . ? F4B B1 F3B F3A 27(3) . . . . ? F4A B1 F3B F3C 45(2) . . . . ? F2A B1 F3B F3C 152.1(18) . . . . ? F2B B1 F3B F3C 137.2(15) . . . . ? F1A B1 F3B F3C -100.0(16) . . . . ? F3A B1 F3B F3C -10(2) . . . . ? F1B B1 F3B F3C -107.4(17) . . . . ? F4C B1 F3B F3C 81(2) . . . . ? F4B B1 F3B F3C 17.0(19) . . . . ? F3C B1 F3B F2A -152.1(18) . . . . ? F4A B1 F3B F2A -106.6(9) . . . . ? F2B B1 F3B F2A -14.9(8) . . . . ? F1A B1 F3B F2A 107.9(7) . . . . ? F3A B1 F3B F2A -163(3) . . . . ? F1B B1 F3B F2A 100.6(8) . . . . ? F4C B1 F3B F2A -71(2) . . . . ? F4B B1 F3B F2A -135.1(6) . . . . ? F2B F2A F3B F3A 16(6) . . . . ? B1 F2A F3B F3A -23(4) . . . . ? F2B F2A F3B F3C 13(3) . . . . ? B1 F2A F3B F3C -25.1(17) . . . . ? F2B F2A F3B B1 38(2) . . . . ? B1 F3A F3C F3B -25(5) . . . . ? F3B F3A F3C F4B 9(7) . . . . ? B1 F3A F3C F4B -17(3) . . . . ? F3B F3A F3C B1 25(5) . . . . ? B1 F3B F3C F3A 152(6) . . . . ? F2A F3B F3C F3A 175(6) . . . . ? F3A F3B F3C F4B -173(5) . . . . ? B1 F3B F3C F4B -21(2) . . . . ? F2A F3B F3C F4B 2(4) . . . . ? F3A F3B F3C B1 -152(6) . . . . ? F2A F3B F3C B1 22.9(15) . . . . ? F4A B1 F3C F3A -156.0(17) . . . . ? F2A B1 F3C F3A -40(2) . . . . ? F2B B1 F3C F3A -74(2) . . . . ? F3B B1 F3C F3A -7.5(15) . . . . ? F1A B1 F3C F3A 95.6(18) . . . . ? F1B B1 F3C F3A 83.7(19) . . . . ? F4C B1 F3C F3A -156.6(16) . . . . ? F4B B1 F3C F3A -169(2) . . . . ? F4A B1 F3C F3B -148.5(17) . . . . ? F2A B1 F3C F3B -33(2) . . . . ? F2B B1 F3C F3B -67(2) . . . . ? F1A B1 F3C F3B 103.2(17) . . . . ? F3A B1 F3C F3B 7.5(15) . . . . ? F1B B1 F3C F3B 91.2(19) . . . . ? F4C B1 F3C F3B -149.1(17) . . . . ? F4B B1 F3C F3B -161(2) . . . . ? F4A B1 F3C F4B 12.6(8) . . . . ? F2A B1 F3C F4B 128.5(7) . . . . ? F2B B1 F3C F4B 94.4(11) . . . . ? F3B B1 F3C F4B 161(2) . . . . ? F1A B1 F3C F4B -95.8(8) . . . . ? F3A B1 F3C F4B 169(2) . . . . ? F1B B1 F3C F4B -107.7(10) . . . . ? F4C B1 F3C F4B 12.0(14) . . . . ? F3C B1 F4A F4C -179(2) . . . . ? F2A B1 F4A F4C 56(2) . . . . ? F2B B1 F4A F4C 47.7(19) . . . . ? F3B B1 F4A F4C 145(2) . . . . ? F1A B1 F4A F4C -69(2) . . . . ? F3A B1 F4A F4C 166.5(19) . . . . ? F1B B1 F4A F4C -66(2) . . . . ? F4B B1 F4A F4C -159(2) . . . . ? F3C B1 F4A F4B -20.0(13) . . . . ? F2A B1 F4A F4B -145.3(10) . . . . ? F2B B1 F4A F4B -153.4(11) . . . . ? F3B B1 F4A F4B -56.3(17) . . . . ? F1A B1 F4A F4B 89.9(11) . . . . ? F3A B1 F4A F4B -34.6(12) . . . . ? F1B B1 F4A F4B 93.0(13) . . . . ? F4C B1 F4A F4B 159(2) . . . . ? F4C F4A F4B F3C 75(5) . . . . ? B1 F4A F4B F3C 23.6(15) . . . . ? B1 F4A F4B F4C -51(5) . . . . ? F4C F4A F4B B1 51(5) . . . . ? F3A F3C F4B F4A -8(5) . . . . ? F3B F3C F4B F4A -5(4) . . . . ? B1 F3C F4B F4A -26.0(16) . . . . ? F3A F3C F4B F4C 6(5) . . . . ? F3B F3C F4B F4C 9(4) . . . . ? B1 F3C F4B F4C -12.2(15) . . . . ? F3A F3C F4B B1 18(4) . . . . ? F3B F3C F4B B1 21(3) . . . . ? F3C B1 F4B F4A 156.0(15) . . . . ? F2A B1 F4B F4A 50.6(15) . . . . ? F2B B1 F4B F4A 29.4(13) . . . . ? F3B B1 F4B F4A 139.3(14) . . . . ? F1A B1 F4B F4A -100.0(11) . . . . ? F3A B1 F4B F4A 149.8(11) . . . . ? F1B B1 F4B F4A -104.2(12) . . . . ? F4C B1 F4B F4A -11.4(13) . . . . ? F4A B1 F4B F3C -156.0(15) . . . . ? F2A B1 F4B F3C -105.4(13) . . . . ? F2B B1 F4B F3C -126.6(11) . . . . ? F3B B1 F4B F3C -16.7(19) . . . . ? F1A B1 F4B F3C 104.0(11) . . . . ? F3A B1 F4B F3C -6.2(12) . . . . ? F1B B1 F4B F3C 99.8(13) . . . . ? F4C B1 F4B F3C -167.4(15) . . . . ? F3C B1 F4B F4C 167.4(15) . . . . ? F4A B1 F4B F4C 11.4(13) . . . . ? F2A B1 F4B F4C 62.0(14) . . . . ? F2B B1 F4B F4C 40.8(12) . . . . ? F3B B1 F4B F4C 150.7(14) . . . . ? F1A B1 F4B F4C -88.6(12) . . . . ? F3A B1 F4B F4C 161.2(11) . . . . ? F1B B1 F4B F4C -92.8(13) . . . . ? B1 F4A F4C F4B 51(5) . . . . ? F4B F4A F4C B1 -51(5) . . . . ? F4B F4A F4C F2B -93(5) . . . . ? B1 F4A F4C F2B -42.3(11) . . . . ? F3C F4B F4C F4A -112(5) . . . . ? B1 F4B F4C F4A -124(5) . . . . ? F4A F4B F4C B1 124(5) . . . . ? F3C F4B F4C B1 11.9(14) . . . . ? F4A F4B F4C F2B 91(5) . . . . ? F3C F4B F4C F2B -21.0(19) . . . . ? B1 F4B F4C F2B -32.9(7) . . . . ? F3C B1 F4C F4A 1(2) . . . . ? F2A B1 F4C F4A -130.1(18) . . . . ? F2B B1 F4C F4A -127(2) . . . . ? F3B B1 F4C F4A -65(3) . . . . ? F1A B1 F4C F4A 116.8(18) . . . . ? F3A B1 F4C F4A -21(3) . . . . ? F1B B1 F4C F4A 124.3(18) . . . . ? F4B B1 F4C F4A 12.9(14) . . . . ? F3C B1 F4C F4B -11.7(14) . . . . ? F4A B1 F4C F4B -12.9(14) . . . . ? F2A B1 F4C F4B -143.0(7) . . . . ? F2B B1 F4C F4B -139.9(10) . . . . ? F3B B1 F4C F4B -77(2) . . . . ? F1A B1 F4C F4B 103.9(8) . . . . ? F3A B1 F4C F4B -33.9(17) . . . . ? F1B B1 F4C F4B 111.5(10) . . . . ? F3C B1 F4C F2B 128.2(11) . . . . ? F4A B1 F4C F2B 127(2) . . . . ? F2A B1 F4C F2B -3.1(8) . . . . ? F3B B1 F4C F2B 63(2) . . . . ? F1A B1 F4C F2B -116.2(7) . . . . ? F3A B1 F4C F2B 105.9(12) . . . . ? F1B B1 F4C F2B -108.6(9) . . . . ? F4B B1 F4C F2B 139.9(10) . . . . ? F2A F2B F4C F4A 59(3) . . . . ? B1 F2B F4C F4A 50.2(17) . . . . ? F2A F2B F4C F4B 44(3) . . . . ? B1 F2B F4C F4B 35.3(9) . . . . ? F2A F2B F4C B1 8(2) . . . . ? O1 C6 Fe1 C7 -165.5(16) . . . . ? O1 C6 Fe1 N3 105.8(16) . . . . ? O1 C6 Fe1 C2 -60.6(16) . . . . ? O1 C6 Fe1 C3 -22.2(16) . . . . ? O1 C6 Fe1 C4 6.6(16) . . . . ? O1 C6 Fe1 C1 -71.9(16) . . . . ? O1 C6 Fe1 C5 -8.9(17) . . . . ? N1 C7 Fe1 C6 -144.30(13) . . . . ? N2 C7 Fe1 C6 37.17(14) . . . . ? N1 C7 Fe1 N3 -54.28(13) . . . . ? N2 C7 Fe1 N3 127.19(13) . . . . ? N1 C7 Fe1 C2 115.22(13) . . . . ? N2 C7 Fe1 C2 -63.31(14) . . . . ? N1 C7 Fe1 C3 118.56(14) . . . . ? N2 C7 Fe1 C3 -59.97(18) . . . . ? N1 C7 Fe1 C4 48.79(18) . . . . ? N2 C7 Fe1 C4 -129.74(14) . . . . ? N1 C7 Fe1 C1 79.96(13) . . . . ? N2 C7 Fe1 C1 -98.57(14) . . . . ? N1 C7 Fe1 C5 46.98(14) . . . . ? N2 C7 Fe1 C5 -131.55(13) . . . . ? C1 C2 Fe1 C6 -167.47(10) . . . . ? C3 C2 Fe1 C6 75.78(11) . . . . ? C1 C2 Fe1 C7 -66.41(11) . . . . ? C3 C2 Fe1 C7 176.84(10) . . . . ? C1 C2 Fe1 N3 71.7(3) . . . . ? C3 C2 Fe1 N3 -45.0(3) . . . . ? C1 C2 Fe1 C3 116.74(15) . . . . ? C1 C2 Fe1 C4 79.68(11) . . . . ? C3 C2 Fe1 C4 -37.07(10) . . . . ? C3 C2 Fe1 C1 -116.74(15) . . . . ? C1 C2 Fe1 C5 36.48(10) . . . . ? C3 C2 Fe1 C5 -80.27(11) . . . . ? C4 C3 Fe1 C6 135.35(11) . . . . ? C2 C3 Fe1 C6 -106.07(11) . . . . ? C4 C3 Fe1 C7 -123.68(12) . . . . ? C2 C3 Fe1 C7 -5.10(16) . . . . ? C4 C3 Fe1 N3 47.22(13) . . . . ? C2 C3 Fe1 N3 165.80(9) . . . . ? C4 C3 Fe1 C2 -118.58(15) . . . . ? C2 C3 Fe1 C4 118.58(15) . . . . ? C4 C3 Fe1 C1 -80.44(11) . . . . ? C2 C3 Fe1 C1 38.14(10) . . . . ? C4 C3 Fe1 C5 -37.77(10) . . . . ? C2 C3 Fe1 C5 80.81(11) . . . . ? C3 C4 Fe1 C6 -50.26(12) . . . . ? C5 C4 Fe1 C6 -168.54(10) . . . . ? C3 C4 Fe1 C7 115.55(13) . . . . ? C5 C4 Fe1 C7 -2.73(16) . . . . ? C3 C4 Fe1 N3 -144.25(10) . . . . ? C5 C4 Fe1 N3 97.47(10) . . . . ? C3 C4 Fe1 C2 37.93(11) . . . . ? C5 C4 Fe1 C2 -80.35(11) . . . . ? C5 C4 Fe1 C3 -118.29(14) . . . . ? C3 C4 Fe1 C1 80.87(11) . . . . ? C5 C4 Fe1 C1 -37.41(10) . . . . ? C3 C4 Fe1 C5 118.29(14) . . . . ? C2 C1 Fe1 C6 17.92(15) . . . . ? C5 C1 Fe1 C6 137.76(11) . . . . ? C2 C1 Fe1 C7 116.64(10) . . . . ? C5 C1 Fe1 C7 -123.52(11) . . . . ? C2 C1 Fe1 N3 -158.86(9) . . . . ? C5 C1 Fe1 N3 -39.02(13) . . . . ? C5 C1 Fe1 C2 119.84(14) . . . . ? C2 C1 Fe1 C3 -38.92(10) . . . . ? C5 C1 Fe1 C3 80.92(11) . . . . ? C2 C1 Fe1 C4 -81.85(11) . . . . ? C5 C1 Fe1 C4 37.99(10) . . . . ? C2 C1 Fe1 C5 -119.84(14) . . . . ? C1 C5 Fe1 C6 -95.33(17) . . . . ? C4 C5 Fe1 C6 22.64(19) . . . . ? C1 C5 Fe1 C7 60.44(11) . . . . ? C4 C5 Fe1 C7 178.41(9) . . . . ? C1 C5 Fe1 N3 152.50(10) . . . . ? C4 C5 Fe1 N3 -89.53(10) . . . . ? C1 C5 Fe1 C2 -36.75(10) . . . . ? C4 C5 Fe1 C2 81.21(10) . . . . ? C1 C5 Fe1 C3 -80.60(11) . . . . ? C4 C5 Fe1 C3 37.36(10) . . . . ? C1 C5 Fe1 C4 -117.97(14) . . . . ? C4 C5 Fe1 C1 117.97(14) . . . . ? N2 C7 N1 C8 -0.63(16) . . . . ? Fe1 C7 N1 C8 -179.46(11) . . . . ? N2 C7 N1 C13 174.98(13) . . . . ? Fe1 C7 N1 C13 -3.8(2) . . . . ? C9 C8 N1 C7 0.21(18) . . . . ? C9 C8 N1 C13 -175.67(14) . . . . ? C15 C13 N1 C7 -109.85(17) . . . . ? C14 C13 N1 C7 125.66(16) . . . . ? C15 C13 N1 C8 65.33(18) . . . . ? C14 C13 N1 C8 -59.16(19) . . . . ? N1 C7 N2 C9 0.83(16) . . . . ? Fe1 C7 N2 C9 179.61(11) . . . . ? N1 C7 N2 C10 -178.94(13) . . . . ? Fe1 C7 N2 C10 -0.2(2) . . . . ? C8 C9 N2 C7 -0.73(18) . . . . ? C8 C9 N2 C10 179.05(14) . . . . ? C11 C10 N2 C7 122.61(16) . . . . ? C12 C10 N2 C7 -112.42(17) . . . . ? C11 C10 N2 C9 -57.13(19) . . . . ? C12 C10 N2 C9 67.83(19) . . . . ? C17 C16 N3 C20 -0.8(2) . . . . ? C17 C16 N3 Fe1 177.84(12) . . . . ? C19 C20 N3 C16 1.0(2) . . . . ? C19 C20 N3 Fe1 -177.78(13) . . . . ? C6 Fe1 N3 C16 -133.04(13) . . . . ? C7 Fe1 N3 C16 128.17(13) . . . . ? C2 Fe1 N3 C16 -11.3(3) . . . . ? C3 Fe1 N3 C16 -46.35(15) . . . . ? C4 Fe1 N3 C16 -18.64(14) . . . . ? C1 Fe1 N3 C16 44.72(16) . . . . ? C5 Fe1 N3 C16 21.10(14) . . . . ? C6 Fe1 N3 C20 45.61(13) . . . . ? C7 Fe1 N3 C20 -53.18(12) . . . . ? C2 Fe1 N3 C20 167.3(2) . . . . ? C3 Fe1 N3 C20 132.30(12) . . . . ? C4 Fe1 N3 C20 160.01(12) . . . . ? C1 Fe1 N3 C20 -136.63(12) . . . . ? C5 Fe1 N3 C20 -160.25(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.284 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.050 #################################################END # Attachment 'albrecht_cplx_3_4_9b_11_12.CIF' data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 726549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 Cl2 Fe2 I2 N4 O2' _chemical_formula_weight 1021.14 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' 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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6665(8) _cell_length_b 12.7160(7) _cell_length_c 15.2275(8) _cell_angle_alpha 66.698(4) _cell_angle_beta 87.838(5) _cell_angle_gamma 79.813(5) _cell_volume 2040.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35310 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 29.61 _exptl_crystal_description block _exptl_crystal_colour grenn _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.391 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.054 _exptl_absorpt_correction_T_max 0.483 _exptl_absorpt_process_details 'DIFrelABS in PLATON; Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26602 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.27 _reflns_number_total 10857 _reflns_number_gt 9449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.26 (STOE, 2005)' _computing_cell_refinement 'X-Area V1.26' _computing_data_reduction 'X-RED32 V1.26 (STOE, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.1300P)^2^+4.7658P] 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 10857 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.2312 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 -0.0720(7) -0.0056(7) 0.5945(5) 0.0699(17) Uani 1 1 d . . . H1 H -0.1483 -0.0031 0.5733 0.084 Uiso 1 1 d R . . C2 C 0.0071(7) -0.1054(6) 0.6512(5) 0.0610(14) Uani 1 1 d . . . H2 H -0.0078 -0.1826 0.6734 0.073 Uiso 1 1 d R . . C3 C 0.1078(6) -0.0731(7) 0.6684(5) 0.0658(16) Uani 1 1 d . . . H3 H 0.1739 -0.1238 0.7061 0.079 Uiso 1 1 d R . . C4 C 0.0954(8) 0.0495(8) 0.6208(6) 0.079(2) Uani 1 1 d . . . H4 H 0.1517 0.0962 0.6185 0.094 Uiso 1 1 d R . . C5 C -0.0183(10) 0.0897(6) 0.5746(5) 0.082(3) Uani 1 1 d . . . H5 H -0.0511 0.1686 0.5377 0.098 Uiso 1 1 d R . . C6 C -0.1374(6) -0.0759(5) 0.7859(5) 0.0563(13) Uani 1 1 d . . . C7 C -0.1138(5) 0.1584(5) 0.7206(4) 0.0497(11) Uani 1 1 d . . . C8 C -0.1535(6) 0.3501(5) 0.7003(5) 0.0579(13) Uani 1 1 d . . . H8 H -0.1414 0.4256 0.6913 0.070 Uiso 1 1 calc R . . C9 C -0.2550(6) 0.3161(5) 0.7057(5) 0.0616(14) Uani 1 1 d . . . H9 H -0.3297 0.3619 0.7026 0.074 Uiso 1 1 calc R . . C10 C -0.3233(5) 0.1327(5) 0.7305(5) 0.0584(13) Uani 1 1 d . . . C11 C -0.3762(6) 0.1316(6) 0.6521(6) 0.0704(17) Uani 1 1 d . . . C12 C -0.4654(7) 0.0661(8) 0.6680(8) 0.088(3) Uani 1 1 d . . . H12 H -0.5021 0.0612 0.6154 0.105 Uiso 1 1 calc R . . C13 C -0.5003(7) 0.0086(8) 0.7601(9) 0.094(3) Uani 1 1 d . . . C14 C -0.4496(6) 0.0190(6) 0.8364(7) 0.076(2) Uani 1 1 d . . . H14 H -0.4780 -0.0160 0.8987 0.091 Uiso 1 1 calc R . . C15 C -0.3600(6) 0.0782(5) 0.8238(5) 0.0650(16) Uani 1 1 d . . . C16 C -0.3435(8) 0.2016(8) 0.5511(6) 0.085(2) Uani 1 1 d . . . H16A H -0.3195 0.1496 0.5179 0.127 Uiso 1 1 calc R . . H16B H -0.2789 0.2405 0.5534 0.127 Uiso 1 1 calc R . . H16C H -0.4108 0.2600 0.5167 0.127 Uiso 1 1 calc R . . C17 C -0.5936(10) -0.0656(13) 0.7717(14) 0.150(7) Uani 1 1 d . . . H17A H -0.6188 -0.0585 0.7086 0.225 Uiso 1 1 calc R . . H17B H -0.6605 -0.0390 0.8032 0.225 Uiso 1 1 calc R . . H17C H -0.5616 -0.1472 0.8107 0.225 Uiso 1 1 calc R . . C18 C -0.3018(8) 0.0811(7) 0.9079(6) 0.077(2) Uani 1 1 d . . . H18A H -0.3117 0.1616 0.9025 0.115 Uiso 1 1 calc R . . H18B H -0.2185 0.0495 0.9098 0.115 Uiso 1 1 calc R . . H18C H -0.3367 0.0340 0.9667 0.115 Uiso 1 1 calc R . . C19 C 0.0566(5) 0.2601(5) 0.7126(4) 0.0497(10) Uani 1 1 d . . . H19A H 0.1041 0.1835 0.7220 0.060 Uiso 1 1 calc R . . H19B H 0.0773 0.3184 0.6511 0.060 Uiso 1 1 calc R . . C20 C 0.4136(9) 0.3561(10) 0.7115(8) 0.104(4) Uani 1 1 d . . . H20 H 0.4559 0.3353 0.7698 0.124 Uiso 1 1 d R . . C21 C 0.4132(7) 0.4578(8) 0.6281(7) 0.079(2) Uani 1 1 d . . . H21 H 0.4561 0.5178 0.6195 0.095 Uiso 1 1 d R . . C22 C 0.3387(9) 0.4539(9) 0.5618(7) 0.092(3) Uani 1 1 d . . . H22 H 0.3184 0.5109 0.4991 0.111 Uiso 1 1 d R . . C23 C 0.2994(12) 0.3471(13) 0.6045(13) 0.131(6) Uani 1 1 d . . . H23 H 0.2483 0.3211 0.5735 0.158 Uiso 1 1 d R . . C24 C 0.3400(13) 0.2904(9) 0.6940(12) 0.135(6) Uani 1 1 d . . . H24 H 0.3232 0.2176 0.7372 0.162 Uiso 1 1 d R . . C25 C 0.2607(7) 0.5647(6) 0.7165(6) 0.0679(17) Uani 1 1 d . . . C26 C 0.1495(5) 0.3687(4) 0.7887(4) 0.0502(11) Uani 1 1 d . . . C27 C 0.0346(6) 0.2427(5) 0.8816(4) 0.0541(12) Uani 1 1 d . . . H27 H -0.0154 0.1867 0.9008 0.065 Uiso 1 1 calc R . . C28 C 0.0755(5) 0.2903(5) 0.9356(4) 0.0528(11) Uani 1 1 d . . . H28 H 0.0595 0.2749 1.0008 0.063 Uiso 1 1 calc R . . C29 C 0.1972(5) 0.4337(5) 0.9167(4) 0.0514(11) Uani 1 1 d . . . C30 C 0.1356(6) 0.5416(5) 0.9078(5) 0.0602(14) Uani 1 1 d . . . C31 C 0.1842(8) 0.6032(6) 0.9498(7) 0.077(2) Uani 1 1 d . . . H31 H 0.1454 0.6789 0.9417 0.092 Uiso 1 1 calc R . . C32 C 0.2898(9) 0.5560(9) 1.0044(8) 0.090(3) Uani 1 1 d . . . C33 C 0.3494(7) 0.4482(8) 1.0103(7) 0.078(2) Uani 1 1 d . . . H33 H 0.4223 0.4169 1.0445 0.093 Uiso 1 1 calc R . . C34 C 0.3040(6) 0.3852(6) 0.9669(5) 0.0587(13) Uani 1 1 d . . . C35 C 0.0190(7) 0.5894(6) 0.8571(5) 0.0718(18) Uani 1 1 d . . . H35A H -0.0372 0.5405 0.8925 0.108 Uiso 1 1 calc R . . H35B H 0.0248 0.5903 0.7925 0.108 Uiso 1 1 calc R . . H35C H -0.0070 0.6689 0.8530 0.108 Uiso 1 1 calc R . . C36 C 0.3385(10) 0.6229(12) 1.0538(11) 0.120(5) Uani 1 1 d . . . H36A H 0.2750 0.6583 1.0828 0.181 Uiso 1 1 calc R . . H36B H 0.3756 0.6840 1.0067 0.181 Uiso 1 1 calc R . . H36C H 0.3962 0.5695 1.1037 0.181 Uiso 1 1 calc R . . C37 C 0.3665(6) 0.2659(6) 0.9801(6) 0.0658(15) Uani 1 1 d . . . H37A H 0.3263 0.2074 1.0269 0.099 Uiso 1 1 calc R . . H37B H 0.4468 0.2550 1.0031 0.099 Uiso 1 1 calc R . . H37C H 0.3671 0.2575 0.9188 0.099 Uiso 1 1 calc R . . Fe1 Fe -0.03513(7) 0.00880(6) 0.72160(5) 0.04708(18) Uani 1 1 d . . . Fe2 Fe 0.24607(9) 0.45054(7) 0.68271(7) 0.0588(2) Uani 1 1 d . . . I1 I 0.08400(4) -0.04797(3) 0.88075(3) 0.05636(14) Uani 1 1 d . . . I2 I 0.05704(6) 0.58259(4) 0.58303(4) 0.07848(18) Uani 1 1 d . . . N1 N -0.0674(4) 0.2545(4) 0.7102(3) 0.0506(9) Uani 1 1 d . . . N2 N -0.2313(4) 0.1997(4) 0.7170(4) 0.0541(10) Uani 1 1 d . . . N3 N 0.0808(5) 0.2925(4) 0.7910(3) 0.0504(9) Uani 1 1 d . . . N4 N 0.1450(4) 0.3657(4) 0.8789(3) 0.0482(9) Uani 1 1 d . . . O1 O -0.1961(4) -0.1425(4) 0.8245(4) 0.0680(12) Uani 1 1 d . . . O2 O 0.2802(6) 0.6437(5) 0.7288(5) 0.0873(18) 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 0.079(4) 0.088(5) 0.049(3) -0.037(3) -0.002(3) -0.004(4) C2 0.080(4) 0.055(3) 0.056(3) -0.030(3) 0.015(3) -0.015(3) C3 0.061(3) 0.079(4) 0.068(4) -0.046(3) 0.013(3) 0.001(3) C4 0.097(6) 0.091(5) 0.073(5) -0.051(4) 0.048(4) -0.046(5) C5 0.144(8) 0.050(3) 0.040(3) -0.015(2) 0.023(4) 0.001(4) C6 0.061(3) 0.047(3) 0.058(3) -0.023(2) 0.005(2) 0.001(2) C7 0.057(3) 0.046(2) 0.040(2) -0.0143(19) 0.0016(19) 0.000(2) C8 0.058(3) 0.048(3) 0.064(3) -0.022(2) 0.000(2) -0.002(2) C9 0.060(3) 0.050(3) 0.069(4) -0.021(3) 0.005(3) 0.000(2) C10 0.047(3) 0.048(3) 0.072(4) -0.019(3) 0.000(2) 0.000(2) C11 0.061(4) 0.057(3) 0.080(5) -0.017(3) -0.012(3) 0.002(3) C12 0.064(4) 0.077(5) 0.114(7) -0.029(5) -0.029(4) -0.006(4) C13 0.056(4) 0.067(4) 0.140(9) -0.021(5) -0.001(5) -0.008(3) C14 0.052(3) 0.055(3) 0.097(5) -0.012(3) 0.011(3) 0.004(3) C15 0.061(3) 0.048(3) 0.075(4) -0.018(3) 0.014(3) 0.001(2) C16 0.084(5) 0.091(6) 0.069(4) -0.021(4) -0.019(4) -0.012(4) C17 0.062(5) 0.124(10) 0.237(19) -0.036(10) -0.026(8) -0.030(6) C18 0.096(6) 0.067(4) 0.063(4) -0.026(3) 0.022(4) -0.011(4) C19 0.057(3) 0.045(2) 0.047(2) -0.019(2) 0.007(2) -0.008(2) C20 0.071(5) 0.103(7) 0.091(6) -0.009(5) 0.032(4) 0.021(5) C21 0.071(4) 0.080(5) 0.086(5) -0.035(4) 0.036(4) -0.015(4) C22 0.102(7) 0.100(6) 0.082(6) -0.042(5) 0.052(5) -0.033(5) C23 0.126(9) 0.138(10) 0.208(15) -0.139(12) 0.106(11) -0.072(8) C24 0.140(10) 0.061(5) 0.166(12) -0.021(6) 0.109(10) 0.000(6) C25 0.070(4) 0.059(3) 0.073(4) -0.025(3) 0.026(3) -0.015(3) C26 0.057(3) 0.038(2) 0.053(3) -0.018(2) 0.010(2) -0.0057(19) C27 0.063(3) 0.053(3) 0.048(3) -0.021(2) 0.013(2) -0.016(2) C28 0.062(3) 0.051(3) 0.044(3) -0.017(2) 0.009(2) -0.010(2) C29 0.055(3) 0.044(2) 0.058(3) -0.024(2) 0.010(2) -0.011(2) C30 0.072(4) 0.043(3) 0.064(3) -0.022(2) 0.024(3) -0.010(2) C31 0.084(5) 0.059(4) 0.104(6) -0.048(4) 0.038(4) -0.025(3) C32 0.094(6) 0.091(6) 0.124(8) -0.074(6) 0.036(5) -0.044(5) C33 0.068(4) 0.090(5) 0.100(6) -0.059(5) 0.013(4) -0.027(4) C34 0.056(3) 0.057(3) 0.068(4) -0.030(3) 0.008(3) -0.011(2) C35 0.081(4) 0.052(3) 0.068(4) -0.019(3) 0.010(3) 0.011(3) C36 0.096(7) 0.147(10) 0.191(13) -0.132(10) 0.046(8) -0.059(7) C37 0.058(3) 0.060(3) 0.079(4) -0.030(3) -0.003(3) -0.005(3) Fe1 0.0548(4) 0.0433(4) 0.0425(4) -0.0182(3) 0.0085(3) -0.0056(3) Fe2 0.0687(5) 0.0440(4) 0.0598(5) -0.0180(3) 0.0231(4) -0.0106(3) I1 0.0655(2) 0.0513(2) 0.0471(2) -0.01716(16) 0.00123(15) -0.00276(16) I2 0.1075(4) 0.0539(3) 0.0597(3) -0.00618(19) -0.0032(2) -0.0158(2) N1 0.057(2) 0.045(2) 0.048(2) -0.0190(18) 0.0018(18) -0.0043(18) N2 0.052(2) 0.047(2) 0.054(3) -0.0160(19) 0.0032(19) 0.0015(18) N3 0.063(3) 0.043(2) 0.044(2) -0.0171(17) 0.0083(18) -0.0095(18) N4 0.054(2) 0.041(2) 0.050(2) -0.0191(17) 0.0067(18) -0.0061(17) O1 0.066(3) 0.051(2) 0.080(3) -0.019(2) 0.023(2) -0.0115(19) O2 0.102(4) 0.069(3) 0.105(4) -0.040(3) 0.040(4) -0.041(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.384(12) . ? C1 C2 1.409(10) . ? C1 Fe1 2.081(6) . ? C1 H1 0.9501 . ? C2 C3 1.377(10) . ? C2 Fe1 2.106(6) . ? C2 H2 0.9500 . ? C3 C4 1.419(12) . ? C3 Fe1 2.116(6) . ? C3 H3 0.9500 . ? C4 C5 1.436(14) . ? C4 Fe1 2.102(6) . ? C4 H4 0.9501 . ? C5 Fe1 2.080(6) . ? C5 H5 0.9499 . ? C6 O1 1.146(8) . ? C6 Fe1 1.753(7) . ? C7 N2 1.373(7) . ? C7 N1 1.374(7) . ? C7 Fe1 1.955(5) . ? C8 C9 1.319(10) . ? C8 N1 1.394(7) . ? C8 H8 0.9500 . ? C9 N2 1.398(8) . ? C9 H9 0.9500 . ? C10 C11 1.371(10) . ? C10 C15 1.400(10) . ? C10 N2 1.445(8) . ? C11 C12 1.401(12) . ? C11 C16 1.515(12) . ? C12 C13 1.386(15) . ? C12 H12 0.9500 . ? C13 C14 1.385(15) . ? C13 C17 1.524(14) . ? C14 C15 1.358(11) . ? C14 H14 0.9500 . ? C15 C18 1.488(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N3 1.461(7) . ? C19 N1 1.464(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.40(2) . ? C20 C21 1.408(13) . ? C20 Fe2 2.067(9) . ? C20 H20 0.9501 . ? C21 C22 1.378(15) . ? C21 Fe2 2.094(7) . ? C21 H21 0.9501 . ? C22 C23 1.406(15) . ? C22 Fe2 2.089(7) . ? C22 H22 0.9500 . ? C23 C24 1.32(2) . ? C23 Fe2 2.104(8) . ? C23 H23 0.9500 . ? C24 Fe2 2.079(9) . ? C24 H24 0.9501 . ? C25 O2 1.152(9) . ? C25 Fe2 1.756(7) . ? C26 N3 1.352(7) . ? C26 N4 1.357(7) . ? C26 Fe2 1.977(6) . ? C27 C28 1.340(8) . ? C27 N3 1.403(7) . ? C27 H27 0.9500 . ? C28 N4 1.375(7) . ? C28 H28 0.9500 . ? C29 C30 1.389(8) . ? C29 C34 1.395(9) . ? C29 N4 1.434(7) . ? C30 C31 1.387(10) . ? C30 C35 1.494(11) . ? C31 C32 1.410(15) . ? C31 H31 0.9500 . ? C32 C33 1.393(12) . ? C32 C36 1.525(12) . ? C33 C34 1.399(9) . ? C33 H33 0.9500 . ? C34 C37 1.499(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Fe1 I1 2.6155(9) . ? Fe2 I2 2.6293(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.6(7) . . ? C5 C1 Fe1 70.5(4) . . ? C2 C1 Fe1 71.3(4) . . ? C5 C1 H1 125.6 . . ? C2 C1 H1 126.9 . . ? Fe1 C1 H1 123.8 . . ? C3 C2 C1 109.5(6) . . ? C3 C2 Fe1 71.3(3) . . ? C1 C2 Fe1 69.4(3) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 124.4 . . ? Fe1 C2 H2 125.8 . . ? C2 C3 C4 108.0(7) . . ? C2 C3 Fe1 70.6(4) . . ? C4 C3 Fe1 69.8(4) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 125.8 . . ? Fe1 C3 H3 124.6 . . ? C3 C4 C5 106.5(7) . . ? C3 C4 Fe1 70.9(4) . . ? C5 C4 Fe1 69.1(4) . . ? C3 C4 H4 127.1 . . ? C5 C4 H4 126.4 . . ? Fe1 C4 H4 126.0 . . ? C1 C5 C4 108.3(7) . . ? C1 C5 Fe1 70.6(4) . . ? C4 C5 Fe1 70.7(4) . . ? C1 C5 H5 126.2 . . ? C4 C5 H5 125.5 . . ? Fe1 C5 H5 123.5 . . ? O1 C6 Fe1 171.0(5) . . ? N2 C7 N1 101.9(5) . . ? N2 C7 Fe1 128.5(4) . . ? N1 C7 Fe1 129.1(4) . . ? C9 C8 N1 107.2(5) . . ? C9 C8 H8 126.4 . . ? N1 C8 H8 126.4 . . ? C8 C9 N2 106.7(5) . . ? C8 C9 H9 126.6 . . ? N2 C9 H9 126.6 . . ? C11 C10 C15 122.8(7) . . ? C11 C10 N2 119.3(6) . . ? C15 C10 N2 117.8(6) . . ? C10 C11 C12 117.7(8) . . ? C10 C11 C16 121.9(7) . . ? C12 C11 C16 120.4(8) . . ? C13 C12 C11 120.2(9) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 119.9(8) . . ? C14 C13 C17 123.2(12) . . ? C12 C13 C17 116.9(12) . . ? C15 C14 C13 121.3(8) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 118.0(8) . . ? C14 C15 C18 120.1(7) . . ? C10 C15 C18 121.9(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 N1 109.0(4) . . ? N3 C19 H19A 109.9 . . ? N1 C19 H19A 109.9 . . ? N3 C19 H19B 109.9 . . ? N1 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C24 C20 C21 108.0(11) . . ? C24 C20 Fe2 70.8(6) . . ? C21 C20 Fe2 71.3(5) . . ? C24 C20 H20 125.5 . . ? C21 C20 H20 126.5 . . ? Fe2 C20 H20 123.4 . . ? C22 C21 C20 107.2(10) . . ? C22 C21 Fe2 70.6(5) . . ? C20 C21 Fe2 69.2(5) . . ? C22 C21 H21 126.6 . . ? C20 C21 H21 126.2 . . ? Fe2 C21 H21 125.1 . . ? C21 C22 C23 106.4(11) . . ? C21 C22 Fe2 71.0(5) . . ? C23 C22 Fe2 71.0(5) . . ? C21 C22 H22 127.3 . . ? C23 C22 H22 126.2 . . ? Fe2 C22 H22 123.8 . . ? C24 C23 C22 110.9(13) . . ? C24 C23 Fe2 70.5(6) . . ? C22 C23 Fe2 69.8(5) . . ? C24 C23 H23 125.1 . . ? C22 C23 H23 124.0 . . ? Fe2 C23 H23 125.1 . . ? C23 C24 C20 107.4(9) . . ? C23 C24 Fe2 72.6(6) . . ? C20 C24 Fe2 69.8(6) . . ? C23 C24 H24 125.7 . . ? C20 C24 H24 126.9 . . ? Fe2 C24 H24 124.2 . . ? O2 C25 Fe2 170.9(6) . . ? N3 C26 N4 103.5(5) . . ? N3 C26 Fe2 127.4(4) . . ? N4 C26 Fe2 128.8(4) . . ? C28 C27 N3 105.9(5) . . ? C28 C27 H27 127.1 . . ? N3 C27 H27 127.1 . . ? C27 C28 N4 107.0(5) . . ? C27 C28 H28 126.5 . . ? N4 C28 H28 126.5 . . ? C30 C29 C34 122.6(6) . . ? C30 C29 N4 118.7(6) . . ? C34 C29 N4 118.5(5) . . ? C31 C30 C29 118.0(7) . . ? C31 C30 C35 120.5(6) . . ? C29 C30 C35 121.5(6) . . ? C30 C31 C32 121.5(7) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 118.5(7) . . ? C33 C32 C36 121.0(11) . . ? C31 C32 C36 120.6(9) . . ? C32 C33 C34 121.3(8) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C29 C34 C33 118.0(6) . . ? C29 C34 C37 122.0(6) . . ? C33 C34 C37 119.9(7) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C6 Fe1 C7 98.1(2) . . ? C6 Fe1 C5 129.7(4) . . ? C7 Fe1 C5 88.6(2) . . ? C6 Fe1 C1 93.7(3) . . ? C7 Fe1 C1 110.5(3) . . ? C5 Fe1 C1 38.9(3) . . ? C6 Fe1 C4 153.5(3) . . ? C7 Fe1 C4 105.1(3) . . ? C5 Fe1 C4 40.2(4) . . ? C1 Fe1 C4 66.3(3) . . ? C6 Fe1 C2 88.4(3) . . ? C7 Fe1 C2 149.7(3) . . ? C5 Fe1 C2 65.1(3) . . ? C1 Fe1 C2 39.3(3) . . ? C4 Fe1 C2 65.0(3) . . ? C6 Fe1 C3 117.6(3) . . ? C7 Fe1 C3 144.0(3) . . ? C5 Fe1 C3 66.1(3) . . ? C1 Fe1 C3 65.7(3) . . ? C4 Fe1 C3 39.3(3) . . ? C2 Fe1 C3 38.1(3) . . ? C6 Fe1 I1 89.9(2) . . ? C7 Fe1 I1 94.03(16) . . ? C5 Fe1 I1 139.6(3) . . ? C1 Fe1 I1 154.4(2) . . ? C4 Fe1 I1 101.0(3) . . ? C2 Fe1 I1 115.6(2) . . ? C3 Fe1 I1 90.2(2) . . ? C25 Fe2 C26 98.1(3) . . ? C25 Fe2 C20 100.6(5) . . ? C26 Fe2 C20 107.3(3) . . ? C25 Fe2 C24 138.9(7) . . ? C26 Fe2 C24 89.3(3) . . ? C20 Fe2 C24 39.4(6) . . ? C25 Fe2 C22 113.5(4) . . ? C26 Fe2 C22 148.3(3) . . ? C20 Fe2 C22 65.3(5) . . ? C24 Fe2 C22 65.3(5) . . ? C25 Fe2 C21 88.2(3) . . ? C26 Fe2 C21 146.7(3) . . ? C20 Fe2 C21 39.6(4) . . ? C24 Fe2 C21 65.9(4) . . ? C22 Fe2 C21 38.5(4) . . ? C25 Fe2 C23 151.3(4) . . ? C26 Fe2 C23 109.2(4) . . ? C20 Fe2 C23 63.4(6) . . ? C24 Fe2 C23 36.9(6) . . ? C22 Fe2 C23 39.2(4) . . ? C21 Fe2 C23 64.2(4) . . ? C25 Fe2 I2 87.7(3) . . ? C26 Fe2 I2 90.16(17) . . ? C20 Fe2 I2 159.2(3) . . ? C24 Fe2 I2 132.8(6) . . ? C22 Fe2 I2 93.9(4) . . ? C21 Fe2 I2 122.9(3) . . ? C23 Fe2 I2 100.5(5) . . ? C7 N1 C8 112.0(5) . . ? C7 N1 C19 126.2(5) . . ? C8 N1 C19 121.7(5) . . ? C7 N2 C9 112.1(5) . . ? C7 N2 C10 126.2(5) . . ? C9 N2 C10 121.5(5) . . ? C26 N3 C27 111.5(5) . . ? C26 N3 C19 126.6(5) . . ? C27 N3 C19 121.8(5) . . ? C26 N4 C28 112.1(5) . . ? C26 N4 C29 128.3(5) . . ? C28 N4 C29 119.5(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 C5 C1 C2 C3 1.3(7) . . . . ? Fe1 C1 C2 C3 -60.2(5) . . . . ? C5 C1 C2 Fe1 61.5(4) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? Fe1 C2 C3 C4 -60.1(4) . . . . ? C1 C2 C3 Fe1 59.0(4) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? Fe1 C3 C4 C5 -60.2(4) . . . . ? C2 C3 C4 Fe1 60.6(4) . . . . ? C2 C1 C5 C4 -1.0(7) . . . . ? Fe1 C1 C5 C4 61.0(5) . . . . ? C2 C1 C5 Fe1 -62.0(4) . . . . ? C3 C4 C5 C1 0.4(7) . . . . ? Fe1 C4 C5 C1 -60.9(5) . . . . ? C3 C4 C5 Fe1 61.4(4) . . . . ? N1 C8 C9 N2 -1.2(7) . . . . ? C15 C10 C11 C12 -4.4(10) . . . . ? N2 C10 C11 C12 -179.7(6) . . . . ? C15 C10 C11 C16 173.4(7) . . . . ? N2 C10 C11 C16 -1.9(10) . . . . ? C10 C11 C12 C13 2.2(12) . . . . ? C16 C11 C12 C13 -175.6(8) . . . . ? C11 C12 C13 C14 2.2(13) . . . . ? C11 C12 C13 C17 -177.0(9) . . . . ? C12 C13 C14 C15 -4.6(12) . . . . ? C17 C13 C14 C15 174.5(9) . . . . ? C13 C14 C15 C10 2.5(10) . . . . ? C13 C14 C15 C18 -175.8(7) . . . . ? C11 C10 C15 C14 2.1(9) . . . . ? N2 C10 C15 C14 177.5(5) . . . . ? C11 C10 C15 C18 -179.6(6) . . . . ? N2 C10 C15 C18 -4.3(9) . . . . ? C24 C20 C21 C22 0.9(9) . . . . ? Fe2 C20 C21 C22 -60.7(6) . . . . ? C24 C20 C21 Fe2 61.6(6) . . . . ? C20 C21 C22 C23 -2.8(9) . . . . ? Fe2 C21 C22 C23 -62.5(6) . . . . ? C20 C21 C22 Fe2 59.8(5) . . . . ? C21 C22 C23 C24 3.9(11) . . . . ? Fe2 C22 C23 C24 -58.7(7) . . . . ? C21 C22 C23 Fe2 62.5(6) . . . . ? C22 C23 C24 C20 -3.3(11) . . . . ? Fe2 C23 C24 C20 -61.5(6) . . . . ? C22 C23 C24 Fe2 58.3(7) . . . . ? C21 C20 C24 C23 1.4(10) . . . . ? Fe2 C20 C24 C23 63.3(7) . . . . ? C21 C20 C24 Fe2 -61.9(6) . . . . ? N3 C27 C28 N4 -0.5(7) . . . . ? C34 C29 C30 C31 0.8(9) . . . . ? N4 C29 C30 C31 176.2(6) . . . . ? C34 C29 C30 C35 -177.5(6) . . . . ? N4 C29 C30 C35 -2.0(9) . . . . ? C29 C30 C31 C32 -3.3(11) . . . . ? C35 C30 C31 C32 175.0(8) . . . . ? C30 C31 C32 C33 4.2(13) . . . . ? C30 C31 C32 C36 -177.1(9) . . . . ? C31 C32 C33 C34 -2.7(14) . . . . ? C36 C32 C33 C34 178.6(9) . . . . ? C30 C29 C34 C33 0.7(10) . . . . ? N4 C29 C34 C33 -174.8(6) . . . . ? C30 C29 C34 C37 176.9(6) . . . . ? N4 C29 C34 C37 1.4(9) . . . . ? C32 C33 C34 C29 0.3(12) . . . . ? C32 C33 C34 C37 -176.0(8) . . . . ? O1 C6 Fe1 C7 170(4) . . . . ? O1 C6 Fe1 C5 75(4) . . . . ? O1 C6 Fe1 C1 58(4) . . . . ? O1 C6 Fe1 C4 19(4) . . . . ? O1 C6 Fe1 C2 19(4) . . . . ? O1 C6 Fe1 C3 -6(4) . . . . ? O1 C6 Fe1 I1 -96(4) . . . . ? N2 C7 Fe1 C6 -33.4(5) . . . . ? N1 C7 Fe1 C6 156.4(5) . . . . ? N2 C7 Fe1 C5 96.5(6) . . . . ? N1 C7 Fe1 C5 -73.7(6) . . . . ? N2 C7 Fe1 C1 63.7(6) . . . . ? N1 C7 Fe1 C1 -106.5(5) . . . . ? N2 C7 Fe1 C4 133.6(5) . . . . ? N1 C7 Fe1 C4 -36.6(6) . . . . ? N2 C7 Fe1 C2 67.6(7) . . . . ? N1 C7 Fe1 C2 -102.6(7) . . . . ? N2 C7 Fe1 C3 140.2(5) . . . . ? N1 C7 Fe1 C3 -30.0(7) . . . . ? N2 C7 Fe1 I1 -123.9(5) . . . . ? N1 C7 Fe1 I1 65.9(5) . . . . ? C1 C5 Fe1 C6 -26.6(6) . . . . ? C4 C5 Fe1 C6 -145.0(5) . . . . ? C1 C5 Fe1 C7 -126.0(5) . . . . ? C4 C5 Fe1 C7 115.5(5) . . . . ? C4 C5 Fe1 C1 -118.4(6) . . . . ? C1 C5 Fe1 C4 118.4(6) . . . . ? C1 C5 Fe1 C2 38.4(5) . . . . ? C4 C5 Fe1 C2 -80.0(5) . . . . ? C1 C5 Fe1 C3 80.3(5) . . . . ? C4 C5 Fe1 C3 -38.1(4) . . . . ? C1 C5 Fe1 I1 139.4(4) . . . . ? C4 C5 Fe1 I1 20.9(6) . . . . ? C5 C1 Fe1 C6 159.8(5) . . . . ? C2 C1 Fe1 C6 -82.9(5) . . . . ? C5 C1 Fe1 C7 59.7(6) . . . . ? C2 C1 Fe1 C7 176.9(4) . . . . ? C2 C1 Fe1 C5 117.2(7) . . . . ? C5 C1 Fe1 C4 -38.3(5) . . . . ? C2 C1 Fe1 C4 79.0(5) . . . . ? C5 C1 Fe1 C2 -117.2(7) . . . . ? C5 C1 Fe1 C3 -81.5(6) . . . . ? C2 C1 Fe1 C3 35.7(4) . . . . ? C5 C1 Fe1 I1 -102.6(7) . . . . ? C2 C1 Fe1 I1 14.6(9) . . . . ? C3 C4 Fe1 C6 -36.1(11) . . . . ? C5 C4 Fe1 C6 81.0(9) . . . . ? C3 C4 Fe1 C7 173.9(4) . . . . ? C5 C4 Fe1 C7 -69.1(5) . . . . ? C3 C4 Fe1 C5 -117.1(6) . . . . ? C3 C4 Fe1 C1 -80.0(5) . . . . ? C5 C4 Fe1 C1 37.1(4) . . . . ? C3 C4 Fe1 C2 -36.7(4) . . . . ? C5 C4 Fe1 C2 80.4(5) . . . . ? C5 C4 Fe1 C3 117.1(6) . . . . ? C3 C4 Fe1 I1 76.6(5) . . . . ? C5 C4 Fe1 I1 -166.3(4) . . . . ? C3 C2 Fe1 C6 -141.9(5) . . . . ? C1 C2 Fe1 C6 97.8(5) . . . . ? C3 C2 Fe1 C7 114.6(6) . . . . ? C1 C2 Fe1 C7 -5.7(8) . . . . ? C3 C2 Fe1 C5 82.4(5) . . . . ? C1 C2 Fe1 C5 -37.9(5) . . . . ? C3 C2 Fe1 C1 120.3(6) . . . . ? C3 C2 Fe1 C4 37.9(5) . . . . ? C1 C2 Fe1 C4 -82.4(6) . . . . ? C1 C2 Fe1 C3 -120.3(6) . . . . ? C3 C2 Fe1 I1 -52.7(5) . . . . ? C1 C2 Fe1 I1 -173.0(4) . . . . ? C2 C3 Fe1 C6 44.1(5) . . . . ? C4 C3 Fe1 C6 162.7(5) . . . . ? C2 C3 Fe1 C7 -128.7(5) . . . . ? C4 C3 Fe1 C7 -10.1(7) . . . . ? C2 C3 Fe1 C5 -79.7(5) . . . . ? C4 C3 Fe1 C5 38.9(5) . . . . ? C2 C3 Fe1 C1 -36.9(4) . . . . ? C4 C3 Fe1 C1 81.7(6) . . . . ? C2 C3 Fe1 C4 -118.6(7) . . . . ? C4 C3 Fe1 C2 118.6(7) . . . . ? C2 C3 Fe1 I1 134.1(4) . . . . ? C4 C3 Fe1 I1 -107.3(5) . . . . ? O2 C25 Fe2 C26 174(5) . . . . ? O2 C25 Fe2 C20 65(5) . . . . ? O2 C25 Fe2 C24 76(5) . . . . ? O2 C25 Fe2 C22 -3(5) . . . . ? O2 C25 Fe2 C21 27(5) . . . . ? O2 C25 Fe2 C23 12(6) . . . . ? O2 C25 Fe2 I2 -96(5) . . . . ? N3 C26 Fe2 C25 159.6(6) . . . . ? N4 C26 Fe2 C25 -27.9(6) . . . . ? N3 C26 Fe2 C20 -96.6(7) . . . . ? N4 C26 Fe2 C20 75.9(7) . . . . ? N3 C26 Fe2 C24 -61.0(8) . . . . ? N4 C26 Fe2 C24 111.5(8) . . . . ? N3 C26 Fe2 C22 -25.8(10) . . . . ? N4 C26 Fe2 C22 146.7(8) . . . . ? N3 C26 Fe2 C21 -101.3(7) . . . . ? N4 C26 Fe2 C21 71.2(7) . . . . ? N3 C26 Fe2 C23 -29.4(8) . . . . ? N4 C26 Fe2 C23 143.1(7) . . . . ? N3 C26 Fe2 I2 71.8(5) . . . . ? N4 C26 Fe2 I2 -115.7(5) . . . . ? C24 C20 Fe2 C25 168.4(7) . . . . ? C21 C20 Fe2 C25 -73.9(7) . . . . ? C24 C20 Fe2 C26 66.4(8) . . . . ? C21 C20 Fe2 C26 -175.9(6) . . . . ? C21 C20 Fe2 C24 117.6(10) . . . . ? C24 C20 Fe2 C22 -80.5(8) . . . . ? C21 C20 Fe2 C22 37.2(6) . . . . ? C24 C20 Fe2 C21 -117.6(10) . . . . ? C24 C20 Fe2 C23 -36.8(7) . . . . ? C21 C20 Fe2 C23 80.8(7) . . . . ? C24 C20 Fe2 I2 -79.2(13) . . . . ? C21 C20 Fe2 I2 38.5(16) . . . . ? C23 C24 Fe2 C25 -134.1(9) . . . . ? C20 C24 Fe2 C25 -17.4(10) . . . . ? C23 C24 Fe2 C26 124.4(8) . . . . ? C20 C24 Fe2 C26 -118.9(7) . . . . ? C23 C24 Fe2 C20 -116.6(9) . . . . ? C23 C24 Fe2 C22 -36.1(7) . . . . ? C20 C24 Fe2 C22 80.6(7) . . . . ? C23 C24 Fe2 C21 -78.5(7) . . . . ? C20 C24 Fe2 C21 38.2(6) . . . . ? C20 C24 Fe2 C23 116.6(9) . . . . ? C23 C24 Fe2 I2 34.9(9) . . . . ? C20 C24 Fe2 I2 151.6(6) . . . . ? C21 C22 Fe2 C25 53.0(7) . . . . ? C23 C22 Fe2 C25 168.8(9) . . . . ? C21 C22 Fe2 C26 -121.2(7) . . . . ? C23 C22 Fe2 C26 -5.4(13) . . . . ? C21 C22 Fe2 C20 -38.2(7) . . . . ? C23 C22 Fe2 C20 77.6(10) . . . . ? C21 C22 Fe2 C24 -81.8(9) . . . . ? C23 C22 Fe2 C24 34.0(10) . . . . ? C23 C22 Fe2 C21 115.8(11) . . . . ? C21 C22 Fe2 C23 -115.8(11) . . . . ? C21 C22 Fe2 I2 142.2(5) . . . . ? C23 C22 Fe2 I2 -102.0(9) . . . . ? C22 C21 Fe2 C25 -132.9(6) . . . . ? C20 C21 Fe2 C25 109.1(8) . . . . ? C22 C21 Fe2 C26 125.1(7) . . . . ? C20 C21 Fe2 C26 7.1(10) . . . . ? C22 C21 Fe2 C20 118.0(10) . . . . ? C22 C21 Fe2 C24 80.0(8) . . . . ? C20 C21 Fe2 C24 -38.0(9) . . . . ? C20 C21 Fe2 C22 -118.0(10) . . . . ? C22 C21 Fe2 C23 39.2(8) . . . . ? C20 C21 Fe2 C23 -78.8(9) . . . . ? C22 C21 Fe2 I2 -46.7(6) . . . . ? C20 C21 Fe2 I2 -164.7(7) . . . . ? C24 C23 Fe2 C25 100.4(14) . . . . ? C22 C23 Fe2 C25 -21.8(18) . . . . ? C24 C23 Fe2 C26 -60.8(9) . . . . ? C22 C23 Fe2 C26 177.0(8) . . . . ? C24 C23 Fe2 C20 39.4(8) . . . . ? C22 C23 Fe2 C20 -82.8(8) . . . . ? C22 C23 Fe2 C24 -122.2(13) . . . . ? C24 C23 Fe2 C22 122.2(13) . . . . ? C24 C23 Fe2 C21 83.7(9) . . . . ? C22 C23 Fe2 C21 -38.5(7) . . . . ? C24 C23 Fe2 I2 -154.7(8) . . . . ? C22 C23 Fe2 I2 83.1(8) . . . . ? N2 C7 N1 C8 -0.3(6) . . . . ? Fe1 C7 N1 C8 171.9(4) . . . . ? N2 C7 N1 C19 177.3(5) . . . . ? Fe1 C7 N1 C19 -10.5(8) . . . . ? C9 C8 N1 C7 1.0(7) . . . . ? C9 C8 N1 C19 -176.7(5) . . . . ? N3 C19 N1 C7 -119.7(5) . . . . ? N3 C19 N1 C8 57.7(7) . . . . ? N1 C7 N2 C9 -0.5(6) . . . . ? Fe1 C7 N2 C9 -172.7(4) . . . . ? N1 C7 N2 C10 -175.8(6) . . . . ? Fe1 C7 N2 C10 11.9(9) . . . . ? C8 C9 N2 C7 1.1(8) . . . . ? C8 C9 N2 C10 176.7(6) . . . . ? C11 C10 N2 C7 -95.2(7) . . . . ? C15 C10 N2 C7 89.3(7) . . . . ? C11 C10 N2 C9 89.9(8) . . . . ? C15 C10 N2 C9 -85.6(7) . . . . ? N4 C26 N3 C27 -0.1(6) . . . . ? Fe2 C26 N3 C27 173.9(4) . . . . ? N4 C26 N3 C19 -178.6(5) . . . . ? Fe2 C26 N3 C19 -4.7(8) . . . . ? C28 C27 N3 C26 0.4(7) . . . . ? C28 C27 N3 C19 179.0(5) . . . . ? N1 C19 N3 C26 -137.8(5) . . . . ? N1 C19 N3 C27 43.8(7) . . . . ? N3 C26 N4 C28 -0.2(6) . . . . ? Fe2 C26 N4 C28 -174.1(4) . . . . ? N3 C26 N4 C29 -176.7(5) . . . . ? Fe2 C26 N4 C29 9.5(8) . . . . ? C27 C28 N4 C26 0.5(7) . . . . ? C27 C28 N4 C29 177.3(5) . . . . ? C30 C29 N4 C26 87.3(7) . . . . ? C34 C29 N4 C26 -97.1(7) . . . . ? C30 C29 N4 C28 -88.9(7) . . . . ? C34 C29 N4 C28 86.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.160 _refine_diff_density_min -3.559 _refine_diff_density_rms 0.157 # start Validation Reply Form _vrf_ABSTM02_Complex3 ; PROBLEM: The ratio of expected to reported Tmax/Tmin(RR') is < 0.50 RESPONSE: The crystals present an asymmetric shape and are strongly absorbing. The indexing of crystal faces was not successful related to the irregular shape of the crystal. As a result, no numerical absorption correction was done. ; _vrf_PLAT061_Complex3 ; PROBLEM: Tmax/Tmin Range Test RR' too Large ............. 0.21 RESPONSE: The crystals present an asymmetric shape and are strongly absorbing. The indexing of crystal faces was not successful related to the irregular shape of the crystal. As a result, no numerical absorption correction was done. ; # end Validation Reply Form #################################################END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 726550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Fe2 I2 N4 O4' _chemical_formula_weight 930.17 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' I I -0.4742 1.8119 '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 7.8161(13) _cell_length_b 9.7331(15) _cell_length_c 12.836(2) _cell_angle_alpha 99.738(13) _cell_angle_beta 104.479(13) _cell_angle_gamma 89.843(13) _cell_volume 931.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7659 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.56 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 458 _exptl_absorpt_coefficient_mu 2.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8252 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.18 _reflns_number_total 3307 _reflns_number_gt 2608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^] 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 3307 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 -0.4567(10) 1.1540(9) 0.8674(7) 0.066(2) Uani 1 1 d . . . H1 H -0.3911 1.1233 0.9316 0.079 Uiso 1 1 calc R . . C2 C -0.4917(9) 1.2932(8) 0.8562(6) 0.0601(18) Uani 1 1 d . . . H2 H -0.4547 1.3731 0.9114 0.072 Uiso 1 1 calc R . . C3 C -0.5902(9) 1.2929(7) 0.7501(6) 0.0548(16) Uani 1 1 d . . . H3 H -0.6310 1.3729 0.7194 0.066 Uiso 1 1 calc R . . C4 C -0.6187(8) 1.1546(7) 0.6962(6) 0.0556(17) Uani 1 1 d . . . H4 H -0.6846 1.1249 0.6228 0.067 Uiso 1 1 calc R . . C5 C -0.5357(9) 1.0674(7) 0.7668(7) 0.064(2) Uani 1 1 d . . . H5 H -0.5327 0.9687 0.7506 0.076 Uiso 1 1 calc R . . C6 C -0.2591(10) 1.3701(7) 0.7331(6) 0.0568(16) Uani 1 1 d . . . C7 C -0.1180(8) 1.1414(6) 0.8243(5) 0.0480(14) Uani 1 1 d . . . C8 C 0.1131(9) 1.0094(7) 0.8833(6) 0.0577(17) Uani 1 1 d . . . H8 H 0.1860 0.9314 0.8897 0.069 Uiso 1 1 calc R . . C9 C 0.1487(9) 1.1390(8) 0.9431(7) 0.0590(18) Uani 1 1 d . . . H9 H 0.2521 1.1697 0.9995 0.071 Uiso 1 1 calc R . . C10 C 0.0017(8) 1.3626(7) 0.9525(6) 0.0512(15) Uani 1 1 d . . . C11 C 0.0968(9) 1.4610(7) 0.9242(6) 0.0539(16) Uani 1 1 d . . . H11 H 0.1636 1.4341 0.8721 0.065 Uiso 1 1 alc R . . C12 C -0.0965(9) 1.4005(7) 1.0290(6) 0.0547(16) Uani 1 1 d . . . H12 H -0.1624 1.3318 1.0488 0.066 Uiso 1 1 calc R . . C13 C -0.1298(10) 0.8884(6) 0.7322(7) 0.0585(17) Uani 1 1 d . . . H13A H -0.2552 0.9044 0.6987 0.070 Uiso 1 1 calc R . . H13B H -0.1269 0.8084 0.7710 0.070 Uiso 1 1 calc R . . C14 C -0.0329(10) 0.8526(8) 0.6425(6) 0.0595(17) Uani 1 1 d . . . H14A H -0.0399 0.9313 0.6020 0.071 Uiso 1 1 calc R . . H14B H 0.0934 0.8404 0.6763 0.071 Uiso 1 1 calc R . . C15 C -0.1090(11) 0.7209(8) 0.5628(7) 0.0652(19) Uani 1 1 d . . . H15A H -0.2346 0.7343 0.5280 0.078 Uiso 1 1 calc R . . H15B H -0.1052 0.6430 0.6039 0.078 Uiso 1 1 calc R . . C16 C -0.0116(12) 0.6806(9) 0.4739(7) 0.073(2) Uani 1 1 d . . . H16A H -0.0327 0.7489 0.4246 0.110 Uiso 1 1 calc R . . H16B H -0.0549 0.5879 0.4324 0.110 Uiso 1 1 calc R . . H16C H 0.1154 0.6789 0.5074 0.110 Uiso 1 1 calc R . . C17 C -0.3264(9) 1.1279(7) 0.6143(7) 0.0609(18) Uani 1 1 d . . . N1 N -0.0506(7) 1.0128(5) 0.8108(5) 0.0529(13) Uani 1 1 d . . . N2 N 0.0076(7) 1.2181(5) 0.9069(5) 0.0508(13) Uani 1 1 d . . . O1 O -0.2083(8) 1.4726(5) 0.7183(5) 0.0718(14) Uani 1 1 d . . . O2 O -0.3222(8) 1.0825(6) 0.5274(5) 0.0798(17) Uani 1 1 d . . . Fe1 Fe -0.34731(12) 1.20535(9) 0.74494(8) 0.0483(3) Uani 1 1 d . . . I1 I 0.43394(6) 0.69260(4) 0.81889(4) 0.0594(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.052(4) 0.086(6) 0.074(5) 0.025(4) 0.035(4) 0.006(4) C2 0.048(4) 0.062(4) 0.069(4) -0.011(3) 0.029(3) -0.003(3) C3 0.048(4) 0.046(4) 0.069(4) -0.001(3) 0.020(3) 0.001(3) C4 0.041(3) 0.050(4) 0.074(4) -0.007(3) 0.023(3) 0.001(3) C5 0.054(4) 0.041(3) 0.109(6) 0.008(4) 0.048(4) -0.002(3) C6 0.060(4) 0.044(4) 0.069(4) -0.004(3) 0.030(3) -0.004(3) C7 0.044(3) 0.041(3) 0.062(4) -0.007(3) 0.027(3) -0.005(3) C8 0.052(4) 0.044(4) 0.082(5) 0.005(3) 0.031(3) 0.006(3) C9 0.045(4) 0.051(4) 0.082(5) 0.000(4) 0.025(3) -0.001(3) C10 0.043(3) 0.041(3) 0.068(4) -0.009(3) 0.023(3) -0.003(3) C11 0.047(3) 0.049(4) 0.067(4) -0.008(3) 0.030(3) -0.005(3) C12 0.050(4) 0.044(4) 0.071(4) -0.009(3) 0.031(3) -0.017(3) C13 0.059(4) 0.030(3) 0.087(5) -0.011(3) 0.032(4) -0.002(3) C14 0.060(4) 0.049(4) 0.074(5) 0.000(3) 0.032(4) 0.002(3) C15 0.079(5) 0.044(4) 0.076(5) -0.002(3) 0.033(4) 0.002(3) C16 0.076(5) 0.067(5) 0.081(5) 0.003(4) 0.037(4) 0.010(4) C17 0.055(4) 0.043(4) 0.087(5) -0.007(4) 0.033(4) -0.010(3) N1 0.047(3) 0.035(3) 0.080(4) -0.007(3) 0.032(3) -0.003(2) N2 0.042(3) 0.038(3) 0.073(3) -0.006(3) 0.027(3) -0.005(2) O1 0.085(4) 0.045(3) 0.094(4) 0.007(3) 0.041(3) -0.010(3) O2 0.087(4) 0.075(4) 0.077(4) -0.024(3) 0.045(3) -0.017(3) Fe1 0.0463(5) 0.0368(5) 0.0646(6) -0.0029(4) 0.0271(4) -0.0049(4) I1 0.0614(3) 0.0393(3) 0.0862(4) 0.0048(2) 0.0388(3) 0.00085(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 C2 1.406(11) . ? C1 C5 1.412(12) . ? C1 Fe1 2.096(7) . ? C1 H1 0.9500 . ? C2 C3 1.387(11) . ? C2 Fe1 2.106(7) . ? C2 H2 0.9500 . ? C3 C4 1.396(10) . ? C3 Fe1 2.090(7) . ? C3 H3 0.9500 . ? C4 C5 1.387(11) . ? C4 Fe1 2.091(7) . ? C4 H4 0.9500 . ? C5 Fe1 2.096(6) . ? C5 H5 0.9500 . ? C6 O1 1.137(8) . ? C6 Fe1 1.792(7) . ? C7 N1 1.357(8) . ? C7 N2 1.364(8) . ? C7 Fe1 1.983(7) . ? C8 C9 1.351(10) . ? C8 N1 1.386(10) . ? C8 H8 0.9500 . ? C9 N2 1.373(9) . ? C9 H9 0.9500 . ? C10 C11 1.364(10) . ? C10 C12 1.394(9) . ? C10 N2 1.434(8) . ? C11 C12 1.380(9) 2_587 ? C11 H11 0.9500 . ? C12 C11 1.380(9) 2_587 ? C12 H12 0.9500 . ? C13 N1 1.465(8) . ? C13 C14 1.522(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O2 1.137(9) . ? C17 Fe1 1.765(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.3(7) . . ? C2 C1 Fe1 70.8(4) . . ? C5 C1 Fe1 70.3(4) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe1 C1 H1 124.6 . . ? C3 C2 C1 107.6(7) . . ? C3 C2 Fe1 70.1(4) . . ? C1 C2 Fe1 70.1(4) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Fe1 C2 H2 125.3 . . ? C2 C3 C4 108.1(7) . . ? C2 C3 Fe1 71.3(4) . . ? C4 C3 Fe1 70.5(4) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Fe1 C3 H3 123.8 . . ? C5 C4 C3 109.2(7) . . ? C5 C4 Fe1 70.8(4) . . ? C3 C4 Fe1 70.4(4) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? Fe1 C4 H4 124.9 . . ? C4 C5 C1 106.7(7) . . ? C4 C5 Fe1 70.5(4) . . ? C1 C5 Fe1 70.3(4) . . ? C4 C5 H5 126.6 . . ? C1 C5 H5 126.6 . . ? Fe1 C5 H5 124.2 . . ? O1 C6 Fe1 175.4(7) . . ? N1 C7 N2 104.2(5) . . ? N1 C7 Fe1 128.6(5) . . ? N2 C7 Fe1 127.2(4) . . ? C9 C8 N1 106.4(6) . . ? C9 C8 H8 126.8 . . ? N1 C8 H8 126.8 . . ? C8 C9 N2 107.2(6) . . ? C8 C9 H9 126.4 . . ? N2 C9 H9 126.4 . . ? C11 C10 C12 120.5(6) . . ? C11 C10 N2 120.1(6) . . ? C12 C10 N2 119.3(6) . . ? C10 C11 C12 120.2(6) . 2_587 ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 2_587 . ? C11 C12 C10 119.3(6) 2_587 . ? C11 C12 H12 120.3 2_587 . ? C10 C12 H12 120.3 . . ? N1 C13 C14 111.8(6) . . ? N1 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N1 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 112.5(6) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 113.6(7) . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 Fe1 175.5(8) . . ? C7 N1 C8 111.1(5) . . ? C7 N1 C13 127.9(6) . . ? C8 N1 C13 121.0(5) . . ? C7 N2 C9 111.1(5) . . ? C7 N2 C10 126.8(5) . . ? C9 N2 C10 122.2(6) . . ? C17 Fe1 C6 92.0(3) . . ? C17 Fe1 C7 94.7(3) . . ? C6 Fe1 C7 95.0(3) . . ? C17 Fe1 C3 115.8(3) . . ? C6 Fe1 C3 90.6(3) . . ? C7 Fe1 C3 148.8(3) . . ? C17 Fe1 C4 90.1(3) . . ? C6 Fe1 C4 122.0(3) . . ? C7 Fe1 C4 142.5(3) . . ? C3 Fe1 C4 39.0(3) . . ? C17 Fe1 C1 138.3(3) . . ? C6 Fe1 C1 129.3(3) . . ? C7 Fe1 C1 88.0(3) . . ? C3 Fe1 C1 65.2(3) . . ? C4 Fe1 C1 64.9(3) . . ? C17 Fe1 C5 100.4(3) . . ? C6 Fe1 C5 156.1(3) . . ? C7 Fe1 C5 104.1(3) . . ? C3 Fe1 C5 65.7(3) . . ? C4 Fe1 C5 38.7(3) . . ? C1 Fe1 C5 39.4(3) . . ? C17 Fe1 C2 153.6(3) . . ? C6 Fe1 C2 94.3(3) . . ? C7 Fe1 C2 110.2(3) . . ? C3 Fe1 C2 38.6(3) . . ? C4 Fe1 C2 64.9(3) . . ? C1 Fe1 C2 39.1(3) . . ? C5 Fe1 C2 65.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.3(8) . . . . ? Fe1 C1 C2 C3 60.3(5) . . . . ? C5 C1 C2 Fe1 -60.6(5) . . . . ? C1 C2 C3 C4 1.0(8) . . . . ? Fe1 C2 C3 C4 61.3(5) . . . . ? C1 C2 C3 Fe1 -60.3(5) . . . . ? C2 C3 C4 C5 -1.3(8) . . . . ? Fe1 C3 C4 C5 60.5(5) . . . . ? C2 C3 C4 Fe1 -61.8(5) . . . . ? C3 C4 C5 C1 1.1(8) . . . . ? Fe1 C4 C5 C1 61.3(5) . . . . ? C3 C4 C5 Fe1 -60.2(5) . . . . ? C2 C1 C5 C4 -0.5(8) . . . . ? Fe1 C1 C5 C4 -61.4(5) . . . . ? C2 C1 C5 Fe1 61.0(5) . . . . ? N1 C8 C9 N2 0.3(8) . . . . ? C12 C10 C11 C12 -0.2(12) . . . 2_587 ? N2 C10 C11 C12 -177.6(6) . . . 2_587 ? C11 C10 C12 C11 0.2(12) . . . 2_587 ? N2 C10 C12 C11 177.6(6) . . . 2_587 ? N1 C13 C14 C15 177.8(7) . . . . ? C13 C14 C15 C16 -178.5(7) . . . . ? N2 C7 N1 C8 0.0(7) . . . . ? Fe1 C7 N1 C8 -179.2(5) . . . . ? N2 C7 N1 C13 -179.7(6) . . . . ? Fe1 C7 N1 C13 1.1(10) . . . . ? C9 C8 N1 C7 -0.2(8) . . . . ? C9 C8 N1 C13 179.5(6) . . . . ? C14 C13 N1 C7 108.9(8) . . . . ? C14 C13 N1 C8 -70.8(9) . . . . ? N1 C7 N2 C9 0.2(7) . . . . ? Fe1 C7 N2 C9 179.4(5) . . . . ? N1 C7 N2 C10 179.4(6) . . . . ? Fe1 C7 N2 C10 -1.3(9) . . . . ? C8 C9 N2 C7 -0.3(8) . . . . ? C8 C9 N2 C10 -179.6(6) . . . . ? C11 C10 N2 C7 -102.2(8) . . . . ? C12 C10 N2 C7 80.4(9) . . . . ? C11 C10 N2 C9 77.0(9) . . . . ? C12 C10 N2 C9 -100.4(8) . . . . ? O2 C17 Fe1 C6 -75(8) . . . . ? O2 C17 Fe1 C7 -171(8) . . . . ? O2 C17 Fe1 C3 16(8) . . . . ? O2 C17 Fe1 C4 47(8) . . . . ? O2 C17 Fe1 C1 97(8) . . . . ? O2 C17 Fe1 C5 84(8) . . . . ? O2 C17 Fe1 C2 28(9) . . . . ? O1 C6 Fe1 C17 33(8) . . . . ? O1 C6 Fe1 C7 128(8) . . . . ? O1 C6 Fe1 C3 -83(8) . . . . ? O1 C6 Fe1 C4 -58(8) . . . . ? O1 C6 Fe1 C1 -141(8) . . . . ? O1 C6 Fe1 C5 -89(8) . . . . ? O1 C6 Fe1 C2 -121(8) . . . . ? N1 C7 Fe1 C17 -46.1(6) . . . . ? N2 C7 Fe1 C17 134.8(6) . . . . ? N1 C7 Fe1 C6 -138.6(6) . . . . ? N2 C7 Fe1 C6 42.3(6) . . . . ? N1 C7 Fe1 C3 121.9(6) . . . . ? N2 C7 Fe1 C3 -57.1(8) . . . . ? N1 C7 Fe1 C4 50.1(8) . . . . ? N2 C7 Fe1 C4 -128.9(6) . . . . ? N1 C7 Fe1 C1 92.2(6) . . . . ? N2 C7 Fe1 C1 -86.9(6) . . . . ? N1 C7 Fe1 C5 55.9(6) . . . . ? N2 C7 Fe1 C5 -123.2(6) . . . . ? N1 C7 Fe1 C2 125.0(6) . . . . ? N2 C7 Fe1 C2 -54.1(6) . . . . ? C2 C3 Fe1 C17 171.3(4) . . . . ? C4 C3 Fe1 C17 53.5(5) . . . . ? C2 C3 Fe1 C6 -96.1(5) . . . . ? C4 C3 Fe1 C6 146.0(5) . . . . ? C2 C3 Fe1 C7 4.6(7) . . . . ? C4 C3 Fe1 C7 -113.3(6) . . . . ? C2 C3 Fe1 C4 117.9(7) . . . . ? C2 C3 Fe1 C1 37.7(5) . . . . ? C4 C3 Fe1 C1 -80.1(5) . . . . ? C2 C3 Fe1 C5 81.2(5) . . . . ? C4 C3 Fe1 C5 -36.6(5) . . . . ? C4 C3 Fe1 C2 -117.9(7) . . . . ? C5 C4 Fe1 C17 106.7(5) . . . . ? C3 C4 Fe1 C17 -133.7(5) . . . . ? C5 C4 Fe1 C6 -160.8(5) . . . . ? C3 C4 Fe1 C6 -41.2(6) . . . . ? C5 C4 Fe1 C7 8.9(7) . . . . ? C3 C4 Fe1 C7 128.5(5) . . . . ? C5 C4 Fe1 C3 -119.6(7) . . . . ? C5 C4 Fe1 C1 -38.7(5) . . . . ? C3 C4 Fe1 C1 80.9(5) . . . . ? C3 C4 Fe1 C5 119.6(7) . . . . ? C5 C4 Fe1 C2 -82.1(5) . . . . ? C3 C4 Fe1 C2 37.5(5) . . . . ? C2 C1 Fe1 C17 -138.9(5) . . . . ? C5 C1 Fe1 C17 -20.4(7) . . . . ? C2 C1 Fe1 C6 31.4(6) . . . . ? C5 C1 Fe1 C6 149.9(5) . . . . ? C2 C1 Fe1 C7 126.2(5) . . . . ? C5 C1 Fe1 C7 -115.2(5) . . . . ? C2 C1 Fe1 C3 -37.3(4) . . . . ? C5 C1 Fe1 C3 81.3(5) . . . . ? C2 C1 Fe1 C4 -80.5(5) . . . . ? C5 C1 Fe1 C4 38.0(4) . . . . ? C2 C1 Fe1 C5 -118.5(7) . . . . ? C5 C1 Fe1 C2 118.5(7) . . . . ? C4 C5 Fe1 C17 -76.8(5) . . . . ? C1 C5 Fe1 C17 166.3(5) . . . . ? C4 C5 Fe1 C6 43.5(11) . . . . ? C1 C5 Fe1 C6 -73.4(10) . . . . ? C4 C5 Fe1 C7 -174.4(4) . . . . ? C1 C5 Fe1 C7 68.8(5) . . . . ? C4 C5 Fe1 C3 36.9(4) . . . . ? C1 C5 Fe1 C3 -79.9(5) . . . . ? C1 C5 Fe1 C4 -116.8(6) . . . . ? C4 C5 Fe1 C1 116.8(6) . . . . ? C4 C5 Fe1 C2 79.4(5) . . . . ? C1 C5 Fe1 C2 -37.4(5) . . . . ? C3 C2 Fe1 C17 -17.8(9) . . . . ? C1 C2 Fe1 C17 100.5(8) . . . . ? C3 C2 Fe1 C6 85.6(5) . . . . ? C1 C2 Fe1 C6 -156.2(5) . . . . ? C3 C2 Fe1 C7 -177.5(4) . . . . ? C1 C2 Fe1 C7 -59.2(5) . . . . ? C1 C2 Fe1 C3 118.3(7) . . . . ? C3 C2 Fe1 C4 -37.9(4) . . . . ? C1 C2 Fe1 C4 80.4(5) . . . . ? C3 C2 Fe1 C1 -118.3(7) . . . . ? C3 C2 Fe1 C5 -80.6(5) . . . . ? C1 C2 Fe1 C5 37.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.199 _refine_diff_density_min -1.504 _refine_diff_density_rms 0.159 #################################################END data_Complex9b _database_code_depnum_ccdc_archive 'CCDC 726551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H74 B2 F8 Fe2 N6 O4' _chemical_formula_weight 1276.61 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1129(17) _cell_length_b 20.0683(19) _cell_length_c 14.218(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.165(11) _cell_angle_gamma 90.00 _cell_volume 3128.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 25.44 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99150 _exptl_absorpt_correction_T_max 1.00983 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14935 _diffrn_reflns_av_R_equivalents 0.1351 _diffrn_reflns_av_sigmaI/netI 0.1625 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4089 _reflns_number_gt 2168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0172P)^2^] 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 4089 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 0.6222(5) 0.0643(3) 0.5577(5) 0.0294(15) Uani 1 1 d . . . H1 H 0.6243 0.0842 0.6190 0.035 Uiso 1 1 d R . . C2 C 0.6760(5) 0.0034(3) 0.5521(5) 0.0283(15) Uani 1 1 d . . . H2 H 0.7220 -0.0248 0.6091 0.034 Uiso 1 1 d R . . C3 C 0.6501(5) -0.0085(3) 0.4467(4) 0.0277(14) Uani 1 1 d . . . H3 H 0.6760 -0.0461 0.4209 0.033 Uiso 1 1 d R . . C4 C 0.5794(5) 0.0443(3) 0.3861(5) 0.0307(15) Uani 1 1 d . . . H4 H 0.5480 0.0484 0.3127 0.037 Uiso 1 1 d R . . C5 C 0.5638(4) 0.0908(3) 0.4560(5) 0.0358(16) Uani 1 1 d . . . H5 H 0.5219 0.1322 0.4374 0.043 Uiso 1 1 d R . . C6 C 0.7413(5) 0.1364(3) 0.3972(5) 0.0257(14) Uani 1 1 d . . . C7 C 0.8369(4) 0.1426(3) 0.6111(4) 0.0190(13) Uani 1 1 d . . . C8 C 0.8785(5) 0.2343(3) 0.7159(4) 0.0249(14) Uani 1 1 d . . . H8 H 0.8741 0.2783 0.7388 0.030 Uiso 1 1 calc R . . C9 C 0.9552(5) 0.1870(3) 0.7705(4) 0.0277(14) Uani 1 1 d . . . H9 H 1.0163 0.1906 0.8397 0.033 Uiso 1 1 calc R . . C10 C 1.0119(5) 0.0740(3) 0.7397(4) 0.0248(13) Uani 1 1 d . . . C11 C 1.1192(4) 0.0795(3) 0.7251(4) 0.0235(12) Uani 1 1 d . . . C12 C 1.2032(5) 0.0280(3) 0.7653(4) 0.0252(14) Uani 1 1 d . . . H12 H 1.2757 0.0295 0.7550 0.030 Uiso 1 1 calc R . . C13 C 1.1864(5) -0.0251(3) 0.8195(4) 0.0271(14) Uani 1 1 d . . . C14 C 1.0800(5) -0.0278(3) 0.8326(4) 0.0313(15) Uani 1 1 d . . . H14 H 1.0666 -0.0644 0.8688 0.038 Uiso 1 1 calc R . . C15 C 0.9910(5) 0.0224(3) 0.7938(4) 0.0302(15) Uani 1 1 d . . . C16 C 1.1458(5) 0.1398(3) 0.6764(4) 0.0309(15) Uani 1 1 d . . . H16A H 1.1778 0.1753 0.7283 0.046 Uiso 1 1 calc R . . H16B H 1.0706 0.1550 0.6186 0.046 Uiso 1 1 calc R . . H16C H 1.2065 0.1285 0.6503 0.046 Uiso 1 1 calc R . . C17 C 1.2840(5) -0.0764(3) 0.8684(4) 0.0450(16) Uani 1 1 d . . . H17A H 1.3349 -0.0640 0.9408 0.068 Uiso 1 1 calc R . . H17B H 1.3346 -0.0788 0.8301 0.068 Uiso 1 1 calc R . . H17C H 1.2464 -0.1199 0.8665 0.068 Uiso 1 1 calc R . . C18 C 0.8804(5) 0.0199(3) 0.8179(4) 0.0397(17) Uani 1 1 d . . . H18A H 0.8192 0.0519 0.7737 0.060 Uiso 1 1 calc R . . H18B H 0.9050 0.0314 0.8911 0.060 Uiso 1 1 calc R . . H18C H 0.8458 -0.0251 0.8046 0.060 Uiso 1 1 calc R . . C19 C 0.7269(5) 0.2504(3) 0.5372(4) 0.0220(14) Uani 1 1 d . . . C20 C 0.6075(5) 0.2611(3) 0.5213(4) 0.0253(15) Uani 1 1 d . . . C21 C 0.5349(5) 0.3026(3) 0.4391(4) 0.0323(16) Uani 1 1 d . . . H21 H 0.4517 0.3089 0.4254 0.039 Uiso 1 1 calc R . . C22 C 0.5805(5) 0.3349(3) 0.3770(5) 0.0347(16) Uani 1 1 d . . . C23 C 0.7043(5) 0.3262(3) 0.4021(4) 0.0339(16) Uani 1 1 d . . . H23 H 0.7387 0.3498 0.3630 0.041 Uiso 1 1 calc R . . C24 C 0.7783(5) 0.2852(3) 0.4808(4) 0.0257(15) Uani 1 1 d . . . C25 C 0.5571(5) 0.2324(3) 0.5934(4) 0.0349(16) Uani 1 1 d . . . H25A H 0.5494 0.2680 0.6375 0.052 Uiso 1 1 calc R . . H25B H 0.6126 0.1980 0.6371 0.052 Uiso 1 1 calc R . . H25C H 0.4768 0.2128 0.5523 0.052 Uiso 1 1 calc R . . C26 C 0.5016(6) 0.3802(4) 0.2909(5) 0.056(2) Uani 1 1 d . . . H26A H 0.4673 0.3554 0.2253 0.085 Uiso 1 1 calc R . . H26B H 0.5506 0.4175 0.2850 0.085 Uiso 1 1 calc R . . H26C H 0.4352 0.3975 0.3061 0.085 Uiso 1 1 calc R . . C27 C 0.9135(5) 0.2795(3) 0.5066(5) 0.0329(17) Uani 1 1 d . . . H27A H 0.9294 0.2364 0.4823 0.049 Uiso 1 1 calc R . . H27B H 0.9613 0.2829 0.5820 0.049 Uiso 1 1 calc R . . H27C H 0.9368 0.3155 0.4722 0.049 Uiso 1 1 calc R . . C28 C 0.9682(4) 0.0602(3) 0.4572(4) 0.0220(14) Uani 1 1 d . . . H28 H 0.9488 0.1030 0.4258 0.026 Uiso 1 1 calc R . . C29 C 0.9335(5) -0.0259(3) 0.5449(4) 0.0229(13) Uani 1 1 d . . . H29 H 0.8883 -0.0462 0.5778 0.028 Uiso 1 1 calc R . . C30 C 0.3341(7) 0.1340(5) 0.1247(6) 0.062(2) Uani 1 1 d . . . C31 C 0.2302(8) 0.1190(4) 0.0252(6) 0.095(3) Uani 1 1 d . . . H31A H 0.2389 0.0738 0.0032 0.142 Uiso 1 1 calc R . . H31B H 0.2283 0.1510 -0.0275 0.142 Uiso 1 1 calc R . . H31C H 0.1542 0.1222 0.0337 0.142 Uiso 1 1 calc R . . C32 C 0.3252(9) 0.1935(5) 0.1792(7) 0.108(4) Uani 1 1 d . . . H32A H 0.4058 0.2047 0.2337 0.162 Uiso 1 1 calc R . . H32B H 0.2685 0.1854 0.2108 0.162 Uiso 1 1 calc R . . H32C H 0.2951 0.2307 0.1300 0.162 Uiso 1 1 calc R . . B1 B 0.1874(7) 0.1814(4) 0.3987(6) 0.0371(19) Uani 1 1 d . . . F1 F 0.0807(3) 0.1917(2) 0.4091(3) 0.0659(13) Uani 1 1 d . . . F2 F 0.2295(3) 0.24162(18) 0.3788(3) 0.0528(10) Uani 1 1 d . . . F3 F 0.2729(3) 0.15516(19) 0.4911(3) 0.0666(13) Uani 1 1 d . . . F4 F 0.1677(4) 0.1369(2) 0.3213(4) 0.0855(14) Uani 1 1 d . . . Fe1 Fe 0.74968(8) 0.08102(4) 0.49428(7) 0.0221(2) Uani 1 1 d . . . N1 N 0.8057(4) 0.2078(2) 0.6192(3) 0.0211(11) Uani 1 1 d . . . N2 N 0.9290(4) 0.1312(2) 0.7069(3) 0.0217(11) Uani 1 1 d . . . N3 N 0.8992(4) 0.0349(2) 0.5022(3) 0.0197(11) Uani 1 1 d . . . O1 O 0.7255(4) 0.1709(2) 0.3259(3) 0.0402(11) Uani 1 1 d . . . O2 O 0.4191(6) 0.0983(4) 0.1568(5) 0.129(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 0.015(3) 0.028(4) 0.049(4) -0.010(3) 0.019(3) -0.007(3) C2 0.018(3) 0.029(4) 0.039(4) 0.004(3) 0.014(3) -0.005(3) C3 0.018(3) 0.025(4) 0.036(4) -0.008(3) 0.008(3) -0.009(3) C4 0.017(3) 0.031(4) 0.039(4) -0.010(3) 0.007(3) -0.008(3) C5 0.011(3) 0.030(4) 0.064(4) -0.006(4) 0.014(3) -0.007(3) C6 0.014(3) 0.030(4) 0.028(4) -0.008(3) 0.004(3) -0.001(3) C7 0.017(3) 0.021(4) 0.020(3) 0.006(3) 0.010(3) 0.000(3) C8 0.032(3) 0.018(4) 0.026(3) -0.001(3) 0.013(3) 0.008(3) C9 0.024(3) 0.034(4) 0.025(3) -0.008(3) 0.010(3) -0.008(3) C10 0.028(3) 0.018(4) 0.023(3) 0.003(3) 0.006(2) 0.002(3) C11 0.023(3) 0.023(3) 0.021(3) -0.001(3) 0.005(2) -0.007(3) C12 0.016(3) 0.022(4) 0.031(3) -0.005(3) 0.004(3) -0.005(3) C13 0.027(3) 0.023(4) 0.026(3) 0.003(3) 0.005(3) 0.002(3) C14 0.047(4) 0.017(4) 0.029(3) 0.004(3) 0.014(3) -0.001(3) C15 0.035(4) 0.032(4) 0.028(4) -0.002(3) 0.017(3) -0.001(3) C16 0.030(3) 0.023(4) 0.040(4) 0.002(3) 0.016(3) -0.002(3) C17 0.042(4) 0.036(4) 0.053(4) 0.005(4) 0.017(3) 0.006(4) C18 0.038(4) 0.044(5) 0.042(4) 0.013(3) 0.021(3) 0.001(3) C19 0.025(3) 0.018(4) 0.022(3) 0.007(3) 0.008(3) 0.010(3) C20 0.018(3) 0.026(4) 0.032(4) -0.009(3) 0.011(3) -0.001(3) C21 0.019(3) 0.036(4) 0.034(4) -0.008(3) 0.004(3) 0.007(3) C22 0.029(4) 0.026(4) 0.042(4) 0.000(3) 0.008(3) 0.011(3) C23 0.032(4) 0.039(5) 0.032(4) 0.010(3) 0.014(3) 0.009(3) C24 0.023(4) 0.029(4) 0.025(4) -0.004(3) 0.009(3) 0.006(3) C25 0.025(3) 0.040(4) 0.042(4) -0.004(3) 0.017(3) 0.001(3) C26 0.048(4) 0.062(6) 0.053(5) 0.017(4) 0.016(4) 0.029(4) C27 0.023(4) 0.039(5) 0.042(4) 0.003(3) 0.019(3) -0.001(3) C28 0.018(3) 0.016(4) 0.030(3) -0.001(3) 0.009(3) -0.001(2) C29 0.024(3) 0.019(4) 0.030(3) 0.004(3) 0.015(3) 0.000(3) C30 0.039(5) 0.083(7) 0.055(5) 0.021(5) 0.010(4) 0.012(4) C31 0.083(7) 0.074(7) 0.082(7) 0.023(5) -0.009(5) -0.003(5) C32 0.144(10) 0.104(9) 0.129(9) -0.033(7) 0.109(8) -0.027(7) B1 0.040(5) 0.029(5) 0.048(5) 0.008(4) 0.024(4) -0.001(4) F1 0.047(2) 0.070(3) 0.100(3) 0.036(3) 0.049(2) 0.017(2) F2 0.052(2) 0.034(3) 0.079(3) 0.012(2) 0.034(2) -0.0094(19) F3 0.041(3) 0.062(3) 0.082(3) 0.029(3) 0.012(2) 0.004(2) F4 0.124(4) 0.061(3) 0.092(3) -0.022(3) 0.066(3) -0.023(3) Fe1 0.0166(3) 0.0222(4) 0.0277(4) -0.0012(5) 0.0095(3) -0.0006(5) N1 0.023(3) 0.022(3) 0.020(3) -0.002(2) 0.011(2) 0.000(2) N2 0.022(3) 0.024(3) 0.019(3) 0.000(2) 0.008(2) 0.003(2) N3 0.018(3) 0.020(3) 0.025(3) -0.005(2) 0.012(2) -0.006(2) O1 0.047(3) 0.039(3) 0.035(3) 0.006(2) 0.017(2) 0.003(2) O2 0.089(5) 0.185(8) 0.092(5) 0.046(5) 0.019(4) 0.072(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 C2 1.403(7) . ? C1 C5 1.416(8) . ? C1 Fe1 2.120(5) . ? C1 H1 0.9501 . ? C2 C3 1.414(7) . ? C2 Fe1 2.127(5) . ? C2 H2 0.9500 . ? C3 C4 1.404(8) . ? C3 Fe1 2.108(5) . ? C3 H3 0.9499 . ? C4 C5 1.433(8) . ? C4 Fe1 2.113(5) . ? C4 H4 0.9500 . ? C5 Fe1 2.088(5) . ? C5 H5 0.9500 . ? C6 O1 1.174(6) . ? C6 Fe1 1.741(6) . ? C7 N2 1.363(6) . ? C7 N1 1.381(6) . ? C7 Fe1 1.977(5) . ? C8 C9 1.324(7) . ? C8 N1 1.386(6) . ? C8 H8 0.9500 . ? C9 N2 1.390(6) . ? C9 H9 0.9500 . ? C10 C15 1.376(7) . ? C10 C11 1.405(6) . ? C10 N2 1.464(7) . ? C11 C12 1.392(7) . ? C11 C16 1.496(7) . ? C12 C13 1.380(7) . ? C12 H12 0.9500 . ? C13 C14 1.380(7) . ? C13 C17 1.496(7) . ? C14 C15 1.406(8) . ? C14 H14 0.9500 . ? C15 C18 1.517(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.383(7) . ? C19 C24 1.394(7) . ? C19 N1 1.433(6) . ? C20 C21 1.401(8) . ? C20 C25 1.511(7) . ? C21 C22 1.385(8) . ? C21 H21 0.9500 . ? C22 C23 1.396(7) . ? C22 C26 1.499(8) . ? C23 C24 1.371(7) . ? C23 H23 0.9500 . ? C24 C27 1.522(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N3 1.349(6) . ? C28 C29 1.386(7) 3_756 ? C28 H28 0.9500 . ? C29 N3 1.349(6) . ? C29 C28 1.386(7) 3_756 ? C29 H29 0.9500 . ? C30 O2 1.176(8) . ? C30 C32 1.453(11) . ? C30 C31 1.470(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? B1 F4 1.358(8) . ? B1 F1 1.377(7) . ? B1 F3 1.385(8) . ? B1 F2 1.386(8) . ? Fe1 N3 1.994(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 C2 C1 C5 108.2(5) . . ? C2 C1 Fe1 71.0(3) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 125.8 . . ? Fe1 C1 H1 125.7 . . ? C1 C2 C3 107.9(5) . . ? C1 C2 Fe1 70.4(3) . . ? C3 C2 Fe1 69.8(3) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 126.2 . . ? Fe1 C2 H2 125.2 . . ? C4 C3 C2 109.1(5) . . ? C4 C3 Fe1 70.8(3) . . ? C2 C3 Fe1 71.2(3) . . ? C4 C3 H3 125.3 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 124.3 . . ? C3 C4 C5 106.9(5) . . ? C3 C4 Fe1 70.4(3) . . ? C5 C4 Fe1 69.1(3) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.6 . . ? Fe1 C4 H4 125.5 . . ? C1 C5 C4 107.9(6) . . ? C1 C5 Fe1 71.6(3) . . ? C4 C5 Fe1 71.0(3) . . ? C1 C5 H5 126.1 . . ? C4 C5 H5 126.0 . . ? Fe1 C5 H5 123.0 . . ? O1 C6 Fe1 173.7(5) . . ? N2 C7 N1 102.3(4) . . ? N2 C7 Fe1 130.7(4) . . ? N1 C7 Fe1 126.5(4) . . ? C9 C8 N1 107.4(5) . . ? C9 C8 H8 126.3 . . ? N1 C8 H8 126.3 . . ? C8 C9 N2 106.7(5) . . ? C8 C9 H9 126.6 . . ? N2 C9 H9 126.6 . . ? C15 C10 C11 122.9(5) . . ? C15 C10 N2 120.2(5) . . ? C11 C10 N2 116.3(5) . . ? C12 C11 C10 116.3(5) . . ? C12 C11 C16 121.8(5) . . ? C10 C11 C16 121.8(5) . . ? C13 C12 C11 123.2(5) . . ? C13 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C12 C13 C14 118.2(5) . . ? C12 C13 C17 121.0(5) . . ? C14 C13 C17 120.6(5) . . ? C13 C14 C15 121.6(5) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C10 C15 C14 117.8(5) . . ? C10 C15 C18 122.8(5) . . ? C14 C15 C18 119.4(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 121.4(5) . . ? C20 C19 N1 120.9(5) . . ? C24 C19 N1 117.5(4) . . ? C19 C20 C21 118.0(5) . . ? C19 C20 C25 121.8(5) . . ? C21 C20 C25 120.1(5) . . ? C22 C21 C20 122.1(5) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 117.1(5) . . ? C21 C22 C26 121.0(5) . . ? C23 C22 C26 121.8(6) . . ? C24 C23 C22 122.8(5) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C23 C24 C19 118.2(5) . . ? C23 C24 C27 120.3(5) . . ? C19 C24 C27 121.4(5) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 122.3(5) . 3_756 ? N3 C28 H28 118.9 . . ? C29 C28 H28 118.9 3_756 . ? N3 C29 C28 122.9(5) . 3_756 ? N3 C29 H29 118.6 . . ? C28 C29 H29 118.6 3_756 . ? O2 C30 C32 123.1(9) . . ? O2 C30 C31 119.9(9) . . ? C32 C30 C31 117.0(8) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? F4 B1 F1 109.6(6) . . ? F4 B1 F3 108.7(6) . . ? F1 B1 F3 108.3(6) . . ? F4 B1 F2 111.1(6) . . ? F1 B1 F2 109.6(6) . . ? F3 B1 F2 109.5(6) . . ? C6 Fe1 C7 95.6(2) . . ? C6 Fe1 N3 94.9(2) . . ? C7 Fe1 N3 95.42(19) . . ? C6 Fe1 C5 92.3(2) . . ? C7 Fe1 C5 106.9(2) . . ? N3 Fe1 C5 155.7(2) . . ? C6 Fe1 C3 117.2(2) . . ? C7 Fe1 C3 146.1(2) . . ? N3 Fe1 C3 90.3(2) . . ? C5 Fe1 C3 65.8(2) . . ? C6 Fe1 C4 86.3(2) . . ? C7 Fe1 C4 146.8(2) . . ? N3 Fe1 C4 117.5(2) . . ? C5 Fe1 C4 39.9(2) . . ? C3 Fe1 C4 38.9(2) . . ? C6 Fe1 C1 129.1(2) . . ? C7 Fe1 C1 88.1(2) . . ? N3 Fe1 C1 135.3(2) . . ? C5 Fe1 C1 39.3(2) . . ? C3 Fe1 C1 65.2(2) . . ? C4 Fe1 C1 66.0(2) . . ? C6 Fe1 C2 151.8(2) . . ? C7 Fe1 C2 107.1(2) . . ? N3 Fe1 C2 99.1(2) . . ? C5 Fe1 C2 65.6(2) . . ? C3 Fe1 C2 39.0(2) . . ? C4 Fe1 C2 65.6(2) . . ? C1 Fe1 C2 38.58(19) . . ? C7 N1 C8 111.4(4) . . ? C7 N1 C19 127.5(4) . . ? C8 N1 C19 120.0(5) . . ? C7 N2 C9 112.2(5) . . ? C7 N2 C10 127.5(5) . . ? C9 N2 C10 119.3(4) . . ? C29 N3 C28 114.9(4) . . ? C29 N3 Fe1 122.9(3) . . ? C28 N3 Fe1 122.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.6(6) . . . . ? Fe1 C1 C2 C3 -60.0(3) . . . . ? C5 C1 C2 Fe1 59.4(3) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? Fe1 C2 C3 C4 -60.9(4) . . . . ? C1 C2 C3 Fe1 60.4(4) . . . . ? C2 C3 C4 C5 1.4(6) . . . . ? Fe1 C3 C4 C5 -59.8(4) . . . . ? C2 C3 C4 Fe1 61.2(4) . . . . ? C2 C1 C5 C4 1.5(6) . . . . ? Fe1 C1 C5 C4 62.0(3) . . . . ? C2 C1 C5 Fe1 -60.5(4) . . . . ? C3 C4 C5 C1 -1.8(6) . . . . ? Fe1 C4 C5 C1 -62.4(3) . . . . ? C3 C4 C5 Fe1 60.6(4) . . . . ? N1 C8 C9 N2 -0.1(6) . . . . ? C15 C10 C11 C12 2.4(8) . . . . ? N2 C10 C11 C12 174.0(5) . . . . ? C15 C10 C11 C16 -173.0(5) . . . . ? N2 C10 C11 C16 -1.4(7) . . . . ? C10 C11 C12 C13 -1.8(8) . . . . ? C16 C11 C12 C13 173.6(5) . . . . ? C11 C12 C13 C14 1.2(8) . . . . ? C11 C12 C13 C17 -175.1(5) . . . . ? C12 C13 C14 C15 -1.0(8) . . . . ? C17 C13 C14 C15 175.3(5) . . . . ? C11 C10 C15 C14 -2.2(8) . . . . ? N2 C10 C15 C14 -173.6(5) . . . . ? C11 C10 C15 C18 174.3(5) . . . . ? N2 C10 C15 C18 2.9(8) . . . . ? C13 C14 C15 C10 1.5(8) . . . . ? C13 C14 C15 C18 -175.1(5) . . . . ? C24 C19 C20 C21 6.7(8) . . . . ? N1 C19 C20 C21 -179.2(5) . . . . ? C24 C19 C20 C25 -169.8(5) . . . . ? N1 C19 C20 C25 4.2(8) . . . . ? C19 C20 C21 C22 -2.7(9) . . . . ? C25 C20 C21 C22 173.9(5) . . . . ? C20 C21 C22 C23 -2.2(9) . . . . ? C20 C21 C22 C26 -178.7(6) . . . . ? C21 C22 C23 C24 3.4(9) . . . . ? C26 C22 C23 C24 179.8(6) . . . . ? C22 C23 C24 C19 0.5(9) . . . . ? C22 C23 C24 C27 -178.1(5) . . . . ? C20 C19 C24 C23 -5.7(8) . . . . ? N1 C19 C24 C23 -179.9(5) . . . . ? C20 C19 C24 C27 172.8(6) . . . . ? N1 C19 C24 C27 -1.4(8) . . . . ? O1 C6 Fe1 C7 -149(5) . . . . ? O1 C6 Fe1 N3 116(5) . . . . ? O1 C6 Fe1 C5 -41(5) . . . . ? O1 C6 Fe1 C3 23(5) . . . . ? O1 C6 Fe1 C4 -2(5) . . . . ? O1 C6 Fe1 C1 -56(5) . . . . ? O1 C6 Fe1 C2 -4(5) . . . . ? N2 C7 Fe1 C6 -140.5(5) . . . . ? N1 C7 Fe1 C6 49.1(4) . . . . ? N2 C7 Fe1 N3 -44.9(5) . . . . ? N1 C7 Fe1 N3 144.7(4) . . . . ? N2 C7 Fe1 C5 125.4(5) . . . . ? N1 C7 Fe1 C5 -45.0(5) . . . . ? N2 C7 Fe1 C3 53.7(6) . . . . ? N1 C7 Fe1 C3 -116.7(5) . . . . ? N2 C7 Fe1 C4 127.8(5) . . . . ? N1 C7 Fe1 C4 -42.6(7) . . . . ? N2 C7 Fe1 C1 90.4(5) . . . . ? N1 C7 Fe1 C1 -80.0(4) . . . . ? N2 C7 Fe1 C2 56.4(5) . . . . ? N1 C7 Fe1 C2 -114.0(4) . . . . ? C1 C5 Fe1 C6 -161.3(4) . . . . ? C4 C5 Fe1 C6 81.4(4) . . . . ? C1 C5 Fe1 C7 -64.7(4) . . . . ? C4 C5 Fe1 C7 178.0(4) . . . . ? C1 C5 Fe1 N3 91.3(6) . . . . ? C4 C5 Fe1 N3 -26.0(7) . . . . ? C1 C5 Fe1 C3 79.8(4) . . . . ? C4 C5 Fe1 C3 -37.5(3) . . . . ? C1 C5 Fe1 C4 117.3(5) . . . . ? C4 C5 Fe1 C1 -117.3(5) . . . . ? C1 C5 Fe1 C2 36.8(3) . . . . ? C4 C5 Fe1 C2 -80.5(4) . . . . ? C4 C3 Fe1 C6 -41.1(4) . . . . ? C2 C3 Fe1 C6 -160.0(3) . . . . ? C4 C3 Fe1 C7 123.0(4) . . . . ? C2 C3 Fe1 C7 4.0(6) . . . . ? C4 C3 Fe1 N3 -136.8(3) . . . . ? C2 C3 Fe1 N3 104.2(3) . . . . ? C4 C3 Fe1 C5 38.5(3) . . . . ? C2 C3 Fe1 C5 -80.5(3) . . . . ? C2 C3 Fe1 C4 -119.0(5) . . . . ? C4 C3 Fe1 C1 81.9(4) . . . . ? C2 C3 Fe1 C1 -37.1(3) . . . . ? C4 C3 Fe1 C2 119.0(5) . . . . ? C3 C4 Fe1 C6 144.2(4) . . . . ? C5 C4 Fe1 C6 -98.1(4) . . . . ? C3 C4 Fe1 C7 -121.3(4) . . . . ? C5 C4 Fe1 C7 -3.5(6) . . . . ? C3 C4 Fe1 N3 50.5(4) . . . . ? C5 C4 Fe1 N3 168.3(3) . . . . ? C3 C4 Fe1 C5 -117.7(5) . . . . ? C5 C4 Fe1 C3 117.7(5) . . . . ? C3 C4 Fe1 C1 -79.7(4) . . . . ? C5 C4 Fe1 C1 38.1(3) . . . . ? C3 C4 Fe1 C2 -37.2(3) . . . . ? C5 C4 Fe1 C2 80.5(4) . . . . ? C2 C1 Fe1 C6 143.3(4) . . . . ? C5 C1 Fe1 C6 24.4(5) . . . . ? C2 C1 Fe1 C7 -121.0(4) . . . . ? C5 C1 Fe1 C7 120.1(4) . . . . ? C2 C1 Fe1 N3 -25.2(5) . . . . ? C5 C1 Fe1 N3 -144.2(3) . . . . ? C2 C1 Fe1 C5 119.0(5) . . . . ? C2 C1 Fe1 C3 37.5(3) . . . . ? C5 C1 Fe1 C3 -81.5(4) . . . . ? C2 C1 Fe1 C4 80.4(4) . . . . ? C5 C1 Fe1 C4 -38.6(4) . . . . ? C5 C1 Fe1 C2 -119.0(5) . . . . ? C1 C2 Fe1 C6 -78.6(6) . . . . ? C3 C2 Fe1 C6 40.0(6) . . . . ? C1 C2 Fe1 C7 63.7(4) . . . . ? C3 C2 Fe1 C7 -177.7(3) . . . . ? C1 C2 Fe1 N3 162.4(3) . . . . ? C3 C2 Fe1 N3 -79.0(3) . . . . ? C1 C2 Fe1 C5 -37.5(3) . . . . ? C3 C2 Fe1 C5 81.1(4) . . . . ? C1 C2 Fe1 C3 -118.6(5) . . . . ? C1 C2 Fe1 C4 -81.5(4) . . . . ? C3 C2 Fe1 C4 37.1(3) . . . . ? C3 C2 Fe1 C1 118.6(5) . . . . ? N2 C7 N1 C8 1.0(5) . . . . ? Fe1 C7 N1 C8 173.5(3) . . . . ? N2 C7 N1 C19 169.3(4) . . . . ? Fe1 C7 N1 C19 -18.1(7) . . . . ? C9 C8 N1 C7 -0.5(6) . . . . ? C9 C8 N1 C19 -169.9(4) . . . . ? C20 C19 N1 C7 100.5(6) . . . . ? C24 C19 N1 C7 -85.2(7) . . . . ? C20 C19 N1 C8 -92.0(6) . . . . ? C24 C19 N1 C8 82.3(6) . . . . ? N1 C7 N2 C9 -1.1(5) . . . . ? Fe1 C7 N2 C9 -173.2(4) . . . . ? N1 C7 N2 C10 -169.3(4) . . . . ? Fe1 C7 N2 C10 18.5(7) . . . . ? C8 C9 N2 C7 0.8(6) . . . . ? C8 C9 N2 C10 170.1(4) . . . . ? C15 C10 N2 C7 -99.3(6) . . . . ? C11 C10 N2 C7 88.8(6) . . . . ? C15 C10 N2 C9 93.2(6) . . . . ? C11 C10 N2 C9 -78.7(6) . . . . ? C28 C29 N3 C28 -0.1(8) 3_756 . . . ? C28 C29 N3 Fe1 174.6(4) 3_756 . . . ? C29 C28 N3 C29 0.1(8) 3_756 . . . ? C29 C28 N3 Fe1 -174.7(4) 3_756 . . . ? C6 Fe1 N3 C29 -161.1(4) . . . . ? C7 Fe1 N3 C29 102.7(4) . . . . ? C5 Fe1 N3 C29 -54.3(7) . . . . ? C3 Fe1 N3 C29 -43.8(4) . . . . ? C4 Fe1 N3 C29 -72.8(4) . . . . ? C1 Fe1 N3 C29 9.9(5) . . . . ? C2 Fe1 N3 C29 -5.7(4) . . . . ? C6 Fe1 N3 C28 13.2(4) . . . . ? C7 Fe1 N3 C28 -82.9(4) . . . . ? C5 Fe1 N3 C28 120.0(6) . . . . ? C3 Fe1 N3 C28 130.5(4) . . . . ? C4 Fe1 N3 C28 101.6(4) . . . . ? C1 Fe1 N3 C28 -175.7(4) . . . . ? C2 Fe1 N3 C28 168.7(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.259 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.057 # start Validation Reply Form _vrf_PLAT023_Complex9b ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.50 Deg. RESPONSE: The crystal did not diffract significantly above 45 in 2Theta and this was set as the 2Theta cutoff limit. ; # end Validation Reply Form #################################################END data_complex11 _database_code_depnum_ccdc_archive 'CCDC 726552' _audit_creation_method SHELXL-97 _audit_creation_date 09-04-01 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C17 H24 B F4 Fe N3 O' _chemical_formula_sum 'C17 H24 B F4 Fe N3 O' _chemical_formula_weight 429.05 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 68 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 96 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; B B 4 0.0013 0.0007 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 16 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Fe Fe 4 0.3463 0.8444 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 12 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 4 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 14 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 9.3055(2) _cell_length_b 21.7066(4) _cell_length_c 10.3747(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.4040(10) _cell_angle_gamma 90.00 _cell_volume 1988.41(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 117656 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sortav; Blessing, 1995)' _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.906 _exptl_special_details ; Solvent used: Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.970(1) Frames collected: 891 Seconds exposure per frame: 64 Degrees rotation per frame: 0.8 Crystal-Detector distance (mm): 32.6 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 45202 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4541 _reflns_number_gt 3725 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2003)' _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 'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+2.6710P] 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 4541 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.54691(4) 0.149420(18) 0.75882(4) 0.01938(13) Uani 1 1 d . . . O1 O 0.5880(3) 0.25285(11) 0.9460(2) 0.0393(6) Uani 1 1 d . . . N1 N 0.8497(3) 0.09664(11) 0.7706(2) 0.0212(5) Uani 1 1 d . . . N2 N 0.8340(3) 0.11002(10) 0.9710(2) 0.0212(5) Uani 1 1 d . . . N3 N 0.5986(3) 0.19822(11) 0.6261(2) 0.0268(5) Uani 1 1 d . . . C7 C 0.7538(3) 0.11690(12) 0.8373(3) 0.0192(5) Uani 1 1 d . . . C8 C 0.9866(3) 0.07866(13) 0.8616(3) 0.0263(6) Uani 1 1 d . . . H8 H 1.0713 0.0632 0.8394 0.032 Uiso 1 1 calc R . . C9 C 0.9780(3) 0.08700(13) 0.9870(3) 0.0256(6) Uani 1 1 d . . . H9 H 1.0551 0.0788 1.0703 0.031 Uiso 1 1 calc R . . C10 C 0.8115(3) 0.08839(14) 0.6219(3) 0.0252(6) Uani 1 1 d . . . H10 H 0.7044 0.1021 0.5785 0.030 Uiso 1 1 calc R . . C11 C 0.8217(4) 0.02044(16) 0.5887(3) 0.0393(8) Uani 1 1 d . . . H11A H 0.9281 0.0075 0.6190 0.059 Uiso 1 1 calc R . . H11B H 0.7788 0.0143 0.4904 0.059 Uiso 1 1 calc R . . H11C H 0.7649 -0.0041 0.6353 0.059 Uiso 1 1 calc R . . C12 C 0.9131(4) 0.1284(2) 0.5666(4) 0.0439(9) Uani 1 1 d . . . H12A H 0.9115 0.1708 0.5982 0.066 Uiso 1 1 calc R . . H12B H 0.8764 0.1275 0.4671 0.066 Uiso 1 1 calc R . . H12C H 1.0170 0.1125 0.5991 0.066 Uiso 1 1 calc R . . C13 C 0.7769(3) 0.12061(13) 1.0868(3) 0.0236(6) Uani 1 1 d . . . H13 H 0.6695 0.1349 1.0496 0.028 Uiso 1 1 calc R . . C14 C 0.7776(4) 0.06051(15) 1.1625(3) 0.0341(7) Uani 1 1 d . . . H14A H 0.7262 0.0285 1.0977 0.051 Uiso 1 1 calc R . . H14B H 0.7247 0.0664 1.2296 0.051 Uiso 1 1 calc R . . H14C H 0.8824 0.0479 1.2088 0.051 Uiso 1 1 calc R . . C15 C 0.8674(4) 0.17119(15) 1.1782(3) 0.0341(7) Uani 1 1 d . . . H15A H 0.9720 0.1573 1.2205 0.051 Uiso 1 1 calc R . . H15B H 0.8217 0.1807 1.2491 0.051 Uiso 1 1 calc R . . H15C H 0.8669 0.2082 1.1241 0.051 Uiso 1 1 calc R . . C16 C 0.6179(4) 0.22744(15) 0.5422(3) 0.0353(7) Uani 1 1 d . . . C17 C 0.6406(6) 0.26363(18) 0.4311(4) 0.0607(12) Uani 1 1 d . . . H17A H 0.7490 0.2715 0.4498 0.091 Uiso 1 1 calc R . . H17B H 0.5866 0.3029 0.4233 0.091 Uiso 1 1 calc R . . H17C H 0.6016 0.2407 0.3458 0.091 Uiso 1 1 calc R . . C6 C 0.5764(3) 0.21223(13) 0.8731(3) 0.0252(6) Uani 1 1 d . . . C1 C 0.4635(4) 0.06379(16) 0.7898(4) 0.0455(9) Uani 1 1 d . . . H1 H 0.5218 0.0325 0.8466 0.055 Uiso 1 1 d R . . C5 C 0.4427(4) 0.07115(17) 0.6503(4) 0.0424(9) Uani 1 1 d . . . H5 H 0.4850 0.0460 0.5965 0.051 Uiso 1 1 d R . . C4 C 0.3487(3) 0.12218(18) 0.6052(3) 0.0376(8) Uani 1 1 d . . . H4 H 0.3158 0.1375 0.5147 0.045 Uiso 1 1 d R . . C3 C 0.3108(3) 0.14701(16) 0.7136(3) 0.0332(7) Uani 1 1 d . . . H3 H 0.2481 0.1819 0.7104 0.040 Uiso 1 1 d R . . C2 C 0.3833(4) 0.11064(18) 0.8308(3) 0.0383(8) Uani 1 1 d . . . H2 H 0.3783 0.1170 0.9199 0.046 Uiso 1 1 d R . . F1 F 0.5449(4) -0.16642(16) 0.8358(3) 0.0928(11) Uani 1 1 d . . . F2 F 0.4882(3) -0.10189(17) 0.6582(2) 0.0839(10) Uani 1 1 d . . . F3 F 0.7212(3) -0.14259(17) 0.7373(3) 0.0883(11) Uani 1 1 d . . . F4 F 0.6474(3) -0.07291(13) 0.8631(3) 0.0684(7) Uani 1 1 d . . . B1 B 0.6005(5) -0.1206(2) 0.7719(4) 0.0419(9) 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 0.0174(2) 0.0218(2) 0.0187(2) -0.00010(15) 0.00534(14) -0.00003(15) O1 0.0530(15) 0.0304(12) 0.0298(12) -0.0054(10) 0.0062(11) 0.0095(10) N1 0.0190(11) 0.0228(12) 0.0214(11) -0.0023(9) 0.0059(9) -0.0012(9) N2 0.0234(11) 0.0212(11) 0.0178(11) -0.0014(9) 0.0050(9) -0.0007(9) N3 0.0305(13) 0.0260(13) 0.0252(12) 0.0015(10) 0.0105(10) 0.0023(10) C7 0.0179(12) 0.0179(13) 0.0221(13) -0.0012(10) 0.0064(10) -0.0025(10) C8 0.0206(13) 0.0267(15) 0.0303(15) -0.0025(12) 0.0062(11) 0.0012(11) C9 0.0228(14) 0.0261(15) 0.0238(14) 0.0005(11) 0.0017(11) 0.0030(11) C10 0.0210(13) 0.0314(15) 0.0235(14) -0.0043(12) 0.0075(11) -0.0008(11) C11 0.0405(18) 0.0389(19) 0.0324(17) -0.0169(14) 0.0025(14) 0.0048(15) C12 0.0361(18) 0.070(3) 0.0288(17) 0.0001(16) 0.0153(14) -0.0159(17) C13 0.0291(14) 0.0251(14) 0.0168(13) 0.0009(11) 0.0077(11) 0.0004(11) C14 0.0463(19) 0.0314(17) 0.0275(16) 0.0073(12) 0.0157(14) 0.0027(14) C15 0.0394(17) 0.0355(17) 0.0255(15) -0.0083(13) 0.0076(13) -0.0039(14) C16 0.050(2) 0.0281(16) 0.0332(17) 0.0031(13) 0.0207(15) 0.0058(14) C17 0.107(4) 0.038(2) 0.055(3) 0.0189(18) 0.051(3) 0.009(2) C6 0.0247(14) 0.0261(15) 0.0235(14) 0.0030(11) 0.0058(11) 0.0042(11) C1 0.0254(16) 0.0289(17) 0.073(3) 0.0133(17) 0.0021(16) -0.0112(13) C5 0.0244(15) 0.045(2) 0.060(2) -0.0268(17) 0.0151(15) -0.0148(14) C4 0.0243(15) 0.058(2) 0.0269(16) -0.0061(15) 0.0032(12) -0.0108(15) C3 0.0162(13) 0.0418(18) 0.0405(18) -0.0053(14) 0.0073(12) -0.0004(12) C2 0.0278(16) 0.059(2) 0.0303(16) -0.0005(15) 0.0119(13) -0.0176(15) F1 0.127(3) 0.086(2) 0.082(2) -0.0033(17) 0.057(2) -0.031(2) F2 0.0603(16) 0.143(3) 0.0361(13) -0.0061(15) -0.0017(12) 0.0397(17) F3 0.0598(17) 0.152(3) 0.0602(17) -0.0007(18) 0.0285(14) 0.0389(18) F4 0.0763(18) 0.0674(17) 0.0503(15) -0.0080(12) 0.0038(13) 0.0037(14) B1 0.040(2) 0.061(3) 0.0264(19) 0.0005(17) 0.0136(16) 0.0081(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C6 1.770(3) . ? Fe1 N3 1.915(2) . ? Fe1 C7 1.969(3) . ? Fe1 C2 2.074(3) . ? Fe1 C1 2.078(3) . ? Fe1 C3 2.097(3) . ? Fe1 C5 2.099(3) . ? Fe1 C4 2.106(3) . ? O1 C6 1.145(4) . ? N1 C7 1.362(3) . ? N1 C8 1.381(4) . ? N1 C10 1.481(4) . ? N2 C7 1.360(3) . ? N2 C9 1.390(4) . ? N2 C13 1.478(3) . ? N3 C16 1.136(4) . ? C8 C9 1.340(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C12 1.523(4) . ? C10 C11 1.524(4) . ? C10 H10 1.0000 . ? 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 C15 1.520(4) . ? C13 C14 1.521(4) . ? C13 H13 1.0000 . ? 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 C17 1.465(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C1 C2 1.404(5) . ? C1 C5 1.408(6) . ? C1 H1 0.9494 . ? C5 C4 1.398(5) . ? C5 H5 0.9505 . ? C4 C3 1.389(5) . ? C4 H4 0.9510 . ? C3 C2 1.428(5) . ? C3 H3 0.9504 . ? C2 H2 0.9502 . ? F1 B1 1.383(5) . ? F2 B1 1.368(5) . ? F3 B1 1.368(5) . ? F4 B1 1.378(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 N3 91.97(12) . . ? C6 Fe1 C7 94.28(12) . . ? N3 Fe1 C7 93.50(11) . . ? C6 Fe1 C2 92.74(14) . . ? N3 Fe1 C2 149.64(13) . . ? C7 Fe1 C2 116.01(13) . . ? C6 Fe1 C1 124.88(16) . . ? N3 Fe1 C1 142.83(15) . . ? C7 Fe1 C1 88.83(12) . . ? C2 Fe1 C1 39.53(15) . . ? C6 Fe1 C3 95.68(13) . . ? N3 Fe1 C3 109.63(12) . . ? C7 Fe1 C3 154.40(12) . . ? C2 Fe1 C3 40.03(13) . . ? C1 Fe1 C3 66.18(14) . . ? C6 Fe1 C5 158.51(14) . . ? N3 Fe1 C5 103.89(14) . . ? C7 Fe1 C5 99.05(13) . . ? C2 Fe1 C5 66.27(14) . . ? C1 Fe1 C5 39.40(16) . . ? C3 Fe1 C5 65.54(13) . . ? C6 Fe1 C4 129.53(14) . . ? N3 Fe1 C4 88.26(12) . . ? C7 Fe1 C4 136.10(13) . . ? C2 Fe1 C4 65.90(13) . . ? C1 Fe1 C4 65.50(15) . . ? C3 Fe1 C4 38.60(13) . . ? C5 Fe1 C4 38.82(15) . . ? C7 N1 C8 110.8(2) . . ? C7 N1 C10 126.0(2) . . ? C8 N1 C10 123.0(2) . . ? C7 N2 C9 111.1(2) . . ? C7 N2 C13 126.1(2) . . ? C9 N2 C13 122.6(2) . . ? C16 N3 Fe1 174.8(3) . . ? N2 C7 N1 104.2(2) . . ? N2 C7 Fe1 127.7(2) . . ? N1 C7 Fe1 128.11(19) . . ? C9 C8 N1 107.5(2) . . ? C9 C8 H8 126.3 . . ? N1 C8 H8 126.3 . . ? C8 C9 N2 106.4(2) . . ? C8 C9 H9 126.8 . . ? N2 C9 H9 126.8 . . ? N1 C10 C12 110.5(2) . . ? N1 C10 C11 109.9(2) . . ? C12 C10 C11 112.1(3) . . ? N1 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C15 110.4(2) . . ? N2 C13 C14 110.0(2) . . ? C15 C13 C14 112.7(2) . . ? N2 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 178.2(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C6 Fe1 176.6(3) . . ? C2 C1 C5 108.4(3) . . ? C2 C1 Fe1 70.08(19) . . ? C5 C1 Fe1 71.10(19) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe1 C1 H1 124.6 . . ? C4 C5 C1 107.6(3) . . ? C4 C5 Fe1 70.88(19) . . ? C1 C5 Fe1 69.50(19) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe1 C5 H5 125.0 . . ? C3 C4 C5 109.2(3) . . ? C3 C4 Fe1 70.34(18) . . ? C5 C4 Fe1 70.30(18) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? Fe1 C4 H4 125.5 . . ? C4 C3 C2 107.6(3) . . ? C4 C3 Fe1 71.06(18) . . ? C2 C3 Fe1 69.12(17) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe1 C3 H3 125.2 . . ? C1 C2 C3 107.2(3) . . ? C1 C2 Fe1 70.39(18) . . ? C3 C2 Fe1 70.85(18) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 126.4 . . ? Fe1 C2 H2 124.0 . . ? F2 B1 F3 110.2(3) . . ? F2 B1 F4 111.0(4) . . ? F3 B1 F4 109.5(4) . . ? F2 B1 F1 109.1(4) . . ? F3 B1 F1 109.8(4) . . ? F4 B1 F1 107.2(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 C6 Fe1 N3 C16 -103(3) . . . . ? C7 Fe1 N3 C16 163(3) . . . . ? C2 Fe1 N3 C16 -4(3) . . . . ? C1 Fe1 N3 C16 70(3) . . . . ? C3 Fe1 N3 C16 -6(3) . . . . ? C5 Fe1 N3 C16 63(3) . . . . ? C4 Fe1 N3 C16 27(3) . . . . ? C9 N2 C7 N1 1.1(3) . . . . ? C13 N2 C7 N1 -174.7(2) . . . . ? C9 N2 C7 Fe1 -178.4(2) . . . . ? C13 N2 C7 Fe1 5.8(4) . . . . ? C8 N1 C7 N2 -0.9(3) . . . . ? C10 N1 C7 N2 173.3(2) . . . . ? C8 N1 C7 Fe1 178.6(2) . . . . ? C10 N1 C7 Fe1 -7.2(4) . . . . ? C6 Fe1 C7 N2 44.5(3) . . . . ? N3 Fe1 C7 N2 136.7(2) . . . . ? C2 Fe1 C7 N2 -50.7(3) . . . . ? C1 Fe1 C7 N2 -80.4(3) . . . . ? C3 Fe1 C7 N2 -68.2(4) . . . . ? C5 Fe1 C7 N2 -118.6(3) . . . . ? C4 Fe1 C7 N2 -132.1(2) . . . . ? C6 Fe1 C7 N1 -134.9(2) . . . . ? N3 Fe1 C7 N1 -42.7(2) . . . . ? C2 Fe1 C7 N1 129.9(2) . . . . ? C1 Fe1 C7 N1 100.2(3) . . . . ? C3 Fe1 C7 N1 112.4(3) . . . . ? C5 Fe1 C7 N1 62.0(3) . . . . ? C4 Fe1 C7 N1 48.4(3) . . . . ? C7 N1 C8 C9 0.5(3) . . . . ? C10 N1 C8 C9 -174.0(3) . . . . ? N1 C8 C9 N2 0.2(3) . . . . ? C7 N2 C9 C8 -0.8(3) . . . . ? C13 N2 C9 C8 175.1(2) . . . . ? C7 N1 C10 C12 120.6(3) . . . . ? C8 N1 C10 C12 -65.9(4) . . . . ? C7 N1 C10 C11 -115.2(3) . . . . ? C8 N1 C10 C11 58.3(3) . . . . ? C7 N2 C13 C15 -119.2(3) . . . . ? C9 N2 C13 C15 65.6(3) . . . . ? C7 N2 C13 C14 115.8(3) . . . . ? C9 N2 C13 C14 -59.5(3) . . . . ? Fe1 N3 C16 C17 -62(14) . . . . ? N3 Fe1 C6 O1 113(4) . . . . ? C7 Fe1 C6 O1 -154(4) . . . . ? C2 Fe1 C6 O1 -37(4) . . . . ? C1 Fe1 C6 O1 -62(5) . . . . ? C3 Fe1 C6 O1 3(4) . . . . ? C5 Fe1 C6 O1 -25(5) . . . . ? C4 Fe1 C6 O1 23(5) . . . . ? C6 Fe1 C1 C2 41.1(3) . . . . ? N3 Fe1 C1 C2 -130.2(2) . . . . ? C7 Fe1 C1 C2 135.5(2) . . . . ? C3 Fe1 C1 C2 -38.7(2) . . . . ? C5 Fe1 C1 C2 -118.6(3) . . . . ? C4 Fe1 C1 C2 -81.2(2) . . . . ? C6 Fe1 C1 C5 159.8(2) . . . . ? N3 Fe1 C1 C5 -11.6(3) . . . . ? C7 Fe1 C1 C5 -105.8(2) . . . . ? C2 Fe1 C1 C5 118.6(3) . . . . ? C3 Fe1 C1 C5 79.9(2) . . . . ? C4 Fe1 C1 C5 37.4(2) . . . . ? C2 C1 C5 C4 -0.5(4) . . . . ? Fe1 C1 C5 C4 -61.0(2) . . . . ? C2 C1 C5 Fe1 60.4(2) . . . . ? C6 Fe1 C5 C4 67.4(5) . . . . ? N3 Fe1 C5 C4 -69.1(2) . . . . ? C7 Fe1 C5 C4 -165.0(2) . . . . ? C2 Fe1 C5 C4 80.5(2) . . . . ? C1 Fe1 C5 C4 118.1(3) . . . . ? C3 Fe1 C5 C4 36.5(2) . . . . ? C6 Fe1 C5 C1 -50.7(5) . . . . ? N3 Fe1 C5 C1 172.8(2) . . . . ? C7 Fe1 C5 C1 76.9(2) . . . . ? C2 Fe1 C5 C1 -37.6(2) . . . . ? C3 Fe1 C5 C1 -81.6(2) . . . . ? C4 Fe1 C5 C1 -118.1(3) . . . . ? C1 C5 C4 C3 0.3(4) . . . . ? Fe1 C5 C4 C3 -59.8(2) . . . . ? C1 C5 C4 Fe1 60.1(2) . . . . ? C6 Fe1 C4 C3 -34.1(3) . . . . ? N3 Fe1 C4 C3 -125.2(2) . . . . ? C7 Fe1 C4 C3 141.5(2) . . . . ? C2 Fe1 C4 C3 38.4(2) . . . . ? C1 Fe1 C4 C3 81.9(2) . . . . ? C5 Fe1 C4 C3 119.9(3) . . . . ? C6 Fe1 C4 C5 -154.0(2) . . . . ? N3 Fe1 C4 C5 114.9(2) . . . . ? C7 Fe1 C4 C5 21.6(3) . . . . ? C2 Fe1 C4 C5 -81.5(2) . . . . ? C1 Fe1 C4 C5 -38.0(2) . . . . ? C3 Fe1 C4 C5 -119.9(3) . . . . ? C5 C4 C3 C2 0.1(4) . . . . ? Fe1 C4 C3 C2 -59.7(2) . . . . ? C5 C4 C3 Fe1 59.8(2) . . . . ? C6 Fe1 C3 C4 154.2(2) . . . . ? N3 Fe1 C3 C4 60.1(2) . . . . ? C7 Fe1 C3 C4 -93.3(3) . . . . ? C2 Fe1 C3 C4 -118.3(3) . . . . ? C1 Fe1 C3 C4 -80.0(2) . . . . ? C5 Fe1 C3 C4 -36.7(2) . . . . ? C6 Fe1 C3 C2 -87.5(2) . . . . ? N3 Fe1 C3 C2 178.4(2) . . . . ? C7 Fe1 C3 C2 24.9(4) . . . . ? C1 Fe1 C3 C2 38.3(2) . . . . ? C5 Fe1 C3 C2 81.6(2) . . . . ? C4 Fe1 C3 C2 118.3(3) . . . . ? C5 C1 C2 C3 0.6(4) . . . . ? Fe1 C1 C2 C3 61.7(2) . . . . ? C5 C1 C2 Fe1 -61.1(2) . . . . ? C4 C3 C2 C1 -0.4(4) . . . . ? Fe1 C3 C2 C1 -61.4(2) . . . . ? C4 C3 C2 Fe1 60.9(2) . . . . ? C6 Fe1 C2 C1 -147.3(2) . . . . ? N3 Fe1 C2 C1 114.1(3) . . . . ? C7 Fe1 C2 C1 -51.2(2) . . . . ? C3 Fe1 C2 C1 117.1(3) . . . . ? C5 Fe1 C2 C1 37.5(2) . . . . ? C4 Fe1 C2 C1 80.1(2) . . . . ? C6 Fe1 C2 C3 95.6(2) . . . . ? N3 Fe1 C2 C3 -3.0(4) . . . . ? C7 Fe1 C2 C3 -168.31(18) . . . . ? C1 Fe1 C2 C3 -117.1(3) . . . . ? C5 Fe1 C2 C3 -79.6(2) . . . . ? C4 Fe1 C2 C3 -37.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.575 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.085