# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Sumio Kaizaki' _publ_contact_author_address ; Department of Chemistry Graduate School of Science, Osaka University Toyonaka Osaka 560-0043 JAPAN ; _publ_contact_author_email KAIZAKI@CHEM.SCI.OSAKA-U.AC.JP _publ_section_title ; Direct Two-Step Spin-Crossover through [HS-HS]للل[LS-LS] at the Plateau in Dinuclear Diiron(II) Complex [{Fe(NCBH3)(4phpy)}2(m-bpypz)2] ; loop_ _publ_author_name 'Sumio Kaizaki' 'Akira Fuyuhiro' 'Satoshi Kawata' 'Syotaro Morimoto' 'Keisaku Nakano' 'Saburo Nasu' ; T.Yagi ; 'Ko Yoneda' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 241137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 B2 Fe2 N12' _chemical_formula_weight 944.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0589(3) _cell_length_b 10.6824(11) _cell_length_c 12.6458(8) _cell_angle_alpha 93.521(8) _cell_angle_beta 109.122(12) _cell_angle_gamma 104.560(8) _cell_volume 1105.17(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8549 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6771 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4314 _reflns_number_gt 3442 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4314 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.00440(5) 0.31616(4) 0.45603(4) 0.02352(18) Uani 1 1 d . . . N1 N 1.2040(3) 0.2491(3) 0.5042(2) 0.0255(6) Uani 1 1 d . . . N2 N 1.1672(3) 0.4749(3) 0.5434(2) 0.0239(5) Uani 1 1 d . . . N3 N 1.1647(3) 0.5983(3) 0.5709(2) 0.0227(5) Uani 1 1 d . . . N4 N 1.1905(4) 0.8322(3) 0.6496(2) 0.0283(6) Uani 1 1 d . . . N5 N 0.9612(3) 0.2459(3) 0.5858(2) 0.0274(6) Uani 1 1 d . . . N6 N 1.0545(3) 0.3640(3) 0.3199(2) 0.0244(5) Uani 1 1 d . . . C1 C 1.2145(5) 0.1262(3) 0.4913(3) 0.0312(7) Uani 1 1 d . . . C2 C 1.3591(5) 0.0943(4) 0.5265(3) 0.0362(8) Uani 1 1 d . . . C3 C 1.5029(5) 0.1918(4) 0.5810(3) 0.0350(8) Uani 1 1 d . . . C4 C 1.4946(4) 0.3198(4) 0.5987(3) 0.0304(7) Uani 1 1 d . . . C5 C 1.3460(4) 0.3449(3) 0.5602(3) 0.0276(7) Uani 1 1 d . . . C6 C 1.3251(4) 0.4736(3) 0.5799(3) 0.0257(6) Uani 1 1 d . . . C7 C 1.4263(4) 0.5966(3) 0.6316(3) 0.0269(7) Uani 1 1 d . . . C8 C 1.3208(4) 0.6724(3) 0.6252(3) 0.0272(7) Uani 1 1 d . . . C9 C 1.3347(4) 0.8040(3) 0.6726(3) 0.0275(7) Uani 1 1 d . . . C10 C 1.4823(5) 0.8898(4) 0.7432(3) 0.0330(7) Uani 1 1 d . . . C11 C 1.4832(5) 1.0062(4) 0.7973(3) 0.0379(9) Uani 1 1 d . . . C12 C 1.3368(5) 1.0332(4) 0.7785(3) 0.0365(8) Uani 1 1 d . . . C13 C 1.1954(5) 0.9463(3) 0.7036(3) 0.0334(8) Uani 1 1 d . . . C14 C 0.9428(4) 0.1937(3) 0.6595(3) 0.0282(7) Uani 1 1 d . . . C15 C 1.0989(4) 0.2835(3) 0.2576(3) 0.0273(7) Uani 1 1 d . . . C16 C 1.1488(4) 0.3193(3) 0.1689(3) 0.0294(7) Uani 1 1 d . . . C17 C 1.1558(4) 0.4440(3) 0.1404(3) 0.0258(7) Uani 1 1 d . . . C18 C 1.1012(4) 0.5236(3) 0.2012(3) 0.0271(7) Uani 1 1 d . . . C19 C 1.0528(4) 0.4821(3) 0.2877(3) 0.0268(7) Uani 1 1 d . . . C20 C 1.2214(4) 0.4903(4) 0.0523(3) 0.0302(7) Uani 1 1 d . . . C21 C 1.2321(5) 0.4026(4) -0.0292(3) 0.0351(8) Uani 1 1 d . . . C22 C 1.2947(5) 0.4462(5) -0.1093(3) 0.0424(9) Uani 1 1 d . . . C23 C 1.3508(5) 0.5796(5) -0.1095(3) 0.0432(9) Uani 1 1 d . . . C24 C 1.3398(6) 0.6669(5) -0.0307(4) 0.0455(10) Uani 1 1 d . . . C25 C 1.2746(5) 0.6238(4) 0.0500(3) 0.0376(8) Uani 1 1 d . . . B1 B 0.9177(6) 0.1196(4) 0.7604(4) 0.0367(9) Uani 1 1 d . . . H1 H 1.108(5) 0.056(4) 0.449(4) 0.038 Uiso 1 1 d . . . H2 H 1.344(5) -0.004(4) 0.515(4) 0.038 Uiso 1 1 d . . . H3 H 1.597(5) 0.169(4) 0.612(4) 0.038 Uiso 1 1 d . . . H4 H 1.583(5) 0.393(4) 0.636(4) 0.038 Uiso 1 1 d . . . H5 H 1.562(5) 0.621(4) 0.671(4) 0.038 Uiso 1 1 d . . . H6 H 1.577(5) 0.873(4) 0.752(4) 0.038 Uiso 1 1 d . . . H7 H 1.585(5) 1.057(4) 0.849(4) 0.038 Uiso 1 1 d . . . H8 H 1.337(5) 1.102(4) 0.814(4) 0.038 Uiso 1 1 d . . . H9 H 1.097(6) 0.966(4) 0.684(4) 0.038 Uiso 1 1 d . . . H10 H 0.832(5) 0.005(4) 0.725(4) 0.038 Uiso 1 1 d . . . H11 H 0.866(5) 0.189(4) 0.810(4) 0.038 Uiso 1 1 d . . . H12 H 1.052(5) 0.116(4) 0.827(4) 0.038 Uiso 1 1 d . . . H13 H 1.096(5) 0.197(4) 0.275(4) 0.038 Uiso 1 1 d . . . H14 H 1.179(5) 0.245(4) 0.127(4) 0.038 Uiso 1 1 d . . . H15 H 1.100(5) 0.603(4) 0.181(4) 0.038 Uiso 1 1 d . . . H16 H 1.013(5) 0.541(4) 0.333(4) 0.038 Uiso 1 1 d . . . H17 H 1.199(5) 0.306(4) -0.030(4) 0.038 Uiso 1 1 d . . . H18 H 1.314(5) 0.387(4) -0.170(4) 0.038 Uiso 1 1 d . . . H19 H 1.389(5) 0.605(4) -0.161(4) 0.038 Uiso 1 1 d . . . H20 H 1.369(5) 0.746(4) -0.028(4) 0.038 Uiso 1 1 d . . . H21 H 1.268(5) 0.685(4) 0.102(4) 0.038 Uiso 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 0.0229(3) 0.0204(3) 0.0276(3) 0.00437(17) 0.01073(18) 0.00445(18) N1 0.0276(14) 0.0257(14) 0.0276(13) 0.0066(10) 0.0150(11) 0.0078(11) N2 0.0259(14) 0.0181(12) 0.0271(13) 0.0049(10) 0.0102(10) 0.0041(10) N3 0.0209(13) 0.0215(13) 0.0259(13) 0.0029(10) 0.0099(10) 0.0048(10) N4 0.0298(14) 0.0242(14) 0.0308(14) 0.0034(11) 0.0139(11) 0.0040(11) N5 0.0275(14) 0.0200(13) 0.0347(15) 0.0004(11) 0.0129(11) 0.0052(11) N6 0.0236(13) 0.0190(13) 0.0281(13) 0.0023(10) 0.0090(10) 0.0026(10) C1 0.0389(19) 0.0238(17) 0.0335(17) 0.0082(13) 0.0153(15) 0.0094(15) C2 0.042(2) 0.0316(19) 0.0394(19) 0.0091(15) 0.0171(16) 0.0146(16) C3 0.0337(19) 0.038(2) 0.0408(19) 0.0110(15) 0.0171(15) 0.0165(16) C4 0.0257(16) 0.0329(19) 0.0318(17) 0.0076(14) 0.0096(13) 0.0074(14) C5 0.0294(17) 0.0281(17) 0.0272(16) 0.0071(13) 0.0131(13) 0.0069(13) C6 0.0248(16) 0.0259(16) 0.0280(15) 0.0086(12) 0.0108(12) 0.0073(13) C7 0.0257(16) 0.0272(16) 0.0262(15) 0.0044(12) 0.0108(12) 0.0025(13) C8 0.0273(16) 0.0241(16) 0.0259(15) 0.0045(12) 0.0105(12) -0.0014(13) C9 0.0273(16) 0.0251(16) 0.0273(15) 0.0044(13) 0.0115(12) 0.0004(13) C10 0.0297(18) 0.0284(18) 0.0379(19) 0.0048(14) 0.0113(14) 0.0045(14) C11 0.038(2) 0.0262(18) 0.0369(19) -0.0019(15) 0.0093(16) -0.0043(15) C12 0.040(2) 0.0264(18) 0.040(2) -0.0002(15) 0.0148(16) 0.0061(15) C13 0.0370(19) 0.0245(17) 0.0372(19) 0.0027(14) 0.0157(15) 0.0034(15) C14 0.0285(17) 0.0209(16) 0.0368(18) 0.0023(13) 0.0151(14) 0.0055(13) C15 0.0278(16) 0.0208(16) 0.0340(17) 0.0034(12) 0.0120(13) 0.0070(13) C16 0.0321(17) 0.0292(17) 0.0277(16) 0.0032(13) 0.0106(13) 0.0103(14) C17 0.0227(15) 0.0272(17) 0.0246(15) 0.0027(12) 0.0073(12) 0.0038(12) C18 0.0275(16) 0.0237(16) 0.0287(16) 0.0041(13) 0.0100(13) 0.0049(13) C19 0.0257(16) 0.0227(16) 0.0313(16) 0.0048(12) 0.0099(13) 0.0056(13) C20 0.0280(17) 0.0361(19) 0.0274(16) 0.0064(13) 0.0111(13) 0.0090(14) C21 0.0351(19) 0.040(2) 0.0316(18) 0.0036(15) 0.0105(14) 0.0155(16) C22 0.043(2) 0.061(3) 0.0305(19) 0.0108(17) 0.0143(16) 0.025(2) C23 0.045(2) 0.062(3) 0.0300(19) 0.0177(18) 0.0200(16) 0.018(2) C24 0.056(3) 0.042(2) 0.045(2) 0.0168(19) 0.0274(19) 0.009(2) C25 0.046(2) 0.035(2) 0.0368(19) 0.0054(15) 0.0236(17) 0.0096(17) B1 0.049(3) 0.030(2) 0.036(2) 0.0103(16) 0.0200(19) 0.0106(18) _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 N3 1.923(3) 2_766 ? Fe1 N2 1.928(3) . ? Fe1 N5 1.958(3) . ? Fe1 N6 1.984(3) . ? Fe1 N1 2.034(3) . ? Fe1 N4 2.050(3) 2_766 ? N1 C1 1.344(4) . ? N1 C5 1.362(4) . ? N2 N3 1.350(4) . ? N2 C6 1.356(4) . ? N3 C8 1.353(4) . ? N3 Fe1 1.923(3) 2_766 ? N4 C13 1.344(5) . ? N4 C9 1.357(5) . ? N4 Fe1 2.050(3) 2_766 ? N5 C14 1.151(5) . ? N6 C15 1.348(4) . ? N6 C19 1.351(4) . ? C1 C2 1.376(5) . ? C1 H1 1.01(4) . ? C2 C3 1.378(6) . ? C2 H2 1.02(4) . ? C3 C4 1.397(5) . ? C3 H3 0.92(4) . ? C4 C5 1.374(5) . ? C4 H4 0.93(4) . ? C5 C6 1.452(5) . ? C6 C7 1.376(5) . ? C7 C8 1.386(5) . ? C7 H5 1.12(4) . ? C8 C9 1.453(5) . ? C9 C10 1.388(5) . ? C10 C11 1.378(5) . ? C10 H6 0.89(4) . ? C11 C12 1.375(6) . ? C11 H7 0.94(4) . ? C12 C13 1.378(5) . ? C12 H8 0.84(4) . ? C13 H9 0.92(4) . ? C14 B1 1.590(5) . ? C15 C16 1.381(5) . ? C15 H13 0.96(4) . ? C16 C17 1.393(5) . ? C16 H14 1.07(4) . ? C17 C18 1.393(5) . ? C17 C20 1.481(5) . ? C18 C19 1.365(5) . ? C18 H15 0.90(4) . ? C19 H16 1.03(4) . ? C20 C25 1.392(5) . ? C20 C21 1.393(5) . ? C21 C22 1.366(6) . ? C21 H17 1.00(4) . ? C22 C23 1.388(6) . ? C22 H18 1.05(4) . ? C23 C24 1.367(6) . ? C23 H19 0.86(5) . ? C24 C25 1.385(5) . ? C24 H20 0.81(4) . ? C25 H21 0.93(4) . ? B1 H10 1.24(4) . ? B1 H11 1.21(4) . ? B1 H12 1.24(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 N3 Fe1 N2 91.22(11) 2_766 . ? N3 Fe1 N5 92.61(11) 2_766 . ? N2 Fe1 N5 95.53(11) . . ? N3 Fe1 N6 93.87(11) 2_766 . ? N2 Fe1 N6 89.06(11) . . ? N5 Fe1 N6 171.98(11) . . ? N3 Fe1 N1 171.17(11) 2_766 . ? N2 Fe1 N1 80.37(11) . . ? N5 Fe1 N1 85.59(11) . . ? N6 Fe1 N1 88.71(11) . . ? N3 Fe1 N4 80.04(11) 2_766 2_766 ? N2 Fe1 N4 170.38(11) . 2_766 ? N5 Fe1 N4 88.92(11) . 2_766 ? N6 Fe1 N4 87.55(11) . 2_766 ? N1 Fe1 N4 108.53(11) . 2_766 ? C1 N1 C5 116.7(3) . . ? C1 N1 Fe1 129.7(2) . . ? C5 N1 Fe1 113.6(2) . . ? N3 N2 C6 107.9(3) . . ? N3 N2 Fe1 134.4(2) . . ? C6 N2 Fe1 117.4(2) . . ? N2 N3 C8 107.8(3) . . ? N2 N3 Fe1 134.3(2) . 2_766 ? C8 N3 Fe1 117.9(2) . 2_766 ? C13 N4 C9 116.5(3) . . ? C13 N4 Fe1 130.4(3) . 2_766 ? C9 N4 Fe1 113.0(2) . 2_766 ? C14 N5 Fe1 172.4(3) . . ? C15 N6 C19 116.5(3) . . ? C15 N6 Fe1 122.1(2) . . ? C19 N6 Fe1 121.3(2) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 116(2) . . ? C2 C1 H1 120(2) . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 114(2) . . ? C3 C2 H2 127(2) . . ? C2 C3 C4 118.0(3) . . ? C2 C3 H3 119(3) . . ? C4 C3 H3 123(3) . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 115(3) . . ? C3 C4 H4 125(3) . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 114.1(3) . . ? C4 C5 C6 123.3(3) . . ? N2 C6 C7 110.2(3) . . ? N2 C6 C5 113.9(3) . . ? C7 C6 C5 135.9(3) . . ? C6 C7 C8 104.2(3) . . ? C6 C7 H5 124(2) . . ? C8 C7 H5 132(2) . . ? N3 C8 C7 110.0(3) . . ? N3 C8 C9 113.4(3) . . ? C7 C8 C9 136.0(3) . . ? N4 C9 C10 122.8(3) . . ? N4 C9 C8 114.6(3) . . ? C10 C9 C8 122.4(3) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H6 119(3) . . ? C9 C10 H6 122(3) . . ? C12 C11 C10 118.5(3) . . ? C12 C11 H7 125(3) . . ? C10 C11 H7 116(3) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 H8 118(3) . . ? C13 C12 H8 122(3) . . ? N4 C13 C12 123.5(4) . . ? N4 C13 H9 115(3) . . ? C12 C13 H9 121(3) . . ? N5 C14 B1 179.2(3) . . ? N6 C15 C16 123.2(3) . . ? N6 C15 H13 119(3) . . ? C16 C15 H13 118(3) . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H14 115(2) . . ? C17 C16 H14 125(2) . . ? C16 C17 C18 116.2(3) . . ? C16 C17 C20 121.8(3) . . ? C18 C17 C20 122.0(3) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H15 122(3) . . ? C17 C18 H15 117(3) . . ? N6 C19 C18 123.2(3) . . ? N6 C19 H16 116(2) . . ? C18 C19 H16 121(2) . . ? C25 C20 C21 118.6(3) . . ? C25 C20 C17 120.0(3) . . ? C21 C20 C17 121.4(3) . . ? C22 C21 C20 121.0(4) . . ? C22 C21 H17 117(3) . . ? C20 C21 H17 122(3) . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H18 125(2) . . ? C23 C22 H18 114(2) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H19 122(3) . . ? C22 C23 H19 118(3) . . ? C23 C24 C25 120.7(4) . . ? C23 C24 H20 124(3) . . ? C25 C24 H20 115(3) . . ? C24 C25 C20 119.9(4) . . ? C24 C25 H21 119(3) . . ? C20 C25 H21 121(3) . . ? C14 B1 H10 111(2) . . ? C14 B1 H11 104(2) . . ? H10 B1 H11 117(3) . . ? C14 B1 H12 110(2) . . ? H10 B1 H12 107(3) . . ? H11 B1 H12 108(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 N3 Fe1 N1 C1 154.3(6) 2_766 . . . ? N2 Fe1 N1 C1 172.2(3) . . . . ? N5 Fe1 N1 C1 75.8(3) . . . . ? N6 Fe1 N1 C1 -98.6(3) . . . . ? N4 Fe1 N1 C1 -11.6(3) 2_766 . . . ? N3 Fe1 N1 C5 -23.7(8) 2_766 . . . ? N2 Fe1 N1 C5 -5.9(2) . . . . ? N5 Fe1 N1 C5 -102.3(2) . . . . ? N6 Fe1 N1 C5 83.4(2) . . . . ? N4 Fe1 N1 C5 170.4(2) 2_766 . . . ? N3 Fe1 N2 N3 -2.4(3) 2_766 . . . ? N5 Fe1 N2 N3 -95.1(3) . . . . ? N6 Fe1 N2 N3 91.5(3) . . . . ? N1 Fe1 N2 N3 -179.7(3) . . . . ? N4 Fe1 N2 N3 22.2(9) 2_766 . . . ? N3 Fe1 N2 C6 -175.0(2) 2_766 . . . ? N5 Fe1 N2 C6 92.2(2) . . . . ? N6 Fe1 N2 C6 -81.2(2) . . . . ? N1 Fe1 N2 C6 7.7(2) . . . . ? N4 Fe1 N2 C6 -150.5(6) 2_766 . . . ? C6 N2 N3 C8 -0.6(3) . . . . ? Fe1 N2 N3 C8 -173.8(2) . . . . ? C6 N2 N3 Fe1 176.5(2) . . . 2_766 ? Fe1 N2 N3 Fe1 3.3(5) . . . 2_766 ? N3 Fe1 N5 C14 154(2) 2_766 . . . ? N2 Fe1 N5 C14 -115(2) . . . . ? N6 Fe1 N5 C14 10(3) . . . . ? N1 Fe1 N5 C14 -35(2) . . . . ? N4 Fe1 N5 C14 74(2) 2_766 . . . ? N3 Fe1 N6 C15 -144.7(3) 2_766 . . . ? N2 Fe1 N6 C15 124.1(3) . . . . ? N5 Fe1 N6 C15 -0.9(9) . . . . ? N1 Fe1 N6 C15 43.7(3) . . . . ? N4 Fe1 N6 C15 -64.9(3) 2_766 . . . ? N3 Fe1 N6 C19 38.3(3) 2_766 . . . ? N2 Fe1 N6 C19 -52.8(3) . . . . ? N5 Fe1 N6 C19 -177.9(7) . . . . ? N1 Fe1 N6 C19 -133.2(3) . . . . ? N4 Fe1 N6 C19 118.2(3) 2_766 . . . ? C5 N1 C1 C2 -3.1(5) . . . . ? Fe1 N1 C1 C2 178.8(3) . . . . ? N1 C1 C2 C3 1.8(6) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C1 N1 C5 C4 2.4(5) . . . . ? Fe1 N1 C5 C4 -179.3(3) . . . . ? C1 N1 C5 C6 -175.0(3) . . . . ? Fe1 N1 C5 C6 3.4(4) . . . . ? C3 C4 C5 N1 -0.4(5) . . . . ? C3 C4 C5 C6 176.7(3) . . . . ? N3 N2 C6 C7 0.0(4) . . . . ? Fe1 N2 C6 C7 174.6(2) . . . . ? N3 N2 C6 C5 177.5(3) . . . . ? Fe1 N2 C6 C5 -8.0(4) . . . . ? N1 C5 C6 N2 2.7(4) . . . . ? C4 C5 C6 N2 -174.6(3) . . . . ? N1 C5 C6 C7 179.3(4) . . . . ? C4 C5 C6 C7 1.9(6) . . . . ? N2 C6 C7 C8 0.5(4) . . . . ? C5 C6 C7 C8 -176.2(4) . . . . ? N2 N3 C8 C7 0.9(4) . . . . ? Fe1 N3 C8 C7 -176.7(2) 2_766 . . . ? N2 N3 C8 C9 -172.5(3) . . . . ? Fe1 N3 C8 C9 9.9(4) 2_766 . . . ? C6 C7 C8 N3 -0.9(4) . . . . ? C6 C7 C8 C9 170.4(4) . . . . ? C13 N4 C9 C10 -3.3(5) . . . . ? Fe1 N4 C9 C10 -179.3(3) 2_766 . . . ? C13 N4 C9 C8 171.7(3) . . . . ? Fe1 N4 C9 C8 -4.3(4) 2_766 . . . ? N3 C8 C9 N4 -3.2(4) . . . . ? C7 C8 C9 N4 -174.2(4) . . . . ? N3 C8 C9 C10 171.8(3) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? N4 C9 C10 C11 3.3(6) . . . . ? C8 C9 C10 C11 -171.3(3) . . . . ? C9 C10 C11 C12 -0.3(6) . . . . ? C10 C11 C12 C13 -2.4(6) . . . . ? C9 N4 C13 C12 0.4(5) . . . . ? Fe1 N4 C13 C12 175.5(3) 2_766 . . . ? C11 C12 C13 N4 2.5(6) . . . . ? Fe1 N5 C14 B1 -17(29) . . . . ? C19 N6 C15 C16 3.2(5) . . . . ? Fe1 N6 C15 C16 -173.9(3) . . . . ? N6 C15 C16 C17 0.4(5) . . . . ? C15 C16 C17 C18 -3.7(5) . . . . ? C15 C16 C17 C20 174.8(3) . . . . ? C16 C17 C18 C19 3.6(5) . . . . ? C20 C17 C18 C19 -175.0(3) . . . . ? C15 N6 C19 C18 -3.4(5) . . . . ? Fe1 N6 C19 C18 173.7(3) . . . . ? C17 C18 C19 N6 0.0(5) . . . . ? C16 C17 C20 C25 -159.7(4) . . . . ? C18 C17 C20 C25 18.8(5) . . . . ? C16 C17 C20 C21 20.1(5) . . . . ? C18 C17 C20 C21 -161.4(3) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? C17 C20 C21 C22 -179.1(3) . . . . ? C20 C21 C22 C23 0.8(6) . . . . ? C21 C22 C23 C24 -1.4(6) . . . . ? C22 C23 C24 C25 0.5(7) . . . . ? C23 C24 C25 C20 0.8(7) . . . . ? C21 C20 C25 C24 -1.4(6) . . . . ? C17 C20 C25 C24 178.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 1.565 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.212 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 241138' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 B2 Fe2 N12' _chemical_formula_weight 944.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3509(2) _cell_length_b 14.91240(10) _cell_length_c 17.1648(4) _cell_angle_alpha 99.6120(10) _cell_angle_beta 94.5510(10) _cell_angle_gamma 98.1740(10) _cell_volume 2322.89(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11936 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _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 ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17830 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.1240 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10011 _reflns_number_gt 4730 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10011 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1614 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12542(7) 0.60719(4) 0.07481(4) 0.0389(2) Uani 1 1 d . . . Fe2 Fe 0.61665(7) 1.12243(4) 0.56817(4) 0.0438(2) Uani 1 1 d . . . N1 N 0.0716(4) 0.7365(3) 0.1075(2) 0.0507(10) Uani 1 1 d . . . N2 N -0.0700(4) 0.5882(2) 0.0219(2) 0.0386(9) Uani 1 1 d . . . N3 N -0.1532(4) 0.5170(2) -0.0291(2) 0.0364(9) Uani 1 1 d . . . N4 N -0.3299(4) 0.3942(3) -0.1271(2) 0.0431(9) Uani 1 1 d . . . N5 N 0.0557(4) 0.5749(3) 0.1754(3) 0.0483(10) Uani 1 1 d . . . N6 N 0.2155(4) 0.6535(2) -0.0160(2) 0.0421(9) Uani 1 1 d . . . N7 N 0.5321(6) 1.2536(3) 0.5829(3) 0.0629(13) Uani 1 1 d . . . N8 N 0.4137(4) 1.0870(3) 0.5086(2) 0.0462(10) Uani 1 1 d . . . N9 N 0.3385(4) 1.0082(3) 0.4649(2) 0.0461(10) Uani 1 1 d . . . N10 N 0.1644(4) 0.8681(3) 0.3768(2) 0.0474(10) Uani 1 1 d . . . N11 N 0.5459(5) 1.1037(3) 0.6778(3) 0.0572(12) Uani 1 1 d . . . N12 N 0.7178(4) 1.1643(3) 0.4682(2) 0.0466(10) Uani 1 1 d . . . C1 C 0.1563(7) 0.8158(4) 0.1436(3) 0.0634(15) Uani 1 1 d . . . C2 C 0.1085(8) 0.8981(4) 0.1566(4) 0.0756(19) Uani 1 1 d . . . C3 C -0.0329(8) 0.9024(4) 0.1352(4) 0.0699(17) Uani 1 1 d . . . C4 C -0.1250(7) 0.8229(4) 0.0980(4) 0.0619(15) Uani 1 1 d . . . C5 C -0.0684(6) 0.7415(3) 0.0834(3) 0.0460(12) Uani 1 1 d . . . C6 C -0.1504(5) 0.6566(3) 0.0363(3) 0.0403(11) Uani 1 1 d . . . C7 C -0.2862(5) 0.6293(3) -0.0041(3) 0.0455(13) Uani 1 1 d . . . C8 C -0.2843(5) 0.5415(3) -0.0443(3) 0.0394(11) Uani 1 1 d . . . C9 C -0.3844(5) 0.4734(3) -0.0995(3) 0.0439(12) Uani 1 1 d . . . C10 C -0.5223(6) 0.4847(4) -0.1271(3) 0.0556(14) Uani 1 1 d . . . C11 C -0.6084(6) 0.4174(4) -0.1832(4) 0.0644(16) Uani 1 1 d . . . C12 C -0.5521(6) 0.3416(4) -0.2116(3) 0.0649(17) Uani 1 1 d . . . C13 C -0.4149(6) 0.3318(4) -0.1830(3) 0.0581(15) Uani 1 1 d . . . C14 C 0.0285(6) 0.5611(3) 0.2370(3) 0.0521(13) Uani 1 1 d . . . C15 C 0.3322(5) 0.7207(3) -0.0056(3) 0.0460(12) Uani 1 1 d . . . C16 C 0.4037(5) 0.7486(3) -0.0667(3) 0.0470(12) Uani 1 1 d . . . C17 C 0.3569(5) 0.7086(3) -0.1450(3) 0.0428(11) Uani 1 1 d . . . C18 C 0.2325(5) 0.6415(3) -0.1563(3) 0.0449(12) Uani 1 1 d . . . C19 C 0.1676(5) 0.6170(3) -0.0927(3) 0.0423(11) Uani 1 1 d . . . C20 C 0.4383(5) 0.7324(3) -0.2118(3) 0.0498(13) Uani 1 1 d . . . C21 C 0.5230(7) 0.8163(4) -0.2065(4) 0.0704(18) Uani 1 1 d . . . C22 C 0.6005(7) 0.8392(5) -0.2669(5) 0.084(2) Uani 1 1 d . . . C23 C 0.5897(8) 0.7751(6) -0.3358(5) 0.089(3) Uani 1 1 d . . . C24 C 0.5077(8) 0.6916(5) -0.3438(4) 0.0780(19) Uani 1 1 d . . . C25 C 0.4323(7) 0.6720(4) -0.2825(4) 0.0680(18) Uani 1 1 d . . . C26 C 0.6025(8) 1.3385(4) 0.6139(4) 0.079(2) Uani 1 1 d . . . C27 C 0.5331(12) 1.4150(5) 0.6152(5) 0.109(3) Uani 1 1 d . . . C28 C 0.3919(12) 1.4063(5) 0.5900(5) 0.103(3) Uani 1 1 d . . . C29 C 0.3187(8) 1.3194(4) 0.5587(4) 0.084(2) Uani 1 1 d . . . C30 C 0.3896(7) 1.2440(4) 0.5532(3) 0.0630(15) Uani 1 1 d . . . C31 C 0.3241(6) 1.1511(3) 0.5132(3) 0.0514(13) Uani 1 1 d . . . C32 C 0.1900(6) 1.1136(4) 0.4730(3) 0.0541(14) Uani 1 1 d . . . C33 C 0.2020(5) 1.0237(3) 0.4429(3) 0.0482(12) Uani 1 1 d . . . C34 C 0.1061(5) 0.9457(4) 0.3943(3) 0.0519(13) Uani 1 1 d . . . C35 C -0.0355(6) 0.9508(5) 0.3678(3) 0.0654(16) Uani 1 1 d . . . C36 C -0.1211(7) 0.8724(6) 0.3216(4) 0.082(2) Uani 1 1 d . . . C37 C -0.0611(7) 0.7952(5) 0.3034(4) 0.081(2) Uani 1 1 d . . . C38 C 0.0805(7) 0.7955(4) 0.3315(3) 0.0631(16) Uani 1 1 d . . . C39 C 0.5074(6) 1.0923(4) 0.7375(4) 0.0540(14) Uani 1 1 d . . . C40 C 0.8185(7) 1.2389(4) 0.4709(4) 0.0638(16) Uani 1 1 d . . . C41 C 0.8907(6) 1.2571(4) 0.4067(4) 0.0626(15) Uani 1 1 d . . . C42 C 0.8609(6) 1.1986(3) 0.3343(3) 0.0534(13) Uani 1 1 d . . . C43 C 0.7506(6) 1.1247(4) 0.3321(3) 0.0574(14) Uani 1 1 d . . . C44 C 0.6827(6) 1.1109(4) 0.3979(3) 0.0568(14) Uani 1 1 d . . . C45 C 0.9419(6) 1.2132(4) 0.2648(4) 0.0655(16) Uani 1 1 d . . . C46 C 1.0594(8) 1.2807(6) 0.2699(4) 0.089(2) Uani 1 1 d . . . C47 C 1.1341(9) 1.2919(7) 0.2043(6) 0.111(3) Uani 1 1 d . . . C48 C 1.0902(11) 1.2377(8) 0.1367(6) 0.106(3) Uani 1 1 d . . . C49 C 0.9738(10) 1.1687(5) 0.1269(5) 0.097(2) Uani 1 1 d . . . C50 C 0.9031(9) 1.1578(5) 0.1921(5) 0.089(2) Uani 1 1 d . . . B1 B -0.0154(10) 0.5426(6) 0.3218(4) 0.084(2) Uani 1 1 d . . . B2 B 0.4593(8) 1.0798(5) 0.8235(5) 0.075(2) Uani 1 1 d . . . H1 H 0.270(5) 0.812(3) 0.164(2) 0.038 Uiso 1 1 d . . . H2 H 0.182(5) 0.946(3) 0.179(2) 0.038 Uiso 1 1 d . . . H3 H -0.097(5) 0.944(3) 0.126(2) 0.038 Uiso 1 1 d . . . H4 H -0.215(5) 0.826(3) 0.074(2) 0.038 Uiso 1 1 d . . . H5 H -0.354(5) 0.651(3) -0.007(3) 0.038 Uiso 1 1 d . . . H6 H -0.558(5) 0.537(3) -0.109(2) 0.038 Uiso 1 1 d . . . H7 H -0.699(5) 0.421(3) -0.202(2) 0.038 Uiso 1 1 d . . . H8 H -0.610(5) 0.296(3) -0.245(2) 0.038 Uiso 1 1 d . . . H9 H -0.376(5) 0.285(3) -0.195(3) 0.038 Uiso 1 1 d . . . H10 H 0.034(4) 0.613(3) 0.363(2) 0.038 Uiso 1 1 d . . . H11 H -0.067(4) 0.469(3) 0.323(2) 0.038 Uiso 1 1 d . . . H12 H 0.096(4) 0.532(2) 0.371(2) 0.038 Uiso 1 1 d . . . H13 H 0.370(4) 0.754(3) 0.050(2) 0.038 Uiso 1 1 d . . . H14 H 0.480(5) 0.797(3) -0.053(2) 0.038 Uiso 1 1 d . . . H15 H 0.197(4) 0.616(3) -0.210(2) 0.038 Uiso 1 1 d . . . H16 H 0.087(5) 0.570(3) -0.100(2) 0.038 Uiso 1 1 d . . . H17 H 0.526(5) 0.859(3) -0.166(3) 0.038 Uiso 1 1 d . . . H18 H 0.654(5) 0.895(3) -0.251(2) 0.038 Uiso 1 1 d . . . H19 H 0.639(5) 0.779(3) -0.370(3) 0.038 Uiso 1 1 d . . . H20 H 0.501(5) 0.650(3) -0.391(3) 0.038 Uiso 1 1 d . . . H21 H 0.383(5) 0.626(3) -0.288(3) 0.038 Uiso 1 1 d . . . H22 H 0.708(5) 1.345(3) 0.633(2) 0.038 Uiso 1 1 d . . . H23 H 0.588(5) 1.459(3) 0.637(3) 0.038 Uiso 1 1 d . . . H24 H 0.315(4) 1.455(3) 0.594(2) 0.038 Uiso 1 1 d . . . H25 H 0.222(5) 1.314(3) 0.534(2) 0.038 Uiso 1 1 d . . . H26 H 0.104(5) 1.138(3) 0.456(2) 0.038 Uiso 1 1 d . . . H27 H -0.063(4) 1.012(3) 0.372(2) 0.038 Uiso 1 1 d . . . H28 H -0.215(5) 0.879(3) 0.301(2) 0.038 Uiso 1 1 d . . . H29 H -0.104(5) 0.745(3) 0.272(2) 0.038 Uiso 1 1 d . . . H30 H 0.127(5) 0.747(3) 0.323(3) 0.038 Uiso 1 1 d . . . H31 H 0.457(4) 1.144(3) 0.865(2) 0.038 Uiso 1 1 d . . . H32 H 0.360(5) 1.045(3) 0.823(2) 0.038 Uiso 1 1 d . . . H33 H 0.546(4) 1.059(2) 0.865(2) 0.038 Uiso 1 1 d . . . H34 H 0.840(4) 1.280(3) 0.519(2) 0.038 Uiso 1 1 d . . . H35 H 0.966(5) 1.310(3) 0.417(2) 0.038 Uiso 1 1 d . . . H36 H 0.734(5) 1.080(3) 0.287(2) 0.038 Uiso 1 1 d . . . H37 H 0.612(5) 1.059(3) 0.397(2) 0.038 Uiso 1 1 d . . . H38 H 1.066(5) 1.325(3) 0.311(3) 0.038 Uiso 1 1 d . . . H39 H 1.188(5) 1.352(3) 0.223(3) 0.038 Uiso 1 1 d . . . H40 H 1.124(6) 1.241(4) 0.106(3) 0.038 Uiso 1 1 d . . . H41 H 0.941(4) 1.132(3) 0.068(3) 0.038 Uiso 1 1 d . . . H42 H 0.824(5) 1.115(3) 0.182(3) 0.038 Uiso 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 0.0315(4) 0.0403(4) 0.0400(4) -0.0005(3) 0.0002(3) 0.0001(3) Fe2 0.0389(4) 0.0435(4) 0.0434(4) 0.0000(3) -0.0001(3) -0.0007(3) N1 0.045(3) 0.045(2) 0.055(3) -0.003(2) 0.009(2) -0.0036(19) N2 0.036(2) 0.035(2) 0.044(2) 0.0029(18) 0.0064(17) 0.0052(16) N3 0.029(2) 0.036(2) 0.041(2) 0.0022(18) 0.0025(17) 0.0011(15) N4 0.035(2) 0.048(2) 0.041(2) 0.0016(19) 0.0007(18) -0.0002(18) N5 0.035(2) 0.046(2) 0.058(3) 0.000(2) 0.001(2) 0.0011(17) N6 0.035(2) 0.039(2) 0.048(2) -0.0001(19) -0.0027(18) 0.0027(17) N7 0.083(4) 0.050(3) 0.051(3) 0.000(2) 0.019(3) -0.004(2) N8 0.049(3) 0.047(2) 0.042(2) 0.005(2) 0.010(2) 0.005(2) N9 0.047(3) 0.047(2) 0.040(2) 0.003(2) 0.0025(19) 0.0032(19) N10 0.042(2) 0.051(2) 0.044(2) 0.001(2) 0.0035(19) -0.0010(19) N11 0.037(3) 0.057(3) 0.071(3) 0.009(3) -0.006(2) -0.005(2) N12 0.037(2) 0.052(2) 0.047(3) 0.003(2) 0.0026(19) 0.0038(19) C1 0.061(4) 0.048(3) 0.068(4) -0.013(3) 0.008(3) -0.007(3) C2 0.073(5) 0.052(4) 0.086(5) -0.018(3) 0.016(4) -0.013(3) C3 0.078(5) 0.047(3) 0.085(5) -0.001(3) 0.020(4) 0.018(3) C4 0.061(4) 0.046(3) 0.077(4) -0.001(3) 0.019(3) 0.011(3) C5 0.054(3) 0.038(3) 0.045(3) 0.002(2) 0.015(2) 0.005(2) C6 0.039(3) 0.042(3) 0.040(3) 0.005(2) 0.007(2) 0.005(2) C7 0.034(3) 0.047(3) 0.059(3) 0.011(3) 0.010(2) 0.012(2) C8 0.027(2) 0.048(3) 0.040(3) 0.004(2) 0.003(2) 0.0001(19) C9 0.038(3) 0.051(3) 0.045(3) 0.018(2) 0.006(2) 0.006(2) C10 0.038(3) 0.064(3) 0.065(4) 0.010(3) 0.000(3) 0.010(3) C11 0.035(3) 0.089(4) 0.066(4) 0.017(3) -0.008(3) 0.001(3) C12 0.049(4) 0.072(4) 0.060(4) -0.001(3) -0.019(3) -0.010(3) C13 0.047(3) 0.066(4) 0.053(3) -0.003(3) -0.007(3) 0.005(3) C14 0.046(3) 0.051(3) 0.051(3) -0.003(3) -0.001(3) -0.003(2) C15 0.040(3) 0.046(3) 0.045(3) -0.003(2) -0.001(2) -0.001(2) C16 0.043(3) 0.046(3) 0.046(3) 0.004(2) -0.001(2) -0.005(2) C17 0.042(3) 0.038(2) 0.046(3) 0.005(2) 0.000(2) 0.003(2) C18 0.048(3) 0.042(3) 0.043(3) 0.007(2) -0.003(2) 0.009(2) C19 0.037(3) 0.042(3) 0.042(3) 0.000(2) -0.004(2) -0.004(2) C20 0.050(3) 0.052(3) 0.049(3) 0.019(3) -0.002(2) 0.005(2) C21 0.080(5) 0.063(4) 0.064(4) 0.021(3) 0.004(4) -0.011(3) C22 0.069(5) 0.086(5) 0.092(6) 0.038(5) -0.001(4) -0.025(4) C23 0.065(5) 0.129(7) 0.081(6) 0.060(6) 0.007(4) -0.006(4) C24 0.081(5) 0.094(5) 0.061(4) 0.018(4) 0.022(4) 0.008(4) C25 0.069(4) 0.065(4) 0.068(4) 0.020(4) 0.015(3) -0.009(3) C26 0.096(5) 0.055(4) 0.075(5) -0.012(3) 0.027(4) -0.013(4) C27 0.163(10) 0.049(4) 0.098(6) -0.015(4) 0.040(7) -0.021(5) C28 0.150(8) 0.050(4) 0.111(7) -0.006(4) 0.050(6) 0.025(5) C29 0.105(6) 0.058(4) 0.095(5) 0.009(4) 0.028(4) 0.028(4) C30 0.077(4) 0.053(3) 0.063(4) 0.007(3) 0.026(3) 0.015(3) C31 0.058(4) 0.047(3) 0.050(3) 0.003(3) 0.018(3) 0.012(3) C32 0.048(3) 0.061(3) 0.058(4) 0.016(3) 0.012(3) 0.014(3) C33 0.044(3) 0.053(3) 0.047(3) 0.011(3) 0.004(2) 0.006(2) C34 0.041(3) 0.070(3) 0.044(3) 0.014(3) 0.002(2) -0.001(3) C35 0.051(4) 0.092(4) 0.056(4) 0.028(4) -0.002(3) 0.008(3) C36 0.030(3) 0.132(6) 0.082(5) 0.025(5) -0.005(3) 0.001(4) C37 0.058(4) 0.099(5) 0.066(4) 0.000(4) -0.020(3) -0.022(4) C38 0.060(4) 0.065(4) 0.054(4) 0.002(3) -0.009(3) -0.005(3) C39 0.036(3) 0.052(3) 0.066(4) 0.005(3) -0.005(3) -0.009(2) C40 0.062(4) 0.056(3) 0.063(4) -0.012(3) 0.006(3) -0.001(3) C41 0.060(4) 0.052(3) 0.073(4) 0.008(3) 0.016(3) -0.001(3) C42 0.047(3) 0.051(3) 0.064(4) 0.015(3) 0.002(3) 0.010(2) C43 0.060(4) 0.064(4) 0.045(3) 0.004(3) 0.003(3) 0.009(3) C44 0.056(4) 0.054(3) 0.055(4) 0.004(3) 0.006(3) -0.002(3) C45 0.057(4) 0.072(4) 0.079(5) 0.036(4) 0.013(3) 0.018(3) C46 0.060(4) 0.138(7) 0.067(5) 0.036(4) 0.004(4) -0.005(4) C47 0.075(5) 0.152(9) 0.111(7) 0.074(7) -0.004(5) -0.020(5) C48 0.084(7) 0.150(8) 0.116(9) 0.074(8) 0.051(6) 0.045(6) C49 0.140(8) 0.081(5) 0.091(6) 0.030(4) 0.058(6) 0.040(5) C50 0.120(7) 0.064(4) 0.093(6) 0.021(4) 0.057(5) 0.010(4) B1 0.105(7) 0.075(5) 0.054(4) 0.003(4) -0.003(4) -0.024(5) B2 0.056(5) 0.076(5) 0.079(5) -0.008(4) 0.010(4) -0.021(4) _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 N2 1.936(4) . ? Fe1 N3 1.949(3) 2_565 ? Fe1 N5 2.002(5) . ? Fe1 N6 2.005(4) . ? Fe1 N4 2.051(4) 2_565 ? Fe1 N1 2.060(4) . ? Fe2 N8 2.038(4) . ? Fe2 N9 2.048(4) 2_676 ? Fe2 N11 2.092(5) . ? Fe2 N10 2.161(4) 2_676 ? Fe2 N12 2.162(4) . ? Fe2 N7 2.195(4) . ? N1 C1 1.350(6) . ? N1 C5 1.357(6) . ? N2 C6 1.353(5) . ? N2 N3 1.358(4) . ? N3 C8 1.346(5) . ? N3 Fe1 1.949(3) 2_565 ? N4 C13 1.337(6) . ? N4 C9 1.381(6) . ? N4 Fe1 2.051(4) 2_565 ? N5 C14 1.151(6) . ? N6 C15 1.351(6) . ? N6 C19 1.352(6) . ? N7 C26 1.342(7) . ? N7 C30 1.367(7) . ? N8 N9 1.351(5) . ? N8 C31 1.354(6) . ? N9 C33 1.365(6) . ? N9 Fe2 2.048(4) 2_676 ? N10 C38 1.331(6) . ? N10 C34 1.348(6) . ? N10 Fe2 2.161(4) 2_676 ? N11 C39 1.144(6) . ? N12 C44 1.319(6) . ? N12 C40 1.344(6) . ? C1 C2 1.355(8) . ? C1 H1 1.10(4) . ? C2 C3 1.358(9) . ? C2 H2 0.92(4) . ? C3 C4 1.387(8) . ? C3 H3 0.95(4) . ? C4 C5 1.385(7) . ? C4 H4 0.92(4) . ? C5 C6 1.458(6) . ? C6 C7 1.370(6) . ? C7 C8 1.377(6) . ? C7 H5 0.75(4) . ? C8 C9 1.440(6) . ? C9 C10 1.381(7) . ? C10 C11 1.381(7) . ? C10 H6 0.90(4) . ? C11 C12 1.348(8) . ? C11 H7 0.90(4) . ? C12 C13 1.374(8) . ? C12 H8 0.89(4) . ? C13 H9 0.83(4) . ? C14 B1 1.600(9) . ? C15 C16 1.378(7) . ? C15 H13 1.01(4) . ? C16 C17 1.384(6) . ? C16 H14 0.92(4) . ? C17 C18 1.401(6) . ? C17 C20 1.489(7) . ? C18 C19 1.367(7) . ? C18 H15 0.95(4) . ? C19 H16 0.94(4) . ? C20 C21 1.367(7) . ? C20 C25 1.377(8) . ? C21 C22 1.372(9) . ? C21 H17 0.86(4) . ? C22 C23 1.378(10) . ? C22 H18 0.90(4) . ? C23 C24 1.346(9) . ? C23 H19 0.78(4) . ? C24 C25 1.361(8) . ? C24 H20 0.93(4) . ? C25 H21 0.75(4) . ? C26 C27 1.389(11) . ? C26 H22 1.00(4) . ? C27 C28 1.338(12) . ? C27 H23 0.79(4) . ? C28 C29 1.376(9) . ? C28 H24 1.09(4) . ? C29 C30 1.378(8) . ? C29 H25 0.96(4) . ? C30 C31 1.463(7) . ? C31 C32 1.377(7) . ? C32 C33 1.378(7) . ? C32 H26 0.97(4) . ? C33 C34 1.454(7) . ? C34 C35 1.382(7) . ? C35 C36 1.400(9) . ? C35 H27 0.97(4) . ? C36 C37 1.354(9) . ? C36 H28 0.94(4) . ? C37 C38 1.371(8) . ? C37 H29 0.87(4) . ? C38 H30 0.89(4) . ? C39 B2 1.610(9) . ? C40 C41 1.383(8) . ? C40 H34 0.93(4) . ? C41 C42 1.377(7) . ? C41 H35 0.96(4) . ? C42 C43 1.391(7) . ? C42 C45 1.493(8) . ? C43 C44 1.370(7) . ? C43 H36 0.93(4) . ? C44 H37 0.94(4) . ? C45 C50 1.367(9) . ? C45 C46 1.367(9) . ? C46 C47 1.393(10) . ? C46 H38 0.87(4) . ? C47 C48 1.298(13) . ? C47 H39 0.95(4) . ? C48 C49 1.366(13) . ? C48 H40 0.64(5) . ? C49 C50 1.365(9) . ? C49 H41 1.07(4) . ? C50 H42 0.89(4) . ? B1 H10 1.17(4) . ? B1 H11 1.14(4) . ? B1 H12 1.33(4) . ? B2 H31 1.09(4) . ? B2 H32 1.00(4) . ? B2 H33 1.15(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 N2 Fe1 N3 91.83(14) . 2_565 ? N2 Fe1 N5 92.65(15) . . ? N3 Fe1 N5 95.77(15) 2_565 . ? N2 Fe1 N6 93.55(15) . . ? N3 Fe1 N6 89.25(15) 2_565 . ? N5 Fe1 N6 171.89(15) . . ? N2 Fe1 N4 171.25(15) . 2_565 ? N3 Fe1 N4 79.79(15) 2_565 2_565 ? N5 Fe1 N4 85.74(15) . 2_565 ? N6 Fe1 N4 88.90(15) . 2_565 ? N2 Fe1 N1 79.76(15) . . ? N3 Fe1 N1 170.70(15) 2_565 . ? N5 Fe1 N1 88.62(16) . . ? N6 Fe1 N1 87.35(15) . . ? N4 Fe1 N1 108.78(16) 2_565 . ? N8 Fe2 N9 91.57(15) . 2_676 ? N8 Fe2 N11 94.01(16) . . ? N9 Fe2 N11 96.36(16) 2_676 . ? N8 Fe2 N10 168.70(15) . 2_676 ? N9 Fe2 N10 77.13(15) 2_676 2_676 ? N11 Fe2 N10 87.21(15) . 2_676 ? N8 Fe2 N12 94.65(15) . . ? N9 Fe2 N12 90.27(15) 2_676 . ? N11 Fe2 N12 168.94(16) . . ? N10 Fe2 N12 85.66(14) 2_676 . ? N8 Fe2 N7 76.99(17) . . ? N9 Fe2 N7 167.94(17) 2_676 . ? N11 Fe2 N7 88.33(16) . . ? N10 Fe2 N7 114.30(17) 2_676 . ? N12 Fe2 N7 86.92(15) . . ? C1 N1 C5 116.8(4) . . ? C1 N1 Fe1 129.7(4) . . ? C5 N1 Fe1 113.3(3) . . ? C6 N2 N3 107.7(3) . . ? C6 N2 Fe1 118.3(3) . . ? N3 N2 Fe1 133.9(3) . . ? C8 N3 N2 107.7(3) . . ? C8 N3 Fe1 118.0(3) . 2_565 ? N2 N3 Fe1 134.2(3) . 2_565 ? C13 N4 C9 116.7(4) . . ? C13 N4 Fe1 130.3(3) . 2_565 ? C9 N4 Fe1 113.0(3) . 2_565 ? C14 N5 Fe1 173.2(4) . . ? C15 N6 C19 114.7(4) . . ? C15 N6 Fe1 122.9(3) . . ? C19 N6 Fe1 122.4(3) . . ? C26 N7 C30 118.4(5) . . ? C26 N7 Fe2 128.7(5) . . ? C30 N7 Fe2 112.9(3) . . ? N9 N8 C31 107.5(4) . . ? N9 N8 Fe2 134.1(3) . . ? C31 N8 Fe2 118.4(3) . . ? N8 N9 C33 108.2(4) . . ? N8 N9 Fe2 134.4(3) . 2_676 ? C33 N9 Fe2 117.3(3) . 2_676 ? C38 N10 C34 117.3(5) . . ? C38 N10 Fe2 128.5(4) . 2_676 ? C34 N10 Fe2 114.2(3) . 2_676 ? C39 N11 Fe2 179.1(5) . . ? C44 N12 C40 115.8(5) . . ? C44 N12 Fe2 118.1(4) . . ? C40 N12 Fe2 126.1(4) . . ? N1 C1 C2 123.6(6) . . ? N1 C1 H1 117(2) . . ? C2 C1 H1 119(2) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 H2 112(3) . . ? C3 C2 H2 128(3) . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 142(3) . . ? C4 C3 H3 97(3) . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H4 120(3) . . ? C3 C4 H4 121(3) . . ? N1 C5 C4 122.2(5) . . ? N1 C5 C6 114.8(4) . . ? C4 C5 C6 122.9(5) . . ? N2 C6 C7 109.7(4) . . ? N2 C6 C5 113.3(4) . . ? C7 C6 C5 136.6(4) . . ? C6 C7 C8 104.9(4) . . ? C6 C7 H5 135(4) . . ? C8 C7 H5 120(4) . . ? N3 C8 C7 109.9(4) . . ? N3 C8 C9 114.3(4) . . ? C7 C8 C9 135.7(4) . . ? N4 C9 C10 120.6(5) . . ? N4 C9 C8 114.5(4) . . ? C10 C9 C8 124.9(5) . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H6 118(3) . . ? C9 C10 H6 121(3) . . ? C12 C11 C10 117.9(5) . . ? C12 C11 H7 118(3) . . ? C10 C11 H7 124(3) . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H8 118(3) . . ? C13 C12 H8 121(3) . . ? N4 C13 C12 123.8(5) . . ? N4 C13 H9 111(3) . . ? C12 C13 H9 125(3) . . ? N5 C14 B1 177.8(6) . . ? N6 C15 C16 124.2(5) . . ? N6 C15 H13 119(2) . . ? C16 C15 H13 117(2) . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H14 117(3) . . ? C17 C16 H14 123(3) . . ? C16 C17 C18 115.4(5) . . ? C16 C17 C20 121.9(4) . . ? C18 C17 C20 122.6(4) . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H15 123(3) . . ? C17 C18 H15 116(3) . . ? N6 C19 C18 124.3(4) . . ? N6 C19 H16 115(3) . . ? C18 C19 H16 120(2) . . ? C21 C20 C25 116.0(6) . . ? C21 C20 C17 121.6(5) . . ? C25 C20 C17 122.4(5) . . ? C20 C21 C22 122.6(6) . . ? C20 C21 H17 121(3) . . ? C22 C21 H17 116(3) . . ? C21 C22 C23 118.2(6) . . ? C21 C22 H18 109(3) . . ? C23 C22 H18 133(3) . . ? C24 C23 C22 121.4(7) . . ? C24 C23 H19 113(4) . . ? C22 C23 H19 125(4) . . ? C23 C24 C25 118.4(7) . . ? C23 C24 H20 120(3) . . ? C25 C24 H20 122(3) . . ? C24 C25 C20 123.4(6) . . ? C24 C25 H21 118(4) . . ? C20 C25 H21 118(4) . . ? N7 C26 C27 121.0(7) . . ? N7 C26 H22 118(3) . . ? C27 C26 H22 121(2) . . ? C28 C27 C26 121.2(7) . . ? C28 C27 H23 130(4) . . ? C26 C27 H23 109(4) . . ? C27 C28 C29 118.0(7) . . ? C27 C28 H24 133(2) . . ? C29 C28 H24 109(2) . . ? C28 C29 C30 120.7(8) . . ? C28 C29 H25 118(3) . . ? C30 C29 H25 121(3) . . ? N7 C30 C29 120.5(6) . . ? N7 C30 C31 115.4(5) . . ? C29 C30 C31 124.0(6) . . ? N8 C31 C32 110.2(4) . . ? N8 C31 C30 115.7(5) . . ? C32 C31 C30 133.8(5) . . ? C31 C32 C33 104.9(5) . . ? C31 C32 H26 135(2) . . ? C33 C32 H26 119(2) . . ? N9 C33 C32 109.2(5) . . ? N9 C33 C34 115.6(4) . . ? C32 C33 C34 135.2(5) . . ? N10 C34 C35 122.2(5) . . ? N10 C34 C33 115.6(4) . . ? C35 C34 C33 122.2(5) . . ? C34 C35 C36 118.7(6) . . ? C34 C35 H27 117(3) . . ? C36 C35 H27 122(3) . . ? C37 C36 C35 118.7(6) . . ? C37 C36 H28 125(3) . . ? C35 C36 H28 117(3) . . ? C36 C37 C38 119.2(6) . . ? C36 C37 H29 124(3) . . ? C38 C37 H29 116(3) . . ? N10 C38 C37 123.8(6) . . ? N10 C38 H30 112(3) . . ? C37 C38 H30 125(3) . . ? N11 C39 B2 177.4(6) . . ? N12 C40 C41 123.5(5) . . ? N12 C40 H34 117(3) . . ? C41 C40 H34 119(3) . . ? C42 C41 C40 120.9(5) . . ? C42 C41 H35 123(3) . . ? C40 C41 H35 116(3) . . ? C41 C42 C43 114.3(6) . . ? C41 C42 C45 122.4(5) . . ? C43 C42 C45 123.2(5) . . ? C44 C43 C42 121.8(5) . . ? C44 C43 H36 120(3) . . ? C42 C43 H36 117(3) . . ? N12 C44 C43 123.4(5) . . ? N12 C44 H37 115(3) . . ? C43 C44 H37 121(3) . . ? C50 C45 C46 116.2(7) . . ? C50 C45 C42 121.2(6) . . ? C46 C45 C42 122.6(6) . . ? C45 C46 C47 121.3(7) . . ? C45 C46 H38 114(3) . . ? C47 C46 H38 122(3) . . ? C48 C47 C46 119.2(8) . . ? C48 C47 H39 138(3) . . ? C46 C47 H39 99(3) . . ? C47 C48 C49 122.8(8) . . ? C47 C48 H40 121(6) . . ? C49 C48 H40 116(6) . . ? C50 C49 C48 117.1(9) . . ? C50 C49 H41 126(3) . . ? C48 C49 H41 117(2) . . ? C49 C50 C45 123.2(7) . . ? C49 C50 H42 114(3) . . ? C45 C50 H42 122(3) . . ? C14 B1 H10 101(2) . . ? C14 B1 H11 115(2) . . ? H10 B1 H11 143(3) . . ? C14 B1 H12 113.7(18) . . ? H10 B1 H12 70(2) . . ? H11 B1 H12 89(2) . . ? C39 B2 H31 116(2) . . ? C39 B2 H32 115(2) . . ? H31 B2 H32 103(3) . . ? C39 B2 H33 115(2) . . ? H31 B2 H33 92(3) . . ? H32 B2 H33 114(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 N2 Fe1 N1 C1 -169.8(5) . . . . ? N3 Fe1 N1 C1 -144.4(9) 2_565 . . . ? N5 Fe1 N1 C1 97.2(5) . . . . ? N6 Fe1 N1 C1 -75.8(5) . . . . ? N4 Fe1 N1 C1 12.2(5) 2_565 . . . ? N2 Fe1 N1 C5 5.2(3) . . . . ? N3 Fe1 N1 C5 30.6(11) 2_565 . . . ? N5 Fe1 N1 C5 -87.8(3) . . . . ? N6 Fe1 N1 C5 99.3(3) . . . . ? N4 Fe1 N1 C5 -172.8(3) 2_565 . . . ? N3 Fe1 N2 C6 176.9(3) 2_565 . . . ? N5 Fe1 N2 C6 81.1(3) . . . . ? N6 Fe1 N2 C6 -93.7(3) . . . . ? N4 Fe1 N2 C6 160.2(9) 2_565 . . . ? N1 Fe1 N2 C6 -7.1(3) . . . . ? N3 Fe1 N2 N3 -1.8(4) 2_565 . . . ? N5 Fe1 N2 N3 -97.7(4) . . . . ? N6 Fe1 N2 N3 87.5(4) . . . . ? N4 Fe1 N2 N3 -18.5(13) 2_565 . . . ? N1 Fe1 N2 N3 174.2(4) . . . . ? C6 N2 N3 C8 -1.2(5) . . . . ? Fe1 N2 N3 C8 177.6(3) . . . . ? C6 N2 N3 Fe1 -176.3(3) . . . 2_565 ? Fe1 N2 N3 Fe1 2.5(6) . . . 2_565 ? N2 Fe1 N5 C14 -158(4) . . . . ? N3 Fe1 N5 C14 109(4) 2_565 . . . ? N6 Fe1 N5 C14 -19(4) . . . . ? N4 Fe1 N5 C14 30(4) 2_565 . . . ? N1 Fe1 N5 C14 -79(4) . . . . ? N2 Fe1 N6 C15 144.4(4) . . . . ? N3 Fe1 N6 C15 -123.8(4) 2_565 . . . ? N5 Fe1 N6 C15 4.6(13) . . . . ? N4 Fe1 N6 C15 -44.0(4) 2_565 . . . ? N1 Fe1 N6 C15 64.9(4) . . . . ? N2 Fe1 N6 C19 -38.5(4) . . . . ? N3 Fe1 N6 C19 53.3(4) 2_565 . . . ? N5 Fe1 N6 C19 -178.4(9) . . . . ? N4 Fe1 N6 C19 133.1(4) 2_565 . . . ? N1 Fe1 N6 C19 -118.1(4) . . . . ? N8 Fe2 N7 C26 -171.9(5) . . . . ? N9 Fe2 N7 C26 -153.2(7) 2_676 . . . ? N11 Fe2 N7 C26 93.6(5) . . . . ? N10 Fe2 N7 C26 7.4(5) 2_676 . . . ? N12 Fe2 N7 C26 -76.4(5) . . . . ? N8 Fe2 N7 C30 5.7(4) . . . . ? N9 Fe2 N7 C30 24.5(10) 2_676 . . . ? N11 Fe2 N7 C30 -88.8(4) . . . . ? N10 Fe2 N7 C30 -174.9(3) 2_676 . . . ? N12 Fe2 N7 C30 101.2(4) . . . . ? N9 Fe2 N8 N9 0.3(5) 2_676 . . . ? N11 Fe2 N8 N9 -96.2(4) . . . . ? N10 Fe2 N8 N9 -0.4(10) 2_676 . . . ? N12 Fe2 N8 N9 90.7(4) . . . . ? N7 Fe2 N8 N9 176.4(4) . . . . ? N9 Fe2 N8 C31 176.8(4) 2_676 . . . ? N11 Fe2 N8 C31 80.3(4) . . . . ? N10 Fe2 N8 C31 176.1(7) 2_676 . . . ? N12 Fe2 N8 C31 -92.8(4) . . . . ? N7 Fe2 N8 C31 -7.1(4) . . . . ? C31 N8 N9 C33 -0.3(5) . . . . ? Fe2 N8 N9 C33 176.5(3) . . . . ? C31 N8 N9 Fe2 -177.2(3) . . . 2_676 ? Fe2 N8 N9 Fe2 -0.4(7) . . . 2_676 ? N8 Fe2 N11 C39 88(28) . . . . ? N9 Fe2 N11 C39 -4(28) 2_676 . . . ? N10 Fe2 N11 C39 -81(28) 2_676 . . . ? N12 Fe2 N11 C39 -131(28) . . . . ? N7 Fe2 N11 C39 164(28) . . . . ? N8 Fe2 N12 C44 -44.4(4) . . . . ? N9 Fe2 N12 C44 47.2(4) 2_676 . . . ? N11 Fe2 N12 C44 174.2(7) . . . . ? N10 Fe2 N12 C44 124.2(4) 2_676 . . . ? N7 Fe2 N12 C44 -121.1(4) . . . . ? N8 Fe2 N12 C40 138.2(4) . . . . ? N9 Fe2 N12 C40 -130.2(4) 2_676 . . . ? N11 Fe2 N12 C40 -3.2(11) . . . . ? N10 Fe2 N12 C40 -53.1(4) 2_676 . . . ? N7 Fe2 N12 C40 61.5(4) . . . . ? C5 N1 C1 C2 0.1(8) . . . . ? Fe1 N1 C1 C2 175.0(5) . . . . ? N1 C1 C2 C3 2.4(10) . . . . ? C1 C2 C3 C4 -2.1(10) . . . . ? C2 C3 C4 C5 -0.6(10) . . . . ? C1 N1 C5 C4 -2.9(7) . . . . ? Fe1 N1 C5 C4 -178.7(4) . . . . ? C1 N1 C5 C6 172.9(4) . . . . ? Fe1 N1 C5 C6 -2.8(5) . . . . ? C3 C4 C5 N1 3.2(9) . . . . ? C3 C4 C5 C6 -172.3(5) . . . . ? N3 N2 C6 C7 1.1(5) . . . . ? Fe1 N2 C6 C7 -178.0(3) . . . . ? N3 N2 C6 C5 -173.5(4) . . . . ? Fe1 N2 C6 C5 7.5(5) . . . . ? N1 C5 C6 N2 -2.7(6) . . . . ? C4 C5 C6 N2 173.1(5) . . . . ? N1 C5 C6 C7 -175.2(5) . . . . ? C4 C5 C6 C7 0.6(9) . . . . ? N2 C6 C7 C8 -0.5(6) . . . . ? C5 C6 C7 C8 172.2(5) . . . . ? N2 N3 C8 C7 0.9(5) . . . . ? Fe1 N3 C8 C7 176.9(3) 2_565 . . . ? N2 N3 C8 C9 178.5(4) . . . . ? Fe1 N3 C8 C9 -5.4(5) 2_565 . . . ? C6 C7 C8 N3 -0.2(6) . . . . ? C6 C7 C8 C9 -177.2(5) . . . . ? C13 N4 C9 C10 2.1(7) . . . . ? Fe1 N4 C9 C10 -178.5(4) 2_565 . . . ? C13 N4 C9 C8 -175.2(4) . . . . ? Fe1 N4 C9 C8 4.2(5) 2_565 . . . ? N3 C8 C9 N4 0.5(6) . . . . ? C7 C8 C9 N4 177.4(5) . . . . ? N3 C8 C9 C10 -176.6(5) . . . . ? C7 C8 C9 C10 0.2(9) . . . . ? N4 C9 C10 C11 -0.3(8) . . . . ? C8 C9 C10 C11 176.7(5) . . . . ? C9 C10 C11 C12 -1.8(9) . . . . ? C10 C11 C12 C13 2.0(9) . . . . ? C9 N4 C13 C12 -2.0(8) . . . . ? Fe1 N4 C13 C12 178.8(4) 2_565 . . . ? C11 C12 C13 N4 -0.1(10) . . . . ? Fe1 N5 C14 B1 139(13) . . . . ? C19 N6 C15 C16 -2.9(7) . . . . ? Fe1 N6 C15 C16 174.4(4) . . . . ? N6 C15 C16 C17 0.9(8) . . . . ? C15 C16 C17 C18 1.6(7) . . . . ? C15 C16 C17 C20 -175.4(4) . . . . ? C16 C17 C18 C19 -1.9(7) . . . . ? C20 C17 C18 C19 175.0(4) . . . . ? C15 N6 C19 C18 2.5(7) . . . . ? Fe1 N6 C19 C18 -174.7(4) . . . . ? C17 C18 C19 N6 -0.2(8) . . . . ? C16 C17 C20 C21 -27.3(7) . . . . ? C18 C17 C20 C21 156.0(5) . . . . ? C16 C17 C20 C25 153.2(5) . . . . ? C18 C17 C20 C25 -23.6(8) . . . . ? C25 C20 C21 C22 -1.3(9) . . . . ? C17 C20 C21 C22 179.1(6) . . . . ? C20 C21 C22 C23 1.2(11) . . . . ? C21 C22 C23 C24 -1.2(11) . . . . ? C22 C23 C24 C25 1.4(12) . . . . ? C23 C24 C25 C20 -1.6(11) . . . . ? C21 C20 C25 C24 1.6(9) . . . . ? C17 C20 C25 C24 -178.8(6) . . . . ? C30 N7 C26 C27 -0.6(9) . . . . ? Fe2 N7 C26 C27 176.9(5) . . . . ? N7 C26 C27 C28 4.1(12) . . . . ? C26 C27 C28 C29 -3.5(13) . . . . ? C27 C28 C29 C30 -0.3(12) . . . . ? C26 N7 C30 C29 -3.1(9) . . . . ? Fe2 N7 C30 C29 179.0(5) . . . . ? C26 N7 C30 C31 174.1(5) . . . . ? Fe2 N7 C30 C31 -3.9(6) . . . . ? C28 C29 C30 N7 3.6(10) . . . . ? C28 C29 C30 C31 -173.3(6) . . . . ? N9 N8 C31 C32 0.5(6) . . . . ? Fe2 N8 C31 C32 -176.9(3) . . . . ? N9 N8 C31 C30 -175.3(4) . . . . ? Fe2 N8 C31 C30 7.3(6) . . . . ? N7 C30 C31 N8 -1.8(7) . . . . ? C29 C30 C31 N8 175.2(6) . . . . ? N7 C30 C31 C32 -176.4(6) . . . . ? C29 C30 C31 C32 0.6(10) . . . . ? N8 C31 C32 C33 -0.5(6) . . . . ? C30 C31 C32 C33 174.3(6) . . . . ? N8 N9 C33 C32 0.0(6) . . . . ? Fe2 N9 C33 C32 177.5(3) 2_676 . . . ? N8 N9 C33 C34 179.3(4) . . . . ? Fe2 N9 C33 C34 -3.2(6) 2_676 . . . ? C31 C32 C33 N9 0.3(6) . . . . ? C31 C32 C33 C34 -178.9(6) . . . . ? C38 N10 C34 C35 0.9(8) . . . . ? Fe2 N10 C34 C35 -176.6(4) 2_676 . . . ? C38 N10 C34 C33 -179.0(4) . . . . ? Fe2 N10 C34 C33 3.5(5) 2_676 . . . ? N9 C33 C34 N10 -0.4(7) . . . . ? C32 C33 C34 N10 178.8(6) . . . . ? N9 C33 C34 C35 179.7(5) . . . . ? C32 C33 C34 C35 -1.2(9) . . . . ? N10 C34 C35 C36 0.3(9) . . . . ? C33 C34 C35 C36 -179.7(5) . . . . ? C34 C35 C36 C37 -1.2(10) . . . . ? C35 C36 C37 C38 0.8(11) . . . . ? C34 N10 C38 C37 -1.4(9) . . . . ? Fe2 N10 C38 C37 175.7(5) 2_676 . . . ? C36 C37 C38 N10 0.6(11) . . . . ? Fe2 N11 C39 B2 122(26) . . . . ? C44 N12 C40 C41 -4.6(8) . . . . ? Fe2 N12 C40 C41 172.8(4) . . . . ? N12 C40 C41 C42 0.9(9) . . . . ? C40 C41 C42 C43 2.5(8) . . . . ? C40 C41 C42 C45 -176.7(5) . . . . ? C41 C42 C43 C44 -2.2(8) . . . . ? C45 C42 C43 C44 176.9(5) . . . . ? C40 N12 C44 C43 4.9(8) . . . . ? Fe2 N12 C44 C43 -172.7(4) . . . . ? C42 C43 C44 N12 -1.6(9) . . . . ? C41 C42 C45 C50 -175.2(6) . . . . ? C43 C42 C45 C50 5.6(8) . . . . ? C41 C42 C45 C46 5.8(9) . . . . ? C43 C42 C45 C46 -173.3(6) . . . . ? C50 C45 C46 C47 0.1(11) . . . . ? C42 C45 C46 C47 179.1(7) . . . . ? C45 C46 C47 C48 0.8(13) . . . . ? C46 C47 C48 C49 -0.8(15) . . . . ? C47 C48 C49 C50 -0.1(14) . . . . ? C48 C49 C50 C45 1.1(12) . . . . ? C46 C45 C50 C49 -1.1(11) . . . . ? C42 C45 C50 C49 179.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.171 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.176 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 241139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 B2 Fe2 N12' _chemical_formula_weight 944.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4567(2) _cell_length_b 10.7576(6) _cell_length_c 13.1355(5) _cell_angle_alpha 92.519(6) _cell_angle_beta 108.793(9) _cell_angle_gamma 105.710(5) _cell_volume 1205.11(9) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7264 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10582 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5236 _reflns_number_gt 3346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp.,2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp.,2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp.,2000)' _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^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5236 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Fe1 Fe 0.50620(5) -0.18932(4) 0.45813(4) 0.05097(19) Uani 1 1 d . . . N1 N 0.7293(3) -0.2399(3) 0.5087(2) 0.0587(7) Uani 1 1 d . . . N2 N 0.6781(3) -0.0162(2) 0.5460(2) 0.0493(6) Uani 1 1 d . . . N3 N 0.6728(3) 0.1047(2) 0.5737(2) 0.0504(6) Uani 1 1 d . . . N4 N 0.7080(4) 0.3466(3) 0.6532(2) 0.0642(8) Uani 1 1 d . . . N5 N 0.4644(4) -0.2763(3) 0.5935(3) 0.0674(8) Uani 1 1 d . . . N6 N 0.5537(3) -0.1420(2) 0.3085(2) 0.0560(7) Uani 1 1 d . . . B1 B 0.4155(8) -0.3882(5) 0.7655(5) 0.0914(16) Uani 1 1 d . . . C1 C 0.7511(5) -0.3546(4) 0.4885(4) 0.0759(11) Uani 1 1 d . . . C10 C 0.9821(5) 0.3953(4) 0.7464(4) 0.0857(13) Uani 1 1 d . . . C11 C 0.9879(6) 0.5140(4) 0.7932(4) 0.1059(17) Uani 1 1 d . . . C12 C 0.8552(7) 0.5476(4) 0.7702(5) 0.1032(17) Uani 1 1 d . . . C13 C 0.7169(5) 0.4641(3) 0.6990(4) 0.0816(12) Uani 1 1 d . . . C14 C 0.4450(4) -0.3217(3) 0.6654(4) 0.0657(10) Uani 1 1 d . . . C15 C 0.5949(5) -0.2175(3) 0.2466(3) 0.0680(10) Uani 1 1 d . . . C16 C 0.6449(5) -0.1784(4) 0.1642(3) 0.0697(10) Uani 1 1 d . . . C17 C 0.6564(4) -0.0540(3) 0.1380(3) 0.0597(8) Uani 1 1 d . . . C18 C 0.6067(4) 0.0221(3) 0.1994(3) 0.0625(9) Uani 1 1 d . . . C19 C 0.5593(4) -0.0229(3) 0.2811(3) 0.0575(8) Uani 1 1 d . . . C2 C 0.8948(6) -0.3738(5) 0.5218(4) 0.0956(15) Uani 1 1 d . . . C20 C 0.7194(4) -0.0041(4) 0.0531(3) 0.0689(10) Uani 1 1 d . . . C21 C 0.7319(7) -0.0880(6) -0.0251(4) 0.1023(15) Uani 1 1 d . . . C22 C 0.7947(8) -0.0395(8) -0.1018(4) 0.123(2) Uani 1 1 d . . . C23 C 0.8427(7) 0.0909(8) -0.1028(5) 0.120(2) Uani 1 1 d . . . C24 C 0.8291(8) 0.1746(7) -0.0291(5) 0.141(3) Uani 1 1 d . . . C25 C 0.7664(7) 0.1271(5) 0.0474(4) 0.1133(19) Uani 1 1 d . . . C3 C 1.0226(6) -0.2741(5) 0.5777(4) 0.0951(15) Uani 1 1 d . . . C4 C 1.0053(5) -0.1533(4) 0.6018(3) 0.0754(11) Uani 1 1 d . . . C5 C 0.8575(4) -0.1391(3) 0.5657(3) 0.0560(8) Uani 1 1 d . . . C6 C 0.8275(4) -0.0155(3) 0.5867(2) 0.0497(7) Uani 1 1 d . . . C7 C 0.9222(4) 0.1054(3) 0.6421(3) 0.0583(8) Uani 1 1 d . . . C8 C 0.8209(4) 0.1788(3) 0.6326(3) 0.0530(8) Uani 1 1 d . . . C9 C 0.8394(4) 0.3119(3) 0.6784(3) 0.0603(9) Uani 1 1 d . . . H1 H 0.6641 -0.4247 0.4498 0.091 Uiso 1 1 calc R . . H2 H 0.9044 -0.4556 0.5060 0.115 Uiso 1 1 calc R . . H3 H 1.1214 -0.2859 0.5999 0.114 Uiso 1 1 calc R . . H4 H 1.0918 -0.0834 0.6417 0.090 Uiso 1 1 calc R . . H5 H 1.0301 0.1316 0.6779 0.070 Uiso 1 1 calc R . . H6 H 1.0730 0.3711 0.7602 0.103 Uiso 1 1 calc R . . H7 H 1.0823 0.5705 0.8402 0.127 Uiso 1 1 calc R . . H8 H 0.8568 0.6270 0.8024 0.124 Uiso 1 1 calc R . . H9 H 0.6267 0.4898 0.6819 0.098 Uiso 1 1 calc R . . H10 H 0.3458 -0.4754 0.7400 0.110 Uiso 1 1 calc R . . H11 H 0.3695 -0.3384 0.8006 0.110 Uiso 1 1 calc R . . H12 H 0.5133 -0.3910 0.8163 0.110 Uiso 1 1 calc R . . H13 H 0.5889 -0.3023 0.2611 0.082 Uiso 1 1 calc R . . H14 H 0.6719 -0.2362 0.1247 0.084 Uiso 1 1 calc R . . H15 H 0.6061 0.1056 0.1840 0.075 Uiso 1 1 calc R . . H16 H 0.5289 0.0321 0.3207 0.069 Uiso 1 1 calc R . . H17 H 0.6976 -0.1777 -0.0256 0.123 Uiso 1 1 calc R . . H18 H 0.8040 -0.0965 -0.1530 0.147 Uiso 1 1 calc R . . H19 H 0.8854 0.1232 -0.1545 0.144 Uiso 1 1 calc R . . H20 H 0.8622 0.2640 -0.0302 0.169 Uiso 1 1 calc R . . H21 H 0.7553 0.1853 0.0966 0.136 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0460(3) 0.0393(3) 0.0684(3) 0.0068(2) 0.0199(2) 0.01407(19) N1 0.0631(17) 0.0545(16) 0.0697(18) 0.0137(14) 0.0285(14) 0.0283(14) N2 0.0445(14) 0.0409(13) 0.0635(16) 0.0064(12) 0.0180(12) 0.0156(11) N3 0.0414(13) 0.0451(13) 0.0617(16) 0.0025(12) 0.0165(12) 0.0109(11) N4 0.069(2) 0.0442(15) 0.077(2) 0.0022(14) 0.0287(15) 0.0099(14) N5 0.069(2) 0.0573(18) 0.083(2) 0.0115(16) 0.0324(17) 0.0228(15) N6 0.0539(15) 0.0464(14) 0.0690(18) 0.0085(13) 0.0217(13) 0.0166(12) C1 0.085(3) 0.060(2) 0.100(3) 0.019(2) 0.037(2) 0.041(2) C2 0.106(4) 0.087(3) 0.124(4) 0.025(3) 0.045(3) 0.068(3) C3 0.088(3) 0.119(4) 0.112(4) 0.039(3) 0.042(3) 0.074(3) C4 0.059(2) 0.094(3) 0.082(3) 0.019(2) 0.0217(19) 0.038(2) C5 0.0528(19) 0.070(2) 0.057(2) 0.0209(17) 0.0242(15) 0.0291(17) C6 0.0448(17) 0.0578(18) 0.0507(18) 0.0109(14) 0.0186(13) 0.0192(14) C7 0.0369(16) 0.071(2) 0.061(2) 0.0071(17) 0.0130(14) 0.0121(16) C8 0.0486(17) 0.0519(18) 0.0550(19) 0.0076(15) 0.0204(14) 0.0064(14) C9 0.061(2) 0.0502(18) 0.064(2) 0.0033(16) 0.0254(17) 0.0040(16) C10 0.070(3) 0.067(2) 0.096(3) -0.014(2) 0.023(2) -0.006(2) C11 0.092(4) 0.068(3) 0.120(4) -0.026(3) 0.023(3) -0.013(3) C12 0.118(4) 0.050(2) 0.127(4) -0.019(3) 0.048(3) 0.001(3) C13 0.095(3) 0.0445(19) 0.108(3) -0.002(2) 0.048(3) 0.010(2) C14 0.066(2) 0.049(2) 0.089(3) 0.0033(19) 0.033(2) 0.0224(17) C15 0.082(3) 0.0451(18) 0.081(3) 0.0070(17) 0.033(2) 0.0207(17) C16 0.082(3) 0.058(2) 0.074(3) 0.0003(18) 0.032(2) 0.0243(19) C17 0.0546(19) 0.061(2) 0.056(2) 0.0025(16) 0.0126(15) 0.0142(16) C18 0.066(2) 0.0502(18) 0.070(2) 0.0143(17) 0.0201(18) 0.0189(16) C19 0.058(2) 0.0497(18) 0.070(2) 0.0098(16) 0.0256(17) 0.0213(15) C20 0.063(2) 0.082(3) 0.055(2) 0.0090(19) 0.0175(17) 0.0163(19) C21 0.129(4) 0.118(4) 0.086(3) 0.022(3) 0.052(3) 0.059(3) C22 0.147(5) 0.180(7) 0.084(4) 0.035(4) 0.066(4) 0.082(5) C23 0.119(4) 0.170(6) 0.084(4) 0.052(4) 0.052(3) 0.040(4) C24 0.187(7) 0.121(5) 0.111(5) 0.022(4) 0.087(5) -0.002(5) C25 0.156(5) 0.086(3) 0.097(4) 0.008(3) 0.073(4) 0.000(3) B1 0.126(5) 0.066(3) 0.107(4) 0.024(3) 0.065(4) 0.038(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 Fe1 N3 2.069(2) 2_656 ? Fe1 N2 2.099(2) . ? Fe1 N5 2.143(4) . ? Fe1 N6 2.203(3) . ? Fe1 N1 2.223(3) . ? Fe1 N4 2.263(3) 2_656 ? N1 C1 1.334(4) . ? N1 C5 1.356(4) . ? N2 C6 1.338(4) . ? N2 N3 1.353(3) . ? N3 C8 1.356(4) . ? N3 Fe1 2.069(2) 2_656 ? N4 C9 1.338(5) . ? N4 C13 1.346(4) . ? N4 Fe1 2.263(3) 2_656 ? N5 C14 1.126(5) . ? N6 C19 1.337(4) . ? N6 C15 1.339(4) . ? C1 C2 1.363(6) . ? C1 H1 0.9300 . ? C2 C3 1.344(7) . ? C2 H2 0.9300 . ? C3 C4 1.389(6) . ? C3 H3 0.9300 . ? C4 C5 1.377(5) . ? C4 H4 0.9300 . ? C5 C6 1.465(4) . ? C6 C7 1.374(5) . ? C7 C8 1.378(5) . ? C7 H5 0.9300 . ? C8 C9 1.470(4) . ? C9 C10 1.386(5) . ? C10 C11 1.372(6) . ? C10 H6 0.9300 . ? C11 C12 1.344(7) . ? C11 H7 0.9300 . ? C12 C13 1.376(7) . ? C12 H8 0.9300 . ? C13 H9 0.9300 . ? C14 B1 1.590(7) . ? C15 C16 1.354(5) . ? C15 H13 0.9300 . ? C16 C17 1.381(5) . ? C16 H14 0.9300 . ? C17 C18 1.392(5) . ? C17 C20 1.481(5) . ? C18 C19 1.351(5) . ? C18 H15 0.9300 . ? C19 H16 0.9300 . ? C20 C25 1.373(6) . ? C20 C21 1.393(6) . ? C21 C22 1.380(7) . ? C21 H17 0.9300 . ? C22 C23 1.355(8) . ? C22 H18 0.9300 . ? C23 C24 1.353(8) . ? C23 H19 0.9300 . ? C24 C25 1.374(7) . ? C24 H20 0.9300 . ? C25 H21 0.9300 . ? B1 H10 0.9600 . ? B1 H11 0.9600 . ? B1 H12 0.9600 . ? 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 N3 Fe1 N2 93.29(9) 2_656 . ? N3 Fe1 N5 95.55(11) 2_656 . ? N2 Fe1 N5 97.70(11) . . ? N3 Fe1 N6 93.47(10) 2_656 . ? N2 Fe1 N6 90.54(10) . . ? N5 Fe1 N6 167.39(10) . . ? N3 Fe1 N1 168.38(10) 2_656 . ? N2 Fe1 N1 75.10(10) . . ? N5 Fe1 N1 86.65(11) . . ? N6 Fe1 N1 86.27(10) . . ? N3 Fe1 N4 75.37(10) 2_656 2_656 ? N2 Fe1 N4 167.65(10) . 2_656 ? N5 Fe1 N4 88.40(12) . 2_656 ? N6 Fe1 N4 85.37(10) . 2_656 ? N1 Fe1 N4 116.15(11) . 2_656 ? C1 N1 C5 117.5(3) . . ? C1 N1 Fe1 128.1(3) . . ? C5 N1 Fe1 114.4(2) . . ? C6 N2 N3 107.8(2) . . ? C6 N2 Fe1 119.0(2) . . ? N3 N2 Fe1 133.24(19) . . ? N2 N3 C8 107.7(2) . . ? N2 N3 Fe1 133.45(19) . 2_656 ? C8 N3 Fe1 118.9(2) . 2_656 ? C9 N4 C13 117.9(3) . . ? C9 N4 Fe1 113.5(2) . 2_656 ? C13 N4 Fe1 128.5(3) . 2_656 ? C14 N5 Fe1 178.9(3) . . ? C19 N6 C15 115.0(3) . . ? C19 N6 Fe1 118.9(2) . . ? C15 N6 Fe1 125.6(2) . . ? N1 C1 C2 123.1(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.7(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.5(3) . . ? C4 C5 C6 122.7(3) . . ? N2 C6 C7 110.6(3) . . ? N2 C6 C5 116.1(3) . . ? C7 C6 C5 133.3(3) . . ? C6 C7 C8 104.3(3) . . ? C6 C7 H5 127.9 . . ? C8 C7 H5 127.9 . . ? N3 C8 C7 109.6(3) . . ? N3 C8 C9 116.4(3) . . ? C7 C8 C9 133.8(3) . . ? N4 C9 C10 121.6(3) . . ? N4 C9 C8 115.6(3) . . ? C10 C9 C8 122.7(4) . . ? C11 C10 C9 119.4(5) . . ? C11 C10 H6 120.3 . . ? C9 C10 H6 120.3 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 H7 120.5 . . ? C10 C11 H7 120.5 . . ? C11 C12 C13 119.8(4) . . ? C11 C12 H8 120.1 . . ? C13 C12 H8 120.1 . . ? N4 C13 C12 122.1(4) . . ? N4 C13 H9 118.9 . . ? C12 C13 H9 118.9 . . ? N5 C14 B1 178.9(4) . . ? N6 C15 C16 124.2(3) . . ? N6 C15 H13 117.9 . . ? C16 C15 H13 117.9 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 H14 119.5 . . ? C17 C16 H14 119.5 . . ? C16 C17 C18 114.5(3) . . ? C16 C17 C20 123.0(3) . . ? C18 C17 C20 122.4(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H15 119.4 . . ? C17 C18 H15 119.4 . . ? N6 C19 C18 123.9(3) . . ? N6 C19 H16 118.0 . . ? C18 C19 H16 118.0 . . ? C25 C20 C21 117.0(4) . . ? C25 C20 C17 121.4(4) . . ? C21 C20 C17 121.5(4) . . ? C22 C21 C20 120.7(5) . . ? C22 C21 H17 119.6 . . ? C20 C21 H17 119.6 . . ? C23 C22 C21 120.1(5) . . ? C23 C22 H18 120.0 . . ? C21 C22 H18 120.0 . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H19 119.8 . . ? C22 C23 H19 119.8 . . ? C23 C24 C25 119.8(6) . . ? C23 C24 H20 120.1 . . ? C25 C24 H20 120.1 . . ? C20 C25 C24 121.8(5) . . ? C20 C25 H21 119.1 . . ? C24 C25 H21 119.1 . . ? C14 B1 H10 109.5 . . ? C14 B1 H11 109.5 . . ? H10 B1 H11 109.5 . . ? C14 B1 H12 109.5 . . ? H10 B1 H12 109.5 . . ? H11 B1 H12 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 N1 C1 -177.7(5) 2_656 . . . ? N2 Fe1 N1 C1 179.9(3) . . . . ? N5 Fe1 N1 C1 81.0(3) . . . . ? N6 Fe1 N1 C1 -88.6(3) . . . . ? N4 Fe1 N1 C1 -5.6(4) 2_656 . . . ? N3 Fe1 N1 C5 1.3(7) 2_656 . . . ? N2 Fe1 N1 C5 -1.2(2) . . . . ? N5 Fe1 N1 C5 -100.1(2) . . . . ? N6 Fe1 N1 C5 90.4(2) . . . . ? N4 Fe1 N1 C5 173.3(2) 2_656 . . . ? N3 Fe1 N2 C6 -178.8(2) 2_656 . . . ? N5 Fe1 N2 C6 85.1(2) . . . . ? N6 Fe1 N2 C6 -85.3(2) . . . . ? N1 Fe1 N2 C6 0.7(2) . . . . ? N4 Fe1 N2 C6 -155.8(4) 2_656 . . . ? N3 Fe1 N2 N3 1.4(3) 2_656 . . . ? N5 Fe1 N2 N3 -94.7(3) . . . . ? N6 Fe1 N2 N3 94.9(3) . . . . ? N1 Fe1 N2 N3 -179.1(3) . . . . ? N4 Fe1 N2 N3 24.4(7) 2_656 . . . ? C6 N2 N3 C8 -0.5(4) . . . . ? Fe1 N2 N3 C8 179.3(2) . . . . ? C6 N2 N3 Fe1 178.3(2) . . . 2_656 ? Fe1 N2 N3 Fe1 -1.9(5) . . . 2_656 ? N3 Fe1 N5 C14 -146(16) 2_656 . . . ? N2 Fe1 N5 C14 -52(16) . . . . ? N6 Fe1 N5 C14 78(16) . . . . ? N1 Fe1 N5 C14 22(16) . . . . ? N4 Fe1 N5 C14 139(16) 2_656 . . . ? N3 Fe1 N6 C19 44.4(2) 2_656 . . . ? N2 Fe1 N6 C19 -49.0(2) . . . . ? N5 Fe1 N6 C19 180.0(4) . . . . ? N1 Fe1 N6 C19 -124.0(2) . . . . ? N4 Fe1 N6 C19 119.4(2) 2_656 . . . ? N3 Fe1 N6 C15 -143.4(3) 2_656 . . . ? N2 Fe1 N6 C15 123.3(3) . . . . ? N5 Fe1 N6 C15 -7.8(7) . . . . ? N1 Fe1 N6 C15 48.2(3) . . . . ? N4 Fe1 N6 C15 -68.4(3) 2_656 . . . ? C5 N1 C1 C2 -0.3(6) . . . . ? Fe1 N1 C1 C2 178.6(3) . . . . ? N1 C1 C2 C3 -0.1(8) . . . . ? C1 C2 C3 C4 0.9(8) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? C1 N1 C5 C4 -0.1(5) . . . . ? Fe1 N1 C5 C4 -179.1(3) . . . . ? C1 N1 C5 C6 -179.4(3) . . . . ? Fe1 N1 C5 C6 1.5(4) . . . . ? C3 C4 C5 N1 0.9(6) . . . . ? C3 C4 C5 C6 -179.8(3) . . . . ? N3 N2 C6 C7 0.3(4) . . . . ? Fe1 N2 C6 C7 -179.5(2) . . . . ? N3 N2 C6 C5 179.7(3) . . . . ? Fe1 N2 C6 C5 -0.1(4) . . . . ? N1 C5 C6 N2 -1.0(4) . . . . ? C4 C5 C6 N2 179.6(3) . . . . ? N1 C5 C6 C7 178.2(3) . . . . ? C4 C5 C6 C7 -1.1(6) . . . . ? N2 C6 C7 C8 0.0(4) . . . . ? C5 C6 C7 C8 -179.3(3) . . . . ? N2 N3 C8 C7 0.5(4) . . . . ? Fe1 N3 C8 C7 -178.5(2) 2_656 . . . ? N2 N3 C8 C9 -175.3(3) . . . . ? Fe1 N3 C8 C9 5.8(4) 2_656 . . . ? C6 C7 C8 N3 -0.3(4) . . . . ? C6 C7 C8 C9 174.4(4) . . . . ? C13 N4 C9 C10 -2.3(6) . . . . ? Fe1 N4 C9 C10 -179.5(3) 2_656 . . . ? C13 N4 C9 C8 175.6(3) . . . . ? Fe1 N4 C9 C8 -1.6(4) 2_656 . . . ? N3 C8 C9 N4 -2.5(5) . . . . ? C7 C8 C9 N4 -176.9(4) . . . . ? N3 C8 C9 C10 175.5(3) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? N4 C9 C10 C11 3.2(6) . . . . ? C8 C9 C10 C11 -174.6(4) . . . . ? C9 C10 C11 C12 -1.3(8) . . . . ? C10 C11 C12 C13 -1.2(8) . . . . ? C9 N4 C13 C12 -0.3(6) . . . . ? Fe1 N4 C13 C12 176.4(4) 2_656 . . . ? C11 C12 C13 N4 2.1(8) . . . . ? Fe1 N5 C14 B1 -120(23) . . . . ? C19 N6 C15 C16 2.4(5) . . . . ? Fe1 N6 C15 C16 -170.1(3) . . . . ? N6 C15 C16 C17 -0.2(6) . . . . ? C15 C16 C17 C18 -2.6(5) . . . . ? C15 C16 C17 C20 176.2(4) . . . . ? C16 C17 C18 C19 3.2(5) . . . . ? C20 C17 C18 C19 -175.6(3) . . . . ? C15 N6 C19 C18 -1.7(5) . . . . ? Fe1 N6 C19 C18 171.3(3) . . . . ? C17 C18 C19 N6 -1.1(6) . . . . ? C16 C17 C20 C25 -163.2(4) . . . . ? C18 C17 C20 C25 15.4(6) . . . . ? C16 C17 C20 C21 17.6(6) . . . . ? C18 C17 C20 C21 -163.8(4) . . . . ? C25 C20 C21 C22 2.4(8) . . . . ? C17 C20 C21 C22 -178.4(4) . . . . ? C20 C21 C22 C23 -1.0(9) . . . . ? C21 C22 C23 C24 -0.3(10) . . . . ? C22 C23 C24 C25 0.1(11) . . . . ? C21 C20 C25 C24 -2.7(8) . . . . ? C17 C20 C25 C24 178.1(5) . . . . ? C23 C24 C25 C20 1.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.953 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.176