# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hung, Chen-Hsiung' 'Ching, Wei-Min' _publ_contact_author_name 'Hung, Chen-Hsiung' _publ_contact_author_email chhung@chem.sinica.edu.tw _publ_section_title ; Interior Aliphatic C-H Bond Activation on Iron(II) N-Confused Porphyrin through Synergistic Nitric Oxide Binding and Iron Oxidation ; # Attachment '- cif_bind.cif' data_i12300mp_FeHCTPPCH3Br_cmpd2 _database_code_depnum_ccdc_archive 'CCDC 866963' #TrackingRef '- cif_bind.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 Br Fe N4 O' _chemical_formula_weight 835.60 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 P2(1)/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 12.4227(9) _cell_length_b 25.958(2) _cell_length_c 13.1178(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.087(5) _cell_angle_gamma 90.00 _cell_volume 3861.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3508 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 21.39 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.470 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8097 _exptl_absorpt_correction_T_max 0.9301 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25699 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.12 _reflns_number_total 6850 _reflns_number_gt 4006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0834P)^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 6850 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.30538(6) 0.07024(3) 0.02472(7) 0.0332(2) Uani 1 1 d . A 1 Br1 Br 0.14792(5) 0.12419(2) 0.02837(5) 0.0401(2) Uani 1 1 d . A 1 N1 N 0.1330(4) 0.12889(16) -0.2565(4) 0.0407(13) Uani 1 1 d . A 1 H1 H 0.1094 0.1599 -0.2832 0.049 Uiso 1 1 calc R A 1 N2 N 0.4404(4) 0.11966(16) 0.0173(4) 0.0356(12) Uani 1 1 d . A 1 N3 N 0.4297(4) 0.04517(17) 0.1754(4) 0.0344(11) Uani 1 1 d . A 1 N4 N 0.2333(4) -0.00587(16) 0.0014(4) 0.0321(11) Uani 1 1 d . A 1 O1 O 1.0922(5) 0.23088(19) 0.7675(6) 0.108(2) Uani 1 1 d . B 1 C1 C 0.2509(4) 0.06146(19) -0.1775(5) 0.0322(14) Uani 1 1 d . A 1 C2 C 0.2503(5) 0.1137(2) -0.2014(5) 0.0340(14) Uani 1 1 d . A 1 C3 C 0.3441(5) 0.1503(2) -0.1767(6) 0.0363(15) Uani 1 1 d . A 1 C4 C 0.4372(5) 0.1482(2) -0.0752(6) 0.0383(15) Uani 1 1 d . A 1 C5 C 0.5485(5) 0.1759(2) -0.0396(6) 0.0451(17) Uani 1 1 d . A 1 H5 H 0.5717 0.1977 -0.0853 0.054 Uiso 1 1 calc R A 1 C6 C 0.6118(5) 0.1657(2) 0.0674(6) 0.0437(16) Uani 1 1 d . A 1 H6 H 0.6882 0.1786 0.1121 0.052 Uiso 1 1 calc R A 1 C7 C 0.5428(5) 0.1310(2) 0.1034(6) 0.0362(14) Uani 1 1 d . A 1 C8 C 0.5814(5) 0.1124(2) 0.2134(5) 0.0372(15) Uani 1 1 d . A 1 C9 C 0.5268(5) 0.0722(2) 0.2466(5) 0.0366(15) Uani 1 1 d . A 1 C10 C 0.5706(5) 0.0496(2) 0.3576(5) 0.0371(14) Uani 1 1 d . A 1 H10 H 0.6350 0.0617 0.4220 0.044 Uiso 1 1 calc R A 1 C11 C 0.5043(5) 0.0092(2) 0.3523(5) 0.0363(14) Uani 1 1 d . A 1 H11 H 0.5117 -0.0129 0.4125 0.044 Uiso 1 1 calc R A 1 C12 C 0.4177(5) 0.00448(19) 0.2372(5) 0.0313(13) Uani 1 1 d . A 1 C13 C 0.3402(5) -0.03629(19) 0.1941(5) 0.0311(13) Uani 1 1 d . A 1 C14 C 0.2586(4) -0.0418(2) 0.0824(5) 0.0308(14) Uani 1 1 d . A 1 C15 C 0.1887(5) -0.0874(2) 0.0406(5) 0.0359(14) Uani 1 1 d . A 1 H15 H 0.1925 -0.1181 0.0812 0.043 Uiso 1 1 calc R A 1 C16 C 0.1166(5) -0.0782(2) -0.0673(5) 0.0353(14) Uani 1 1 d . A 1 H16 H 0.0593 -0.1011 -0.1167 0.042 Uiso 1 1 calc R A 1 C17 C 0.1435(5) -0.0268(2) -0.0929(5) 0.0341(14) Uani 1 1 d . A 1 C18 C 0.0839(5) -0.0009(2) -0.1934(5) 0.0326(13) Uani 1 1 d . A 1 C19 C 0.1298(5) 0.04614(19) -0.2147(5) 0.0328(14) Uani 1 1 d . A 1 C20 C 0.0615(5) 0.08920(19) -0.2629(5) 0.0338(14) Uani 1 1 d . A 1 H20 H -0.0222 0.0903 -0.2951 0.041 Uiso 1 1 calc R A 1 C21 C 0.3330(5) 0.1887(2) -0.2630(5) 0.0376(15) Uani 1 1 d . A 1 C22 C 0.2824(5) 0.1745(2) -0.3760(6) 0.0470(17) Uani 1 1 d . A 1 H22 H 0.2549 0.1402 -0.3955 0.056 Uiso 1 1 calc R A 1 C23 C 0.2716(6) 0.2091(2) -0.4595(6) 0.0556(19) Uani 1 1 d . A 1 H23 H 0.2373 0.1986 -0.5355 0.067 Uiso 1 1 calc R A 1 C24 C 0.3110(6) 0.2589(3) -0.4317(7) 0.060(2) Uani 1 1 d . A 1 H24 H 0.3047 0.2828 -0.4886 0.072 Uiso 1 1 calc R A 1 C25 C 0.3596(5) 0.2740(3) -0.3210(7) 0.056(2) Uani 1 1 d . A 1 H25 H 0.3859 0.3085 -0.3024 0.068 Uiso 1 1 calc R A 1 C26 C 0.3706(5) 0.2393(2) -0.2364(6) 0.0477(17) Uani 1 1 d . A 1 H26 H 0.4037 0.2502 -0.1607 0.057 Uiso 1 1 calc R A 1 C27 C 0.6917(5) 0.1345(2) 0.2988(5) 0.0398(15) Uani 1 1 d . A 1 C28 C 0.6948(5) 0.1849(2) 0.3362(5) 0.0408(15) Uani 1 1 d . A 1 H28 H 0.6253 0.2053 0.3071 0.049 Uiso 1 1 calc R A 1 C29 C 0.7976(5) 0.2056(2) 0.4154(5) 0.0467(16) Uani 1 1 d . A 1 H29 H 0.7979 0.2399 0.4410 0.056 Uiso 1 1 calc R A 1 C30 C 0.8999(5) 0.1767(3) 0.4572(6) 0.0520(18) Uani 1 1 d . A 1 H30 H 0.9706 0.1910 0.5111 0.062 Uiso 1 1 calc R A 1 C31 C 0.8985(5) 0.1269(2) 0.4200(6) 0.058(2) Uani 1 1 d . A 1 H31 H 0.9686 0.1069 0.4475 0.069 Uiso 1 1 calc R A 1 C32 C 0.7969(5) 0.1065(2) 0.3444(6) 0.0530(18) Uani 1 1 d . A 1 H32 H 0.7971 0.0718 0.3214 0.064 Uiso 1 1 calc R A 1 C33 C 0.3463(4) -0.08004(19) 0.2719(5) 0.0318(13) Uani 1 1 d . A 1 C34 C 0.2715(5) -0.0833(2) 0.3254(5) 0.0417(16) Uani 1 1 d . A 1 H34 H 0.2171 -0.0563 0.3170 0.050 Uiso 1 1 calc R A 1 C35 C 0.2744(5) -0.1253(2) 0.3910(5) 0.0420(15) Uani 1 1 d . A 1 H35 H 0.2224 -0.1266 0.4276 0.050 Uiso 1 1 calc R A 1 C36 C 0.3509(5) -0.1649(2) 0.4040(5) 0.0396(15) Uani 1 1 d . A 1 H36 H 0.3509 -0.1941 0.4477 0.048 Uiso 1 1 calc R A 1 C37 C 0.4282(6) -0.1622(2) 0.3530(6) 0.064(2) Uani 1 1 d . A 1 H37 H 0.4831 -0.1892 0.3624 0.077 Uiso 1 1 calc R A 1 C38 C 0.4254(6) -0.1197(2) 0.2877(6) 0.064(2) Uani 1 1 d . A 1 H38 H 0.4792 -0.1178 0.2532 0.077 Uiso 1 1 calc R A 1 C39 C -0.0298(5) -0.0197(2) -0.2762(5) 0.0335(14) Uani 1 1 d . A 1 C40 C -0.1134(5) -0.04337(19) -0.2446(5) 0.0348(14) Uani 1 1 d . A 1 H40 H -0.0982 -0.0461 -0.1678 0.042 Uiso 1 1 calc R A 1 C41 C -0.2176(5) -0.0628(2) -0.3245(5) 0.0360(14) Uani 1 1 d . A 1 H41 H -0.2718 -0.0798 -0.3016 0.043 Uiso 1 1 calc R A 1 C42 C -0.2438(5) -0.0577(2) -0.4370(5) 0.0388(15) Uani 1 1 d . A 1 H42 H -0.3155 -0.0710 -0.4915 0.047 Uiso 1 1 calc R A 1 C43 C -0.1635(5) -0.0329(2) -0.4692(5) 0.0408(15) Uani 1 1 d . A 1 H43 H -0.1807 -0.0290 -0.5463 0.049 Uiso 1 1 calc R A 1 C44 C -0.0597(5) -0.0139(2) -0.3907(5) 0.0400(15) Uani 1 1 d . A 1 H44 H -0.0069 0.0036 -0.4146 0.048 Uiso 1 1 calc R A 1 C45 C 0.3556(5) 0.02619(19) -0.1498(5) 0.0404(15) Uani 1 1 d . A 1 H45A H 0.4108 0.0413 -0.1776 0.061 Uiso 1 1 calc R A 1 H45B H 0.3288 -0.0074 -0.1851 0.061 Uiso 1 1 calc R A 1 H45C H 0.3952 0.0218 -0.0687 0.061 Uiso 1 1 calc R A 1 C46 C 1.0776(6) 0.2771(3) 0.6985(8) 0.088(3) Uani 1 1 d . B 1 H46A H 1.1392 0.3030 0.7380 0.106 Uiso 1 1 calc R B 1 H46B H 1.0816 0.2683 0.6267 0.106 Uiso 1 1 calc R B 1 C47 C 0.9637(7) 0.2959(3) 0.6809(8) 0.090(3) Uani 1 1 d . B 1 H47A H 0.9182 0.3049 0.6015 0.108 Uiso 1 1 calc R B 1 H47B H 0.9700 0.3268 0.7272 0.108 Uiso 1 1 calc R B 1 C48 C 0.9038(8) 0.2511(3) 0.7161(7) 0.082(3) Uani 1 1 d . B 1 H48A H 0.8422 0.2636 0.7397 0.099 Uiso 1 1 calc R B 1 H48B H 0.8692 0.2254 0.6556 0.099 Uiso 1 1 calc R B 1 C49 C 1.0031(6) 0.2309(3) 0.8076(7) 0.065(2) Uani 1 1 d . B 1 H49A H 1.0247 0.2531 0.8744 0.078 Uiso 1 1 calc R B 1 H49B H 0.9874 0.1956 0.8266 0.078 Uiso 1 1 calc R B 1 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 0.0339(5) 0.0291(4) 0.0483(6) 0.0038(4) 0.0287(4) 0.0013(3) Br1 0.0390(3) 0.0360(3) 0.0586(5) 0.0024(3) 0.0335(3) 0.0025(3) N1 0.045(3) 0.031(3) 0.059(4) 0.015(3) 0.035(3) 0.004(2) N2 0.036(3) 0.031(3) 0.051(3) 0.004(3) 0.030(3) 0.003(2) N3 0.034(3) 0.031(3) 0.046(3) 0.001(2) 0.025(3) 0.002(2) N4 0.031(3) 0.033(3) 0.038(3) 0.005(2) 0.020(2) -0.001(2) O1 0.139(5) 0.062(3) 0.192(7) 0.034(4) 0.136(5) 0.025(3) C1 0.038(3) 0.030(3) 0.039(4) 0.007(3) 0.028(3) 0.005(2) C2 0.040(3) 0.034(3) 0.042(4) 0.000(3) 0.031(3) -0.004(3) C3 0.042(3) 0.026(3) 0.057(4) 0.003(3) 0.036(4) 0.002(3) C4 0.044(4) 0.025(3) 0.062(5) 0.005(3) 0.038(4) 0.003(3) C5 0.039(3) 0.036(3) 0.076(5) 0.005(4) 0.040(4) -0.005(3) C6 0.041(4) 0.036(3) 0.063(5) 0.006(3) 0.030(4) -0.003(3) C7 0.032(3) 0.032(3) 0.054(4) 0.000(3) 0.026(3) 0.000(3) C8 0.030(3) 0.029(3) 0.059(5) -0.005(3) 0.025(3) -0.003(2) C9 0.035(3) 0.033(3) 0.052(4) -0.003(3) 0.029(3) 0.006(3) C10 0.035(3) 0.033(3) 0.045(4) -0.006(3) 0.019(3) -0.002(3) C11 0.037(3) 0.035(3) 0.044(4) 0.001(3) 0.024(3) 0.000(3) C12 0.037(3) 0.025(3) 0.047(4) 0.003(3) 0.031(3) 0.007(2) C13 0.034(3) 0.026(3) 0.044(4) 0.004(3) 0.026(3) 0.006(2) C14 0.027(3) 0.029(3) 0.047(4) 0.001(3) 0.026(3) 0.004(2) C15 0.039(3) 0.025(3) 0.052(4) 0.005(3) 0.027(3) 0.002(3) C16 0.035(3) 0.028(3) 0.044(4) -0.001(3) 0.017(3) -0.004(2) C17 0.037(3) 0.028(3) 0.049(4) 0.001(3) 0.030(3) 0.002(3) C18 0.036(3) 0.028(3) 0.043(4) 0.005(3) 0.026(3) 0.005(3) C19 0.040(3) 0.026(3) 0.041(4) 0.001(3) 0.025(3) -0.004(3) C20 0.033(3) 0.030(3) 0.046(4) 0.010(3) 0.024(3) 0.001(3) C21 0.042(3) 0.029(3) 0.055(4) 0.008(3) 0.033(3) 0.006(3) C22 0.063(4) 0.031(3) 0.070(5) 0.006(4) 0.051(4) 0.003(3) C23 0.075(5) 0.047(4) 0.070(5) 0.014(4) 0.055(4) 0.007(3) C24 0.064(5) 0.049(4) 0.096(7) 0.027(5) 0.060(5) 0.014(4) C25 0.047(4) 0.042(4) 0.089(6) 0.019(4) 0.036(4) 0.000(3) C26 0.042(4) 0.035(3) 0.077(5) 0.009(4) 0.036(4) 0.000(3) C27 0.036(3) 0.037(3) 0.057(4) 0.002(3) 0.029(3) -0.003(3) C28 0.040(3) 0.041(4) 0.050(4) 0.002(3) 0.026(3) 0.001(3) C29 0.055(4) 0.039(4) 0.053(4) -0.004(3) 0.028(4) -0.008(3) C30 0.043(4) 0.058(4) 0.059(5) 0.001(4) 0.025(4) -0.017(3) C31 0.030(3) 0.049(4) 0.093(6) 0.003(4) 0.025(4) -0.002(3) C32 0.036(4) 0.040(4) 0.084(6) -0.007(4) 0.025(4) -0.001(3) C33 0.030(3) 0.029(3) 0.042(4) 0.002(3) 0.021(3) 0.000(2) C34 0.041(3) 0.029(3) 0.068(5) 0.006(3) 0.035(3) 0.009(3) C35 0.043(3) 0.039(3) 0.057(4) 0.004(3) 0.034(3) -0.003(3) C36 0.046(3) 0.031(3) 0.049(4) 0.004(3) 0.026(3) -0.001(3) C37 0.074(5) 0.052(4) 0.094(6) 0.038(4) 0.062(5) 0.035(4) C38 0.073(5) 0.053(4) 0.098(6) 0.029(4) 0.069(5) 0.030(4) C39 0.034(3) 0.031(3) 0.042(4) 0.003(3) 0.022(3) 0.004(2) C40 0.038(3) 0.027(3) 0.048(4) 0.010(3) 0.026(3) 0.011(3) C41 0.030(3) 0.034(3) 0.051(4) 0.001(3) 0.023(3) -0.001(3) C42 0.037(3) 0.034(3) 0.046(4) -0.006(3) 0.017(3) 0.001(3) C43 0.045(4) 0.046(4) 0.035(4) 0.000(3) 0.020(3) 0.008(3) C44 0.042(4) 0.041(3) 0.044(4) 0.002(3) 0.025(3) 0.002(3) C45 0.048(4) 0.030(3) 0.059(4) -0.008(3) 0.039(3) -0.003(3) C46 0.071(5) 0.064(5) 0.154(9) 0.073(5) 0.071(6) 0.026(4) C47 0.102(7) 0.055(5) 0.114(8) 0.014(5) 0.046(6) 0.010(5) C48 0.104(7) 0.069(6) 0.091(7) -0.015(5) 0.057(6) -0.003(5) C49 0.068(5) 0.061(5) 0.088(6) 0.008(4) 0.055(5) 0.020(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 N3 2.055(5) . ? Fe1 N4 2.139(4) . ? Fe1 N2 2.145(4) . ? Fe1 Br1 2.4220(9) . ? Fe1 C1 2.466(6) . ? N1 C20 1.341(6) . ? N1 C2 1.393(7) . ? N1 H1 0.8800 . ? N2 C7 1.345(7) . ? N2 C4 1.409(7) . ? N3 C12 1.376(6) . ? N3 C9 1.379(7) . ? N4 C14 1.352(7) . ? N4 C17 1.394(7) . ? O1 C49 1.405(7) . ? O1 C46 1.469(8) . ? C1 C2 1.392(7) . ? C1 C19 1.435(7) . ? C1 C45 1.509(7) . ? C2 C3 1.434(7) . ? C3 C4 1.362(8) . ? C3 C21 1.472(8) . ? C4 C5 1.455(7) . ? C5 C6 1.327(8) . ? C5 H5 0.9500 . ? C6 C7 1.449(7) . ? C6 H6 0.9500 . ? C7 C8 1.407(8) . ? C8 C9 1.407(7) . ? C8 C27 1.486(8) . ? C9 C10 1.453(8) . ? C10 C11 1.319(7) . ? C10 H10 0.9500 . ? C11 C12 1.459(8) . ? C11 H11 0.9500 . ? C12 C13 1.386(7) . ? C13 C14 1.408(8) . ? C13 C33 1.508(7) . ? C14 C15 1.436(7) . ? C15 C16 1.352(8) . ? C15 H15 0.9500 . ? C16 C17 1.450(7) . ? C16 H16 0.9500 . ? C17 C18 1.392(8) . ? C18 C19 1.422(7) . ? C18 C39 1.470(8) . ? C19 C20 1.390(7) . ? C20 H20 0.9500 . ? C21 C26 1.392(8) . ? C21 C22 1.403(8) . ? C22 C23 1.380(8) . ? C22 H22 0.9500 . ? C23 C24 1.378(9) . ? C23 H23 0.9500 . ? C24 C25 1.383(10) . ? C24 H24 0.9500 . ? C25 C26 1.391(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.392(7) . ? C27 C32 1.398(8) . ? C28 C29 1.385(8) . ? C28 H28 0.9500 . ? C29 C30 1.382(8) . ? C29 H29 0.9500 . ? C30 C31 1.380(9) . ? C30 H30 0.9500 . ? C31 C32 1.355(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.376(7) . ? C33 C38 1.378(7) . ? C34 C35 1.380(7) . ? C34 H34 0.9500 . ? C35 C36 1.362(7) . ? C35 H35 0.9500 . ? C36 C37 1.379(7) . ? C36 H36 0.9500 . ? C37 C38 1.388(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.400(8) . ? C39 C40 1.407(7) . ? C40 C41 1.386(7) . ? C40 H40 0.9500 . ? C41 C42 1.382(8) . ? C41 H41 0.9500 . ? C42 C43 1.390(7) . ? C42 H42 0.9500 . ? C43 C44 1.372(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.424(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.549(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.425(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N4 87.21(18) . . ? N3 Fe1 N2 86.47(18) . . ? N4 Fe1 N2 146.65(15) . . ? N3 Fe1 Br1 117.39(12) . . ? N4 Fe1 Br1 104.04(11) . . ? N2 Fe1 Br1 107.93(11) . . ? N3 Fe1 C1 140.71(16) . . ? N4 Fe1 C1 81.12(17) . . ? N2 Fe1 C1 83.28(18) . . ? Br1 Fe1 C1 101.85(12) . . ? C20 N1 C2 110.0(4) . . ? C20 N1 H1 125.0 . . ? C2 N1 H1 125.0 . . ? C7 N2 C4 107.0(4) . . ? C7 N2 Fe1 125.6(4) . . ? C4 N2 Fe1 127.3(4) . . ? C12 N3 C9 105.5(5) . . ? C12 N3 Fe1 126.1(4) . . ? C9 N3 Fe1 126.6(4) . . ? C14 N4 C17 105.9(4) . . ? C14 N4 Fe1 125.2(4) . . ? C17 N4 Fe1 128.5(4) . . ? C49 O1 C46 108.2(5) . . ? C2 C1 C19 106.6(4) . . ? C2 C1 C45 124.8(4) . . ? C19 C1 C45 126.5(5) . . ? C2 C1 Fe1 97.3(4) . . ? C19 C1 Fe1 100.4(3) . . ? C45 C1 Fe1 88.0(3) . . ? C1 C2 N1 107.5(4) . . ? C1 C2 C3 131.7(5) . . ? N1 C2 C3 120.8(5) . . ? C4 C3 C2 118.9(5) . . ? C4 C3 C21 123.6(5) . . ? C2 C3 C21 117.5(6) . . ? C3 C4 N2 125.2(5) . . ? C3 C4 C5 127.6(6) . . ? N2 C4 C5 107.2(6) . . ? C6 C5 C4 108.4(5) . . ? C6 C5 H5 125.8 . . ? C4 C5 H5 125.8 . . ? C5 C6 C7 107.2(6) . . ? C5 C6 H6 126.4 . . ? C7 C6 H6 126.4 . . ? N2 C7 C8 126.6(5) . . ? N2 C7 C6 110.2(6) . . ? C8 C7 C6 123.2(6) . . ? C7 C8 C9 124.5(6) . . ? C7 C8 C27 117.7(5) . . ? C9 C8 C27 117.7(6) . . ? N3 C9 C8 124.5(6) . . ? N3 C9 C10 109.8(5) . . ? C8 C9 C10 125.4(6) . . ? C11 C10 C9 107.4(6) . . ? C11 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? C10 C11 C12 107.6(5) . . ? C10 C11 H11 126.2 . . ? C12 C11 H11 126.2 . . ? N3 C12 C13 124.8(5) . . ? N3 C12 C11 109.5(5) . . ? C13 C12 C11 125.6(5) . . ? C12 C13 C14 126.0(5) . . ? C12 C13 C33 117.7(5) . . ? C14 C13 C33 116.3(5) . . ? N4 C14 C13 125.8(5) . . ? N4 C14 C15 111.0(5) . . ? C13 C14 C15 123.2(5) . . ? C16 C15 C14 107.1(5) . . ? C16 C15 H15 126.4 . . ? C14 C15 H15 126.4 . . ? C15 C16 C17 106.7(5) . . ? C15 C16 H16 126.7 . . ? C17 C16 H16 126.7 . . ? C18 C17 N4 125.2(5) . . ? C18 C17 C16 125.5(5) . . ? N4 C17 C16 109.2(5) . . ? C17 C18 C19 119.9(5) . . ? C17 C18 C39 121.3(5) . . ? C19 C18 C39 118.7(5) . . ? C20 C19 C18 124.1(5) . . ? C20 C19 C1 107.0(4) . . ? C18 C19 C1 128.3(5) . . ? N1 C20 C19 108.9(5) . . ? N1 C20 H20 125.6 . . ? C19 C20 H20 125.6 . . ? C26 C21 C22 118.2(6) . . ? C26 C21 C3 122.0(6) . . ? C22 C21 C3 119.7(5) . . ? C23 C22 C21 121.6(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 119.5(7) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.0(7) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 119.8(7) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C28 C27 C32 116.8(5) . . ? C28 C27 C8 120.8(5) . . ? C32 C27 C8 122.4(5) . . ? C29 C28 C27 120.9(5) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 120.2(6) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 119.4(6) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C31 C30 119.9(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 122.6(6) . . ? C31 C32 H32 118.7 . . ? C27 C32 H32 118.7 . . ? C34 C33 C38 117.7(5) . . ? C34 C33 C13 122.3(5) . . ? C38 C33 C13 119.9(5) . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 120.9(5) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 119.3(5) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C38 119.5(5) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C33 C38 C37 121.5(5) . . ? C33 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C44 C39 C40 117.2(5) . . ? C44 C39 C18 120.8(5) . . ? C40 C39 C18 122.0(5) . . ? C41 C40 C39 120.7(6) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C42 C41 C40 120.8(5) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 118.9(6) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C44 C43 C42 120.7(6) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C39 121.5(5) . . ? C43 C44 H44 119.2 . . ? C39 C44 H44 119.2 . . ? C47 C46 O1 104.1(5) . . ? C47 C46 H46A 110.9 . . ? O1 C46 H46A 110.9 . . ? C47 C46 H46B 110.9 . . ? O1 C46 H46B 110.9 . . ? H46A C46 H46B 109.0 . . ? C46 C47 C48 105.1(6) . . ? C46 C47 H47A 110.7 . . ? C48 C47 H47A 110.7 . . ? C46 C47 H47B 110.7 . . ? C48 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? C49 C48 C47 99.9(7) . . ? C49 C48 H48A 111.8 . . ? C47 C48 H48A 111.8 . . ? C49 C48 H48B 111.8 . . ? C47 C48 H48B 111.8 . . ? H48A C48 H48B 109.5 . . ? O1 C49 C48 103.2(7) . . ? O1 C49 H49A 111.1 . . ? C48 C49 H49A 111.1 . . ? O1 C49 H49B 111.1 . . ? C48 C49 H49B 111.1 . . ? H49A C49 H49B 109.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.263 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.105 #==END data_i11526p2_FeCTPPCH3NO_cmpd3 _database_code_depnum_ccdc_archive 'CCDC 866964' #TrackingRef '- cif_bind.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H32 Cl2 Fe N5 O' _chemical_formula_weight 797.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 11.7119(11) _cell_length_b 12.9672(10) _cell_length_c 14.6335(11) _cell_angle_alpha 64.680(5) _cell_angle_beta 86.090(6) _cell_angle_gamma 65.569(5) _cell_volume 1813.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 697 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 18.19 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9416 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11569 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1786 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.28 _reflns_number_total 6304 _reflns_number_gt 3009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0974P)^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 6304 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1688 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2157 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 0.71107(9) 0.94577(9) 0.62658(7) 0.0246(3) Uani 1 1 d . A 1 O1 O 0.9555(6) 0.8649(5) 0.7084(5) 0.073(2) Uani 1 1 d . A 1 N1 N 0.9457(6) 0.5772(6) 0.7411(5) 0.0332(17) Uani 0.50 1 d P A 1 N2 N 0.6212(5) 0.8803(5) 0.7464(4) 0.0240(14) Uani 1 1 d . A 1 N3 N 0.5775(5) 1.1210(5) 0.5889(4) 0.0244(13) Uani 1 1 d . A 1 N4 N 0.7552(5) 1.0062(5) 0.4833(4) 0.0247(14) Uani 1 1 d . A 1 N5 N 0.8446(6) 0.9167(5) 0.6882(4) 0.0318(15) Uani 1 1 d . A 1 N1A N 0.9906(7) 0.6198(6) 0.6535(5) 0.0344(18) Uani 0.50 1 d P B 2 C1 C 0.7834(6) 0.7683(6) 0.6306(5) 0.0233(16) Uani 1 1 d . A 1 C2 C 0.8226(6) 0.6639(6) 0.7342(5) 0.0240(16) Uani 1 1 d . A 1 C3 C 0.7533(7) 0.6516(6) 0.8148(5) 0.0284(17) Uani 1 1 d . A 1 C4 C 0.6456(7) 0.7559(6) 0.8135(5) 0.0261(17) Uani 1 1 d . A 1 C5 C 0.5547(7) 0.7509(6) 0.8819(5) 0.0282(17) Uani 1 1 d . A 1 H5 H 0.5519 0.6768 0.9340 0.034 Uiso 1 1 calc R A 1 C6 C 0.4728(6) 0.8706(6) 0.8594(5) 0.0276(17) Uani 1 1 d . A 1 H6 H 0.4005 0.8970 0.8917 0.033 Uiso 1 1 calc R A 1 C7 C 0.5156(7) 0.9507(6) 0.7771(5) 0.0270(17) Uani 1 1 d . A 1 C8 C 0.4605(6) 1.0825(6) 0.7360(5) 0.0252(17) Uani 1 1 d . A 1 C9 C 0.4936(6) 1.1590(6) 0.6514(5) 0.0216(16) Uani 1 1 d . A 1 C10 C 0.4398(6) 1.2947(6) 0.6085(5) 0.0267(17) Uani 1 1 d . A 1 H10 H 0.3804 1.3451 0.6369 0.032 Uiso 1 1 calc R A 1 C11 C 0.4877(6) 1.3376(6) 0.5221(5) 0.0243(16) Uani 1 1 d . A 1 H11 H 0.4694 1.4231 0.4781 0.029 Uiso 1 1 calc R A 1 C12 C 0.5714(6) 1.2296(6) 0.5089(5) 0.0255(17) Uani 1 1 d . A 1 C13 C 0.6305(6) 1.2353(6) 0.4213(5) 0.0241(16) Uani 1 1 d . A 1 C14 C 0.7100(7) 1.1278(6) 0.4095(5) 0.0263(17) Uani 1 1 d . A 1 C15 C 0.7577(7) 1.1338(6) 0.3154(5) 0.0300(18) Uani 1 1 d . A 1 H15 H 0.7369 1.2072 0.2524 0.036 Uiso 1 1 calc R A 1 C16 C 0.8378(7) 1.0151(6) 0.3341(5) 0.0297(18) Uani 1 1 d . A 1 H16 H 0.8858 0.9886 0.2869 0.036 Uiso 1 1 calc R A 1 C17 C 0.8372(6) 0.9365(6) 0.4379(5) 0.0253(17) Uani 1 1 d . A 1 C18 C 0.9180(6) 0.8077(6) 0.4878(5) 0.0252(17) Uani 1 1 d . A 1 C19 C 0.8987(7) 0.7346(6) 0.5843(5) 0.0277(17) Uani 1 1 d . A 1 C20 C 0.9906(7) 0.6198(6) 0.6535(5) 0.0344(18) Uani 0.50 1 d P A 1 H20 H 1.064(14) 0.596(14) 0.648(11) 0.041 Uiso 0.50 1 d P C 1 C21 C 0.7925(7) 0.5260(6) 0.9059(5) 0.0273(17) Uani 1 1 d . A 1 C22 C 0.8134(7) 0.5132(6) 1.0017(5) 0.037(2) Uani 1 1 d . A 1 H22 H 0.8008 0.5845 1.0120 0.045 Uiso 1 1 calc R A 1 C23 C 0.8537(8) 0.3934(7) 1.0848(6) 0.045(2) Uani 1 1 d . A 1 H23 H 0.8686 0.3841 1.1515 0.054 Uiso 1 1 calc R A 1 C24 C 0.8720(7) 0.2897(6) 1.0713(5) 0.035(2) Uani 1 1 d . A 1 H24 H 0.8984 0.2092 1.1282 0.043 Uiso 1 1 calc R A 1 C25 C 0.8519(6) 0.3035(6) 0.9754(5) 0.0283(17) Uani 1 1 d . A 1 H25 H 0.8640 0.2323 0.9651 0.034 Uiso 1 1 calc R A 1 C26 C 0.8139(6) 0.4206(6) 0.8929(5) 0.0269(17) Uani 1 1 d . A 1 H26 H 0.8023 0.4287 0.8261 0.032 Uiso 1 1 calc R A 1 C27 C 0.3582(6) 1.1410(6) 0.7897(5) 0.0249(17) Uani 1 1 d . A 1 C28 C 0.3887(6) 1.1278(6) 0.8854(5) 0.0231(16) Uani 1 1 d . A 1 H28 H 0.4741 1.0817 0.9167 0.028 Uiso 1 1 calc R A 1 C29 C 0.2952(7) 1.1813(6) 0.9351(5) 0.0311(18) Uani 1 1 d . A 1 H29 H 0.3164 1.1723 1.0005 0.037 Uiso 1 1 calc R A 1 C30 C 0.1704(7) 1.2482(6) 0.8897(5) 0.0329(19) Uani 1 1 d . A 1 H30 H 0.1055 1.2849 0.9237 0.039 Uiso 1 1 calc R A 1 C31 C 0.1422(7) 1.2607(6) 0.7952(6) 0.0325(18) Uani 1 1 d . A 1 H31 H 0.0567 1.3067 0.7638 0.039 Uiso 1 1 calc R A 1 C32 C 0.2335(6) 1.2089(6) 0.7452(5) 0.0283(17) Uani 1 1 d . A 1 H32 H 0.2115 1.2195 0.6795 0.034 Uiso 1 1 calc R A 1 C33 C 0.6088(7) 1.3605(6) 0.3367(5) 0.0253(17) Uani 1 1 d . A 1 C34 C 0.5059(7) 1.4238(6) 0.2601(5) 0.0328(18) Uani 1 1 d . A 1 H34 H 0.4479 1.3887 0.2634 0.039 Uiso 1 1 calc R A 1 C35 C 0.4894(7) 1.5374(6) 0.1799(5) 0.0327(18) Uani 1 1 d . A 1 H35 H 0.4186 1.5820 0.1286 0.039 Uiso 1 1 calc R A 1 C36 C 0.5745(7) 1.5857(6) 0.1740(5) 0.0286(17) Uani 1 1 d . A 1 H36 H 0.5634 1.6627 0.1172 0.034 Uiso 1 1 calc R A 1 C37 C 0.6751(7) 1.5265(6) 0.2475(5) 0.0311(18) Uani 1 1 d . A 1 H37 H 0.7325 1.5625 0.2430 0.037 Uiso 1 1 calc R A 1 C38 C 0.6923(7) 1.4125(7) 0.3291(5) 0.0343(19) Uani 1 1 d . A 1 H38 H 0.7627 1.3698 0.3804 0.041 Uiso 1 1 calc R A 1 C39 C 1.0297(7) 0.7516(6) 0.4416(5) 0.0292(18) Uani 1 1 d . A 1 C40 C 1.0535(7) 0.6401(6) 0.4360(5) 0.0321(18) Uani 1 1 d . A 1 H40 H 0.9988 0.5995 0.4613 0.039 Uiso 1 1 calc R A 1 C41 C 1.1587(7) 0.5892(6) 0.3928(5) 0.036(2) Uani 1 1 d . A 1 H41 H 1.1748 0.5138 0.3879 0.043 Uiso 1 1 calc R A 1 C42 C 1.2394(7) 0.6449(6) 0.3572(5) 0.0322(18) Uani 1 1 d . A 1 H42 H 1.3108 0.6086 0.3278 0.039 Uiso 1 1 calc R A 1 C43 C 1.2163(7) 0.7537(6) 0.3641(5) 0.0343(19) Uani 1 1 d . A 1 H43 H 1.2722 0.7928 0.3398 0.041 Uiso 1 1 calc R A 1 C44 C 1.1122(6) 0.8069(6) 0.4063(5) 0.0274(17) Uani 1 1 d . A 1 H44 H 1.0973 0.8822 0.4109 0.033 Uiso 1 1 calc R A 1 C45 C 0.6617(7) 0.7957(8) 0.5736(6) 0.0318(19) Uani 1 1 d . A 1 C46 C 0.1346(7) 0.9916(7) 0.1079(7) 0.049(2) Uani 1 1 d . D 1 H46A H 0.1091 1.0673 0.0413 0.059 Uiso 1 1 calc R D 1 H46B H 0.1436 1.0166 0.1612 0.059 Uiso 1 1 calc R D 1 C20A C 0.9457(6) 0.5772(6) 0.7411(5) 0.0332(17) Uani 0.50 1 d P B 2 H20A H 0.998(13) 0.501(12) 0.813(10) 0.040 Uiso 0.50 1 d P E 2 Cl1 Cl 0.0156(2) 0.93661(19) 0.13243(15) 0.0487(6) Uani 1 1 d . D 1 Cl2 Cl 0.2812(2) 0.8760(2) 0.10593(17) 0.0542(6) Uani 1 1 d . D 1 H51 H 0.647(5) 0.864(5) 0.506(5) 0.015(16) Uiso 1 1 d . F 1 H50 H 0.666(7) 0.728(7) 0.561(5) 0.05(2) Uiso 1 1 d . G 1 H52 H 0.577(6) 0.820(6) 0.609(5) 0.030(18) Uiso 1 1 d . H 1 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 0.0242(6) 0.0176(5) 0.0259(6) -0.0081(5) 0.0031(4) -0.0050(4) O1 0.044(4) 0.041(4) 0.120(6) -0.032(4) -0.034(4) -0.002(3) N1 0.031(4) 0.027(4) 0.030(4) -0.010(3) 0.007(3) -0.005(3) N2 0.025(3) 0.017(3) 0.021(3) -0.005(3) -0.001(3) -0.004(3) N3 0.020(3) 0.020(3) 0.023(3) -0.004(3) 0.001(3) -0.006(3) N4 0.028(3) 0.011(3) 0.025(3) -0.002(3) 0.003(3) -0.005(2) N5 0.025(4) 0.028(3) 0.035(4) -0.010(3) -0.003(3) -0.008(3) N1A 0.032(4) 0.032(4) 0.032(4) -0.014(3) 0.004(4) -0.007(4) C1 0.027(4) 0.019(4) 0.020(4) -0.008(3) 0.008(3) -0.006(3) C2 0.029(4) 0.017(4) 0.025(4) -0.009(3) 0.010(3) -0.009(3) C3 0.027(4) 0.020(4) 0.032(4) -0.009(3) -0.007(3) -0.004(3) C4 0.033(4) 0.020(4) 0.024(4) -0.011(3) -0.003(3) -0.008(3) C5 0.034(4) 0.026(4) 0.022(4) -0.010(3) 0.005(3) -0.011(3) C6 0.022(4) 0.029(4) 0.031(4) -0.016(4) 0.005(3) -0.007(3) C7 0.029(4) 0.023(4) 0.031(4) -0.015(3) 0.003(3) -0.010(3) C8 0.027(4) 0.020(4) 0.022(4) -0.009(3) -0.002(3) -0.004(3) C9 0.017(4) 0.025(4) 0.017(4) -0.005(3) 0.000(3) -0.008(3) C10 0.027(4) 0.019(4) 0.029(4) -0.010(3) 0.006(3) -0.006(3) C11 0.032(4) 0.014(3) 0.015(4) 0.001(3) 0.003(3) -0.007(3) C12 0.025(4) 0.017(4) 0.026(4) -0.006(3) -0.002(3) -0.004(3) C13 0.024(4) 0.014(3) 0.027(4) -0.006(3) -0.003(3) -0.004(3) C14 0.032(4) 0.019(4) 0.025(4) -0.009(3) 0.001(3) -0.009(3) C15 0.030(4) 0.026(4) 0.028(4) -0.010(3) 0.005(3) -0.008(3) C16 0.032(4) 0.025(4) 0.029(4) -0.012(4) 0.006(3) -0.009(3) C17 0.026(4) 0.019(4) 0.026(4) -0.010(3) 0.003(3) -0.005(3) C18 0.027(4) 0.013(3) 0.025(4) -0.004(3) 0.002(3) -0.002(3) C19 0.030(4) 0.019(4) 0.036(5) -0.014(4) 0.004(4) -0.011(3) C20 0.032(4) 0.032(4) 0.032(4) -0.014(3) 0.004(4) -0.007(4) C21 0.034(4) 0.014(4) 0.023(4) -0.003(3) 0.003(3) -0.006(3) C22 0.053(5) 0.020(4) 0.033(5) -0.014(4) 0.002(4) -0.009(4) C23 0.063(6) 0.030(4) 0.022(4) -0.008(4) 0.004(4) -0.004(4) C24 0.038(5) 0.020(4) 0.026(4) 0.000(3) 0.010(4) -0.003(3) C25 0.031(4) 0.013(3) 0.037(5) -0.010(3) 0.007(4) -0.007(3) C26 0.023(4) 0.025(4) 0.031(4) -0.013(4) 0.008(3) -0.008(3) C27 0.030(4) 0.017(3) 0.025(4) -0.010(3) 0.010(3) -0.007(3) C28 0.025(4) 0.016(3) 0.022(4) -0.004(3) 0.008(3) -0.009(3) C29 0.038(5) 0.021(4) 0.029(4) -0.009(3) 0.003(4) -0.009(3) C30 0.032(5) 0.024(4) 0.041(5) -0.016(4) 0.009(4) -0.009(3) C31 0.016(4) 0.033(4) 0.046(5) -0.020(4) 0.000(4) -0.004(3) C32 0.024(4) 0.025(4) 0.036(4) -0.015(4) 0.005(3) -0.008(3) C33 0.031(4) 0.015(4) 0.024(4) -0.008(3) 0.012(3) -0.006(3) C34 0.025(4) 0.028(4) 0.042(5) -0.012(4) 0.006(4) -0.012(3) C35 0.029(4) 0.026(4) 0.030(4) -0.005(4) 0.001(3) -0.008(3) C36 0.030(4) 0.014(4) 0.032(4) -0.005(3) 0.008(4) -0.008(3) C37 0.036(5) 0.028(4) 0.034(4) -0.012(4) 0.007(4) -0.019(4) C38 0.038(5) 0.036(5) 0.034(5) -0.018(4) 0.009(4) -0.019(4) C39 0.029(4) 0.018(4) 0.023(4) -0.004(3) 0.000(3) 0.000(3) C40 0.030(4) 0.019(4) 0.040(5) -0.011(4) 0.004(4) -0.006(3) C41 0.036(5) 0.020(4) 0.034(5) -0.009(4) 0.000(4) 0.001(4) C42 0.025(4) 0.030(4) 0.030(4) -0.013(4) 0.000(3) -0.002(3) C43 0.034(5) 0.033(4) 0.023(4) -0.006(4) -0.005(3) -0.008(4) C44 0.026(4) 0.022(4) 0.025(4) -0.007(3) 0.000(3) -0.005(3) C45 0.031(5) 0.027(4) 0.024(5) -0.006(4) -0.006(4) -0.004(4) C46 0.045(6) 0.036(5) 0.063(6) -0.022(5) 0.004(5) -0.014(4) C20A 0.031(4) 0.027(4) 0.030(4) -0.010(3) 0.007(3) -0.005(3) Cl1 0.0449(13) 0.0502(13) 0.0453(13) -0.0221(11) 0.0092(10) -0.0146(10) Cl2 0.0467(14) 0.0496(13) 0.0637(15) -0.0274(12) 0.0164(12) -0.0171(11) _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 N5 1.678(6) . ? Fe1 N3 2.005(5) . ? Fe1 N4 2.015(6) . ? Fe1 N2 2.029(6) . ? Fe1 C1 2.072(6) . ? O1 N5 1.177(7) . ? N1 C2 1.390(8) . ? N1 H20A 1.08(13) . ? N2 C7 1.381(8) . ? N2 C4 1.396(8) . ? N3 C12 1.370(8) . ? N3 C9 1.380(8) . ? N4 C14 1.365(8) . ? N4 C17 1.374(8) . ? N1A H20 0.80(15) . ? C1 C19 1.454(9) . ? C1 C2 1.472(9) . ? C1 C45 1.530(10) . ? C2 C3 1.376(9) . ? C3 C4 1.410(9) . ? C3 C21 1.499(9) . ? C4 C5 1.413(9) . ? C5 C6 1.346(8) . ? C5 H5 0.9500 . ? C6 C7 1.435(10) . ? C6 H6 0.9500 . ? C7 C8 1.400(8) . ? C8 C9 1.368(9) . ? C8 C27 1.503(9) . ? C9 C10 1.442(8) . ? C10 C11 1.335(9) . ? C10 H10 0.9500 . ? C11 C12 1.425(8) . ? C11 H11 0.9500 . ? C12 C13 1.402(9) . ? C13 C14 1.397(8) . ? C13 C33 1.489(9) . ? C14 C15 1.433(9) . ? C15 C16 1.343(9) . ? C15 H15 0.9500 . ? C16 C17 1.423(9) . ? C16 H16 0.9500 . ? C17 C18 1.401(8) . ? C18 C19 1.391(9) . ? C18 C39 1.486(9) . ? C21 C22 1.366(9) . ? C21 C26 1.379(9) . ? C22 C23 1.404(9) . ? C22 H22 0.9500 . ? C23 C24 1.369(10) . ? C23 H23 0.9500 . ? C24 C25 1.362(9) . ? C24 H24 0.9500 . ? C25 C26 1.381(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.381(9) . ? C27 C28 1.390(9) . ? C28 C29 1.380(9) . ? C28 H28 0.9500 . ? C29 C30 1.386(9) . ? C29 H29 0.9500 . ? C30 C31 1.370(9) . ? C30 H30 0.9500 . ? C31 C32 1.360(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.374(10) . ? C33 C34 1.400(9) . ? C34 C35 1.379(9) . ? C34 H34 0.9500 . ? C35 C36 1.360(10) . ? C35 H35 0.9500 . ? C36 C37 1.361(9) . ? C36 H36 0.9500 . ? C37 C38 1.389(9) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.379(10) . ? C39 C40 1.394(9) . ? C40 C41 1.390(9) . ? C40 H40 0.9500 . ? C41 C42 1.364(10) . ? C41 H41 0.9500 . ? C42 C43 1.371(9) . ? C42 H42 0.9500 . ? C43 C44 1.382(9) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H51 0.97(6) . ? C45 H50 0.95(7) . ? C45 H52 1.08(7) . ? C46 Cl2 1.760(8) . ? C46 Cl1 1.765(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Fe1 N3 112.3(2) . . ? N5 Fe1 N4 98.5(3) . . ? N3 Fe1 N4 88.7(2) . . ? N5 Fe1 N2 100.5(3) . . ? N3 Fe1 N2 89.1(2) . . ? N4 Fe1 N2 160.2(2) . . ? N5 Fe1 C1 93.5(3) . . ? N3 Fe1 C1 154.2(2) . . ? N4 Fe1 C1 86.5(2) . . ? N2 Fe1 C1 87.0(2) . . ? C2 N1 H20A 122(7) . . ? C7 N2 C4 103.6(6) . . ? C7 N2 Fe1 127.2(4) . . ? C4 N2 Fe1 129.2(4) . . ? C12 N3 C9 105.8(5) . . ? C12 N3 Fe1 126.5(4) . . ? C9 N3 Fe1 125.9(4) . . ? C14 N4 C17 104.5(6) . . ? C14 N4 Fe1 127.0(4) . . ? C17 N4 Fe1 128.5(4) . . ? O1 N5 Fe1 150.5(6) . . ? C19 C1 C2 101.5(5) . . ? C19 C1 C45 117.2(6) . . ? C2 C1 C45 116.2(6) . . ? C19 C1 Fe1 115.4(5) . . ? C2 C1 Fe1 114.1(4) . . ? C45 C1 Fe1 93.3(4) . . ? C3 C2 N1 123.4(6) . . ? C3 C2 C1 127.1(6) . . ? N1 C2 C1 109.5(6) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 C21 119.9(6) . . ? C4 C3 C21 119.2(7) . . ? N2 C4 C3 122.7(7) . . ? N2 C4 C5 111.3(6) . . ? C3 C4 C5 125.9(6) . . ? C6 C5 C4 107.3(6) . . ? C6 C5 H5 126.3 . . ? C4 C5 H5 126.3 . . ? C5 C6 C7 106.8(6) . . ? C5 C6 H6 126.6 . . ? C7 C6 H6 126.6 . . ? N2 C7 C8 124.5(7) . . ? N2 C7 C6 111.0(6) . . ? C8 C7 C6 124.5(6) . . ? C9 C8 C7 124.3(6) . . ? C9 C8 C27 119.2(6) . . ? C7 C8 C27 116.6(6) . . ? C8 C9 N3 126.2(6) . . ? C8 C9 C10 125.3(6) . . ? N3 C9 C10 108.4(6) . . ? C11 C10 C9 108.5(6) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? C10 C11 C12 106.4(6) . . ? C10 C11 H11 126.8 . . ? C12 C11 H11 126.8 . . ? N3 C12 C13 124.9(6) . . ? N3 C12 C11 110.8(6) . . ? C13 C12 C11 124.0(6) . . ? C14 C13 C12 122.8(6) . . ? C14 C13 C33 117.8(6) . . ? C12 C13 C33 119.4(5) . . ? N4 C14 C13 126.2(6) . . ? N4 C14 C15 111.2(6) . . ? C13 C14 C15 122.6(6) . . ? C16 C15 C14 106.3(6) . . ? C16 C15 H15 126.9 . . ? C14 C15 H15 126.9 . . ? C15 C16 C17 107.2(6) . . ? C15 C16 H16 126.4 . . ? C17 C16 H16 126.4 . . ? N4 C17 C18 125.4(6) . . ? N4 C17 C16 110.8(5) . . ? C18 C17 C16 123.7(6) . . ? C19 C18 C17 119.5(6) . . ? C19 C18 C39 120.1(6) . . ? C17 C18 C39 120.2(6) . . ? C18 C19 C1 125.9(6) . . ? C22 C21 C26 119.2(6) . . ? C22 C21 C3 120.9(6) . . ? C26 C21 C3 119.8(6) . . ? C21 C22 C23 119.2(7) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 121.1(7) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 119.1(7) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 121.0(7) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C32 C27 C28 119.0(6) . . ? C32 C27 C8 121.1(6) . . ? C28 C27 C8 119.9(6) . . ? C29 C28 C27 120.2(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.0(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.0(7) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C32 C31 C30 121.5(7) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C27 120.3(7) . . ? C31 C32 H32 119.9 . . ? C27 C32 H32 119.9 . . ? C38 C33 C34 119.0(6) . . ? C38 C33 C13 121.0(6) . . ? C34 C33 C13 119.9(6) . . ? C35 C34 C33 119.5(7) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C34 120.1(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.7(7) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 118.8(7) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C33 C38 C37 120.9(7) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C44 C39 C40 119.3(7) . . ? C44 C39 C18 120.9(6) . . ? C40 C39 C18 119.7(7) . . ? C41 C40 C39 118.8(7) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C42 C41 C40 121.7(7) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C43 119.2(7) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C44 120.5(8) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C39 C44 C43 120.6(6) . . ? C39 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C1 C45 H51 109(4) . . ? C1 C45 H50 114(4) . . ? H51 C45 H50 103(5) . . ? C1 C45 H52 117(3) . . ? H51 C45 H52 108(5) . . ? H50 C45 H52 105(6) . . ? Cl2 C46 Cl1 111.8(4) . . ? Cl2 C46 H46A 109.3 . . ? Cl1 C46 H46A 109.3 . . ? Cl2 C46 H46B 109.3 . . ? Cl1 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.673 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.115 #==END data_i10995mp_FeHCTPPCH3_2_O_BF4_2_cmpd4 _database_code_depnum_ccdc_archive 'CCDC 866965' #TrackingRef '- cif_bind.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H68 B2 Cl6 F8 Fe2 N8 O' _chemical_formula_weight 1811.57 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/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 18.0177(11) _cell_length_b 16.7896(10) _cell_length_c 28.1291(17) _cell_angle_alpha 90.00 _cell_angle_beta 106.170(3) _cell_angle_gamma 90.00 _cell_volume 8172.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8852 _exptl_absorpt_correction_T_max 0.9401 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53926 _diffrn_reflns_av_R_equivalents 0.1261 _diffrn_reflns_av_sigmaI/netI 0.1696 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.19 _reflns_number_total 14636 _reflns_number_gt 6399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1200P)^2^+0.5777P] 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 14636 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2052 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2719 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Fe2 Fe 0.04552(6) 0.48815(7) 0.24454(4) 0.0260(3) Uani 1 1 d . A 4 Fe1 Fe 0.01369(6) 0.28921(7) 0.24127(4) 0.0271(3) Uani 1 1 d . A 4 N1 N 0.1505(4) 0.2727(4) 0.3754(2) 0.0340(17) Uani 1 1 d . A 4 H1 H 0.1568 0.2897 0.4059 0.041 Uiso 1 1 calc R A 4 N2 N 0.0901(3) 0.2600(4) 0.1996(2) 0.0288(15) Uani 1 1 d . A 4 N3 N -0.0740(3) 0.2841(4) 0.1779(2) 0.0281(15) Uani 1 1 d . A 4 N4 N -0.0661(3) 0.2578(4) 0.2803(2) 0.0286(15) Uani 1 1 d . A 4 N5 N 0.1630(4) 0.4759(4) 0.3859(2) 0.0301(16) Uani 1 1 d . A 4 H5 H 0.2026 0.4525 0.4067 0.036 Uiso 1 1 calc R A 4 N6 N 0.1579(3) 0.5067(4) 0.2387(2) 0.0262(15) Uani 1 1 d . A 4 N7 N 0.0055(3) 0.5104(4) 0.1707(2) 0.0280(15) Uani 1 1 d . A 4 N8 N -0.0621(3) 0.5256(4) 0.2509(2) 0.0276(15) Uani 1 1 d . A 4 O1 O 0.0431(3) 0.3872(3) 0.25965(18) 0.0290(12) Uani 1 1 d . A 4 C1 C 0.0995(4) 0.2135(5) 0.3026(3) 0.0288(18) Uani 1 1 d . A 4 C2 C 0.0863(4) 0.2352(5) 0.3477(3) 0.0282(19) Uani 1 1 d . A 4 C3 C 0.0184(5) 0.2284(5) 0.3634(3) 0.0306(19) Uani 1 1 d . A 4 C4 C -0.0530(5) 0.2322(5) 0.3295(3) 0.032(2) Uani 1 1 d . A 4 C5 C -0.1259(4) 0.2163(5) 0.3376(3) 0.036(2) Uani 1 1 d . A 4 H5A H -0.1336 0.1959 0.3674 0.043 Uiso 1 1 calc R A 4 C6 C -0.1818(5) 0.2343(5) 0.2971(3) 0.038(2) Uani 1 1 d . A 4 H6 H -0.2359 0.2305 0.2929 0.046 Uiso 1 1 calc R A 4 C7 C -0.1446(5) 0.2608(5) 0.2610(3) 0.0316(19) Uani 1 1 d . A 4 C8 C -0.1850(4) 0.2844(5) 0.2126(3) 0.0308(19) Uani 1 1 d . A 4 C9 C -0.1515(4) 0.2941(5) 0.1739(3) 0.0305(19) Uani 1 1 d . A 4 C10 C -0.1926(4) 0.3083(5) 0.1225(3) 0.0303(19) Uani 1 1 d . A 4 H10 H -0.2463 0.3187 0.1099 0.036 Uiso 1 1 calc R A 4 C11 C -0.1428(5) 0.3042(5) 0.0966(3) 0.034(2) Uani 1 1 d . A 4 H11 H -0.1541 0.3110 0.0618 0.041 Uiso 1 1 calc R A 4 C12 C -0.0681(4) 0.2878(4) 0.1296(3) 0.0274(18) Uani 1 1 d . A 4 C13 C -0.0011(4) 0.2735(4) 0.1163(3) 0.0298(19) Uani 1 1 d . A 4 C14 C 0.0716(4) 0.2576(5) 0.1489(3) 0.0299(19) Uani 1 1 d . A 4 C15 C 0.1401(4) 0.2390(5) 0.1342(3) 0.033(2) Uani 1 1 d . A 4 H15 H 0.1427 0.2327 0.1012 0.040 Uiso 1 1 calc R A 4 C16 C 0.1993(5) 0.2321(4) 0.1749(3) 0.0305(19) Uani 1 1 d . A 4 H16 H 0.2513 0.2200 0.1761 0.037 Uiso 1 1 calc R A 4 C17 C 0.1696(4) 0.2462(4) 0.2166(3) 0.0286(19) Uani 1 1 d . A 4 C18 C 0.2115(4) 0.2465(4) 0.2663(3) 0.0277(18) Uani 1 1 d . A 4 C19 C 0.1742(4) 0.2444(4) 0.3045(3) 0.0272(18) Uani 1 1 d . A 4 C20 C 0.2030(4) 0.2801(4) 0.3501(3) 0.0282(18) Uani 1 1 d . A 4 H20 H 0.2518 0.3056 0.3616 0.034 Uiso 1 1 calc R A 4 C21 C 0.0270(5) 0.2222(5) 0.4174(3) 0.034(2) Uani 1 1 d . A 4 C22 C 0.0835(5) 0.1745(5) 0.4465(3) 0.045(2) Uani 1 1 d . A 4 H22 H 0.1172 0.1458 0.4321 0.055 Uiso 1 1 calc R A 4 C23 C 0.0919(6) 0.1679(6) 0.4978(3) 0.062(3) Uani 1 1 d . A 4 H23 H 0.1303 0.1339 0.5177 0.075 Uiso 1 1 calc R A 4 C24 C 0.0452(7) 0.2099(7) 0.5183(3) 0.064(3) Uani 1 1 d . A 4 H24 H 0.0517 0.2062 0.5529 0.077 Uiso 1 1 calc R A 4 C25 C -0.0123(6) 0.2585(6) 0.4897(3) 0.059(3) Uani 1 1 d . A 4 H25 H -0.0459 0.2865 0.5045 0.071 Uiso 1 1 calc R A 4 C26 C -0.0206(5) 0.2659(5) 0.4397(3) 0.043(2) Uani 1 1 d . A 4 H26 H -0.0586 0.3008 0.4203 0.052 Uiso 1 1 calc R A 4 C27 C -0.2705(5) 0.2917(5) 0.2020(3) 0.036(2) Uani 1 1 d . A 4 C28 C -0.3197(5) 0.2410(5) 0.1696(3) 0.036(2) Uani 1 1 d . A 4 H28 H -0.2992 0.2037 0.1513 0.043 Uiso 1 1 calc R A 4 C29 C -0.3981(5) 0.2436(5) 0.1634(3) 0.044(2) Uani 1 1 d . A 4 H29 H -0.4316 0.2085 0.1408 0.053 Uiso 1 1 calc R A 4 C30 C -0.4272(5) 0.2974(6) 0.1901(4) 0.051(3) Uani 1 1 d . A 4 H30 H -0.4812 0.2985 0.1863 0.061 Uiso 1 1 calc R A 4 C31 C -0.3809(5) 0.3488(6) 0.2217(4) 0.056(3) Uani 1 1 d . A 4 H31 H -0.4023 0.3865 0.2394 0.067 Uiso 1 1 calc R A 4 C32 C -0.3029(5) 0.3460(5) 0.2281(3) 0.044(2) Uani 1 1 d . A 4 H32 H -0.2701 0.3816 0.2507 0.052 Uiso 1 1 calc R A 4 C33 C -0.0054(5) 0.2694(5) 0.0617(3) 0.034(2) Uani 1 1 d . A 4 C34 C 0.0378(5) 0.3197(5) 0.0412(3) 0.038(2) Uani 1 1 d . A 4 H34 H 0.0691 0.3600 0.0605 0.046 Uiso 1 1 calc R A 4 C35 C 0.0345(5) 0.3098(6) -0.0088(3) 0.049(3) Uani 1 1 d . A 4 H35 H 0.0642 0.3439 -0.0233 0.059 Uiso 1 1 calc R A 4 C36 C -0.0097(6) 0.2533(7) -0.0367(3) 0.054(3) Uani 1 1 d . A 4 H36 H -0.0097 0.2469 -0.0702 0.064 Uiso 1 1 calc R A 4 C37 C -0.0541(5) 0.2053(6) -0.0173(3) 0.049(3) Uani 1 1 d . A 4 H37 H -0.0870 0.1673 -0.0378 0.059 Uiso 1 1 calc R A 4 C38 C -0.0522(4) 0.2112(5) 0.0326(3) 0.038(2) Uani 1 1 d . A 4 H38 H -0.0822 0.1763 0.0464 0.046 Uiso 1 1 calc R A 4 C39 C 0.2972(4) 0.2540(5) 0.2782(3) 0.0295(19) Uani 1 1 d . A 4 C40 C 0.3442(5) 0.2088(5) 0.3162(3) 0.0323(19) Uani 1 1 d . A 4 H40 H 0.3215 0.1740 0.3349 0.039 Uiso 1 1 calc R A 4 C41 C 0.4238(5) 0.2140(5) 0.3270(3) 0.040(2) Uani 1 1 d . A 4 H41 H 0.4555 0.1805 0.3517 0.048 Uiso 1 1 calc R A 4 C42 C 0.4570(5) 0.2667(6) 0.3026(3) 0.050(3) Uani 1 1 d . A 4 H42 H 0.5117 0.2711 0.3111 0.060 Uiso 1 1 calc R A 4 C43 C 0.4118(5) 0.3138(6) 0.2655(3) 0.045(2) Uani 1 1 d . A 4 H43 H 0.4355 0.3504 0.2485 0.054 Uiso 1 1 calc R A 4 C44 C 0.3318(5) 0.3080(5) 0.2530(3) 0.035(2) Uani 1 1 d . A 4 H44 H 0.3007 0.3405 0.2274 0.042 Uiso 1 1 calc R A 4 C45 C 0.0608(5) 0.1413(5) 0.2728(3) 0.036(2) Uani 1 1 d . A 4 H45A H 0.0314 0.1121 0.2917 0.054 Uiso 1 1 calc R A 4 H45B H 0.1003 0.1063 0.2662 0.054 Uiso 1 1 calc R A 4 H45C H 0.0257 0.1592 0.2414 0.054 Uiso 1 1 calc R A 4 C46 C 0.0927(4) 0.5480(4) 0.3214(3) 0.0259(18) Uani 1 1 d . A 4 C47 C 0.1666(4) 0.5161(4) 0.3436(2) 0.0243(17) Uani 1 1 d . A 4 C48 C 0.2327(4) 0.5135(5) 0.3266(3) 0.0314(19) Uani 1 1 d . A 4 C49 C 0.2264(4) 0.5147(5) 0.2763(3) 0.0300(19) Uani 1 1 d . A 4 C50 C 0.2895(4) 0.5214(5) 0.2553(3) 0.0320(19) Uani 1 1 d . A 4 H50 H 0.3425 0.5274 0.2727 0.038 Uiso 1 1 calc R A 4 C51 C 0.2593(4) 0.5176(5) 0.2058(3) 0.0327(19) Uani 1 1 d . A 4 H51 H 0.2875 0.5213 0.1819 0.039 Uiso 1 1 calc R A 4 C52 C 0.1784(4) 0.5070(4) 0.1955(3) 0.0283(18) Uani 1 1 d . A 4 C53 C 0.1281(4) 0.5030(5) 0.1476(3) 0.0300(19) Uani 1 1 d . A 4 C54 C 0.0488(4) 0.5038(4) 0.1370(3) 0.0289(19) Uani 1 1 d . A 4 C55 C -0.0041(4) 0.5024(5) 0.0873(3) 0.035(2) Uani 1 1 d . A 4 H55 H 0.0098 0.4970 0.0573 0.041 Uiso 1 1 calc R A 4 C56 C -0.0771(5) 0.5102(5) 0.0916(3) 0.038(2) Uani 1 1 d . A 4 H56 H -0.1234 0.5112 0.0653 0.046 Uiso 1 1 calc R A 4 C57 C -0.0710(4) 0.5167(5) 0.1437(3) 0.0296(19) Uani 1 1 d . A 4 C58 C -0.1335(4) 0.5307(5) 0.1621(3) 0.0309(19) Uani 1 1 d . A 4 C59 C -0.1278(5) 0.5374(4) 0.2131(3) 0.0308(19) Uani 1 1 d . A 4 C60 C -0.1916(5) 0.5547(5) 0.2325(3) 0.036(2) Uani 1 1 d . A 4 H60 H -0.2431 0.5661 0.2138 0.044 Uiso 1 1 calc R A 4 C61 C -0.1651(5) 0.5516(5) 0.2816(3) 0.038(2) Uani 1 1 d . A 4 H61 H -0.1944 0.5601 0.3045 0.045 Uiso 1 1 calc R A 4 C62 C -0.0844(4) 0.5335(5) 0.2937(3) 0.033(2) Uani 1 1 d . A 4 C63 C -0.0366(4) 0.5239(5) 0.3412(3) 0.0303(19) Uani 1 1 d . A 4 C64 C 0.0451(4) 0.5203(4) 0.3511(3) 0.0266(18) Uani 1 1 d . A 4 C65 C 0.0922(4) 0.4772(5) 0.3908(3) 0.0293(18) Uani 1 1 d . A 4 H65 H 0.0760 0.4530 0.4168 0.035 Uiso 1 1 calc R A 4 C66 C 0.3101(4) 0.5043(5) 0.3631(3) 0.0297(19) Uani 1 1 d . A 4 C67 C 0.3624(5) 0.4482(5) 0.3569(3) 0.036(2) Uani 1 1 d . A 4 H67 H 0.3483 0.4127 0.3295 0.043 Uiso 1 1 calc R A 4 C68 C 0.4346(5) 0.4428(5) 0.3899(3) 0.044(2) Uani 1 1 d . A 4 H68 H 0.4698 0.4033 0.3855 0.052 Uiso 1 1 calc R A 4 C69 C 0.4561(5) 0.4950(6) 0.4297(3) 0.048(2) Uani 1 1 d . A 4 H69 H 0.5067 0.4925 0.4517 0.057 Uiso 1 1 calc R A 4 C70 C 0.4043(5) 0.5498(5) 0.4371(3) 0.041(2) Uani 1 1 d . A 4 H70 H 0.4188 0.5849 0.4647 0.049 Uiso 1 1 calc R A 4 C71 C 0.3300(5) 0.5545(5) 0.4042(3) 0.035(2) Uani 1 1 d . A 4 H71 H 0.2934 0.5915 0.4099 0.042 Uiso 1 1 calc R A 4 C72 C 0.1637(4) 0.5045(5) 0.1054(3) 0.0295(19) Uani 1 1 d . A 4 C73 C 0.2032(4) 0.4402(5) 0.0944(3) 0.038(2) Uani 1 1 d . A 4 H73 H 0.2078 0.3933 0.1139 0.045 Uiso 1 1 calc R A 4 C74 C 0.2362(5) 0.4420(6) 0.0557(3) 0.043(2) Uani 1 1 d . A 4 H74 H 0.2622 0.3965 0.0481 0.052 Uiso 1 1 calc R A 4 C75 C 0.2311(5) 0.5113(6) 0.0279(3) 0.045(2) Uani 1 1 d . A 4 H75 H 0.2547 0.5132 0.0017 0.054 Uiso 1 1 calc R A 4 C76 C 0.1924(5) 0.5770(5) 0.0377(3) 0.043(2) Uani 1 1 d . A 4 H76 H 0.1890 0.6241 0.0186 0.052 Uiso 1 1 calc R A 4 C77 C 0.1579(5) 0.5727(5) 0.0767(3) 0.040(2) Uani 1 1 d . A 4 H77 H 0.1302 0.6174 0.0836 0.048 Uiso 1 1 calc R A 4 C78 C -0.2113(5) 0.5430(5) 0.1272(3) 0.040(2) Uani 1 1 d . A 4 C79 C -0.2719(5) 0.4930(6) 0.1291(3) 0.054(3) Uani 1 1 d . A 4 H79 H -0.2631 0.4498 0.1518 0.065 Uiso 1 1 calc R A 4 C80 C -0.3451(6) 0.5060(7) 0.0978(4) 0.072(3) Uani 1 1 d . A 4 H80 H -0.3869 0.4723 0.0990 0.087 Uiso 1 1 calc R A 4 C81 C -0.3566(7) 0.5690(8) 0.0649(4) 0.073(4) Uani 1 1 d . A 4 H81 H -0.4070 0.5779 0.0436 0.087 Uiso 1 1 calc R A 4 C82 C -0.2999(7) 0.6177(7) 0.0619(4) 0.063(3) Uani 1 1 d . A 4 H82 H -0.3094 0.6604 0.0388 0.075 Uiso 1 1 calc R A 4 C83 C -0.2255(6) 0.6044(6) 0.0937(3) 0.053(3) Uani 1 1 d . A 4 H83 H -0.1844 0.6386 0.0920 0.064 Uiso 1 1 calc R A 4 C84 C -0.0699(4) 0.5128(5) 0.3835(3) 0.0305(19) Uani 1 1 d . A 4 C85 C -0.1273(5) 0.4553(5) 0.3798(3) 0.047(2) Uani 1 1 d . A 4 H85 H -0.1445 0.4241 0.3506 0.057 Uiso 1 1 calc R A 4 C86 C -0.1589(5) 0.4438(6) 0.4187(4) 0.058(3) Uani 1 1 d . A 4 H86 H -0.1968 0.4036 0.4168 0.070 Uiso 1 1 calc R A 4 C87 C -0.1345(5) 0.4922(6) 0.4614(3) 0.054(3) Uani 1 1 d . A 4 H87 H -0.1567 0.4854 0.4881 0.065 Uiso 1 1 calc R A 4 C88 C -0.0794(5) 0.5485(6) 0.4642(3) 0.049(2) Uani 1 1 d . A 4 H88 H -0.0635 0.5814 0.4927 0.059 Uiso 1 1 calc R A 4 C89 C -0.0455(5) 0.5584(5) 0.4252(3) 0.039(2) Uani 1 1 d . A 4 H89 H -0.0058 0.5968 0.4279 0.047 Uiso 1 1 calc R A 4 C90 C 0.0804(4) 0.6257(4) 0.2939(3) 0.032(2) Uani 1 1 d . A 4 H90A H 0.0497 0.6613 0.3085 0.048 Uiso 1 1 calc R A 4 H90B H 0.0529 0.6161 0.2590 0.048 Uiso 1 1 calc R A 4 H90C H 0.1305 0.6504 0.2961 0.048 Uiso 1 1 calc R A 4 C91 C 0.6458(6) 0.5787(7) 0.3497(4) 0.082(4) Uani 1 1 d . B 4 H91A H 0.6654 0.6332 0.3592 0.098 Uiso 1 1 calc R B 4 H91B H 0.6814 0.5406 0.3716 0.098 Uiso 1 1 calc R B 4 C92 C 0.8188(8) 0.8362(7) 0.0378(5) 0.099(4) Uani 1 1 d . C 4 H92A H 0.8523 0.8099 0.0199 0.118 Uiso 1 1 calc R C 4 H92B H 0.7646 0.8199 0.0224 0.118 Uiso 1 1 calc R C 4 C93 C 0.5606(7) 0.5883(6) 0.8933(4) 0.077(3) Uani 1 1 d . D 4 H93A H 0.5151 0.6241 0.8850 0.093 Uiso 1 1 calc R D 4 H93B H 0.6074 0.6219 0.9044 0.093 Uiso 1 1 calc R D 4 B1 B 0.7474(6) 0.1552(7) 0.9865(4) 0.045(3) Uani 1 1 d . E 4 B2 B 0.3476(14) 0.2115(16) 0.0744(9) 0.072(3) Uani 0.620(13) 1 d P F 4 Cl1 Cl 0.55459(19) 0.5690(2) 0.35817(12) 0.0945(10) Uani 1 1 d . B 4 Cl2 Cl 0.64531(19) 0.5614(2) 0.28933(13) 0.1034(12) Uani 1 1 d . B 4 Cl3 Cl 0.8280(2) 0.9388(3) 0.03604(14) 0.1123(13) Uani 1 1 d . C 4 Cl4 Cl 0.8488(3) 0.8099(3) 0.10325(18) 0.1565(19) Uani 1 1 d . C 4 Cl5 Cl 0.55508(19) 0.5275(2) 0.94121(13) 0.1098(12) Uani 1 1 d . D 4 Cl6 Cl 0.5639(3) 0.5378(3) 0.84182(14) 0.1484(19) Uani 1 1 d . D 4 F1 F 0.7641(3) 0.2332(3) 0.98247(18) 0.0570(14) Uani 1 1 d . E 4 F2 F 0.7796(3) 0.1122(3) 0.9539(2) 0.0746(18) Uani 1 1 d . E 4 F3 F 0.6670(3) 0.1452(3) 0.96766(15) 0.0450(12) Uani 1 1 d . E 4 F4 F 0.7739(3) 0.1292(4) 1.0329(2) 0.083(2) Uani 1 1 d . E 4 F5 F 0.4218(8) 0.2211(9) 0.0954(7) 0.072(3) Uani 0.620(13) 1 d P F 4 F6 F 0.3388(5) 0.1378(6) 0.0515(4) 0.072(3) Uani 0.620(13) 1 d P F 4 F7 F 0.3321(8) 0.2647(13) 0.0392(6) 0.072(3) Uani 0.620(13) 1 d P F 4 F8 F 0.3016(6) 0.2110(7) 0.1039(3) 0.072(3) Uani 0.620(13) 1 d P F 4 B2A B 0.3494(10) 0.2225(9) 0.0791(6) 0.080(5) Uani 0.380(13) 1 d PD F 2 F6A F 0.3113(9) 0.1486(10) 0.0816(7) 0.080(5) Uani 0.380(13) 1 d PD F 2 F8A F 0.3328(10) 0.2680(10) 0.1179(6) 0.080(5) Uani 0.380(13) 1 d PD F 2 F5A F 0.4301(12) 0.2053(16) 0.0976(12) 0.080(5) Uani 0.380(13) 1 d PD F 2 F7A F 0.3158(14) 0.266(2) 0.0348(11) 0.080(5) Uani 0.380(13) 1 d PD F 2 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 Fe2 0.0282(6) 0.0302(7) 0.0170(6) 0.0002(5) 0.0021(5) -0.0004(5) Fe1 0.0311(7) 0.0316(7) 0.0185(6) -0.0009(5) 0.0069(5) -0.0014(5) N1 0.039(4) 0.045(5) 0.016(3) -0.001(3) 0.006(3) -0.002(3) N2 0.030(4) 0.035(4) 0.019(4) -0.001(3) 0.003(3) -0.001(3) N3 0.028(4) 0.036(4) 0.020(3) -0.003(3) 0.006(3) -0.001(3) N4 0.032(4) 0.034(4) 0.017(3) 0.002(3) 0.001(3) 0.005(3) N5 0.037(4) 0.033(4) 0.016(3) 0.001(3) 0.000(3) 0.004(3) N6 0.032(4) 0.031(4) 0.013(3) -0.002(3) 0.003(3) -0.003(3) N7 0.032(4) 0.037(4) 0.016(3) 0.002(3) 0.007(3) 0.000(3) N8 0.030(4) 0.032(4) 0.018(3) 0.004(3) 0.003(3) 0.007(3) O1 0.033(3) 0.029(3) 0.026(3) -0.002(2) 0.010(2) -0.001(2) C1 0.028(5) 0.034(5) 0.025(4) -0.001(4) 0.009(3) -0.002(4) C2 0.033(5) 0.032(5) 0.019(4) 0.001(3) 0.005(3) 0.002(4) C3 0.037(5) 0.031(5) 0.027(5) 0.003(4) 0.013(4) -0.002(4) C4 0.038(5) 0.041(5) 0.019(4) 0.004(4) 0.013(4) 0.000(4) C5 0.038(5) 0.048(6) 0.028(5) -0.002(4) 0.021(4) -0.012(4) C6 0.029(5) 0.057(6) 0.029(5) 0.003(4) 0.007(4) -0.010(4) C7 0.034(5) 0.030(5) 0.033(5) 0.002(4) 0.012(4) 0.008(4) C8 0.034(5) 0.031(5) 0.027(5) 0.001(4) 0.008(4) -0.003(4) C9 0.028(5) 0.032(5) 0.028(5) -0.004(4) 0.002(3) -0.008(4) C10 0.027(5) 0.038(5) 0.024(4) 0.002(4) 0.004(3) 0.000(4) C11 0.044(5) 0.038(5) 0.019(4) 0.001(4) 0.005(4) 0.001(4) C12 0.035(5) 0.029(5) 0.015(4) -0.002(3) 0.002(3) 0.000(4) C13 0.036(5) 0.029(5) 0.021(4) -0.004(3) 0.003(4) -0.001(4) C14 0.029(5) 0.039(5) 0.022(4) 0.001(4) 0.008(3) -0.003(4) C15 0.039(5) 0.039(5) 0.020(4) 0.000(4) 0.007(4) 0.001(4) C16 0.035(5) 0.031(5) 0.026(5) 0.002(4) 0.009(4) 0.007(4) C17 0.032(5) 0.030(5) 0.028(4) -0.001(4) 0.015(4) 0.002(4) C18 0.032(5) 0.028(5) 0.022(4) 0.002(3) 0.005(3) 0.005(4) C19 0.031(5) 0.032(5) 0.016(4) 0.000(3) 0.002(3) 0.006(4) C20 0.029(5) 0.035(5) 0.020(4) 0.004(4) 0.007(3) -0.007(4) C21 0.048(5) 0.039(5) 0.016(4) 0.002(4) 0.008(4) -0.015(4) C22 0.059(6) 0.051(6) 0.026(5) 0.007(4) 0.010(4) -0.010(5) C23 0.083(8) 0.074(8) 0.029(6) 0.017(5) 0.014(5) -0.018(6) C24 0.090(9) 0.081(8) 0.023(5) -0.001(6) 0.020(6) -0.044(7) C25 0.081(8) 0.077(8) 0.033(6) -0.029(5) 0.039(6) -0.038(6) C26 0.045(6) 0.050(6) 0.039(5) -0.012(4) 0.017(4) -0.008(5) C27 0.030(5) 0.051(6) 0.026(5) 0.003(4) 0.007(4) 0.003(4) C28 0.031(5) 0.039(5) 0.037(5) 0.002(4) 0.009(4) 0.003(4) C29 0.038(6) 0.046(6) 0.044(6) 0.001(5) 0.004(4) -0.001(5) C30 0.027(5) 0.063(7) 0.062(7) 0.006(6) 0.013(5) 0.006(5) C31 0.042(6) 0.067(7) 0.063(7) -0.007(6) 0.020(5) 0.008(5) C32 0.033(6) 0.052(6) 0.046(6) -0.009(5) 0.012(4) -0.003(4) C33 0.034(5) 0.046(6) 0.020(4) -0.002(4) 0.005(4) 0.008(4) C34 0.042(5) 0.037(5) 0.037(5) 0.003(4) 0.013(4) 0.008(4) C35 0.061(6) 0.063(7) 0.027(5) 0.022(5) 0.019(5) 0.020(5) C36 0.062(7) 0.081(8) 0.014(5) 0.002(5) 0.004(5) 0.020(6) C37 0.044(6) 0.075(7) 0.020(5) -0.018(5) -0.005(4) 0.008(5) C38 0.030(5) 0.048(6) 0.033(5) -0.004(4) 0.003(4) -0.002(4) C39 0.036(5) 0.034(5) 0.020(4) -0.009(4) 0.010(4) 0.001(4) C40 0.040(5) 0.034(5) 0.022(4) -0.002(4) 0.007(4) 0.000(4) C41 0.040(6) 0.046(6) 0.026(5) -0.006(4) -0.002(4) 0.002(5) C42 0.038(6) 0.066(7) 0.045(6) -0.020(5) 0.009(5) -0.007(5) C43 0.052(6) 0.058(7) 0.029(5) -0.011(4) 0.019(4) -0.014(5) C44 0.034(5) 0.045(6) 0.027(5) -0.006(4) 0.010(4) 0.001(4) C45 0.042(5) 0.032(5) 0.035(5) -0.003(4) 0.011(4) 0.002(4) C46 0.033(5) 0.026(5) 0.018(4) -0.001(3) 0.006(3) 0.001(4) C47 0.040(5) 0.021(4) 0.010(4) 0.004(3) 0.004(3) -0.004(4) C48 0.032(5) 0.041(5) 0.016(4) 0.000(4) 0.000(3) -0.003(4) C49 0.025(4) 0.040(5) 0.021(4) 0.002(4) 0.000(3) 0.001(4) C50 0.029(5) 0.045(5) 0.020(4) 0.004(4) 0.003(3) -0.008(4) C51 0.033(5) 0.040(5) 0.025(4) -0.001(4) 0.008(4) -0.010(4) C52 0.037(5) 0.025(5) 0.025(4) 0.006(3) 0.011(4) -0.003(4) C53 0.035(5) 0.037(5) 0.017(4) 0.003(3) 0.005(3) 0.000(4) C54 0.036(5) 0.032(5) 0.016(4) -0.001(3) 0.004(3) -0.004(4) C55 0.036(5) 0.047(6) 0.017(4) 0.001(4) 0.001(3) 0.002(4) C56 0.033(5) 0.055(6) 0.020(4) -0.009(4) -0.001(4) 0.000(4) C57 0.031(5) 0.031(5) 0.026(4) 0.003(4) 0.006(4) 0.003(4) C58 0.033(5) 0.033(5) 0.019(4) -0.004(3) -0.005(3) 0.006(4) C59 0.041(5) 0.026(5) 0.024(4) 0.001(3) 0.008(4) 0.006(4) C60 0.032(5) 0.045(6) 0.029(5) -0.003(4) 0.005(4) 0.007(4) C61 0.034(5) 0.046(6) 0.037(5) 0.002(4) 0.016(4) 0.010(4) C62 0.029(5) 0.047(6) 0.023(5) -0.002(4) 0.006(4) 0.001(4) C63 0.038(5) 0.034(5) 0.019(4) -0.002(4) 0.007(4) 0.006(4) C64 0.035(5) 0.029(5) 0.015(4) -0.006(3) 0.005(3) 0.003(4) C65 0.022(5) 0.041(5) 0.026(4) 0.000(4) 0.008(3) -0.001(4) C66 0.033(5) 0.039(5) 0.016(4) -0.001(4) 0.004(3) -0.009(4) C67 0.037(5) 0.049(6) 0.022(5) 0.003(4) 0.009(4) -0.001(4) C68 0.046(6) 0.052(6) 0.031(5) 0.010(5) 0.007(4) 0.005(5) C69 0.033(5) 0.066(7) 0.037(5) 0.018(5) -0.001(4) -0.005(5) C70 0.034(5) 0.060(6) 0.022(5) 0.001(4) -0.005(4) -0.002(5) C71 0.038(5) 0.033(5) 0.028(5) 0.001(4) 0.000(4) -0.008(4) C72 0.026(4) 0.036(5) 0.023(4) 0.001(4) 0.002(3) -0.004(4) C73 0.036(5) 0.048(6) 0.026(5) 0.002(4) 0.004(4) 0.001(4) C74 0.038(5) 0.062(7) 0.032(5) -0.010(5) 0.013(4) 0.001(5) C75 0.039(5) 0.077(7) 0.017(4) -0.010(5) 0.005(4) -0.012(5) C76 0.061(6) 0.047(6) 0.023(5) 0.008(4) 0.012(4) -0.004(5) C77 0.052(6) 0.045(6) 0.021(5) 0.001(4) 0.007(4) 0.001(4) C78 0.041(6) 0.049(6) 0.023(5) -0.007(4) 0.000(4) 0.015(5) C79 0.031(6) 0.060(7) 0.059(7) -0.010(5) -0.006(4) 0.013(5) C80 0.043(7) 0.082(9) 0.083(9) -0.045(7) 0.003(6) 0.000(6) C81 0.064(8) 0.110(11) 0.032(6) -0.013(7) -0.006(5) 0.047(8) C82 0.061(8) 0.088(9) 0.043(6) -0.002(6) 0.020(6) 0.031(7) C83 0.059(7) 0.076(7) 0.026(5) 0.000(5) 0.015(5) 0.027(6) C84 0.027(5) 0.043(5) 0.023(4) 0.001(4) 0.009(3) 0.007(4) C85 0.052(6) 0.058(7) 0.035(5) -0.001(5) 0.019(5) -0.004(5) C86 0.049(6) 0.076(8) 0.057(7) -0.011(6) 0.027(5) -0.016(5) C87 0.053(6) 0.079(8) 0.036(6) 0.003(5) 0.023(5) -0.006(6) C88 0.054(6) 0.062(7) 0.032(5) -0.006(5) 0.011(4) -0.012(5) C89 0.037(5) 0.053(6) 0.031(5) 0.004(4) 0.014(4) 0.008(4) C90 0.032(5) 0.036(5) 0.024(4) 0.001(4) 0.003(4) -0.002(4) C91 0.069(8) 0.097(10) 0.087(9) -0.012(7) 0.032(7) 0.008(7) C92 0.111(11) 0.053(8) 0.139(13) -0.003(8) 0.048(9) 0.035(7) C93 0.099(9) 0.066(8) 0.060(7) -0.001(6) 0.011(6) 0.017(7) B1 0.049(7) 0.055(8) 0.024(6) -0.002(5) 0.000(5) -0.005(6) B2 0.067(4) 0.081(5) 0.067(4) 0.004(3) 0.016(3) 0.010(3) Cl1 0.093(2) 0.111(3) 0.088(2) 0.017(2) 0.0395(19) 0.007(2) Cl2 0.078(2) 0.138(3) 0.104(3) 0.009(2) 0.041(2) 0.016(2) Cl3 0.094(3) 0.146(4) 0.111(3) -0.023(2) 0.052(2) -0.023(2) Cl4 0.136(4) 0.141(4) 0.155(4) 0.039(3) -0.023(3) 0.015(3) Cl5 0.080(2) 0.135(3) 0.106(3) 0.035(2) 0.013(2) 0.021(2) Cl6 0.185(4) 0.175(4) 0.080(3) -0.024(3) 0.029(3) 0.097(3) F1 0.055(3) 0.049(4) 0.056(4) -0.002(3) -0.003(3) -0.008(3) F2 0.051(4) 0.082(4) 0.085(5) -0.038(4) 0.009(3) -0.004(3) F3 0.043(3) 0.066(3) 0.023(3) -0.005(2) 0.006(2) -0.003(3) F4 0.085(4) 0.095(5) 0.048(4) 0.026(3) -0.016(3) -0.025(4) F5 0.067(4) 0.081(5) 0.067(4) 0.004(3) 0.016(3) 0.010(3) F6 0.067(4) 0.081(5) 0.067(4) 0.004(3) 0.016(3) 0.010(3) F7 0.067(4) 0.081(5) 0.067(4) 0.004(3) 0.016(3) 0.010(3) F8 0.067(4) 0.081(5) 0.067(4) 0.004(3) 0.016(3) 0.010(3) B2A 0.092(8) 0.072(8) 0.080(7) 0.044(5) 0.030(6) 0.010(6) F6A 0.092(8) 0.072(8) 0.080(7) 0.044(5) 0.030(6) 0.010(6) F8A 0.092(8) 0.072(8) 0.080(7) 0.044(5) 0.030(6) 0.010(6) F5A 0.092(8) 0.072(8) 0.080(7) 0.044(5) 0.030(6) 0.010(6) F7A 0.092(8) 0.072(8) 0.080(7) 0.044(5) 0.030(6) 0.010(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 Fe2 O1 1.751(5) . ? Fe2 N7 2.036(6) . ? Fe2 N8 2.093(6) . ? Fe2 N6 2.100(6) . ? Fe2 C46 2.319(7) . ? Fe1 O1 1.761(5) . ? Fe1 N3 2.028(6) . ? Fe1 N2 2.101(6) . ? Fe1 N4 2.104(6) . ? Fe1 C1 2.345(8) . ? N1 C20 1.338(8) . ? N1 C2 1.355(9) . ? N2 C14 1.371(9) . ? N2 C17 1.397(9) . ? N3 C9 1.381(9) . ? N3 C12 1.394(8) . ? N4 C7 1.367(9) . ? N4 C4 1.405(9) . ? N5 C65 1.320(9) . ? N5 C47 1.385(8) . ? N6 C52 1.365(8) . ? N6 C49 1.391(9) . ? N7 C57 1.381(9) . ? N7 C54 1.388(9) . ? N8 C59 1.367(9) . ? N8 C62 1.377(9) . ? C1 C2 1.404(9) . ? C1 C19 1.429(10) . ? C1 C45 1.528(10) . ? C2 C3 1.418(10) . ? C3 C4 1.373(10) . ? C3 C21 1.487(10) . ? C4 C5 1.422(10) . ? C5 C6 1.329(11) . ? C6 C7 1.435(10) . ? C7 C8 1.410(10) . ? C8 C9 1.393(10) . ? C8 C27 1.491(10) . ? C9 C10 1.449(10) . ? C10 C11 1.306(9) . ? C11 C12 1.432(10) . ? C12 C13 1.381(10) . ? C13 C14 1.400(10) . ? C13 C33 1.518(10) . ? C14 C15 1.440(10) . ? C15 C16 1.335(10) . ? C16 C17 1.438(10) . ? C17 C18 1.391(10) . ? C18 C19 1.418(9) . ? C18 C39 1.491(10) . ? C19 C20 1.380(10) . ? C21 C22 1.373(11) . ? C21 C26 1.402(11) . ? C22 C23 1.410(11) . ? C23 C24 1.345(14) . ? C24 C25 1.386(14) . ? C25 C26 1.378(11) . ? C27 C28 1.374(11) . ? C27 C32 1.396(11) . ? C28 C29 1.375(11) . ? C29 C30 1.369(12) . ? C30 C31 1.348(12) . ? C31 C32 1.368(11) . ? C33 C34 1.378(11) . ? C33 C38 1.398(11) . ? C34 C35 1.400(11) . ? C35 C36 1.341(13) . ? C36 C37 1.353(12) . ? C37 C38 1.397(10) . ? C39 C40 1.389(10) . ? C39 C44 1.401(10) . ? C40 C41 1.385(10) . ? C41 C42 1.356(12) . ? C42 C43 1.381(12) . ? C43 C44 1.388(11) . ? C46 C47 1.410(10) . ? C46 C64 1.432(10) . ? C46 C90 1.502(10) . ? C47 C48 1.403(10) . ? C48 C49 1.386(10) . ? C48 C66 1.491(10) . ? C49 C50 1.425(10) . ? C50 C51 1.347(10) . ? C51 C52 1.417(10) . ? C52 C53 1.400(10) . ? C53 C54 1.376(10) . ? C53 C72 1.500(10) . ? C54 C55 1.458(10) . ? C55 C56 1.360(10) . ? C56 C57 1.443(10) . ? C57 C58 1.383(10) . ? C58 C59 1.414(10) . ? C58 C78 1.485(10) . ? C59 C60 1.432(10) . ? C60 C61 1.331(10) . ? C61 C62 1.430(10) . ? C62 C63 1.384(10) . ? C63 C64 1.421(10) . ? C63 C84 1.485(10) . ? C64 C65 1.401(10) . ? C66 C67 1.376(10) . ? C66 C71 1.396(10) . ? C67 C68 1.375(11) . ? C68 C69 1.389(12) . ? C69 C70 1.368(11) . ? C70 C71 1.402(10) . ? C72 C73 1.376(10) . ? C72 C77 1.388(10) . ? C73 C74 1.377(10) . ? C74 C75 1.390(12) . ? C75 C76 1.373(12) . ? C76 C77 1.404(10) . ? C78 C83 1.372(12) . ? C78 C79 1.390(12) . ? C79 C80 1.384(12) . ? C80 C81 1.383(15) . ? C81 C82 1.329(15) . ? C82 C83 1.406(13) . ? C84 C89 1.368(11) . ? C84 C85 1.398(11) . ? C85 C86 1.379(11) . ? C86 C87 1.418(12) . ? C87 C88 1.357(12) . ? C88 C89 1.405(11) . ? C91 Cl2 1.719(11) . ? C91 Cl1 1.733(10) . ? C92 Cl3 1.733(12) . ? C92 Cl4 1.823(13) . ? C93 Cl6 1.695(10) . ? C93 Cl5 1.715(11) . ? B1 F4 1.331(11) . ? B1 F1 1.356(12) . ? B1 F3 1.407(11) . ? B1 F2 1.414(11) . ? B2 F7 1.30(3) . ? B2 F5 1.31(2) . ? B2 F8 1.32(2) . ? B2 F6 1.38(3) . ? B2A F7A 1.4297(10) . ? B2A F5A 1.4298(10) . ? B2A F6A 1.4298(10) . ? B2A F8A 1.4299(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe2 N7 113.6(2) . . ? O1 Fe2 N8 100.6(2) . . ? N7 Fe2 N8 87.7(2) . . ? O1 Fe2 N6 104.6(2) . . ? N7 Fe2 N6 88.2(2) . . ? N8 Fe2 N6 154.0(2) . . ? O1 Fe2 C46 102.7(2) . . ? N7 Fe2 C46 143.7(3) . . ? N8 Fe2 C46 84.2(2) . . ? N6 Fe2 C46 84.1(2) . . ? O1 Fe1 N3 113.3(2) . . ? O1 Fe1 N2 101.0(2) . . ? N3 Fe1 N2 88.3(2) . . ? O1 Fe1 N4 106.0(2) . . ? N3 Fe1 N4 88.3(2) . . ? N2 Fe1 N4 151.9(2) . . ? O1 Fe1 C1 102.0(2) . . ? N3 Fe1 C1 144.7(3) . . ? N2 Fe1 C1 83.3(2) . . ? N4 Fe1 C1 83.5(2) . . ? C20 N1 C2 110.7(6) . . ? C14 N2 C17 106.3(6) . . ? C14 N2 Fe1 125.5(5) . . ? C17 N2 Fe1 128.0(5) . . ? C9 N3 C12 105.4(6) . . ? C9 N3 Fe1 126.1(5) . . ? C12 N3 Fe1 127.1(5) . . ? C7 N4 C4 105.9(6) . . ? C7 N4 Fe1 124.5(5) . . ? C4 N4 Fe1 129.6(5) . . ? C65 N5 C47 111.1(6) . . ? C52 N6 C49 105.9(6) . . ? C52 N6 Fe2 125.2(5) . . ? C49 N6 Fe2 128.7(5) . . ? C57 N7 C54 107.3(6) . . ? C57 N7 Fe2 126.2(5) . . ? C54 N7 Fe2 125.1(5) . . ? C59 N8 C62 105.4(6) . . ? C59 N8 Fe2 126.8(5) . . ? C62 N8 Fe2 127.3(5) . . ? Fe2 O1 Fe1 149.2(3) . . ? C2 C1 C19 105.5(6) . . ? C2 C1 C45 122.4(7) . . ? C19 C1 C45 126.2(6) . . ? C2 C1 Fe1 106.3(5) . . ? C19 C1 Fe1 104.6(5) . . ? C45 C1 Fe1 85.4(4) . . ? N1 C2 C1 107.9(6) . . ? N1 C2 C3 122.1(7) . . ? C1 C2 C3 129.8(7) . . ? C4 C3 C2 120.1(7) . . ? C4 C3 C21 121.7(7) . . ? C2 C3 C21 118.1(7) . . ? C3 C4 N4 124.6(7) . . ? C3 C4 C5 127.4(7) . . ? N4 C4 C5 107.9(7) . . ? C6 C5 C4 109.5(7) . . ? C5 C6 C7 106.5(7) . . ? N4 C7 C8 126.3(7) . . ? N4 C7 C6 110.2(7) . . ? C8 C7 C6 123.5(7) . . ? C9 C8 C7 124.6(7) . . ? C9 C8 C27 118.8(7) . . ? C7 C8 C27 116.3(7) . . ? N3 C9 C8 124.8(7) . . ? N3 C9 C10 108.9(6) . . ? C8 C9 C10 126.0(7) . . ? C11 C10 C9 108.1(7) . . ? C10 C11 C12 108.4(7) . . ? C13 C12 N3 124.5(6) . . ? C13 C12 C11 126.4(7) . . ? N3 C12 C11 109.1(6) . . ? C12 C13 C14 125.8(7) . . ? C12 C13 C33 118.7(7) . . ? C14 C13 C33 115.4(7) . . ? N2 C14 C13 126.0(7) . . ? N2 C14 C15 108.9(6) . . ? C13 C14 C15 125.0(7) . . ? C16 C15 C14 108.5(7) . . ? C15 C16 C17 107.2(7) . . ? C18 C17 N2 124.3(6) . . ? C18 C17 C16 126.7(7) . . ? N2 C17 C16 109.0(7) . . ? C17 C18 C19 121.4(7) . . ? C17 C18 C39 117.7(6) . . ? C19 C18 C39 120.8(7) . . ? C20 C19 C18 124.0(7) . . ? C20 C19 C1 107.4(6) . . ? C18 C19 C1 128.4(7) . . ? N1 C20 C19 108.4(7) . . ? C22 C21 C26 118.9(8) . . ? C22 C21 C3 120.0(8) . . ? C26 C21 C3 121.1(8) . . ? C21 C22 C23 120.4(9) . . ? C24 C23 C22 119.7(10) . . ? C23 C24 C25 121.1(9) . . ? C26 C25 C24 119.7(9) . . ? C25 C26 C21 120.2(9) . . ? C28 C27 C32 117.8(8) . . ? C28 C27 C8 121.4(7) . . ? C32 C27 C8 120.5(8) . . ? C27 C28 C29 121.0(8) . . ? C30 C29 C28 119.2(9) . . ? C31 C30 C29 121.6(9) . . ? C30 C31 C32 119.3(9) . . ? C31 C32 C27 121.2(9) . . ? C34 C33 C38 120.2(7) . . ? C34 C33 C13 121.3(7) . . ? C38 C33 C13 118.4(7) . . ? C33 C34 C35 118.4(8) . . ? C36 C35 C34 121.6(9) . . ? C35 C36 C37 120.4(8) . . ? C36 C37 C38 120.7(8) . . ? C37 C38 C33 118.6(8) . . ? C40 C39 C44 118.8(7) . . ? C40 C39 C18 119.8(7) . . ? C44 C39 C18 121.3(7) . . ? C41 C40 C39 120.4(8) . . ? C42 C41 C40 120.4(8) . . ? C41 C42 C43 120.5(9) . . ? C42 C43 C44 120.2(8) . . ? C43 C44 C39 119.6(8) . . ? C47 C46 C64 105.3(6) . . ? C47 C46 C90 123.0(7) . . ? C64 C46 C90 123.8(7) . . ? C47 C46 Fe2 107.8(5) . . ? C64 C46 Fe2 106.2(5) . . ? C90 C46 Fe2 86.2(4) . . ? N5 C47 C48 121.7(7) . . ? N5 C47 C46 107.6(6) . . ? C48 C47 C46 130.4(6) . . ? C49 C48 C47 120.7(7) . . ? C49 C48 C66 119.9(7) . . ? C47 C48 C66 119.3(6) . . ? C48 C49 N6 125.3(7) . . ? C48 C49 C50 125.2(7) . . ? N6 C49 C50 109.4(6) . . ? C51 C50 C49 106.7(7) . . ? C50 C51 C52 108.2(7) . . ? N6 C52 C53 126.4(7) . . ? N6 C52 C51 109.7(7) . . ? C53 C52 C51 123.8(7) . . ? C54 C53 C52 124.2(7) . . ? C54 C53 C72 118.4(7) . . ? C52 C53 C72 117.1(7) . . ? C53 C54 N7 126.9(7) . . ? C53 C54 C55 124.7(7) . . ? N7 C54 C55 108.3(7) . . ? C56 C55 C54 107.6(7) . . ? C55 C56 C57 107.3(7) . . ? N7 C57 C58 126.9(7) . . ? N7 C57 C56 109.5(6) . . ? C58 C57 C56 123.6(7) . . ? C57 C58 C59 123.8(7) . . ? C57 C58 C78 119.5(7) . . ? C59 C58 C78 116.6(7) . . ? N8 C59 C58 125.4(7) . . ? N8 C59 C60 110.2(6) . . ? C58 C59 C60 124.3(7) . . ? C61 C60 C59 107.0(7) . . ? C60 C61 C62 107.6(7) . . ? N8 C62 C63 125.4(7) . . ? N8 C62 C61 109.7(7) . . ? C63 C62 C61 124.9(7) . . ? C62 C63 C64 121.7(7) . . ? C62 C63 C84 120.4(7) . . ? C64 C63 C84 117.8(7) . . ? C65 C64 C63 122.9(7) . . ? C65 C64 C46 107.7(7) . . ? C63 C64 C46 129.0(7) . . ? N5 C65 C64 108.3(7) . . ? C67 C66 C71 119.5(7) . . ? C67 C66 C48 121.7(7) . . ? C71 C66 C48 118.8(7) . . ? C68 C67 C66 120.8(8) . . ? C67 C68 C69 120.1(8) . . ? C70 C69 C68 119.9(8) . . ? C69 C70 C71 120.2(8) . . ? C66 C71 C70 119.3(8) . . ? C73 C72 C77 118.4(7) . . ? C73 C72 C53 121.8(7) . . ? C77 C72 C53 119.7(7) . . ? C72 C73 C74 121.7(8) . . ? C73 C74 C75 119.1(8) . . ? C76 C75 C74 121.2(8) . . ? C75 C76 C77 118.4(8) . . ? C72 C77 C76 121.2(8) . . ? C83 C78 C79 118.8(8) . . ? C83 C78 C58 121.3(9) . . ? C79 C78 C58 119.9(8) . . ? C80 C79 C78 120.0(10) . . ? C81 C80 C79 118.9(11) . . ? C82 C81 C80 122.6(10) . . ? C81 C82 C83 118.4(11) . . ? C78 C83 C82 121.3(10) . . ? C89 C84 C85 120.3(7) . . ? C89 C84 C63 120.8(7) . . ? C85 C84 C63 118.9(7) . . ? C86 C85 C84 119.9(9) . . ? C85 C86 C87 119.6(9) . . ? C88 C87 C86 119.8(8) . . ? C87 C88 C89 120.5(9) . . ? C84 C89 C88 119.9(8) . . ? Cl2 C91 Cl1 112.1(6) . . ? Cl3 C92 Cl4 105.4(7) . . ? Cl6 C93 Cl5 113.4(7) . . ? F4 B1 F1 111.8(8) . . ? F4 B1 F3 112.3(8) . . ? F1 B1 F3 108.2(8) . . ? F4 B1 F2 111.6(9) . . ? F1 B1 F2 107.4(8) . . ? F3 B1 F2 105.1(7) . . ? F7 B2 F5 104(2) . . ? F7 B2 F8 116(2) . . ? F5 B2 F8 117(2) . . ? F7 B2 F6 107(2) . . ? F5 B2 F6 107(2) . . ? F8 B2 F6 106(2) . . ? F7A B2A F5A 124.2(18) . . ? F7A B2A F6A 113.4(18) . . ? F5A B2A F6A 105.1(18) . . ? F7A B2A F8A 105(2) . . ? F5A B2A F8A 103.7(19) . . ? F6A B2A F8A 102.8(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.881 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.190 #==END data_i11970mc_FeHCTPPCH2NO_BF4_cmpd5 _database_code_depnum_ccdc_archive 'CCDC 866966' #TrackingRef '- cif_bind.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46.50 H33 B Cl3 F4 Fe N5 O' _chemical_formula_weight 926.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.1501(17) _cell_length_b 13.7918(6) _cell_length_c 19.1196(9) _cell_angle_alpha 90.00 _cell_angle_beta 119.319(3) _cell_angle_gamma 90.00 _cell_volume 8081.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6275 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.81 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3784 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9509 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26554 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.13 _reflns_number_total 7214 _reflns_number_gt 5606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.6866P] 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 7214 _refine_ls_number_parameters 595 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.686780(12) 0.52982(3) 0.60474(2) 0.01486(15) Uani 1 1 d . A 1 N1 N 0.80346(8) 0.57344(19) 0.61559(15) 0.0218(6) Uani 1 1 d . A 1 N2 N 0.70638(7) 0.39022(17) 0.61256(14) 0.0165(5) Uani 1 1 d . A 1 N3 N 0.63205(7) 0.48410(17) 0.60131(14) 0.0171(5) Uani 1 1 d . A 1 N4 N 0.67282(7) 0.66759(17) 0.62144(13) 0.0150(5) Uani 1 1 d . A 1 N5 N 0.67601(8) 0.55587(18) 0.50963(15) 0.0206(6) Uani 1 1 d . A 1 O1 O 0.68699(8) 0.59357(18) 0.46760(13) 0.0340(6) Uani 1 1 d . A 1 C1 C 0.75260(9) 0.5716(2) 0.65655(17) 0.0163(6) Uani 1 1 d . A 1 C2 C 0.77955(9) 0.5120(2) 0.63629(17) 0.0174(6) Uani 1 1 d . A 1 C3 C 0.78196(9) 0.4118(2) 0.63533(16) 0.0174(6) Uani 1 1 d . A 1 C4 C 0.74753(9) 0.3563(2) 0.63209(16) 0.0168(6) Uani 1 1 d . A 1 C5 C 0.75056(9) 0.2550(2) 0.64831(17) 0.0183(6) Uani 1 1 d . A 1 H5 H 0.7756 0.2154 0.6640 0.022 Uiso 1 1 calc R A 1 C6 C 0.71155(9) 0.2258(2) 0.63731(17) 0.0200(6) Uani 1 1 d . A 1 H6 H 0.7037 0.1617 0.6434 0.024 Uiso 1 1 calc R A 1 C7 C 0.68388(9) 0.3101(2) 0.61463(16) 0.0174(6) Uani 1 1 d . A 1 C8 C 0.64097(9) 0.3075(2) 0.59865(16) 0.0171(6) Uani 1 1 d . A 1 C9 C 0.61614(9) 0.3908(2) 0.58764(17) 0.0181(6) Uani 1 1 d . A 1 C10 C 0.57083(9) 0.3908(2) 0.56606(18) 0.0211(7) Uani 1 1 d . A 1 H10 H 0.5523 0.3358 0.5527 0.025 Uiso 1 1 calc R A 1 C11 C 0.55972(10) 0.4832(2) 0.56834(18) 0.0213(7) Uani 1 1 d . A 1 H11 H 0.5317 0.5058 0.5570 0.026 Uiso 1 1 calc R A 1 C12 C 0.59769(9) 0.5418(2) 0.59099(17) 0.0173(6) Uani 1 1 d . A 1 C13 C 0.59942(9) 0.6404(2) 0.60425(16) 0.0168(6) Uani 1 1 d . A 1 C14 C 0.63594(9) 0.6977(2) 0.62209(16) 0.0159(6) Uani 1 1 d . A 1 C15 C 0.63924(9) 0.7983(2) 0.64342(17) 0.0178(6) Uani 1 1 d . A 1 H15 H 0.6183 0.8354 0.6496 0.021 Uiso 1 1 calc R A 1 C16 C 0.67750(9) 0.8301(2) 0.65296(16) 0.0181(6) Uani 1 1 d . A 1 H16 H 0.6885 0.8943 0.6664 0.022 Uiso 1 1 calc R A 1 C17 C 0.69876(9) 0.7496(2) 0.63925(16) 0.0165(6) Uani 1 1 d . A 1 C18 C 0.73891(9) 0.7549(2) 0.64082(16) 0.0167(6) Uani 1 1 d . A 1 C19 C 0.76028(9) 0.6700(2) 0.63922(16) 0.0174(6) Uani 1 1 d . A 1 C20 C 0.79180(9) 0.6651(2) 0.61607(16) 0.0160(6) Uani 1 1 d . A 1 H20 H 0.8035 0.7194 0.6025 0.019 Uiso 1 1 calc R A 1 C21 C 0.82004(9) 0.3631(2) 0.63664(17) 0.0178(6) Uani 1 1 d . A 1 C22 C 0.86208(10) 0.3943(2) 0.69020(18) 0.0217(7) Uani 1 1 d . A 1 H22 H 0.8661 0.4487 0.7236 0.026 Uiso 1 1 calc R A 1 C23 C 0.89816(10) 0.3471(2) 0.69545(19) 0.0252(7) Uani 1 1 d . A 1 H23 H 0.9267 0.3691 0.7322 0.030 Uiso 1 1 calc R A 1 C24 C 0.89256(10) 0.2678(2) 0.64709(19) 0.0262(7) Uani 1 1 d . A 1 H24 H 0.9173 0.2344 0.6515 0.031 Uiso 1 1 calc R A 1 C25 C 0.85119(10) 0.2373(2) 0.59257(18) 0.0239(7) Uani 1 1 d . A 1 H25 H 0.8473 0.1835 0.5587 0.029 Uiso 1 1 calc R A 1 C26 C 0.81516(9) 0.2851(2) 0.58714(17) 0.0202(7) Uani 1 1 d . A 1 H26 H 0.7867 0.2642 0.5489 0.024 Uiso 1 1 calc R A 1 C27 C 0.62110(9) 0.2123(2) 0.60008(18) 0.0188(6) Uani 1 1 d . A 1 C28 C 0.61807(9) 0.1368(2) 0.54891(18) 0.0215(7) Uani 1 1 d . A 1 H28 H 0.6285 0.1461 0.5120 0.026 Uiso 1 1 calc R A 1 C29 C 0.59997(10) 0.0487(2) 0.55146(19) 0.0242(7) Uani 1 1 d . A 1 H29 H 0.5978 -0.0022 0.5162 0.029 Uiso 1 1 calc R A 1 C30 C 0.58498(10) 0.0349(2) 0.60579(19) 0.0245(7) Uani 1 1 d . A 1 H30 H 0.5722 -0.0253 0.6070 0.029 Uiso 1 1 calc R A 1 C31 C 0.58850(10) 0.1078(2) 0.65793(19) 0.0243(7) Uani 1 1 d . A 1 H31 H 0.5788 0.0975 0.6959 0.029 Uiso 1 1 calc R A 1 C32 C 0.60628(9) 0.1966(2) 0.65460(18) 0.0211(7) Uani 1 1 d . A 1 H32 H 0.6083 0.2472 0.6900 0.025 Uiso 1 1 calc R A 1 C33 C 0.56072(9) 0.6891(2) 0.60082(17) 0.0185(6) Uani 1 1 d . A 1 C34 C 0.54490(10) 0.6593(2) 0.65134(18) 0.0222(7) Uani 1 1 d . A 1 H34 H 0.5587 0.6073 0.6877 0.027 Uiso 1 1 calc R A 1 C35 C 0.50897(10) 0.7053(2) 0.64896(19) 0.0259(7) Uani 1 1 d . A 1 H35 H 0.4983 0.6843 0.6834 0.031 Uiso 1 1 calc R A 1 C36 C 0.48903(10) 0.7809(2) 0.59687(19) 0.0261(7) Uani 1 1 d . A 1 H36 H 0.4648 0.8129 0.5959 0.031 Uiso 1 1 calc R A 1 C37 C 0.50426(9) 0.8105(2) 0.54573(19) 0.0241(7) Uani 1 1 d . A 1 H37 H 0.4903 0.8626 0.5095 0.029 Uiso 1 1 calc R A 1 C38 C 0.53976(9) 0.7644(2) 0.54721(18) 0.0200(6) Uani 1 1 d . A 1 H38 H 0.5498 0.7844 0.5115 0.024 Uiso 1 1 calc R A 1 C39 C 0.75906(9) 0.8497(2) 0.64310(17) 0.0170(6) Uani 1 1 d . A 1 C40 C 0.80326(9) 0.8645(2) 0.69674(17) 0.0194(6) Uani 1 1 d . A 1 H40 H 0.8199 0.8137 0.7320 0.023 Uiso 1 1 calc R A 1 C41 C 0.82310(10) 0.9513(2) 0.69941(18) 0.0223(7) Uani 1 1 d . A 1 H41 H 0.8532 0.9604 0.7367 0.027 Uiso 1 1 calc R A 1 C42 C 0.79927(11) 1.0255(2) 0.6476(2) 0.0253(7) Uani 1 1 d . A 1 H42 H 0.8129 1.0853 0.6487 0.030 Uiso 1 1 calc R A 1 C43 C 0.75527(11) 1.0118(2) 0.59427(19) 0.0229(7) Uani 1 1 d . A 1 H43 H 0.7387 1.0630 0.5593 0.028 Uiso 1 1 calc R A 1 C44 C 0.73527(10) 0.9249(2) 0.59145(17) 0.0195(6) Uani 1 1 d . A 1 H44 H 0.7052 0.9162 0.5542 0.023 Uiso 1 1 calc R A 1 C45 C 0.73803(9) 0.5451(2) 0.71239(17) 0.0141(6) Uani 1 1 d . A 1 C46 C 0.0000 0.5800(4) 0.7500 0.0472(14) Uani 1 2 d S . 1 H46A H 0.0261 0.6221 0.7708 0.057 Uiso 0.50 1 calc PR . 1 H46B H -0.0261 0.6221 0.7292 0.057 Uiso 0.50 1 calc PR . 1 C47 C 0.9368(2) 0.8967(5) 0.6322(5) 0.0442(16) Uani 0.780(3) 1 d P B 2 H47A H 0.9366 0.8526 0.6729 0.053 Uiso 0.780(3) 1 calc PR B 2 H47B H 0.9146 0.8733 0.5786 0.053 Uiso 0.780(3) 1 calc PR B 2 C47A C 0.9295(9) 0.8907(11) 0.6590(7) 0.052(7) Uani 0.220(3) 1 d PD B 3 H47C H 0.8989 0.8679 0.6292 0.062 Uiso 0.220(3) 1 calc PR B 3 H47D H 0.9478 0.8430 0.6503 0.062 Uiso 0.220(3) 1 calc PR B 3 Cl1 Cl 0.00300(4) 0.50744(10) 0.82772(9) 0.0771(4) Uani 1 1 d . C 1 Cl2 Cl 0.92298(6) 1.01514(14) 0.64742(13) 0.0563(5) Uani 0.780(3) 1 d P B 2 Cl3 Cl 0.98851(4) 0.89307(12) 0.63885(8) 0.0587(5) Uani 0.780(3) 1 d P B 2 Cl2A Cl 0.94596(17) 0.8950(4) 0.7613(3) 0.0559(16) Uani 0.220(3) 1 d PD B 3 Cl3A Cl 0.9334(3) 1.0035(6) 0.6200(4) 0.063(2) Uani 0.220(3) 1 d PD B 3 B1 B 0.61531(12) 0.8381(3) 0.4112(2) 0.0307(9) Uani 1 1 d . D 1 F1 F 0.63060(7) 0.93317(16) 0.42811(14) 0.0467(6) Uani 1 1 d . D 1 F2 F 0.64971(7) 0.77820(15) 0.45430(13) 0.0509(6) Uani 1 1 d . D 1 F3 F 0.59933(7) 0.81989(19) 0.33077(12) 0.0519(6) Uani 1 1 d . D 1 F4 F 0.58291(8) 0.8279(2) 0.43067(15) 0.0752(9) Uani 1 1 d . D 1 H1 H 0.8225(10) 0.554(2) 0.5978(17) 0.014(8) Uiso 1 1 d . E 1 H45A H 0.7483(11) 0.490(2) 0.7393(19) 0.020(8) Uiso 1 1 d . . . H45B H 0.7352(9) 0.595(2) 0.7397(17) 0.010(7) 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 0.0140(2) 0.0134(2) 0.0163(2) -0.00051(17) 0.00671(18) 0.00119(16) N1 0.0232(14) 0.0220(14) 0.0249(14) -0.0003(12) 0.0153(12) -0.0010(11) N2 0.0172(12) 0.0144(12) 0.0182(12) -0.0021(10) 0.0089(10) -0.0009(10) N3 0.0144(12) 0.0159(13) 0.0188(13) -0.0013(10) 0.0063(10) 0.0007(10) N4 0.0140(12) 0.0136(12) 0.0168(12) 0.0002(10) 0.0072(10) 0.0003(9) N5 0.0215(13) 0.0179(13) 0.0195(13) 0.0011(11) 0.0079(11) 0.0067(10) O1 0.0436(15) 0.0401(14) 0.0272(12) 0.0075(11) 0.0243(12) 0.0091(11) C1 0.0130(14) 0.0135(14) 0.0187(15) -0.0010(12) 0.0050(12) 0.0015(11) C2 0.0131(14) 0.0230(16) 0.0147(14) -0.0012(13) 0.0057(12) 0.0010(12) C3 0.0175(15) 0.0182(15) 0.0151(14) 0.0002(12) 0.0068(12) 0.0030(12) C4 0.0142(14) 0.0194(16) 0.0150(14) -0.0007(12) 0.0057(12) 0.0034(12) C5 0.0192(15) 0.0142(15) 0.0202(15) 0.0000(12) 0.0085(13) 0.0032(12) C6 0.0216(16) 0.0157(15) 0.0216(15) -0.0002(13) 0.0097(13) 0.0010(12) C7 0.0201(15) 0.0135(15) 0.0157(14) -0.0019(12) 0.0066(12) -0.0005(12) C8 0.0183(15) 0.0143(15) 0.0162(14) -0.0022(12) 0.0066(12) -0.0022(12) C9 0.0176(15) 0.0173(15) 0.0192(15) -0.0026(13) 0.0087(13) -0.0010(12) C10 0.0178(15) 0.0189(16) 0.0266(16) -0.0018(13) 0.0109(13) -0.0015(12) C11 0.0150(15) 0.0217(17) 0.0239(16) -0.0018(13) 0.0069(13) 0.0014(12) C12 0.0153(14) 0.0189(16) 0.0171(14) -0.0002(12) 0.0075(12) 0.0015(12) C13 0.0153(14) 0.0191(15) 0.0146(14) 0.0003(12) 0.0061(12) 0.0016(12) C14 0.0164(14) 0.0155(15) 0.0144(14) 0.0008(12) 0.0064(12) 0.0021(11) C15 0.0183(15) 0.0164(15) 0.0182(15) -0.0021(12) 0.0084(12) 0.0025(12) C16 0.0217(15) 0.0137(15) 0.0179(14) -0.0025(12) 0.0088(12) 0.0007(12) C17 0.0174(15) 0.0155(15) 0.0144(14) 0.0010(12) 0.0060(12) 0.0018(12) C18 0.0179(15) 0.0156(15) 0.0143(14) 0.0008(12) 0.0062(12) 0.0009(11) C19 0.0145(14) 0.0196(15) 0.0157(14) 0.0003(13) 0.0057(12) 0.0003(12) C20 0.0149(14) 0.0144(15) 0.0180(14) 0.0011(12) 0.0076(12) 0.0003(11) C21 0.0196(15) 0.0172(15) 0.0164(14) 0.0021(12) 0.0087(12) 0.0019(12) C22 0.0245(16) 0.0192(16) 0.0218(16) 0.0031(13) 0.0116(14) 0.0026(13) C23 0.0175(15) 0.0256(17) 0.0316(17) 0.0072(15) 0.0113(14) 0.0027(13) C24 0.0242(17) 0.0275(18) 0.0342(18) 0.0087(15) 0.0200(15) 0.0098(14) C25 0.0333(18) 0.0202(16) 0.0264(17) 0.0033(14) 0.0210(15) 0.0058(14) C26 0.0203(16) 0.0226(16) 0.0175(15) 0.0022(13) 0.0091(13) 0.0031(12) C27 0.0126(14) 0.0167(15) 0.0239(16) -0.0001(13) 0.0065(12) 0.0006(12) C28 0.0182(15) 0.0189(16) 0.0251(16) -0.0008(13) 0.0089(13) -0.0004(12) C29 0.0223(16) 0.0152(15) 0.0270(17) -0.0026(13) 0.0059(14) 0.0036(12) C30 0.0183(16) 0.0156(16) 0.0347(18) 0.0056(14) 0.0091(14) 0.0008(12) C31 0.0209(16) 0.0236(17) 0.0280(17) 0.0028(14) 0.0118(14) 0.0009(13) C32 0.0188(15) 0.0202(16) 0.0219(15) -0.0031(13) 0.0080(13) 0.0001(12) C33 0.0153(14) 0.0178(15) 0.0210(15) -0.0062(13) 0.0078(12) -0.0021(12) C34 0.0213(16) 0.0227(16) 0.0216(16) -0.0008(14) 0.0097(13) -0.0012(13) C35 0.0223(17) 0.0330(19) 0.0263(17) -0.0053(15) 0.0150(14) -0.0029(14) C36 0.0172(15) 0.0267(18) 0.0332(18) -0.0107(15) 0.0114(14) 0.0018(13) C37 0.0185(16) 0.0184(16) 0.0295(17) -0.0056(14) 0.0072(14) 0.0018(12) C38 0.0167(15) 0.0182(15) 0.0233(15) -0.0031(13) 0.0084(13) -0.0018(12) C39 0.0196(15) 0.0162(15) 0.0178(14) -0.0001(12) 0.0112(12) 0.0002(12) C40 0.0197(15) 0.0210(16) 0.0180(15) 0.0005(13) 0.0096(13) 0.0010(12) C41 0.0216(16) 0.0241(17) 0.0228(16) -0.0070(14) 0.0121(14) -0.0057(13) C42 0.0344(19) 0.0171(16) 0.0352(19) -0.0055(14) 0.0255(16) -0.0041(14) C43 0.0332(18) 0.0158(16) 0.0278(17) 0.0039(13) 0.0212(15) 0.0065(13) C44 0.0203(15) 0.0200(16) 0.0200(15) 0.0009(13) 0.0113(13) 0.0042(12) C45 0.0123(14) 0.0123(15) 0.0155(15) -0.0004(13) 0.0052(12) 0.0025(11) C46 0.037(3) 0.043(3) 0.064(4) 0.000 0.027(3) 0.000 C47 0.044(4) 0.039(3) 0.045(4) -0.005(3) 0.019(3) -0.006(3) C47A 0.038(13) 0.046(13) 0.053(17) 0.020(12) 0.007(11) 0.005(10) Cl1 0.0418(7) 0.0776(9) 0.1105(11) 0.0477(8) 0.0362(7) 0.0147(6) Cl2 0.0486(10) 0.0454(9) 0.0593(13) -0.0069(9) 0.0144(8) 0.0027(7) Cl3 0.0455(8) 0.0830(11) 0.0530(8) -0.0075(8) 0.0285(7) -0.0057(7) Cl2A 0.058(3) 0.068(3) 0.045(3) -0.004(2) 0.027(2) -0.012(3) Cl3A 0.072(5) 0.055(4) 0.045(4) 0.006(3) 0.016(3) -0.019(3) B1 0.0219(19) 0.045(3) 0.0263(19) 0.0032(19) 0.0129(16) -0.0049(17) F1 0.0528(14) 0.0386(13) 0.0600(14) 0.0042(11) 0.0362(12) 0.0133(10) F2 0.0582(15) 0.0306(12) 0.0407(12) 0.0070(10) 0.0062(11) 0.0077(10) F3 0.0427(13) 0.0853(18) 0.0252(11) -0.0002(12) 0.0147(10) 0.0022(12) F4 0.0544(15) 0.131(3) 0.0600(15) -0.0297(17) 0.0437(13) -0.0455(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 1.704(3) . ? Fe1 C45 1.974(3) . ? Fe1 N3 1.995(2) . ? Fe1 N2 2.026(2) . ? Fe1 N4 2.026(2) . ? Fe1 C1 2.103(3) . ? N1 C20 1.331(4) . ? N1 C2 1.381(4) . ? N1 H1 0.93(3) . ? N2 C7 1.371(4) . ? N2 C4 1.386(4) . ? N3 C9 1.376(4) . ? N3 C12 1.377(4) . ? N4 C14 1.367(3) . ? N4 C17 1.386(4) . ? N5 O1 1.170(3) . ? C1 C45 1.439(4) . ? C1 C2 1.443(4) . ? C1 C19 1.453(4) . ? C2 C3 1.385(4) . ? C3 C4 1.408(4) . ? C3 C21 1.487(4) . ? C4 C5 1.423(4) . ? C5 C6 1.343(4) . ? C5 H5 0.9500 . ? C6 C7 1.439(4) . ? C6 H6 0.9500 . ? C7 C8 1.385(4) . ? C8 C9 1.395(4) . ? C8 C27 1.494(4) . ? C9 C10 1.437(4) . ? C10 C11 1.340(4) . ? C10 H10 0.9500 . ? C11 C12 1.434(4) . ? C11 H11 0.9500 . ? C12 C13 1.380(4) . ? C13 C14 1.400(4) . ? C13 C33 1.489(4) . ? C14 C15 1.435(4) . ? C15 C16 1.339(4) . ? C15 H15 0.9500 . ? C16 C17 1.433(4) . ? C16 H16 0.9500 . ? C17 C18 1.399(4) . ? C18 C19 1.400(4) . ? C18 C39 1.477(4) . ? C19 C20 1.382(4) . ? C20 H20 0.9500 . ? C21 C26 1.387(4) . ? C21 C22 1.391(4) . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.376(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(4) . ? C27 C28 1.397(4) . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 C31 1.378(4) . ? C30 H30 0.9500 . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.390(4) . ? C33 C34 1.392(4) . ? C34 C35 1.394(4) . ? C34 H34 0.9500 . ? C35 C36 1.374(5) . ? C35 H35 0.9500 . ? C36 C37 1.386(4) . ? C36 H36 0.9500 . ? C37 C38 1.388(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.394(4) . ? C39 C40 1.395(4) . ? C40 C41 1.374(4) . ? C40 H40 0.9500 . ? C41 C42 1.384(5) . ? C41 H41 0.9500 . ? C42 C43 1.387(5) . ? C42 H42 0.9500 . ? C43 C44 1.377(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.88(3) . ? C45 H45B 0.90(3) . ? C46 Cl1 1.751(4) . ? C46 Cl1 1.751(4) 2_556 ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 Cl3 1.759(7) . ? C47 Cl2 1.769(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47A Cl2A 1.748(10) . ? C47A Cl3A 1.759(10) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? B1 F2 1.359(4) . ? B1 F4 1.368(4) . ? B1 F3 1.377(4) . ? B1 F1 1.394(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 N5 Fe1 C45 134.64(12) . . ? N5 Fe1 N3 108.95(11) . . ? C45 Fe1 N3 116.18(11) . . ? N5 Fe1 N2 99.73(10) . . ? C45 Fe1 N2 85.46(11) . . ? N3 Fe1 N2 89.41(9) . . ? N5 Fe1 N4 91.49(10) . . ? C45 Fe1 N4 84.45(11) . . ? N3 Fe1 N4 89.86(9) . . ? N2 Fe1 N4 168.37(9) . . ? N5 Fe1 C1 93.62(12) . . ? C45 Fe1 C1 41.20(11) . . ? N3 Fe1 C1 157.38(11) . . ? N2 Fe1 C1 88.28(10) . . ? N4 Fe1 C1 87.94(10) . . ? C20 N1 C2 110.4(3) . . ? C20 N1 H1 124.1(19) . . ? C2 N1 H1 125.1(19) . . ? C7 N2 C4 105.1(2) . . ? C7 N2 Fe1 126.03(19) . . ? C4 N2 Fe1 127.82(19) . . ? C9 N3 C12 105.5(2) . . ? C9 N3 Fe1 126.68(19) . . ? C12 N3 Fe1 125.88(19) . . ? C14 N4 C17 105.2(2) . . ? C14 N4 Fe1 126.16(19) . . ? C17 N4 Fe1 128.52(18) . . ? O1 N5 Fe1 148.3(2) . . ? C45 C1 C2 124.9(3) . . ? C45 C1 C19 125.4(3) . . ? C2 C1 C19 104.6(2) . . ? C45 C1 Fe1 64.58(15) . . ? C2 C1 Fe1 115.6(2) . . ? C19 C1 Fe1 115.67(19) . . ? N1 C2 C3 124.0(3) . . ? N1 C2 C1 107.4(3) . . ? C3 C2 C1 128.7(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 C21 120.7(3) . . ? C4 C3 C21 120.2(3) . . ? N2 C4 C3 126.1(3) . . ? N2 C4 C5 110.3(2) . . ? C3 C4 C5 123.6(3) . . ? C6 C5 C4 107.3(3) . . ? C6 C5 H5 126.3 . . ? C4 C5 H5 126.3 . . ? C5 C6 C7 107.0(3) . . ? C5 C6 H6 126.5 . . ? C7 C6 H6 126.5 . . ? N2 C7 C8 126.6(3) . . ? N2 C7 C6 110.2(2) . . ? C8 C7 C6 123.2(3) . . ? C7 C8 C9 123.1(3) . . ? C7 C8 C27 119.1(3) . . ? C9 C8 C27 117.6(2) . . ? N3 C9 C8 125.1(3) . . ? N3 C9 C10 110.2(2) . . ? C8 C9 C10 124.5(3) . . ? C11 C10 C9 106.9(3) . . ? C11 C10 H10 126.6 . . ? C9 C10 H10 126.6 . . ? C10 C11 C12 107.6(3) . . ? C10 C11 H11 126.2 . . ? C12 C11 H11 126.2 . . ? N3 C12 C13 125.9(3) . . ? N3 C12 C11 109.8(2) . . ? C13 C12 C11 124.2(3) . . ? C12 C13 C14 123.6(3) . . ? C12 C13 C33 118.6(3) . . ? C14 C13 C33 117.7(3) . . ? N4 C14 C13 125.9(3) . . ? N4 C14 C15 110.6(2) . . ? C13 C14 C15 123.5(3) . . ? C16 C15 C14 106.9(2) . . ? C16 C15 H15 126.5 . . ? C14 C15 H15 126.5 . . ? C15 C16 C17 107.5(3) . . ? C15 C16 H16 126.3 . . ? C17 C16 H16 126.3 . . ? N4 C17 C18 125.7(3) . . ? N4 C17 C16 109.8(2) . . ? C18 C17 C16 124.5(3) . . ? C17 C18 C19 120.1(3) . . ? C17 C18 C39 120.7(2) . . ? C19 C18 C39 119.1(2) . . ? C20 C19 C18 124.8(3) . . ? C20 C19 C1 107.2(2) . . ? C18 C19 C1 127.9(3) . . ? N1 C20 C19 110.3(3) . . ? N1 C20 H20 124.9 . . ? C19 C20 H20 124.9 . . ? C26 C21 C22 118.3(3) . . ? C26 C21 C3 122.0(3) . . ? C22 C21 C3 119.7(3) . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 121.0(3) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 118.7(3) . . ? C32 C27 C8 120.0(3) . . ? C28 C27 C8 121.2(3) . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.7(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 119.5(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C27 120.9(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C38 C33 C34 119.0(3) . . ? C38 C33 C13 120.8(3) . . ? C34 C33 C13 120.2(3) . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 119.9(3) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 120.3(3) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C44 C39 C40 118.5(3) . . ? C44 C39 C18 121.7(3) . . ? C40 C39 C18 119.8(3) . . ? C41 C40 C39 121.2(3) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C40 C41 C42 119.9(3) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 119.5(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 120.7(3) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C39 120.2(3) . . ? C43 C44 H44 119.9 . . ? C39 C44 H44 119.9 . . ? C1 C45 Fe1 74.22(16) . . ? C1 C45 H45A 117(2) . . ? Fe1 C45 H45A 115(2) . . ? C1 C45 H45B 114.4(18) . . ? Fe1 C45 H45B 112.5(17) . . ? H45A C45 H45B 117(3) . . ? Cl1 C46 Cl1 110.3(3) . 2_556 ? Cl1 C46 H46A 109.6 . . ? Cl1 C46 H46A 109.6 2_556 . ? Cl1 C46 H46B 109.6 . . ? Cl1 C46 H46B 109.6 2_556 . ? H46A C46 H46B 108.1 . . ? Cl3 C47 Cl2 111.8(4) . . ? Cl3 C47 H47A 109.2 . . ? Cl2 C47 H47A 109.2 . . ? Cl3 C47 H47B 109.2 . . ? Cl2 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? Cl2A C47A Cl3A 113.1(8) . . ? Cl2A C47A H47C 109.0 . . ? Cl3A C47A H47C 109.0 . . ? Cl2A C47A H47D 109.0 . . ? Cl3A C47A H47D 109.0 . . ? H47C C47A H47D 107.8 . . ? F2 B1 F4 112.6(3) . . ? F2 B1 F3 108.8(3) . . ? F4 B1 F3 110.3(3) . . ? F2 B1 F1 107.6(3) . . ? F4 B1 F1 108.1(3) . . ? F3 B1 F1 109.3(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.226 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.151 #==END