# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dongfeng Li' _publ_contact_author_email DFLI@MAIL.CCNU.EDU.CN _publ_section_title ; Non-heme iron(II/III) complexes that model the reactivity of lipoxygenase with redox switch ; loop_ _publ_author_name 'Dongfeng Li.' 'Ji Li.' 'Zhan-Ru Liao.' 'Fusheng Mei.' 'Xianggao Meng.' ; Chunping Ou ; # Attachment '755332.cif' data_Fe(II)CTB(ClO4)2.EtOH _database_code_depnum_ccdc_archive 'CCDC 755332' #TrackingRef '755332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 Cl2 Fe N10 O9' _chemical_formula_weight 935.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 14.3899(9) _cell_length_b 16.1238(10) _cell_length_c 18.8845(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.1700(10) _cell_angle_gamma 90.00 _cell_volume 4266.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3283 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 20.41 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7727 _exptl_absorpt_correction_T_max 0.9476 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 23054 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8360 _reflns_number_gt 5281 _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^)+(0.0836P)^2^+0.4855P] 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 8360 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.48949(3) 0.51004(3) 0.25908(3) 0.03332(17) Uani 1 1 d . . . C1 C 0.5645(2) 0.6950(2) 0.2745(2) 0.0402(9) Uani 1 1 d . . . H1 H 0.5750 0.6913 0.2251 0.048 Uiso 1 1 calc R . . C2 C 0.6210(3) 0.7704(2) 0.3105(2) 0.0549(11) Uani 1 1 d . . . H2A H 0.6230 0.7698 0.3622 0.066 Uiso 1 1 calc R . . H2B H 0.6861 0.7668 0.3045 0.066 Uiso 1 1 calc R . . C3 C 0.5766(3) 0.8513(2) 0.2778(3) 0.0611(12) Uani 1 1 d . . . H3A H 0.6136 0.8978 0.3018 0.073 Uiso 1 1 calc R . . H3B H 0.5769 0.8534 0.2265 0.073 Uiso 1 1 calc R . . C4 C 0.4758(3) 0.8570(2) 0.2872(3) 0.0625(12) Uani 1 1 d . . . H4A H 0.4492 0.9108 0.2708 0.075 Uiso 1 1 calc R . . H4B H 0.4752 0.8512 0.3382 0.075 Uiso 1 1 calc R . . C5 C 0.4156(3) 0.7888(2) 0.2434(2) 0.0538(11) Uani 1 1 d . . . H5A H 0.4137 0.7967 0.1922 0.065 Uiso 1 1 calc R . . H5B H 0.3508 0.7926 0.2499 0.065 Uiso 1 1 calc R . . C6 C 0.4555(2) 0.7027(2) 0.2668(2) 0.0383(8) Uani 1 1 d . . . H6 H 0.4437 0.6926 0.3151 0.046 Uiso 1 1 calc R . . C7 C 0.6898(2) 0.5864(2) 0.2970(2) 0.0434(9) Uani 1 1 d . . . H7A H 0.7424 0.6143 0.3296 0.052 Uiso 1 1 calc R . . H7B H 0.6925 0.5989 0.2473 0.052 Uiso 1 1 calc R . . C8 C 0.6956(2) 0.4945(2) 0.3098(2) 0.0390(9) Uani 1 1 d . . . C9 C 0.7508(3) 0.3691(2) 0.34267(19) 0.0417(9) Uani 1 1 d . . . C10 C 0.8033(3) 0.2996(3) 0.3696(2) 0.0580(11) Uani 1 1 d . . . H10 H 0.8695 0.3009 0.3840 0.070 Uiso 1 1 calc R . . C11 C 0.7519(4) 0.2279(3) 0.3739(3) 0.0682(13) Uani 1 1 d . . . H11 H 0.7842 0.1796 0.3915 0.082 Uiso 1 1 calc R . . C12 C 0.6531(3) 0.2269(3) 0.3524(2) 0.0601(12) Uani 1 1 d . . . H12 H 0.6209 0.1776 0.3560 0.072 Uiso 1 1 calc R . . C13 C 0.6017(3) 0.2955(2) 0.3262(2) 0.0484(10) Uani 1 1 d . . . H13 H 0.5354 0.2940 0.3126 0.058 Uiso 1 1 calc R . . C14 C 0.6514(2) 0.3677(2) 0.32064(18) 0.0380(8) Uani 1 1 d . . . C15 C 0.6007(3) 0.6123(2) 0.39068(19) 0.0438(9) Uani 1 1 d . . . H15A H 0.6121 0.6679 0.4104 0.053 Uiso 1 1 calc R . . H15B H 0.6533 0.5774 0.4149 0.053 Uiso 1 1 calc R . . C16 C 0.5094(3) 0.5797(2) 0.40520(18) 0.0369(8) Uani 1 1 d . . . C17 C 0.3863(3) 0.5633(2) 0.4542(2) 0.0448(9) Uani 1 1 d . . . C18 C 0.3147(3) 0.5691(3) 0.4939(2) 0.0585(12) Uani 1 1 d . . . H18 H 0.3185 0.6064 0.5320 0.070 Uiso 1 1 calc R . . C19 C 0.2386(3) 0.5159(3) 0.4724(3) 0.0644(13) Uani 1 1 d . . . H19 H 0.1887 0.5182 0.4961 0.077 Uiso 1 1 calc R . . C20 C 0.2336(3) 0.4593(3) 0.4167(2) 0.0639(12) Uani 1 1 d . . . H20 H 0.1815 0.4237 0.4050 0.077 Uiso 1 1 calc R . . C21 C 0.3042(3) 0.4542(3) 0.3780(2) 0.0537(11) Uani 1 1 d . . . H21 H 0.3011 0.4153 0.3411 0.064 Uiso 1 1 calc R . . C22 C 0.3793(3) 0.5091(2) 0.39621(19) 0.0404(9) Uani 1 1 d . . . C23 C 0.3100(2) 0.6157(2) 0.2271(2) 0.0400(9) Uani 1 1 d . . . H23A H 0.2657 0.6561 0.2002 0.048 Uiso 1 1 calc R . . H23B H 0.3070 0.6178 0.2778 0.048 Uiso 1 1 calc R . . C24 C 0.2860(2) 0.5307(2) 0.19695(18) 0.0362(8) Uani 1 1 d . . . C25 C 0.2139(3) 0.4277(2) 0.1285(2) 0.0422(9) Uani 1 1 d . . . C26 C 0.1562(3) 0.3768(3) 0.0789(2) 0.0540(11) Uani 1 1 d . . . H26 H 0.0960 0.3936 0.0536 0.065 Uiso 1 1 calc R . . C27 C 0.1918(3) 0.3001(3) 0.0684(3) 0.0676(13) Uani 1 1 d . . . H27 H 0.1546 0.2641 0.0352 0.081 Uiso 1 1 calc R . . C28 C 0.2813(3) 0.2747(3) 0.1057(2) 0.0658(13) Uani 1 1 d . . . H28 H 0.3026 0.2220 0.0970 0.079 Uiso 1 1 calc R . . C29 C 0.3398(3) 0.3252(2) 0.1555(2) 0.0572(11) Uani 1 1 d . . . H29 H 0.3999 0.3078 0.1806 0.069 Uiso 1 1 calc R . . C30 C 0.3053(2) 0.4032(2) 0.1668(2) 0.0400(9) Uani 1 1 d . . . C31 C 0.4099(3) 0.6449(2) 0.14066(19) 0.0418(9) Uani 1 1 d . . . H31A H 0.3483 0.6291 0.1107 0.050 Uiso 1 1 calc R . . H31B H 0.4201 0.7031 0.1317 0.050 Uiso 1 1 calc R . . C32 C 0.4853(2) 0.5950(2) 0.11966(18) 0.0341(8) Uani 1 1 d . . . C33 C 0.5871(2) 0.5519(2) 0.05642(19) 0.0367(8) Uani 1 1 d . . . C34 C 0.6471(3) 0.5408(3) 0.0093(2) 0.0499(10) Uani 1 1 d . . . H34 H 0.6481 0.5780 -0.0281 0.060 Uiso 1 1 calc R . . C35 C 0.7049(3) 0.4721(3) 0.0206(2) 0.0542(11) Uani 1 1 d . . . H35 H 0.7470 0.4630 -0.0093 0.065 Uiso 1 1 calc R . . C36 C 0.7019(3) 0.4158(3) 0.0758(2) 0.0596(12) Uani 1 1 d . . . H36 H 0.7398 0.3685 0.0802 0.071 Uiso 1 1 calc R . . C37 C 0.6443(3) 0.4280(2) 0.1244(2) 0.0504(10) Uani 1 1 d . . . H37 H 0.6440 0.3906 0.1619 0.060 Uiso 1 1 calc R . . C38 C 0.5875(3) 0.4975(2) 0.11501(19) 0.0374(8) Uani 1 1 d . . . N1 N 0.59690(19) 0.61420(17) 0.31131(15) 0.0364(7) Uani 1 1 d . . . N2 N 0.40882(18) 0.63330(16) 0.21925(14) 0.0336(7) Uani 1 1 d . . . N3 N 0.6195(2) 0.44733(17) 0.29979(16) 0.0382(7) Uani 1 1 d . . . N4 N 0.7770(2) 0.45116(19) 0.33498(16) 0.0429(7) Uani 1 1 d . . . H4 H 0.8342 0.4706 0.3444 0.051 Uiso 1 1 calc R . . N5 N 0.4577(2) 0.52145(17) 0.36461(16) 0.0393(7) Uani 1 1 d . . . N6 N 0.4701(2) 0.60647(18) 0.45885(16) 0.0443(8) Uani 1 1 d . . . H6A H 0.4930 0.6439 0.4905 0.053 Uiso 1 1 calc R . . N7 N 0.3492(2) 0.47009(17) 0.20891(15) 0.0363(7) Uani 1 1 d . . . N8 N 0.2047(2) 0.50848(18) 0.15080(17) 0.0428(8) Uani 1 1 d . . . H8 H 0.1550 0.5393 0.1373 0.051 Uiso 1 1 calc R . . N9 N 0.5221(2) 0.52715(18) 0.15349(16) 0.0388(7) Uani 1 1 d . . . N10 N 0.5217(2) 0.61285(17) 0.06180(16) 0.0396(7) Uani 1 1 d . . . H10A H 0.5068 0.6547 0.0333 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.5951(14) 0.7991(13) 0.5554(13) 0.057(2) Uani 0.580(13) 1 d P A 1 O1 O 0.5724(7) 0.8069(6) 0.4781(4) 0.118(4) Uani 0.580(13) 1 d P A 1 O2 O 0.6947(8) 0.7898(8) 0.5822(6) 0.106(4) Uani 0.580(13) 1 d P A 1 O3 O 0.5476(7) 0.7258(5) 0.5725(5) 0.104(4) Uani 0.580(13) 1 d P A 1 O4 O 0.561(4) 0.867(5) 0.591(4) 0.103(11) Uani 0.580(13) 1 d P A 1 Cl1' Cl 0.598(2) 0.8018(19) 0.567(2) 0.076(6) Uani 0.420(13) 1 d P A 2 O1' O 0.5255(7) 0.7604(6) 0.5161(8) 0.092(6) Uani 0.420(13) 1 d P A 2 O2' O 0.6816(12) 0.8150(11) 0.5403(10) 0.111(5) Uani 0.420(13) 1 d P A 2 O3' O 0.6245(9) 0.7541(8) 0.6330(7) 0.129(6) Uani 0.420(13) 1 d P A 2 O4' O 0.561(6) 0.882(7) 0.582(6) 0.12(2) Uani 0.420(13) 1 d P A 2 Cl2 Cl 0.05226(10) 0.32370(9) 0.51981(8) 0.0819(4) Uani 1 1 d . . . O5 O 0.0114(4) 0.2538(3) 0.5419(3) 0.1369(17) Uani 1 1 d . . . O6 O 0.0548(3) 0.3101(3) 0.4457(3) 0.1395(19) Uani 1 1 d . . . O7 O 0.1401(3) 0.3431(4) 0.5613(3) 0.162(2) Uani 1 1 d . . . O8 O -0.0096(4) 0.3907(3) 0.5221(3) 0.145(2) Uani 1 1 d . . . C39 C 0.0554(5) 0.6018(4) 0.2869(4) 0.113(2) Uani 1 1 d . . . H39A H 0.0840 0.6316 0.3305 0.170 Uiso 1 1 calc R . . H39B H 0.0524 0.6371 0.2455 0.170 Uiso 1 1 calc R . . H39C H 0.0930 0.5537 0.2828 0.170 Uiso 1 1 calc R . . C40 C -0.0394(4) 0.5766(4) 0.2900(3) 0.0966(18) Uani 1 1 d . . . H40A H -0.0709 0.5539 0.2431 0.116 Uiso 1 1 calc R . . H40B H -0.0750 0.6252 0.2985 0.116 Uiso 1 1 calc R . . O9 O -0.0427(2) 0.5156(2) 0.34583(19) 0.0746(9) Uani 1 1 d . . . H9 H -0.0196 0.5355 0.3859 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0320(3) 0.0328(3) 0.0332(3) 0.0004(2) 0.0034(2) 0.0037(2) C1 0.037(2) 0.0309(19) 0.052(2) 0.0012(16) 0.0079(17) 0.0005(15) C2 0.054(3) 0.037(2) 0.072(3) -0.003(2) 0.011(2) -0.0068(18) C3 0.067(3) 0.030(2) 0.089(3) -0.001(2) 0.023(2) -0.0054(19) C4 0.076(3) 0.030(2) 0.086(3) 0.001(2) 0.028(3) 0.006(2) C5 0.051(2) 0.035(2) 0.075(3) -0.002(2) 0.013(2) 0.0079(18) C6 0.040(2) 0.0299(19) 0.046(2) -0.0005(16) 0.0112(17) 0.0003(15) C7 0.0313(19) 0.040(2) 0.058(2) -0.0007(18) 0.0077(17) -0.0009(16) C8 0.034(2) 0.040(2) 0.042(2) 0.0015(16) 0.0064(16) 0.0055(16) C9 0.043(2) 0.050(2) 0.033(2) 0.0050(17) 0.0102(17) 0.0148(18) C10 0.047(2) 0.072(3) 0.054(3) 0.013(2) 0.010(2) 0.026(2) C11 0.078(3) 0.052(3) 0.075(3) 0.024(2) 0.019(3) 0.027(2) C12 0.073(3) 0.043(2) 0.062(3) 0.012(2) 0.012(2) 0.004(2) C13 0.051(2) 0.046(2) 0.047(2) 0.0038(18) 0.0079(19) 0.0047(19) C14 0.043(2) 0.037(2) 0.034(2) -0.0002(15) 0.0089(16) 0.0069(16) C15 0.044(2) 0.041(2) 0.042(2) -0.0028(17) 0.0017(18) -0.0003(17) C16 0.046(2) 0.0345(19) 0.0282(19) 0.0019(15) 0.0034(16) 0.0029(16) C17 0.055(2) 0.041(2) 0.039(2) 0.0087(17) 0.0117(19) 0.0050(18) C18 0.076(3) 0.065(3) 0.039(2) 0.009(2) 0.024(2) 0.018(2) C19 0.058(3) 0.087(3) 0.055(3) 0.018(3) 0.026(2) -0.001(3) C20 0.062(3) 0.080(3) 0.053(3) 0.003(2) 0.020(2) -0.018(2) C21 0.062(3) 0.054(3) 0.048(3) 0.000(2) 0.018(2) -0.006(2) C22 0.048(2) 0.042(2) 0.033(2) 0.0041(16) 0.0117(17) -0.0003(17) C23 0.036(2) 0.041(2) 0.043(2) 0.0001(16) 0.0087(17) 0.0088(16) C24 0.035(2) 0.040(2) 0.032(2) 0.0015(15) 0.0057(16) -0.0008(16) C25 0.037(2) 0.046(2) 0.044(2) 0.0049(18) 0.0099(17) -0.0042(17) C26 0.045(2) 0.061(3) 0.051(3) -0.004(2) -0.001(2) -0.011(2) C27 0.068(3) 0.061(3) 0.066(3) -0.020(2) -0.002(2) -0.018(2) C28 0.078(3) 0.045(3) 0.069(3) -0.016(2) 0.007(3) 0.000(2) C29 0.052(3) 0.042(2) 0.071(3) -0.003(2) 0.001(2) 0.0031(19) C30 0.039(2) 0.038(2) 0.043(2) 0.0004(16) 0.0098(17) -0.0055(16) C31 0.046(2) 0.041(2) 0.038(2) 0.0055(16) 0.0080(17) 0.0112(17) C32 0.0350(19) 0.040(2) 0.0253(18) -0.0018(15) 0.0022(15) 0.0022(15) C33 0.0356(19) 0.040(2) 0.034(2) -0.0044(16) 0.0069(16) -0.0023(16) C34 0.052(2) 0.056(3) 0.044(2) -0.0038(19) 0.015(2) -0.007(2) C35 0.048(2) 0.072(3) 0.045(2) -0.009(2) 0.017(2) 0.005(2) C36 0.057(3) 0.068(3) 0.052(3) -0.009(2) 0.008(2) 0.020(2) C37 0.059(3) 0.054(2) 0.039(2) 0.0049(19) 0.013(2) 0.016(2) C38 0.037(2) 0.040(2) 0.033(2) -0.0036(16) 0.0060(16) 0.0012(16) N1 0.0349(16) 0.0341(16) 0.0399(18) 0.0005(13) 0.0083(13) 0.0008(12) N2 0.0345(16) 0.0332(16) 0.0327(16) -0.0004(12) 0.0067(13) 0.0029(12) N3 0.0340(16) 0.0341(17) 0.0441(18) 0.0012(13) 0.0040(14) 0.0053(13) N4 0.0327(16) 0.0479(19) 0.0469(19) 0.0009(15) 0.0067(14) 0.0055(14) N5 0.0441(18) 0.0345(16) 0.0386(18) -0.0027(13) 0.0077(14) -0.0019(13) N6 0.060(2) 0.0400(18) 0.0311(17) -0.0054(13) 0.0071(15) -0.0005(15) N7 0.0354(16) 0.0364(17) 0.0356(17) 0.0001(13) 0.0052(13) 0.0015(13) N8 0.0299(16) 0.0459(19) 0.050(2) -0.0002(15) 0.0036(14) 0.0045(13) N9 0.0412(17) 0.0418(18) 0.0329(17) 0.0023(13) 0.0075(14) 0.0073(14) N10 0.0455(18) 0.0337(17) 0.0400(18) 0.0033(13) 0.0108(14) 0.0011(13) Cl1 0.045(4) 0.061(3) 0.064(3) -0.022(2) 0.009(2) -0.010(3) O1 0.130(8) 0.142(8) 0.076(6) 0.007(5) 0.015(5) 0.021(6) O2 0.064(5) 0.137(10) 0.108(9) -0.022(7) 0.001(7) 0.001(5) O3 0.129(8) 0.091(6) 0.101(8) -0.024(5) 0.044(7) -0.045(5) O4 0.087(15) 0.077(18) 0.15(2) -0.06(2) 0.036(18) -0.021(11) Cl1' 0.056(5) 0.070(7) 0.099(15) -0.016(8) 0.006(6) -0.025(4) O1' 0.071(6) 0.060(7) 0.121(12) -0.033(7) -0.027(7) -0.014(5) O2' 0.070(10) 0.143(12) 0.127(14) -0.004(10) 0.040(11) -0.026(8) O3' 0.119(10) 0.138(11) 0.118(11) 0.026(8) 0.002(8) -0.010(8) O4' 0.10(3) 0.09(4) 0.15(2) -0.04(2) 0.01(2) -0.005(19) Cl2 0.0803(9) 0.0717(9) 0.0955(10) -0.0393(7) 0.0238(8) -0.0178(7) O5 0.186(5) 0.096(3) 0.134(4) -0.011(3) 0.047(3) -0.034(3) O6 0.144(4) 0.154(4) 0.137(4) -0.090(3) 0.066(3) -0.039(3) O7 0.094(3) 0.216(6) 0.156(5) -0.086(4) -0.010(3) -0.031(3) O8 0.179(5) 0.116(4) 0.127(4) -0.054(3) 0.005(3) 0.059(3) C39 0.118(5) 0.106(5) 0.123(5) 0.011(4) 0.043(4) -0.033(4) C40 0.102(5) 0.090(4) 0.098(5) 0.001(4) 0.025(4) -0.009(4) O9 0.073(2) 0.075(2) 0.076(2) -0.0163(18) 0.0172(18) -0.0190(17) _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 2.112(3) . ? Fe1 N7 2.125(3) . ? Fe1 N5 2.152(3) . ? Fe1 N9 2.167(3) . ? Fe1 N2 2.338(3) . ? Fe1 N1 2.343(3) . ? C1 N1 1.501(4) . ? C1 C2 1.532(5) . ? C1 C6 1.546(5) . ? C1 H1 0.9800 . ? C2 C3 1.521(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.504(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.522(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.529(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N2 1.495(4) . ? C6 H6 0.9800 . ? C7 N1 1.492(4) . ? C7 C8 1.501(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.311(4) . ? C8 N4 1.354(4) . ? C9 C10 1.382(5) . ? C9 N4 1.393(5) . ? C9 C14 1.396(5) . ? C10 C11 1.384(6) . ? C10 H10 0.9300 . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 C13 1.360(5) . ? C12 H12 0.9300 . ? C13 C14 1.383(5) . ? C13 H13 0.9300 . ? C14 N3 1.389(4) . ? C15 N1 1.487(4) . ? C15 C16 1.498(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N5 1.328(4) . ? C16 N6 1.339(4) . ? C17 N6 1.378(5) . ? C17 C22 1.386(5) . ? C17 C18 1.409(5) . ? C18 C19 1.378(6) . ? C18 H18 0.9300 . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.383(5) . ? C20 H20 0.9300 . ? C21 C22 1.380(5) . ? C21 H21 0.9300 . ? C22 N5 1.405(4) . ? C23 N2 1.490(4) . ? C23 C24 1.494(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N7 1.319(4) . ? C24 N8 1.339(4) . ? C25 C26 1.373(5) . ? C25 N8 1.384(5) . ? C25 C30 1.406(5) . ? C26 C27 1.370(6) . ? C26 H26 0.9300 . ? C27 C28 1.382(6) . ? C27 H27 0.9300 . ? C28 C29 1.377(5) . ? C28 H28 0.9300 . ? C29 C30 1.384(5) . ? C29 H29 0.9300 . ? C30 N7 1.403(4) . ? C31 C32 1.477(5) . ? C31 N2 1.499(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N9 1.316(4) . ? C32 N10 1.346(4) . ? C33 N10 1.380(4) . ? C33 C34 1.385(5) . ? C33 C38 1.411(5) . ? C34 C35 1.372(6) . ? C34 H34 0.9300 . ? C35 C36 1.391(6) . ? C35 H35 0.9300 . ? C36 C37 1.384(5) . ? C36 H36 0.9300 . ? C37 C38 1.375(5) . ? C37 H37 0.9300 . ? C38 N9 1.398(4) . ? N4 H4 0.8600 . ? N6 H6A 0.8600 . ? N8 H8 0.8600 . ? N10 H10A 0.8600 . ? Cl1 O2 1.42(2) . ? Cl1 O4 1.42(5) . ? Cl1 O1 1.43(3) . ? Cl1 O3 1.44(2) . ? Cl1' O1' 1.42(3) . ? Cl1' O2' 1.42(3) . ? Cl1' O3' 1.44(4) . ? Cl1' O4' 1.45(9) . ? Cl2 O7 1.363(4) . ? Cl2 O5 1.379(5) . ? Cl2 O8 1.407(4) . ? Cl2 O6 1.425(4) . ? C39 C40 1.436(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O9 1.451(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? O9 H9 0.8200 . ? 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 N7 133.64(11) . . ? N3 Fe1 N5 93.54(11) . . ? N7 Fe1 N5 93.31(11) . . ? N3 Fe1 N9 92.09(11) . . ? N7 Fe1 N9 90.63(11) . . ? N5 Fe1 N9 167.78(11) . . ? N3 Fe1 N2 149.10(10) . . ? N7 Fe1 N2 76.27(10) . . ? N5 Fe1 N2 91.74(10) . . ? N9 Fe1 N2 77.96(10) . . ? N3 Fe1 N1 75.23(10) . . ? N7 Fe1 N1 150.88(10) . . ? N5 Fe1 N1 78.93(10) . . ? N9 Fe1 N1 92.06(11) . . ? N2 Fe1 N1 75.97(10) . . ? N1 C1 C2 113.9(3) . . ? N1 C1 C6 108.4(3) . . ? C2 C1 C6 113.8(3) . . ? N1 C1 H1 106.8 . . ? C2 C1 H1 106.8 . . ? C6 C1 H1 106.8 . . ? C3 C2 C1 111.7(3) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 109.4(3) . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C3 C4 C5 109.6(3) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 111.7(3) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C5 114.8(3) . . ? N2 C6 C1 107.7(3) . . ? C5 C6 C1 114.0(3) . . ? N2 C6 H6 106.6 . . ? C5 C6 H6 106.6 . . ? C1 C6 H6 106.6 . . ? N1 C7 C8 106.7(3) . . ? N1 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? N1 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? N3 C8 N4 112.2(3) . . ? N3 C8 C7 122.4(3) . . ? N4 C8 C7 125.3(3) . . ? C10 C9 N4 132.1(4) . . ? C10 C9 C14 122.2(4) . . ? N4 C9 C14 105.5(3) . . ? C9 C10 C11 116.4(4) . . ? C9 C10 H10 121.8 . . ? C11 C10 H10 121.8 . . ? C10 C11 C12 121.2(4) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 122.2(4) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 117.7(4) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C13 C14 N3 131.0(3) . . ? C13 C14 C9 120.2(3) . . ? N3 C14 C9 108.7(3) . . ? N1 C15 C16 111.0(3) . . ? N1 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N1 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N5 C16 N6 112.8(3) . . ? N5 C16 C15 122.8(3) . . ? N6 C16 C15 124.4(3) . . ? N6 C17 C22 105.9(3) . . ? N6 C17 C18 131.9(4) . . ? C22 C17 C18 122.1(4) . . ? C19 C18 C17 115.5(4) . . ? C19 C18 H18 122.3 . . ? C17 C18 H18 122.3 . . ? C18 C19 C20 122.4(4) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C21 121.7(4) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 117.2(4) . . ? C22 C21 H21 121.4 . . ? C20 C21 H21 121.4 . . ? C21 C22 C17 120.9(4) . . ? C21 C22 N5 130.1(3) . . ? C17 C22 N5 109.0(3) . . ? N2 C23 C24 106.3(3) . . ? N2 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? N2 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? N7 C24 N8 112.3(3) . . ? N7 C24 C23 121.6(3) . . ? N8 C24 C23 125.8(3) . . ? C26 C25 N8 133.3(4) . . ? C26 C25 C30 122.1(4) . . ? N8 C25 C30 104.6(3) . . ? C27 C26 C25 116.8(4) . . ? C27 C26 H26 121.6 . . ? C25 C26 H26 121.6 . . ? C26 C27 C28 122.0(4) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C29 C28 C27 121.7(4) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 117.2(4) . . ? C28 C29 H29 121.4 . . ? C30 C29 H29 121.4 . . ? C29 C30 N7 130.9(3) . . ? C29 C30 C25 120.2(3) . . ? N7 C30 C25 108.8(3) . . ? C32 C31 N2 111.8(3) . . ? C32 C31 H31A 109.3 . . ? N2 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? N2 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? N9 C32 N10 112.6(3) . . ? N9 C32 C31 124.2(3) . . ? N10 C32 C31 123.2(3) . . ? N10 C33 C34 132.4(3) . . ? N10 C33 C38 105.4(3) . . ? C34 C33 C38 122.1(3) . . ? C35 C34 C33 116.7(4) . . ? C35 C34 H34 121.6 . . ? C33 C34 H34 121.6 . . ? C34 C35 C36 121.5(4) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 122.0(4) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C38 C37 C36 117.3(4) . . ? C38 C37 H37 121.4 . . ? C36 C37 H37 121.4 . . ? C37 C38 N9 131.5(3) . . ? C37 C38 C33 120.3(3) . . ? N9 C38 C33 108.2(3) . . ? C15 N1 C7 110.3(3) . . ? C15 N1 C1 114.9(3) . . ? C7 N1 C1 112.0(3) . . ? C15 N1 Fe1 106.2(2) . . ? C7 N1 Fe1 103.9(2) . . ? C1 N1 Fe1 108.77(19) . . ? C23 N2 C6 113.1(3) . . ? C23 N2 C31 110.3(3) . . ? C6 N2 C31 113.3(3) . . ? C23 N2 Fe1 102.80(19) . . ? C6 N2 Fe1 108.72(18) . . ? C31 N2 Fe1 107.98(19) . . ? C8 N3 C14 106.5(3) . . ? C8 N3 Fe1 114.6(2) . . ? C14 N3 Fe1 138.9(2) . . ? C8 N4 C9 107.1(3) . . ? C8 N4 H4 126.5 . . ? C9 N4 H4 126.5 . . ? C16 N5 C22 104.7(3) . . ? C16 N5 Fe1 112.7(2) . . ? C22 N5 Fe1 137.9(2) . . ? C16 N6 C17 107.6(3) . . ? C16 N6 H6A 126.2 . . ? C17 N6 H6A 126.2 . . ? C24 N7 C30 105.6(3) . . ? C24 N7 Fe1 113.5(2) . . ? C30 N7 Fe1 138.2(2) . . ? C24 N8 C25 108.7(3) . . ? C24 N8 H8 125.7 . . ? C25 N8 H8 125.7 . . ? C32 N9 C38 106.0(3) . . ? C32 N9 Fe1 113.9(2) . . ? C38 N9 Fe1 138.3(2) . . ? C32 N10 C33 107.8(3) . . ? C32 N10 H10A 126.1 . . ? C33 N10 H10A 126.1 . . ? O2 Cl1 O4 110(3) . . ? O2 Cl1 O1 110.7(14) . . ? O4 Cl1 O1 113(4) . . ? O2 Cl1 O3 109.1(16) . . ? O4 Cl1 O3 107(3) . . ? O1 Cl1 O3 107.0(16) . . ? O1' Cl1' O2' 113(3) . . ? O1' Cl1' O3' 110(2) . . ? O2' Cl1' O3' 108(2) . . ? O1' Cl1' O4' 108(5) . . ? O2' Cl1' O4' 108(5) . . ? O3' Cl1' O4' 110(5) . . ? O7 Cl2 O5 114.7(4) . . ? O7 Cl2 O8 108.4(3) . . ? O5 Cl2 O8 107.6(4) . . ? O7 Cl2 O6 111.8(3) . . ? O5 Cl2 O6 106.2(3) . . ? O8 Cl2 O6 107.8(3) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C39 C40 O9 114.2(5) . . ? C39 C40 H40A 108.7 . . ? O9 C40 H40A 108.7 . . ? C39 C40 H40B 108.7 . . ? O9 C40 H40B 108.7 . . ? H40A C40 H40B 107.6 . . ? C40 O9 H9 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.475 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.067 # Attachment '755333.cif' data_FeIII(OEt)(HCTB)(ClO4)3.EtOH _database_code_depnum_ccdc_archive 'CCDC 755333' #TrackingRef '755333.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 Cl3 Fe N10 O14' _chemical_formula_weight 1081.12 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 14.3060(10) _cell_length_b 24.6698(17) _cell_length_c 14.8559(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.7840(10) _cell_angle_gamma 90.00 _cell_volume 5069.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5827 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 20.42 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 25366 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8902 _reflns_number_gt 6308 _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^)+(0.1369P)^2^+0.8567P] 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 8902 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.79104(4) 0.14487(2) 0.79919(4) 0.0451(2) Uani 1 1 d . A . O1 O 0.8539(2) 0.09034(12) 0.8686(2) 0.0684(8) Uani 1 1 d . . . C39 C 0.869(2) 0.0432(19) 0.921(3) 0.122(10) Uani 0.52(2) 1 d P A 1 H39A H 0.9366 0.0411 0.9542 0.146 Uiso 0.52(2) 1 calc PR A 1 H39B H 0.8546 0.0123 0.8790 0.146 Uiso 0.52(2) 1 calc PR A 1 C40 C 0.8074(14) 0.0405(7) 0.9888(15) 0.139(8) Uani 0.52(2) 1 d P A 1 H40A H 0.7948 0.0766 1.0071 0.209 Uiso 0.52(2) 1 calc PR A 1 H40B H 0.8408 0.0204 1.0428 0.209 Uiso 0.52(2) 1 calc PR A 1 H40C H 0.7474 0.0229 0.9602 0.209 Uiso 0.52(2) 1 calc PR A 1 C39' C 0.824(2) 0.0438(19) 0.911(3) 0.103(8) Uani 0.48(2) 1 d P A 2 H39C H 0.7913 0.0183 0.8630 0.123 Uiso 0.48(2) 1 calc PR A 2 H39D H 0.7787 0.0542 0.9467 0.123 Uiso 0.48(2) 1 calc PR A 2 C40' C 0.9123(16) 0.0180(9) 0.9730(15) 0.143(8) Uani 0.48(2) 1 d P A 2 H40D H 0.9298 -0.0135 0.9430 0.215 Uiso 0.48(2) 1 calc PR A 2 H40E H 0.8990 0.0076 1.0308 0.215 Uiso 0.48(2) 1 calc PR A 2 H40F H 0.9648 0.0434 0.9851 0.215 Uiso 0.48(2) 1 calc PR A 2 N1 N 0.7245(2) 0.21442(12) 0.6994(2) 0.0477(8) Uani 1 1 d . . . N2 N 0.7739(2) 0.10738(12) 0.6496(2) 0.0437(7) Uani 1 1 d . . . N3 N 0.6531(2) 0.10752(12) 0.7681(2) 0.0437(7) Uani 1 1 d . . . N4 N 0.5590(2) 0.04334(14) 0.6908(2) 0.0555(9) Uani 1 1 d . . . H4A H 0.5397 0.0171 0.6524 0.067 Uiso 1 1 calc R A . N5 N 0.8719(2) 0.00332(13) 0.5563(2) 0.0496(8) Uani 1 1 d . A . H5N H 0.8766 -0.0208 0.5984 0.059 Uiso 1 1 d R . . N6 N 0.8757(2) 0.07409(13) 0.4719(2) 0.0530(8) Uani 1 1 d . A . H6N H 0.8782 0.1075 0.4574 0.064 Uiso 1 1 d R . . N7 N 0.7670(2) 0.20468(12) 0.8896(2) 0.0483(8) Uani 1 1 d . . . N8 N 0.7130(3) 0.28621(13) 0.9091(2) 0.0571(9) Uani 1 1 d . . . H8A H 0.6827 0.3165 0.8966 0.069 Uiso 1 1 calc R A . N9 N 0.9122(2) 0.18385(14) 0.7803(2) 0.0551(8) Uani 1 1 d . . . N10 N 0.9835(3) 0.24657(18) 0.7154(3) 0.0743(11) Uani 1 1 d . . . H10A H 0.9906 0.2741 0.6822 0.089 Uiso 1 1 calc R A . C1 C 0.6645(3) 0.18963(15) 0.6116(2) 0.0472(9) Uani 1 1 d . A . H1A H 0.6116 0.1705 0.6288 0.057 Uiso 1 1 calc R . . C2 C 0.6168(3) 0.23099(18) 0.5369(3) 0.0623(11) Uani 1 1 d . . . H2A H 0.5799 0.2569 0.5629 0.075 Uiso 1 1 calc R A . H2B H 0.6661 0.2506 0.5160 0.075 Uiso 1 1 calc R . . C3 C 0.5511(3) 0.2021(2) 0.4560(3) 0.0657(12) Uani 1 1 d . A . H3A H 0.4997 0.1843 0.4764 0.079 Uiso 1 1 calc R . . H3B H 0.5219 0.2283 0.4084 0.079 Uiso 1 1 calc R . . C4 C 0.6057(4) 0.1611(2) 0.4158(3) 0.0693(13) Uani 1 1 d . . . H4B H 0.6548 0.1792 0.3922 0.083 Uiso 1 1 calc R A . H4C H 0.5619 0.1428 0.3641 0.083 Uiso 1 1 calc R . . C5 C 0.6538(3) 0.11923(18) 0.4895(3) 0.0540(10) Uani 1 1 d . A . H5B H 0.6903 0.0937 0.4623 0.065 Uiso 1 1 calc R . . H5C H 0.6043 0.0992 0.5095 0.065 Uiso 1 1 calc R . . C6 C 0.7219(3) 0.14641(15) 0.5744(2) 0.0457(9) Uani 1 1 d . A . H6B H 0.7716 0.1654 0.5519 0.055 Uiso 1 1 calc R . . C7 C 0.7188(3) 0.05700(15) 0.6565(3) 0.0456(9) Uani 1 1 d . A . H7A H 0.6903 0.0427 0.5948 0.055 Uiso 1 1 calc R . . H7B H 0.7621 0.0298 0.6916 0.055 Uiso 1 1 calc R . . C8 C 0.6420(3) 0.06949(14) 0.7037(2) 0.0431(8) Uani 1 1 d . A . C9 C 0.5088(3) 0.06566(18) 0.7500(3) 0.0594(11) Uani 1 1 d . A . C10 C 0.4199(4) 0.0540(3) 0.7638(4) 0.0893(17) Uani 1 1 d . . . H10B H 0.3806 0.0269 0.7306 0.107 Uiso 1 1 calc R A . C11 C 0.3921(4) 0.0849(3) 0.8302(4) 0.0948(19) Uani 1 1 d . A . H11A H 0.3315 0.0793 0.8407 0.114 Uiso 1 1 calc R . . C12 C 0.4525(4) 0.1242(2) 0.8814(4) 0.0809(15) Uani 1 1 d . . . H12A H 0.4322 0.1431 0.9272 0.097 Uiso 1 1 calc R A . C13 C 0.5404(3) 0.13610(19) 0.8667(3) 0.0626(11) Uani 1 1 d . A . H13A H 0.5796 0.1632 0.9001 0.075 Uiso 1 1 calc R . . C14 C 0.5691(3) 0.10574(16) 0.7990(3) 0.0489(9) Uani 1 1 d . A . C15 C 0.8712(3) 0.09211(16) 0.6387(3) 0.0503(9) Uani 1 1 d . A . H15A H 0.9056 0.0732 0.6946 0.060 Uiso 1 1 calc R . . H15B H 0.9067 0.1251 0.6346 0.060 Uiso 1 1 calc R . . C16 C 0.8729(3) 0.05708(15) 0.5558(3) 0.0466(9) Uani 1 1 d . . . C17 C 0.8763(3) 0.03027(17) 0.4156(3) 0.0517(10) Uani 1 1 d . . . C18 C 0.8805(3) 0.0260(2) 0.3233(3) 0.0721(13) Uani 1 1 d . A . H18A H 0.8828 0.0564 0.2869 0.087 Uiso 1 1 calc R . . C19 C 0.8812(4) -0.0260(3) 0.2889(4) 0.0853(17) Uani 1 1 d . . . H19A H 0.8835 -0.0306 0.2274 0.102 Uiso 1 1 calc R A . C20 C 0.8785(3) -0.0705(2) 0.3418(4) 0.0769(15) Uani 1 1 d . A . H20A H 0.8780 -0.1046 0.3148 0.092 Uiso 1 1 calc R . . C21 C 0.8764(3) -0.06736(18) 0.4330(4) 0.0690(13) Uani 1 1 d . . . H21A H 0.8767 -0.0981 0.4692 0.083 Uiso 1 1 calc R A . C22 C 0.8740(3) -0.01534(16) 0.4687(3) 0.0498(9) Uani 1 1 d . A . C23 C 0.6633(3) 0.24528(17) 0.7493(3) 0.0562(10) Uani 1 1 d . A . H23A H 0.6529 0.2819 0.7250 0.067 Uiso 1 1 calc R . . H23B H 0.6008 0.2278 0.7405 0.067 Uiso 1 1 calc R . . C24 C 0.7140(3) 0.24651(15) 0.8492(3) 0.0500(9) Uani 1 1 d . A . C25 C 0.7703(3) 0.27009(16) 0.9964(3) 0.0526(10) Uani 1 1 d . A . C26 C 0.7950(4) 0.29548(18) 1.0828(3) 0.0654(12) Uani 1 1 d . . . H26A H 0.7722 0.3299 1.0916 0.078 Uiso 1 1 calc R A . C27 C 0.8541(4) 0.2676(2) 1.1538(3) 0.0694(12) Uani 1 1 d . A . H27A H 0.8714 0.2832 1.2128 0.083 Uiso 1 1 calc R . . C28 C 0.8897(3) 0.2163(2) 1.1406(3) 0.0657(12) Uani 1 1 d . . . H28A H 0.9305 0.1986 1.1908 0.079 Uiso 1 1 calc R A . C29 C 0.8660(3) 0.19144(18) 1.0554(3) 0.0585(10) Uani 1 1 d . A . H29A H 0.8904 0.1575 1.0466 0.070 Uiso 1 1 calc R . . C30 C 0.8045(3) 0.21879(15) 0.9832(3) 0.0469(9) Uani 1 1 d . A . C31 C 0.8033(3) 0.24998(17) 0.6831(3) 0.0629(11) Uani 1 1 d . A . H31A H 0.7953 0.2544 0.6167 0.075 Uiso 1 1 calc R . . H31B H 0.7988 0.2855 0.7097 0.075 Uiso 1 1 calc R . . C32 C 0.8990(3) 0.22651(18) 0.7253(3) 0.0576(11) Uani 1 1 d . A . C33 C 1.0559(4) 0.2150(2) 0.7680(4) 0.0768(15) Uani 1 1 d . A . C34 C 1.1573(4) 0.2185(3) 0.7873(6) 0.105(2) Uani 1 1 d . . . H34A H 1.1872 0.2447 0.7592 0.126 Uiso 1 1 calc R A . C35 C 1.2079(5) 0.1837(3) 0.8460(6) 0.106(2) Uani 1 1 d . A . H35A H 1.2750 0.1856 0.8597 0.127 Uiso 1 1 calc R . . C36 C 1.1668(5) 0.1444(3) 0.8885(5) 0.106(2) Uani 1 1 d . . . H36A H 1.2067 0.1207 0.9299 0.127 Uiso 1 1 calc R A . C37 C 1.0638(4) 0.1388(2) 0.8710(4) 0.0869(17) Uani 1 1 d . A . H37A H 1.0350 0.1120 0.8989 0.104 Uiso 1 1 calc R . . C38 C 1.0116(3) 0.17552(19) 0.8107(3) 0.0641(12) Uani 1 1 d . A . Cl1 Cl 0.94212(9) 0.21561(5) 0.45610(8) 0.0690(3) Uani 1 1 d . . . O4 O 0.8977(4) 0.25666(18) 0.4978(3) 0.1167(15) Uani 1 1 d . . . O5 O 0.9874(4) 0.2373(2) 0.3926(4) 0.1281(17) Uani 1 1 d . . . O6 O 0.8667(3) 0.18029(18) 0.4049(4) 0.1192(15) Uani 1 1 d . . . O7 O 1.0013(4) 0.18249(19) 0.5234(4) 0.1333(18) Uani 1 1 d . . . Cl2 Cl 0.37322(8) 0.06809(5) 0.48109(9) 0.0665(3) Uani 1 1 d . . . O8 O 0.4255(3) 0.10832(14) 0.5413(3) 0.0880(11) Uani 1 1 d . . . O9 O 0.4206(4) 0.05655(19) 0.4106(4) 0.1236(17) Uani 1 1 d . . . O10 O 0.2783(3) 0.08634(18) 0.4413(3) 0.1015(12) Uani 1 1 d . . . O11 O 0.3690(3) 0.01944(15) 0.5327(3) 0.1021(13) Uani 1 1 d . . . Cl3 Cl 0.08161(10) 0.09264(5) 0.23765(9) 0.0774(4) Uani 1 1 d . . . O12 O 0.0751(3) 0.12191(19) 0.3182(3) 0.1147(15) Uani 1 1 d . . . O13 O 0.1441(5) 0.1206(2) 0.1966(5) 0.173(3) Uani 1 1 d . . . O14 O 0.1147(3) 0.03942(13) 0.2635(2) 0.0831(10) Uani 1 1 d . . . O15 O -0.0117(4) 0.0888(2) 0.1762(3) 0.1296(18) Uani 1 1 d . . . O1M O 0.8529(13) 0.3805(7) 0.7422(12) 0.176(7) Uani 0.435(7) 1 d P B 1 H1M H 0.7957 0.3867 0.7100 0.263 Uiso 0.435(7) 1 d PR B 1 C1M C 0.921(2) 0.4052(14) 0.707(2) 0.178(10) Uani 0.435(7) 1 d P B 1 H1MA H 0.9688 0.3789 0.6995 0.213 Uiso 0.435(7) 1 calc PR B 1 H1MB H 0.9540 0.4329 0.7504 0.213 Uiso 0.435(7) 1 calc PR B 1 C2M C 0.874(2) 0.4299(13) 0.617(2) 0.214(13) Uani 0.435(7) 1 d P B 1 H2MA H 0.8126 0.4445 0.6199 0.321 Uiso 0.435(7) 1 calc PR B 1 H2MB H 0.8647 0.4029 0.5694 0.321 Uiso 0.435(7) 1 calc PR B 1 H2MC H 0.9141 0.4585 0.6041 0.321 Uiso 0.435(7) 1 calc PR B 1 O2M O 0.0459(7) 0.3393(4) 0.6533(6) 0.132(4) Uani 0.565(7) 1 d P B 2 H2M H 0.0068 0.3658 0.6474 0.197 Uiso 0.565(7) 1 d PR B 2 C3M C 0.1321(11) 0.3483(7) 0.6280(10) 0.127(5) Uani 0.565(7) 1 d P B 2 H3MA H 0.1184 0.3557 0.5618 0.153 Uiso 0.565(7) 1 calc PR B 2 H3MB H 0.1727 0.3163 0.6412 0.153 Uiso 0.565(7) 1 calc PR B 2 C4M C 0.1811(15) 0.3933(9) 0.6790(14) 0.187(8) Uani 0.565(7) 1 d P B 2 H4MA H 0.2403 0.3997 0.6616 0.280 Uiso 0.565(7) 1 calc PR B 2 H4MB H 0.1952 0.3856 0.7445 0.280 Uiso 0.565(7) 1 calc PR B 2 H4MC H 0.1408 0.4249 0.6655 0.280 Uiso 0.565(7) 1 calc PR B 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 Fe1 0.0486(3) 0.0338(3) 0.0478(3) -0.0052(2) 0.0032(2) 0.0062(2) O1 0.071(2) 0.0458(17) 0.075(2) 0.0025(15) -0.0054(16) 0.0173(15) C39 0.14(2) 0.107(14) 0.109(15) 0.026(11) 0.01(2) 0.03(2) C40 0.157(17) 0.129(14) 0.127(16) 0.017(11) 0.028(12) -0.001(11) C39' 0.11(2) 0.095(13) 0.096(15) 0.021(10) 0.023(18) 0.027(19) C40' 0.157(19) 0.128(16) 0.124(14) 0.032(13) 0.000(13) 0.025(13) N1 0.0565(19) 0.0336(17) 0.0506(18) -0.0016(13) 0.0091(15) 0.0050(13) N2 0.0462(17) 0.0356(16) 0.0492(17) -0.0050(13) 0.0120(14) 0.0012(13) N3 0.0502(18) 0.0376(17) 0.0424(16) -0.0021(13) 0.0098(14) 0.0052(13) N4 0.055(2) 0.053(2) 0.058(2) -0.0199(16) 0.0140(16) -0.0074(16) N5 0.0563(19) 0.0371(18) 0.058(2) -0.0020(14) 0.0200(16) 0.0034(14) N6 0.061(2) 0.0398(19) 0.063(2) -0.0027(15) 0.0232(17) -0.0016(15) N7 0.0568(19) 0.0350(17) 0.0488(18) -0.0049(14) 0.0056(15) 0.0066(14) N8 0.077(2) 0.0379(18) 0.055(2) -0.0032(15) 0.0154(17) 0.0172(16) N9 0.0488(19) 0.046(2) 0.068(2) -0.0175(17) 0.0116(16) -0.0028(15) N10 0.076(3) 0.071(3) 0.078(3) -0.022(2) 0.025(2) -0.018(2) C1 0.054(2) 0.042(2) 0.042(2) 0.0030(16) 0.0061(17) 0.0005(17) C2 0.079(3) 0.053(3) 0.051(2) 0.0119(19) 0.011(2) 0.012(2) C3 0.073(3) 0.066(3) 0.050(2) 0.020(2) 0.000(2) 0.005(2) C4 0.079(3) 0.079(3) 0.042(2) 0.005(2) 0.001(2) -0.008(3) C5 0.058(2) 0.055(2) 0.045(2) -0.0065(18) 0.0058(18) -0.0033(19) C6 0.049(2) 0.046(2) 0.041(2) 0.0012(16) 0.0081(16) -0.0031(16) C7 0.049(2) 0.037(2) 0.050(2) -0.0042(16) 0.0106(17) 0.0023(16) C8 0.049(2) 0.0355(19) 0.0429(19) -0.0002(15) 0.0090(16) 0.0038(16) C9 0.058(3) 0.060(3) 0.060(3) -0.013(2) 0.015(2) 0.000(2) C10 0.062(3) 0.097(4) 0.114(4) -0.039(4) 0.033(3) -0.020(3) C11 0.064(3) 0.116(5) 0.118(5) -0.039(4) 0.049(3) -0.013(3) C12 0.072(3) 0.091(4) 0.090(4) -0.023(3) 0.038(3) 0.008(3) C13 0.061(3) 0.062(3) 0.065(3) -0.016(2) 0.017(2) 0.009(2) C14 0.051(2) 0.048(2) 0.047(2) -0.0001(17) 0.0109(17) 0.0075(17) C15 0.046(2) 0.043(2) 0.062(2) -0.0141(18) 0.0139(18) -0.0008(17) C16 0.040(2) 0.042(2) 0.056(2) -0.0083(17) 0.0104(17) -0.0001(16) C17 0.046(2) 0.057(3) 0.054(2) -0.0093(19) 0.0158(18) 0.0019(18) C18 0.070(3) 0.090(4) 0.058(3) -0.005(2) 0.019(2) 0.011(3) C19 0.078(3) 0.112(5) 0.066(3) -0.034(3) 0.018(3) 0.014(3) C20 0.067(3) 0.080(4) 0.086(4) -0.042(3) 0.022(3) -0.003(3) C21 0.063(3) 0.045(3) 0.103(4) -0.022(2) 0.029(3) -0.002(2) C22 0.043(2) 0.046(2) 0.060(2) -0.0141(19) 0.0127(17) -0.0002(16) C23 0.070(3) 0.043(2) 0.051(2) 0.0008(18) 0.0087(19) 0.0208(19) C24 0.059(2) 0.037(2) 0.053(2) -0.0028(17) 0.0118(18) 0.0072(17) C25 0.062(2) 0.044(2) 0.053(2) -0.0058(18) 0.0166(19) 0.0018(18) C26 0.085(3) 0.046(2) 0.065(3) -0.011(2) 0.019(2) 0.003(2) C27 0.085(3) 0.070(3) 0.052(3) -0.012(2) 0.013(2) -0.006(3) C28 0.067(3) 0.070(3) 0.054(3) -0.003(2) 0.003(2) 0.005(2) C29 0.063(3) 0.052(2) 0.056(2) -0.0043(19) 0.005(2) 0.009(2) C30 0.052(2) 0.040(2) 0.049(2) -0.0051(16) 0.0119(17) 0.0026(16) C31 0.078(3) 0.041(2) 0.068(3) -0.005(2) 0.014(2) -0.010(2) C32 0.057(3) 0.052(3) 0.065(3) -0.021(2) 0.018(2) -0.013(2) C33 0.058(3) 0.075(4) 0.099(4) -0.051(3) 0.024(3) -0.015(3) C34 0.072(4) 0.094(5) 0.156(6) -0.057(5) 0.043(4) -0.019(3) C35 0.062(4) 0.099(5) 0.148(6) -0.043(5) 0.010(4) -0.001(4) C36 0.079(4) 0.101(5) 0.122(5) -0.044(4) -0.004(4) 0.035(4) C37 0.060(3) 0.080(4) 0.107(4) -0.039(3) -0.004(3) 0.014(3) C38 0.052(3) 0.061(3) 0.074(3) -0.034(2) 0.007(2) 0.006(2) Cl1 0.0814(8) 0.0520(7) 0.0769(8) 0.0084(5) 0.0259(6) 0.0040(6) O4 0.163(4) 0.097(3) 0.097(3) 0.009(2) 0.046(3) 0.051(3) O5 0.149(4) 0.097(3) 0.166(4) 0.006(3) 0.090(4) -0.022(3) O6 0.102(3) 0.087(3) 0.149(4) 0.010(3) -0.004(3) -0.028(2) O7 0.157(4) 0.084(3) 0.131(4) 0.003(3) -0.014(3) 0.036(3) Cl2 0.0580(7) 0.0538(7) 0.0831(8) -0.0139(5) 0.0097(6) -0.0045(5) O8 0.086(2) 0.061(2) 0.110(3) -0.0241(19) 0.011(2) -0.0177(18) O9 0.154(4) 0.100(3) 0.143(4) -0.040(3) 0.086(3) -0.019(3) O10 0.064(2) 0.103(3) 0.122(3) 0.013(2) -0.004(2) -0.003(2) O11 0.137(3) 0.057(2) 0.093(3) -0.0017(19) -0.006(2) -0.014(2) Cl3 0.0942(9) 0.0488(7) 0.0851(9) 0.0097(6) 0.0153(7) 0.0107(6) O12 0.107(3) 0.089(3) 0.137(4) -0.048(3) 0.010(3) 0.013(2) O13 0.206(6) 0.102(4) 0.249(7) 0.046(5) 0.129(5) -0.001(4) O14 0.119(3) 0.0502(19) 0.078(2) 0.0095(16) 0.021(2) 0.0257(18) O15 0.127(4) 0.123(4) 0.103(3) 0.016(3) -0.035(3) 0.024(3) O1M 0.178(15) 0.167(15) 0.159(13) -0.061(12) 0.001(11) -0.040(12) C1M 0.19(3) 0.19(3) 0.16(2) -0.02(2) 0.06(2) 0.02(2) C2M 0.18(3) 0.22(3) 0.22(3) -0.02(3) 0.01(2) 0.03(2) O2M 0.151(8) 0.112(7) 0.130(7) 0.010(5) 0.031(6) -0.065(6) C3M 0.131(12) 0.148(14) 0.116(10) 0.002(9) 0.055(9) 0.008(10) C4M 0.180(18) 0.19(2) 0.196(19) -0.005(17) 0.061(15) -0.012(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 O1 1.791(3) . ? Fe1 N9 2.063(3) . ? Fe1 N7 2.082(3) . ? Fe1 N3 2.120(3) . ? Fe1 N1 2.308(3) . ? Fe1 N2 2.362(3) . ? O1 C39 1.38(4) . ? O1 C39' 1.43(5) . ? C39 C40 1.51(4) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C39' C40' 1.51(4) . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? C40' H40D 0.9600 . ? C40' H40E 0.9600 . ? C40' H40F 0.9600 . ? N1 C23 1.492(5) . ? N1 C31 1.497(5) . ? N1 C1 1.497(5) . ? N2 C7 1.489(5) . ? N2 C15 1.490(5) . ? N2 C6 1.518(5) . ? N3 C8 1.320(5) . ? N3 C14 1.393(5) . ? N4 C8 1.322(5) . ? N4 C9 1.384(5) . ? N4 H4A 0.8600 . ? N5 C16 1.326(5) . ? N5 C22 1.387(5) . ? N5 H5N 0.8530 . ? N6 C16 1.324(5) . ? N6 C17 1.369(5) . ? N6 H6N 0.8553 . ? N7 C24 1.330(5) . ? N7 C30 1.400(5) . ? N8 C24 1.326(5) . ? N8 C25 1.403(5) . ? N8 H8A 0.8600 . ? N9 C32 1.316(6) . ? N9 C38 1.392(5) . ? N10 C32 1.348(5) . ? N10 C33 1.370(7) . ? N10 H10A 0.8600 . ? C1 C6 1.532(5) . ? C1 C2 1.533(5) . ? C1 H1A 0.9800 . ? C2 C3 1.503(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.492(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.535(6) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.536(5) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6B 0.9800 . ? C7 C8 1.479(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.369(7) . ? C9 C14 1.390(6) . ? C10 C11 1.383(7) . ? C10 H10B 0.9300 . ? C11 C12 1.389(8) . ? C11 H11A 0.9300 . ? C12 C13 1.363(7) . ? C12 H12A 0.9300 . ? C13 C14 1.396(5) . ? C13 H13A 0.9300 . ? C15 C16 1.510(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C22 1.379(6) . ? C17 C18 1.391(6) . ? C18 C19 1.382(8) . ? C18 H18A 0.9300 . ? C19 C20 1.357(8) . ? C19 H19A 0.9300 . ? C20 C21 1.365(7) . ? C20 H20A 0.9300 . ? C21 C22 1.392(6) . ? C21 H21A 0.9300 . ? C23 C24 1.477(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C30 1.389(5) . ? C25 C26 1.390(6) . ? C26 C27 1.358(6) . ? C26 H26A 0.9300 . ? C27 C28 1.399(7) . ? C27 H27A 0.9300 . ? C28 C29 1.368(6) . ? C28 H28A 0.9300 . ? C29 C30 1.378(5) . ? C29 H29A 0.9300 . ? C31 C32 1.471(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 C38 1.400(7) . ? C33 C34 1.408(7) . ? C34 C35 1.304(10) . ? C34 H34A 0.9300 . ? C35 C36 1.368(10) . ? C35 H35A 0.9300 . ? C36 C37 1.437(8) . ? C36 H36A 0.9300 . ? C37 C38 1.357(7) . ? C37 H37A 0.9300 . ? Cl1 O5 1.381(4) . ? Cl1 O7 1.397(4) . ? Cl1 O4 1.419(4) . ? Cl1 O6 1.443(4) . ? Cl2 O10 1.409(4) . ? Cl2 O9 1.415(4) . ? Cl2 O8 1.415(3) . ? Cl2 O11 1.434(4) . ? Cl3 O13 1.387(5) . ? Cl3 O15 1.415(5) . ? Cl3 O14 1.415(3) . ? Cl3 O12 1.421(4) . ? O1M C1M 1.36(3) . ? O1M H1M 0.8499 . ? C1M C2M 1.47(3) . ? C1M H1MA 0.9700 . ? C1M H1MB 0.9700 . ? C2M H2MA 0.9600 . ? C2M H2MB 0.9600 . ? C2M H2MC 0.9600 . ? O2M C3M 1.396(15) . ? O2M H2M 0.8501 . ? C3M C4M 1.42(2) . ? C3M H3MA 0.9700 . ? C3M H3MB 0.9700 . ? C4M H4MA 0.9600 . ? C4M H4MB 0.9600 . ? C4M H4MC 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N9 96.47(15) . . ? O1 Fe1 N7 107.57(13) . . ? N9 Fe1 N7 92.31(13) . . ? O1 Fe1 N3 95.84(14) . . ? N9 Fe1 N3 160.20(13) . . ? N7 Fe1 N3 98.67(12) . . ? O1 Fe1 N1 172.87(14) . . ? N9 Fe1 N1 77.84(13) . . ? N7 Fe1 N1 77.21(11) . . ? N3 Fe1 N1 88.54(11) . . ? O1 Fe1 N2 99.46(12) . . ? N9 Fe1 N2 86.76(12) . . ? N7 Fe1 N2 152.89(11) . . ? N3 Fe1 N2 75.95(11) . . ? N1 Fe1 N2 76.11(10) . . ? C39 O1 C39' 25.8(15) . . ? C39 O1 Fe1 159.7(13) . . ? C39' O1 Fe1 133.9(11) . . ? O1 C39 C40 112(2) . . ? O1 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O1 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? O1 C39' C40' 108(2) . . ? O1 C39' H39C 110.1 . . ? C40' C39' H39C 110.1 . . ? O1 C39' H39D 110.1 . . ? C40' C39' H39D 110.1 . . ? H39C C39' H39D 108.5 . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? C23 N1 C31 110.1(3) . . ? C23 N1 C1 111.3(3) . . ? C31 N1 C1 112.7(3) . . ? C23 N1 Fe1 105.0(2) . . ? C31 N1 Fe1 109.6(2) . . ? C1 N1 Fe1 107.9(2) . . ? C7 N2 C15 108.8(3) . . ? C7 N2 C6 114.3(3) . . ? C15 N2 C6 112.1(3) . . ? C7 N2 Fe1 101.0(2) . . ? C15 N2 Fe1 109.0(2) . . ? C6 N2 Fe1 111.0(2) . . ? C8 N3 C14 105.3(3) . . ? C8 N3 Fe1 113.5(2) . . ? C14 N3 Fe1 140.9(2) . . ? C8 N4 C9 107.8(3) . . ? C8 N4 H4A 126.1 . . ? C9 N4 H4A 126.1 . . ? C16 N5 C22 108.9(3) . . ? C16 N5 H5N 134.5 . . ? C22 N5 H5N 116.1 . . ? C16 N6 C17 109.4(3) . . ? C16 N6 H6N 123.8 . . ? C17 N6 H6N 126.9 . . ? C24 N7 C30 106.6(3) . . ? C24 N7 Fe1 115.3(2) . . ? C30 N7 Fe1 137.1(2) . . ? C24 N8 C25 107.9(3) . . ? C24 N8 H8A 126.0 . . ? C25 N8 H8A 126.0 . . ? C32 N9 C38 107.0(4) . . ? C32 N9 Fe1 117.7(3) . . ? C38 N9 Fe1 135.3(3) . . ? C32 N10 C33 107.3(4) . . ? C32 N10 H10A 126.3 . . ? C33 N10 H10A 126.3 . . ? N1 C1 C6 111.0(3) . . ? N1 C1 C2 114.1(3) . . ? C6 C1 C2 112.5(3) . . ? N1 C1 H1A 106.2 . . ? C6 C1 H1A 106.2 . . ? C2 C1 H1A 106.2 . . ? C3 C2 C1 109.6(4) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 110.9(4) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 110.9(4) . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? C5 C4 H4C 109.5 . . ? H4B C4 H4C 108.0 . . ? C4 C5 C6 111.5(3) . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5C 109.3 . . ? C6 C5 H5C 109.3 . . ? H5B C5 H5C 108.0 . . ? N2 C6 C1 112.5(3) . . ? N2 C6 C5 114.6(3) . . ? C1 C6 C5 108.3(3) . . ? N2 C6 H6B 107.0 . . ? C1 C6 H6B 107.0 . . ? C5 C6 H6B 107.0 . . ? C8 C7 N2 109.2(3) . . ? C8 C7 H7A 109.8 . . ? N2 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? N2 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N3 C8 N4 112.9(3) . . ? N3 C8 C7 121.7(3) . . ? N4 C8 C7 125.3(3) . . ? C10 C9 N4 131.6(4) . . ? C10 C9 C14 123.1(4) . . ? N4 C9 C14 105.3(4) . . ? C9 C10 C11 116.0(5) . . ? C9 C10 H10B 122.0 . . ? C11 C10 H10B 122.0 . . ? C10 C11 C12 121.6(5) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C13 C12 C11 122.2(4) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? C12 C13 C14 116.9(4) . . ? C12 C13 H13A 121.5 . . ? C14 C13 H13A 121.5 . . ? C9 C14 N3 108.7(3) . . ? C9 C14 C13 120.2(4) . . ? N3 C14 C13 131.1(4) . . ? N2 C15 C16 116.2(3) . . ? N2 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? N2 C15 H15B 108.2 . . ? C16 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? N6 C16 N5 109.0(3) . . ? N6 C16 C15 126.6(4) . . ? N5 C16 C15 124.4(4) . . ? N6 C17 C22 106.8(3) . . ? N6 C17 C18 132.1(4) . . ? C22 C17 C18 121.0(4) . . ? C19 C18 C17 116.1(5) . . ? C19 C18 H18A 121.9 . . ? C17 C18 H18A 121.9 . . ? C20 C19 C18 122.2(5) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C19 C20 C21 122.6(5) . . ? C19 C20 H20A 118.7 . . ? C21 C20 H20A 118.7 . . ? C20 C21 C22 116.1(5) . . ? C20 C21 H21A 121.9 . . ? C22 C21 H21A 121.9 . . ? C17 C22 N5 106.0(3) . . ? C17 C22 C21 121.8(4) . . ? N5 C22 C21 132.2(4) . . ? C24 C23 N1 108.0(3) . . ? C24 C23 H23A 110.1 . . ? N1 C23 H23A 110.1 . . ? C24 C23 H23B 110.1 . . ? N1 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N8 C24 N7 111.9(3) . . ? N8 C24 C23 127.1(3) . . ? N7 C24 C23 121.0(3) . . ? C30 C25 C26 121.7(4) . . ? C30 C25 N8 105.7(3) . . ? C26 C25 N8 132.6(4) . . ? C27 C26 C25 116.8(4) . . ? C27 C26 H26A 121.6 . . ? C25 C26 H26A 121.6 . . ? C26 C27 C28 121.7(4) . . ? C26 C27 H27A 119.1 . . ? C28 C27 H27A 119.1 . . ? C29 C28 C27 121.5(4) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C30 117.4(4) . . ? C28 C29 H29A 121.3 . . ? C30 C29 H29A 121.3 . . ? C29 C30 C25 120.9(4) . . ? C29 C30 N7 131.1(4) . . ? C25 C30 N7 107.9(3) . . ? C32 C31 N1 111.0(4) . . ? C32 C31 H31A 109.4 . . ? N1 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? N1 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? N9 C32 N10 111.7(4) . . ? N9 C32 C31 123.4(4) . . ? N10 C32 C31 124.8(4) . . ? N10 C33 C38 106.8(4) . . ? N10 C33 C34 132.2(6) . . ? C38 C33 C34 120.9(6) . . ? C35 C34 C33 117.6(7) . . ? C35 C34 H34A 121.2 . . ? C33 C34 H34A 121.2 . . ? C34 C35 C36 123.0(6) . . ? C34 C35 H35A 118.5 . . ? C36 C35 H35A 118.5 . . ? C35 C36 C37 121.8(6) . . ? C35 C36 H36A 119.1 . . ? C37 C36 H36A 119.1 . . ? C38 C37 C36 114.9(6) . . ? C38 C37 H37A 122.5 . . ? C36 C37 H37A 122.5 . . ? C37 C38 N9 131.1(5) . . ? C37 C38 C33 121.8(5) . . ? N9 C38 C33 107.1(4) . . ? O5 Cl1 O7 114.3(4) . . ? O5 Cl1 O4 111.2(3) . . ? O7 Cl1 O4 111.2(3) . . ? O5 Cl1 O6 107.0(3) . . ? O7 Cl1 O6 105.0(3) . . ? O4 Cl1 O6 107.6(3) . . ? O10 Cl2 O9 110.2(3) . . ? O10 Cl2 O8 109.8(2) . . ? O9 Cl2 O8 109.5(3) . . ? O10 Cl2 O11 108.9(3) . . ? O9 Cl2 O11 108.8(3) . . ? O8 Cl2 O11 109.7(2) . . ? O13 Cl3 O15 111.0(4) . . ? O13 Cl3 O14 111.8(3) . . ? O15 Cl3 O14 107.9(3) . . ? O13 Cl3 O12 107.8(4) . . ? O15 Cl3 O12 108.9(3) . . ? O14 Cl3 O12 109.4(3) . . ? C1M O1M H1M 112.8 . . ? O1M C1M C2M 109(3) . . ? O1M C1M H1MA 109.9 . . ? C2M C1M H1MA 109.9 . . ? O1M C1M H1MB 109.9 . . ? C2M C1M H1MB 109.9 . . ? H1MA C1M H1MB 108.3 . . ? C1M C2M H2MA 109.5 . . ? C1M C2M H2MB 109.5 . . ? H2MA C2M H2MB 109.5 . . ? C1M C2M H2MC 109.5 . . ? H2MA C2M H2MC 109.5 . . ? H2MB C2M H2MC 109.5 . . ? C3M O2M H2M 116.9 . . ? O2M C3M C4M 109.2(13) . . ? O2M C3M H3MA 109.8 . . ? C4M C3M H3MA 109.8 . . ? O2M C3M H3MB 109.8 . . ? C4M C3M H3MB 109.8 . . ? H3MA C3M H3MB 108.3 . . ? C3M C4M H4MA 109.5 . . ? C3M C4M H4MB 109.5 . . ? H4MA C4M H4MB 109.5 . . ? C3M C4M H4MC 109.5 . . ? H4MA C4M H4MC 109.5 . . ? H4MB C4M H4MC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.861 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.091 # Attachment '755334.cif' data_FeIII(OMe)(HCTB)(ClO4)3.3MeOH.4.5H2O _database_code_depnum_ccdc_archive 'CCDC 755334' #TrackingRef '755334.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H63 Cl3 Fe N10 O20.50' _chemical_formula_weight 1198.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 41.3876(14) _cell_length_b 14.1082(5) _cell_length_c 18.3504(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.582(2) _cell_angle_gamma 90.00 _cell_volume 10565.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 65446 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5008 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 15724 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9275 _reflns_number_gt 7212 _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. The bond lengths of Cl-O for the disordered perchlorate anion (Cl3) were restrained with the command DFIX and the anisotropic displacement parameters of the related atoms were refined with the command SIMU and DELU for the instability of disordered perchlorate during the refinement. ; _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^)+(0.2133P)^2^+25.5474P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9275 _refine_ls_number_parameters 724 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2817 _refine_ls_wR_factor_gt 0.2249 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.630386(15) 0.73514(4) 0.55894(3) 0.0215(3) Uani 1 1 d . . . N1 N 0.64157(9) 0.7468(3) 0.6876(2) 0.0247(8) Uani 1 1 d . . . N2 N 0.57990(9) 0.7669(3) 0.5900(2) 0.0264(9) Uani 1 1 d . . . N3 N 0.67779(9) 0.6876(3) 0.58341(19) 0.0224(8) Uani 1 1 d . . . N4 N 0.71790(9) 0.6226(3) 0.6622(2) 0.0251(8) Uani 1 1 d . . . H4 H 0.7289 0.6010 0.7041 0.030 Uiso 1 1 calc R . . N5 N 0.64582(8) 0.8739(3) 0.5734(2) 0.0211(8) Uani 1 1 d . . . N6 N 0.67124(9) 0.9875(3) 0.6446(2) 0.0246(8) Uani 1 1 d . . . H6 H 0.6801 1.0181 0.6848 0.030 Uiso 1 1 calc R . . N7 N 0.61168(10) 0.5968(3) 0.5716(2) 0.0287(9) Uani 1 1 d . . . N8 N 0.56755(11) 0.5091(3) 0.5780(3) 0.0463(13) Uani 1 1 d . . . H8 H 0.5470 0.4949 0.5798 0.056 Uiso 1 1 calc R . . N9 N 0.50739(10) 0.8457(3) 0.5126(3) 0.0336(10) Uani 1 1 d . . . H9 H 0.5090 0.8086 0.4774 0.040 Uiso 1 1 d R . . N10 N 0.52494(8) 0.9454(2) 0.60126(18) 0.0316(9) Uani 1 1 d . . . H10 H 0.5375 0.9689 0.6321 0.038 Uiso 1 1 d R . . C1 C 0.61089(8) 0.7239(2) 0.71648(18) 0.0295(11) Uani 1 1 d R . . H1 H 0.6068 0.6546 0.7082 0.035 Uiso 1 1 calc R . . C2 C 0.61325(14) 0.7419(4) 0.7998(3) 0.0391(13) Uani 1 1 d . . . H2A H 0.6318 0.7051 0.8271 0.047 Uiso 1 1 calc R . . H2B H 0.6176 0.8099 0.8102 0.047 Uiso 1 1 calc R . . C3 C 0.58166(15) 0.7133(5) 0.8265(3) 0.0475(15) Uani 1 1 d . . . H3A H 0.5784 0.6440 0.8205 0.057 Uiso 1 1 calc R . . H3B H 0.5834 0.7285 0.8797 0.057 Uiso 1 1 calc R . . C4 C 0.55255(16) 0.7648(5) 0.7832(4) 0.0520(17) Uani 1 1 d . . . H4A H 0.5549 0.8338 0.7923 0.062 Uiso 1 1 calc R . . H4B H 0.5322 0.7436 0.8001 0.062 Uiso 1 1 calc R . . C5 C 0.55008(13) 0.7452(4) 0.7014(3) 0.0403(13) Uani 1 1 d . . . H5A H 0.5309 0.7793 0.6740 0.048 Uiso 1 1 calc R . . H5B H 0.5466 0.6766 0.6922 0.048 Uiso 1 1 calc R . . C6 C 0.58131(11) 0.7768(3) 0.6721(3) 0.0293(11) Uani 1 1 d . . . H6A H 0.5845 0.8457 0.6840 0.035 Uiso 1 1 calc R . . C7 C 0.66727(12) 0.6737(3) 0.7113(2) 0.0277(10) Uani 1 1 d . . . H7A H 0.6568 0.6123 0.7194 0.033 Uiso 1 1 calc R . . H7B H 0.6809 0.6931 0.7584 0.033 Uiso 1 1 calc R . . C8 C 0.68828(10) 0.6626(3) 0.6528(2) 0.0226(9) Uani 1 1 d . . . C9 C 0.72833(11) 0.6211(3) 0.5940(2) 0.0242(10) Uani 1 1 d . . . C10 C 0.75672(11) 0.5885(3) 0.5709(3) 0.0291(10) Uani 1 1 d . . . H10A H 0.7739 0.5595 0.6042 0.035 Uiso 1 1 calc R . . C11 C 0.75857(13) 0.6006(4) 0.4972(3) 0.0348(12) Uani 1 1 d . . . H11 H 0.7776 0.5796 0.4794 0.042 Uiso 1 1 calc R . . C12 C 0.73300(13) 0.6432(4) 0.4471(3) 0.0318(11) Uani 1 1 d . . . H12 H 0.7354 0.6504 0.3968 0.038 Uiso 1 1 calc R . . C13 C 0.70490(12) 0.6742(3) 0.4694(3) 0.0292(10) Uani 1 1 d . . . H13 H 0.6877 0.7024 0.4356 0.035 Uiso 1 1 calc R . . C14 C 0.70247(11) 0.6628(3) 0.5434(2) 0.0233(9) Uani 1 1 d . . . C15 C 0.65375(12) 0.8440(3) 0.7083(2) 0.0266(10) Uani 1 1 d . . . H15A H 0.6753 0.8396 0.7411 0.032 Uiso 1 1 calc R . . H15B H 0.6383 0.8759 0.7361 0.032 Uiso 1 1 calc R . . C16 C 0.65721(10) 0.9018(3) 0.6418(2) 0.0224(9) Uani 1 1 d . . . C17 C 0.65364(10) 0.9461(3) 0.5273(2) 0.0217(9) Uani 1 1 d . . . C18 C 0.64957(11) 0.9531(3) 0.4506(2) 0.0252(10) Uani 1 1 d . . . H18 H 0.6394 0.9039 0.4195 0.030 Uiso 1 1 calc R . . C19 C 0.66093(12) 1.0351(4) 0.4213(3) 0.0312(11) Uani 1 1 d . . . H19 H 0.6585 1.0421 0.3692 0.037 Uiso 1 1 calc R . . C20 C 0.67579(12) 1.1072(4) 0.4669(3) 0.0358(12) Uani 1 1 d . . . H20 H 0.6830 1.1625 0.4448 0.043 Uiso 1 1 calc R . . C21 C 0.68046(12) 1.1010(3) 0.5434(3) 0.0317(11) Uani 1 1 d . . . H21 H 0.6907 1.1503 0.5741 0.038 Uiso 1 1 calc R . . C22 C 0.66932(11) 1.0192(3) 0.5723(2) 0.0247(10) Uani 1 1 d . . . C23 C 0.55975(11) 0.6851(3) 0.5561(3) 0.0327(11) Uani 1 1 d . . . H23A H 0.5396 0.6796 0.5782 0.039 Uiso 1 1 calc R . . H23B H 0.5533 0.6955 0.5023 0.039 Uiso 1 1 calc R . . C24 C 0.57936(12) 0.5966(3) 0.5696(3) 0.0306(11) Uani 1 1 d . . . C25 C 0.59305(14) 0.4458(4) 0.5830(4) 0.0482(15) Uani 1 1 d . . . C26 C 0.59453(17) 0.3493(5) 0.5910(5) 0.069(2) Uani 1 1 d . . . H26 H 0.5756 0.3132 0.5955 0.083 Uiso 1 1 calc R . . C27 C 0.62430(17) 0.3070(4) 0.5921(5) 0.071(2) Uani 1 1 d . . . H27 H 0.6260 0.2400 0.5957 0.085 Uiso 1 1 calc R . . C28 C 0.65215(16) 0.3601(4) 0.5880(4) 0.0581(18) Uani 1 1 d . . . H28 H 0.6725 0.3284 0.5898 0.070 Uiso 1 1 calc R . . C29 C 0.65115(14) 0.4577(4) 0.5814(3) 0.0396(13) Uani 1 1 d . . . H29 H 0.6704 0.4936 0.5793 0.047 Uiso 1 1 calc R . . C30 C 0.62113(12) 0.5007(3) 0.5779(3) 0.0331(11) Uani 1 1 d . . . C31 C 0.56818(11) 0.8560(3) 0.5496(3) 0.0312(11) Uani 1 1 d . . . H31A H 0.5827 0.9087 0.5701 0.037 Uiso 1 1 calc R . . H31B H 0.5704 0.8485 0.4971 0.037 Uiso 1 1 calc R . . C32 C 0.53352(12) 0.8826(3) 0.5534(3) 0.0298(11) Uani 1 1 d . . . C33 C 0.48013(12) 0.8854(4) 0.5346(3) 0.0332(11) Uani 1 1 d . . . C34 C 0.44670(13) 0.8725(4) 0.5089(3) 0.0418(13) Uani 1 1 d . . . H34 H 0.4389 0.8298 0.4699 0.050 Uiso 1 1 calc R . . C35 C 0.42546(13) 0.9256(4) 0.5437(3) 0.0443(14) Uani 1 1 d . . . H35 H 0.4025 0.9189 0.5280 0.053 Uiso 1 1 calc R . . C36 C 0.43665(13) 0.9881(4) 0.6004(3) 0.0411(13) Uani 1 1 d . . . H36 H 0.4210 1.0223 0.6226 0.049 Uiso 1 1 calc R . . C37 C 0.46946(13) 1.0028(4) 0.6260(3) 0.0374(12) Uani 1 1 d . . . H37 H 0.4770 1.0465 0.6645 0.045 Uiso 1 1 calc R . . C38 C 0.49101(11) 0.9490(3) 0.5916(3) 0.0294(11) Uani 1 1 d . . . O1 O 0.61822(9) 0.7425(2) 0.45963(19) 0.0337(8) Uani 1 1 d . . . C39 C 0.6026(2) 0.6960(7) 0.3983(4) 0.082(2) Uani 1 1 d U . . H39A H 0.5968 0.6318 0.4120 0.098 Uiso 1 1 calc R . . H39B H 0.6171 0.6923 0.3613 0.098 Uiso 1 1 calc R . . H39C H 0.5826 0.7306 0.3775 0.098 Uiso 1 1 calc R . . Cl1 Cl 0.59231(3) 0.07906(9) 0.71389(7) 0.0352(4) Uani 1 1 d . . . O2 O 0.61395(13) 0.0285(4) 0.7684(3) 0.0718(15) Uani 1 1 d . . . O3 O 0.59613(18) 0.1765(4) 0.7242(4) 0.103(2) Uani 1 1 d . . . O4 O 0.55895(11) 0.0545(5) 0.7194(3) 0.0758(16) Uani 1 1 d . . . O5 O 0.59876(12) 0.0537(5) 0.6431(2) 0.0735(16) Uani 1 1 d . . . Cl2 Cl 0.74949(3) 0.83382(9) 0.80643(7) 0.0357(4) Uani 1 1 d . . . O6 O 0.76901(13) 0.9118(3) 0.8350(3) 0.0672(14) Uani 1 1 d . . . O7 O 0.76801(14) 0.7482(3) 0.8228(3) 0.0703(15) Uani 1 1 d . . . O8 O 0.72060(11) 0.8276(5) 0.8403(2) 0.0741(16) Uani 1 1 d . . . O9 O 0.73909(12) 0.8451(3) 0.7280(2) 0.0559(12) Uani 1 1 d . . . Cl3 Cl 0.47952(15) 0.5359(6) 0.6175(5) 0.086(2) Uani 0.50 1 d PDU A 1 O10 O 0.5023(4) 0.4682(11) 0.5959(8) 0.077(3) Uani 0.50 1 d PDU A 1 O11 O 0.44680(16) 0.5039(6) 0.5922(5) 0.127(3) Uani 0.50 1 d PDU A 1 O12 O 0.4848(5) 0.6244(10) 0.5852(10) 0.108(4) Uani 0.50 1 d PDU A 1 O13 O 0.4838(5) 0.5506(13) 0.6956(6) 0.113(5) Uani 0.50 1 d PDU A 1 Cl3' Cl 0.4778(2) 0.5468(8) 0.5894(6) 0.114(3) Uani 0.50 1 d PDU B 2 O10' O 0.4982(4) 0.4759(11) 0.5617(8) 0.077(3) Uani 0.50 1 d PDU B 2 O11' O 0.44680(16) 0.5039(6) 0.5922(5) 0.127(3) Uani 0.50 1 d PDU B 2 O12' O 0.4759(5) 0.6303(12) 0.5464(10) 0.123(6) Uani 0.50 1 d PDU B 2 O13' O 0.4915(6) 0.5719(16) 0.6640(8) 0.134(6) Uani 0.50 1 d PDU B 2 C1M C 0.68307(19) 0.1847(5) 0.7817(4) 0.0657(19) Uani 1 1 d . . . H1MA H 0.6642 0.1639 0.8014 0.099 Uiso 1 1 d R . . H1MB H 0.6975 0.2176 0.8199 0.099 Uiso 1 1 d R . . H1MC H 0.6766 0.2255 0.7399 0.099 Uiso 1 1 d R . . O1M O 0.69891(11) 0.1072(3) 0.7550(2) 0.0525(11) Uani 1 1 d . . . H1M H 0.7162 0.1353 0.7474 0.063 Uiso 1 1 d R . . C2M C 0.7249(3) 0.6376(7) 0.9803(5) 0.105(4) Uani 1 1 d . . . H2MA H 0.7083 0.6068 1.0025 0.158 Uiso 1 1 d R . . H2MB H 0.7276 0.7009 0.9997 0.158 Uiso 1 1 d R . . H2MC H 0.7452 0.6037 0.9927 0.158 Uiso 1 1 d R . . O2M O 0.71521(19) 0.6405(5) 0.9052(3) 0.099(2) Uani 1 1 d . . . H2M H 0.7173 0.6966 0.8899 0.119 Uiso 1 1 d R . . C3M C 0.6531(4) 0.4241(11) 0.7718(9) 0.164(6) Uani 1 1 d DU . . H3MA H 0.6488 0.3917 0.7252 0.246 Uiso 1 1 d R . . H3MB H 0.6561 0.3770 0.8100 0.246 Uiso 1 1 d R . . H3MC H 0.6729 0.4598 0.7732 0.246 Uiso 1 1 d R . . O3M O 0.6250(2) 0.4909(5) 0.7764(5) 0.130(3) Uani 1 1 d D . . H3M H 0.6287 0.5171 0.8186 0.156 Uiso 1 1 d R . . O1W O 0.75636(13) 0.0467(3) 0.6992(2) 0.0594(13) Uani 1 1 d . . . H1WA H 0.7534 -0.0129 0.6980 0.071 Uiso 1 1 d R . . H1WB H 0.7653 0.0628 0.6626 0.071 Uiso 1 1 d R . . O2W O 0.50731(15) 0.7261(4) 0.3970(4) 0.094(2) Uani 1 1 d . . . H2WA H 0.5064 0.6685 0.4102 0.113 Uiso 1 1 d R . . H2WB H 0.4956 0.7323 0.3546 0.113 Uiso 1 1 d R . . O3W O 0.5593(2) 0.4401(8) 0.7467(5) 0.157(4) Uani 1 1 d . . . H3WA H 0.5765 0.4725 0.7449 0.189 Uiso 1 1 d R . . H3WB H 0.5434 0.4656 0.7181 0.189 Uiso 1 1 d R . . O4W O 0.9692(3) 0.7622(9) 0.7575(7) 0.191(5) Uani 1 1 d U . . H4WA H 0.9525 0.7292 0.7627 0.229 Uiso 1 1 d R . . H4WB H 0.9635 0.8202 0.7556 0.229 Uiso 1 1 d R . . O5W O 0.6512(5) 0.5645(15) 0.9061(8) 0.166(8) Uani 0.50 1 d PDU . . H5WA H 0.6604 0.6186 0.9111 0.200 Uiso 0.50 1 d PR . . H5WB H 0.6447 0.5409 0.9437 0.200 Uiso 0.50 1 d PR . . 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 0.0171(4) 0.0176(4) 0.0308(4) -0.0004(2) 0.0070(3) 0.0010(2) N1 0.021(2) 0.024(2) 0.031(2) 0.0010(15) 0.0092(16) 0.0015(15) N2 0.0158(19) 0.0176(19) 0.047(2) -0.0011(16) 0.0092(17) 0.0025(15) N3 0.0197(19) 0.0207(19) 0.0285(19) -0.0005(15) 0.0089(15) 0.0031(15) N4 0.025(2) 0.024(2) 0.0270(19) 0.0032(15) 0.0061(15) 0.0053(16) N5 0.0146(18) 0.0202(19) 0.0296(19) 0.0016(15) 0.0072(14) 0.0011(14) N6 0.027(2) 0.0200(19) 0.0277(19) -0.0039(15) 0.0085(15) -0.0021(16) N7 0.027(2) 0.0158(19) 0.045(2) -0.0015(16) 0.0109(17) 0.0022(16) N8 0.024(2) 0.023(2) 0.097(4) -0.005(2) 0.023(2) -0.0052(18) N9 0.021(2) 0.025(2) 0.054(3) -0.0062(19) 0.0042(18) 0.0038(17) N10 0.021(2) 0.025(2) 0.048(2) -0.0003(18) 0.0032(17) 0.0032(16) C1 0.028(3) 0.024(2) 0.041(3) 0.001(2) 0.019(2) -0.001(2) C2 0.041(3) 0.043(3) 0.038(3) 0.001(2) 0.020(2) -0.001(2) C3 0.048(4) 0.051(4) 0.053(3) 0.002(3) 0.035(3) 0.000(3) C4 0.048(4) 0.049(4) 0.070(4) 0.000(3) 0.042(3) 0.002(3) C5 0.028(3) 0.031(3) 0.068(4) 0.002(2) 0.026(3) 0.000(2) C6 0.023(2) 0.022(2) 0.048(3) -0.001(2) 0.018(2) 0.0009(19) C7 0.027(2) 0.029(3) 0.029(2) 0.0068(19) 0.0088(19) 0.007(2) C8 0.019(2) 0.020(2) 0.030(2) 0.0025(17) 0.0072(18) 0.0035(17) C9 0.019(2) 0.023(2) 0.031(2) -0.0007(18) 0.0053(18) 0.0010(18) C10 0.019(2) 0.028(3) 0.041(3) 0.000(2) 0.0067(19) 0.0059(19) C11 0.029(3) 0.030(3) 0.050(3) -0.004(2) 0.021(2) 0.003(2) C12 0.037(3) 0.029(3) 0.033(2) -0.006(2) 0.018(2) -0.003(2) C13 0.031(3) 0.027(2) 0.030(2) 0.0000(19) 0.008(2) 0.003(2) C14 0.021(2) 0.018(2) 0.032(2) -0.0002(17) 0.0108(18) 0.0006(17) C15 0.027(2) 0.026(2) 0.029(2) -0.0028(18) 0.0093(19) -0.0022(19) C16 0.017(2) 0.022(2) 0.029(2) -0.0020(18) 0.0093(17) 0.0033(18) C17 0.012(2) 0.018(2) 0.036(2) 0.0013(17) 0.0066(17) 0.0026(16) C18 0.018(2) 0.027(2) 0.032(2) -0.0018(18) 0.0072(18) 0.0041(18) C19 0.025(2) 0.038(3) 0.033(2) 0.008(2) 0.0089(19) 0.004(2) C20 0.032(3) 0.031(3) 0.047(3) 0.010(2) 0.015(2) -0.004(2) C21 0.032(3) 0.021(2) 0.044(3) -0.003(2) 0.011(2) -0.007(2) C22 0.022(2) 0.021(2) 0.033(2) -0.0020(18) 0.0112(18) 0.0015(18) C23 0.019(2) 0.023(2) 0.056(3) -0.004(2) 0.009(2) -0.0005(19) C24 0.023(2) 0.022(2) 0.049(3) -0.007(2) 0.012(2) -0.0015(19) C25 0.035(3) 0.021(3) 0.090(5) -0.004(3) 0.015(3) -0.002(2) C26 0.044(4) 0.027(3) 0.139(7) 0.000(4) 0.025(4) -0.005(3) C27 0.052(4) 0.019(3) 0.144(7) -0.005(4) 0.021(4) -0.003(3) C28 0.048(4) 0.024(3) 0.106(5) 0.000(3) 0.025(4) 0.013(3) C29 0.034(3) 0.021(3) 0.067(4) -0.001(2) 0.016(3) 0.003(2) C30 0.030(3) 0.019(2) 0.052(3) -0.004(2) 0.012(2) 0.000(2) C31 0.021(2) 0.019(2) 0.054(3) 0.006(2) 0.008(2) 0.0042(19) C32 0.024(2) 0.022(2) 0.044(3) 0.004(2) 0.008(2) 0.0060(19) C33 0.019(2) 0.027(3) 0.054(3) 0.006(2) 0.007(2) 0.0055(19) C34 0.023(3) 0.040(3) 0.060(3) 0.000(3) 0.001(2) 0.004(2) C35 0.018(3) 0.055(4) 0.059(3) 0.010(3) 0.005(2) 0.008(2) C36 0.026(3) 0.051(3) 0.049(3) 0.013(3) 0.016(2) 0.017(2) C37 0.036(3) 0.040(3) 0.039(3) 0.006(2) 0.011(2) 0.011(2) C38 0.020(2) 0.028(3) 0.041(3) 0.007(2) 0.008(2) 0.0077(19) O1 0.034(2) 0.0317(19) 0.0338(18) -0.0017(14) 0.0001(15) -0.0046(15) C39 0.085(5) 0.100(6) 0.059(4) -0.028(4) 0.007(4) -0.035(5) Cl1 0.0364(7) 0.0354(7) 0.0333(6) -0.0010(5) 0.0039(5) 0.0037(5) O2 0.063(3) 0.097(4) 0.052(3) 0.018(3) -0.001(2) 0.022(3) O3 0.106(5) 0.043(3) 0.163(6) -0.012(3) 0.028(4) 0.004(3) O4 0.040(3) 0.135(5) 0.054(3) -0.017(3) 0.009(2) -0.016(3) O5 0.059(3) 0.121(5) 0.042(2) -0.008(3) 0.013(2) 0.016(3) Cl2 0.0352(7) 0.0299(7) 0.0428(7) -0.0051(5) 0.0090(5) 0.0012(5) O6 0.080(3) 0.037(2) 0.073(3) -0.004(2) -0.019(3) -0.011(2) O7 0.076(4) 0.032(2) 0.106(4) 0.001(2) 0.025(3) 0.016(2) O8 0.043(3) 0.134(5) 0.048(3) 0.015(3) 0.016(2) 0.017(3) O9 0.070(3) 0.059(3) 0.042(2) -0.0066(19) 0.020(2) -0.015(2) Cl3 0.056(3) 0.073(3) 0.140(6) -0.033(4) 0.049(3) -0.018(2) O10 0.058(4) 0.075(4) 0.105(7) -0.005(5) 0.031(5) 0.003(3) O11 0.102(4) 0.131(5) 0.156(5) -0.013(4) 0.046(4) -0.027(4) O12 0.119(8) 0.083(7) 0.124(8) 0.003(7) 0.028(7) -0.038(6) O13 0.135(9) 0.101(8) 0.106(8) -0.008(7) 0.027(7) -0.008(7) Cl3' 0.088(4) 0.107(5) 0.151(7) -0.025(5) 0.026(4) -0.006(4) O10' 0.058(4) 0.075(4) 0.105(7) -0.005(5) 0.031(5) 0.003(3) O11' 0.102(4) 0.131(5) 0.156(5) -0.013(4) 0.046(4) -0.027(4) O12' 0.121(9) 0.111(8) 0.136(9) 0.010(7) 0.020(8) -0.002(7) O13' 0.141(9) 0.116(8) 0.136(8) -0.039(8) -0.002(7) -0.020(7) C1M 0.070(5) 0.061(5) 0.067(4) -0.004(3) 0.012(4) -0.008(4) O1M 0.062(3) 0.051(3) 0.044(2) -0.0139(18) 0.0062(19) -0.011(2) C2M 0.150(10) 0.088(7) 0.091(7) 0.036(5) 0.058(7) 0.051(7) O2M 0.133(6) 0.091(5) 0.080(4) 0.000(3) 0.035(4) -0.004(4) C3M 0.204(10) 0.133(9) 0.154(9) 0.010(7) 0.025(8) 0.002(8) O3M 0.141(7) 0.073(5) 0.185(8) 0.033(5) 0.051(6) 0.009(5) O1W 0.100(4) 0.037(2) 0.040(2) -0.0034(17) 0.005(2) -0.018(2) O2W 0.088(4) 0.060(3) 0.124(5) -0.043(3) -0.018(4) 0.011(3) O3W 0.110(6) 0.237(12) 0.129(7) 0.028(7) 0.031(5) 0.044(7) O4W 0.176(8) 0.179(8) 0.217(9) 0.042(7) 0.033(7) -0.041(7) O5W 0.170(9) 0.167(9) 0.161(9) 0.007(5) 0.025(5) 0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.811(3) . ? Fe1 N3 2.051(4) . ? Fe1 N5 2.062(4) . ? Fe1 N7 2.127(4) . ? Fe1 N2 2.300(4) . ? Fe1 N1 2.334(4) . ? N1 C15 1.488(6) . ? N1 C1 1.491(5) . ? N1 C7 1.494(6) . ? N2 C23 1.497(6) . ? N2 C31 1.498(6) . ? N2 C6 1.505(6) . ? N3 C8 1.323(6) . ? N3 C14 1.398(5) . ? N4 C8 1.334(6) . ? N4 C9 1.391(6) . ? N4 H4 0.8800 . ? N5 C16 1.325(6) . ? N5 C17 1.397(6) . ? N6 C16 1.338(6) . ? N6 C22 1.390(6) . ? N6 H6 0.8800 . ? N7 C24 1.332(6) . ? N7 C30 1.410(6) . ? N8 C24 1.345(6) . ? N8 C25 1.374(7) . ? N8 H8 0.8800 . ? N9 C32 1.315(6) . ? N9 C33 1.378(6) . ? N9 H9 0.8436 . ? N10 C32 1.337(6) . ? N10 C38 1.387(6) . ? N10 H10 0.7754 . ? C1 C2 1.536(6) . ? C1 C6 1.545(6) . ? C1 H1 1.0000 . ? C2 C3 1.525(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.514(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.546(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 1.0000 . ? C7 C8 1.497(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.392(6) . ? C9 C14 1.422(6) . ? C10 C11 1.379(7) . ? C10 H10A 0.9500 . ? C11 C12 1.415(8) . ? C11 H11 0.9500 . ? C12 C13 1.367(7) . ? C12 H12 0.9500 . ? C13 C14 1.388(6) . ? C13 H13 0.9500 . ? C15 C16 1.495(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.393(6) . ? C17 C22 1.411(6) . ? C18 C19 1.390(7) . ? C18 H18 0.9500 . ? C19 C20 1.394(8) . ? C19 H19 0.9500 . ? C20 C21 1.388(7) . ? C20 H20 0.9500 . ? C21 C22 1.381(7) . ? C21 H21 0.9500 . ? C23 C24 1.488(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.370(9) . ? C25 C30 1.412(8) . ? C26 C27 1.366(10) . ? C26 H26 0.9500 . ? C27 C28 1.387(9) . ? C27 H27 0.9500 . ? C28 C29 1.383(8) . ? C28 H28 0.9500 . ? C29 C30 1.375(7) . ? C29 H29 0.9500 . ? C31 C32 1.496(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C33 C38 1.394(7) . ? C33 C34 1.397(7) . ? C34 C35 1.388(8) . ? C34 H34 0.9500 . ? C35 C36 1.384(9) . ? C35 H35 0.9500 . ? C36 C37 1.377(8) . ? C36 H36 0.9500 . ? C37 C38 1.400(7) . ? C37 H37 0.9500 . ? O1 C39 1.369(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Cl1 O3 1.393(6) . ? Cl1 O5 1.415(5) . ? Cl1 O2 1.418(5) . ? Cl1 O4 1.443(5) . ? Cl2 O6 1.413(5) . ? Cl2 O7 1.435(5) . ? Cl2 O8 1.439(5) . ? Cl2 O9 1.442(4) . ? Cl3 O12 1.414(9) . ? Cl3 O11 1.430(8) . ? Cl3 O13 1.430(9) . ? Cl3 O10 1.444(9) . ? Cl3' O12' 1.413(10) . ? Cl3' O13' 1.436(10) . ? Cl3' O10' 1.454(9) . ? C1M O1M 1.405(8) . ? C1M H1MA 0.9603 . ? C1M H1MB 0.9599 . ? C1M H1MC 0.9600 . ? O1M H1M 0.8500 . ? C2M O2M 1.371(11) . ? C2M H2MA 0.9603 . ? C2M H2MB 0.9600 . ? C2M H2MC 0.9598 . ? O2M H2M 0.8500 . ? C3M O3M 1.510(9) . ? C3M H3MA 0.9600 . ? C3M H3MB 0.9600 . ? C3M H3MC 0.9598 . ? O3M H3M 0.8500 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8498 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8502 . ? O5W H5WB 0.8498 . ? 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 Fe1 N3 109.55(15) . . ? O1 Fe1 N5 95.95(15) . . ? N3 Fe1 N5 91.03(14) . . ? O1 Fe1 N7 96.73(16) . . ? N3 Fe1 N7 91.60(15) . . ? N5 Fe1 N7 165.36(15) . . ? O1 Fe1 N2 97.26(16) . . ? N3 Fe1 N2 152.23(14) . . ? N5 Fe1 N2 93.33(13) . . ? N7 Fe1 N2 77.83(14) . . ? O1 Fe1 N1 171.33(15) . . ? N3 Fe1 N1 77.31(14) . . ? N5 Fe1 N1 78.33(14) . . ? N7 Fe1 N1 88.20(15) . . ? N2 Fe1 N1 76.77(14) . . ? C15 N1 C1 112.4(3) . . ? C15 N1 C7 111.6(4) . . ? C1 N1 C7 110.7(3) . . ? C15 N1 Fe1 109.0(3) . . ? C1 N1 Fe1 107.9(2) . . ? C7 N1 Fe1 104.9(3) . . ? C23 N2 C31 109.2(4) . . ? C23 N2 C6 114.5(4) . . ? C31 N2 C6 111.8(4) . . ? C23 N2 Fe1 102.3(3) . . ? C31 N2 Fe1 105.9(3) . . ? C6 N2 Fe1 112.4(3) . . ? C8 N3 C14 106.7(4) . . ? C8 N3 Fe1 116.5(3) . . ? C14 N3 Fe1 136.3(3) . . ? C8 N4 C9 107.8(4) . . ? C8 N4 H4 126.1 . . ? C9 N4 H4 126.1 . . ? C16 N5 C17 106.0(4) . . ? C16 N5 Fe1 117.3(3) . . ? C17 N5 Fe1 135.4(3) . . ? C16 N6 C22 107.4(4) . . ? C16 N6 H6 126.3 . . ? C22 N6 H6 126.3 . . ? C24 N7 C30 105.3(4) . . ? C24 N7 Fe1 112.4(3) . . ? C30 N7 Fe1 142.2(3) . . ? C24 N8 C25 108.3(4) . . ? C24 N8 H8 125.8 . . ? C25 N8 H8 125.8 . . ? C32 N9 C33 108.0(4) . . ? C32 N9 H9 121.3 . . ? C33 N9 H9 130.5 . . ? C32 N10 C38 108.3(4) . . ? C32 N10 H10 123.1 . . ? C38 N10 H10 128.1 . . ? N1 C1 C2 113.7(3) . . ? N1 C1 C6 110.8(3) . . ? C2 C1 C6 111.0(3) . . ? N1 C1 H1 107.0 . . ? C2 C1 H1 107.0 . . ? C6 C1 H1 107.0 . . ? C3 C2 C1 111.1(5) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 110.7(5) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 C5 110.5(5) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 111.7(5) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C1 112.2(3) . . ? N2 C6 C5 115.2(4) . . ? C1 C6 C5 108.2(4) . . ? N2 C6 H6A 106.9 . . ? C1 C6 H6A 106.9 . . ? C5 C6 H6A 106.9 . . ? N1 C7 C8 109.5(3) . . ? N1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N3 C8 N4 112.6(4) . . ? N3 C8 C7 121.7(4) . . ? N4 C8 C7 125.6(4) . . ? C10 C9 N4 133.1(4) . . ? C10 C9 C14 121.3(4) . . ? N4 C9 C14 105.6(4) . . ? C11 C10 C9 116.5(4) . . ? C11 C10 H10A 121.8 . . ? C9 C10 H10A 121.8 . . ? C10 C11 C12 122.2(4) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 121.5(4) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 117.4(5) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C13 C14 N3 131.6(4) . . ? C13 C14 C9 121.2(4) . . ? N3 C14 C9 107.2(4) . . ? N1 C15 C16 111.6(4) . . ? N1 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N1 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N5 C16 N6 112.9(4) . . ? N5 C16 C15 123.0(4) . . ? N6 C16 C15 124.2(4) . . ? C18 C17 N5 131.5(4) . . ? C18 C17 C22 120.4(4) . . ? N5 C17 C22 108.0(4) . . ? C19 C18 C17 117.2(4) . . ? C19 C18 H18 121.4 . . ? C17 C18 H18 121.4 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 122.4(4) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 116.2(5) . . ? C22 C21 H21 121.9 . . ? C20 C21 H21 121.9 . . ? C21 C22 N6 131.8(4) . . ? C21 C22 C17 122.5(4) . . ? N6 C22 C17 105.7(4) . . ? C24 C23 N2 109.1(4) . . ? C24 C23 H23A 109.9 . . ? N2 C23 H23A 109.9 . . ? C24 C23 H23B 109.9 . . ? N2 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N7 C24 N8 112.4(4) . . ? N7 C24 C23 121.3(4) . . ? N8 C24 C23 126.2(4) . . ? C26 C25 N8 132.3(6) . . ? C26 C25 C30 122.0(6) . . ? N8 C25 C30 105.7(5) . . ? C27 C26 C25 117.4(6) . . ? C27 C26 H26 121.3 . . ? C25 C26 H26 121.3 . . ? C26 C27 C28 121.3(6) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 122.0(6) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C30 C29 C28 117.2(5) . . ? C30 C29 H29 121.4 . . ? C28 C29 H29 121.4 . . ? C29 C30 N7 131.6(5) . . ? C29 C30 C25 120.2(5) . . ? N7 C30 C25 108.2(4) . . ? C32 C31 N2 115.0(4) . . ? C32 C31 H31A 108.5 . . ? N2 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? N2 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? N9 C32 N10 110.7(4) . . ? N9 C32 C31 125.3(4) . . ? N10 C32 C31 123.9(4) . . ? N9 C33 C38 107.6(4) . . ? N9 C33 C34 131.4(5) . . ? C38 C33 C34 121.0(5) . . ? C35 C34 C33 116.3(5) . . ? C35 C34 H34 121.9 . . ? C33 C34 H34 121.9 . . ? C36 C35 C34 122.1(5) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C37 C36 C35 122.7(5) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C36 C37 C38 115.5(5) . . ? C36 C37 H37 122.2 . . ? C38 C37 H37 122.2 . . ? N10 C38 C33 105.4(4) . . ? N10 C38 C37 132.1(5) . . ? C33 C38 C37 122.5(5) . . ? C39 O1 Fe1 144.5(5) . . ? O1 C39 H39A 109.5 . . ? O1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 Cl1 O5 109.9(4) . . ? O3 Cl1 O2 110.9(4) . . ? O5 Cl1 O2 109.1(3) . . ? O3 Cl1 O4 108.4(4) . . ? O5 Cl1 O4 109.4(3) . . ? O2 Cl1 O4 109.2(3) . . ? O6 Cl2 O7 109.0(3) . . ? O6 Cl2 O8 110.7(4) . . ? O7 Cl2 O8 108.1(3) . . ? O6 Cl2 O9 109.9(3) . . ? O7 Cl2 O9 111.3(3) . . ? O8 Cl2 O9 107.8(3) . . ? O12 Cl3 O11 110.2(10) . . ? O12 Cl3 O13 106.9(11) . . ? O11 Cl3 O13 109.0(10) . . ? O12 Cl3 O10 108.4(12) . . ? O11 Cl3 O10 109.2(9) . . ? O13 Cl3 O10 113.1(12) . . ? O12' Cl3' O13' 107.6(14) . . ? O12' Cl3' O10' 111.1(13) . . ? O13' Cl3' O10' 110.0(14) . . ? O1M C1M H1MA 110.4 . . ? O1M C1M H1MB 111.2 . . ? H1MA C1M H1MB 108.6 . . ? O1M C1M H1MC 105.7 . . ? H1MA C1M H1MC 110.4 . . ? H1MB C1M H1MC 110.5 . . ? C1M O1M H1M 98.6 . . ? O2M C2M H2MA 109.2 . . ? O2M C2M H2MB 109.9 . . ? H2MA C2M H2MB 108.1 . . ? O2M C2M H2MC 110.5 . . ? H2MA C2M H2MC 109.5 . . ? H2MB C2M H2MC 109.6 . . ? C2M O2M H2M 109.3 . . ? O3M C3M H3MA 108.5 . . ? O3M C3M H3MB 113.5 . . ? H3MA C3M H3MB 107.7 . . ? O3M C3M H3MC 109.6 . . ? H3MA C3M H3MC 107.7 . . ? H3MB C3M H3MC 109.7 . . ? C3M O3M H3M 107.4 . . ? H1WA O1W H1WB 108.9 . . ? H2WA O2W H2WB 108.3 . . ? H3WA O3W H3WB 108.4 . . ? H4WA O4W H4WB 108.0 . . ? H5WA O5W H5WB 117.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.472 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.266