# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mikio Nakamura ' _publ_contact_author_email mnakamu@med.toho-u.ac.jp _publ_author_name 'Mikio Nakamura' data_tiprpfe2mebzim2 _database_code_depnum_ccdc_archive 'CCDC 807917' #TrackingRef '- TiPrPFe2MeBzIm2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(5,10,15,20-tetraisopropylporphyrinato)iron(III) (2-methylbenzimidazole)2]perchlorate ; _chemical_name_common '[Fe(TiPrP)(2-MeBzIm)2]ClO4' _chemical_melting_point ? _chemical_formula_moiety 'C48 H52 Fe N8, Cl O4, C1 H1 Cl3, C1 H1 Cl3' _chemical_formula_sum 'C50 H54 Cl7 Fe N8 O4' _chemical_formula_weight 1135.01 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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 43.200(9) _cell_length_b 11.700(2) _cell_length_c 10.682(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5399.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223 _cell_measurement_reflns_used 3488 _cell_measurement_theta_min 5.151 _cell_measurement_theta_max 39.412 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7372 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details ; XPREP Bruker AXS 2000 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27760 _diffrn_reflns_av_R_equivalents 0.1792 _diffrn_reflns_av_sigmaI/netI 0.1527 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 25.17 _reflns_number_total 9301 _reflns_number_gt 5817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0445P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 9301 _refine_ls_number_parameters 641 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 0.123746(18) 0.95002(6) 0.16138(9) 0.0224(2) Uani 1 1 d . . . C4 C 0.17022(14) 1.1339(5) 0.1506(7) 0.0310(15) Uani 1 1 d . . . C1 C 0.19031(14) 0.9601(5) 0.1099(6) 0.0277(15) Uani 1 1 d . . . C2 C 0.21563(15) 1.0425(6) 0.1049(7) 0.0416(18) Uani 1 1 d . . . H2 H 0.2367 1.0259 0.0913 0.050 Uiso 1 1 calc R . . C3 C 0.20311(14) 1.1477(5) 0.1235(6) 0.0352(18) Uani 1 1 d . . . H3 H 0.2138 1.2175 0.1195 0.042 Uiso 1 1 calc R . . C6 C 0.12384(14) 1.1800(5) 0.2726(6) 0.0300(16) Uani 1 1 d . . . C5 C 0.14939(15) 1.2143(5) 0.2003(6) 0.0271(15) Uani 1 1 d . . . C8 C 0.09096(16) 1.1734(6) 0.4328(7) 0.0411(19) Uani 1 1 d . . . H8 H 0.0795 1.1916 0.5050 0.049 Uiso 1 1 calc R . . C7 C 0.10885(16) 1.2454(6) 0.3689(7) 0.0427(19) Uani 1 1 d . . . H7 H 0.1112 1.3241 0.3840 0.051 Uiso 1 1 calc R . . C9 C 0.09197(15) 1.0621(5) 0.3724(6) 0.0282(15) Uani 1 1 d . . . C10 C 0.07107(15) 0.9694(5) 0.3895(6) 0.0326(16) Uani 1 1 d . . . C14 C 0.06804(13) 0.8143(5) 0.0995(6) 0.0252(14) Uani 1 1 d . . . C13 C 0.03906(14) 0.7822(5) 0.1545(8) 0.0342(15) Uani 1 1 d . . . H13 H 0.0235 0.7389 0.1155 0.041 Uiso 1 1 calc R . . C11 C 0.06598(14) 0.8935(5) 0.2915(6) 0.0245(14) Uani 1 1 d . . . C12 C 0.03804(14) 0.8248(5) 0.2718(7) 0.0353(17) Uani 1 1 d . . . H12 H 0.0222 0.8126 0.3306 0.042 Uiso 1 1 calc R . . C15 C 0.08196(15) 0.7671(5) -0.0070(6) 0.0304(16) Uani 1 1 d . . . C16 C 0.11437(14) 0.7684(5) -0.0260(6) 0.0266(15) Uani 1 1 d . . . C19 C 0.16440(14) 0.7909(5) 0.0231(6) 0.0275(15) Uani 1 1 d . . . C17 C 0.13192(15) 0.6900(6) -0.1007(6) 0.0343(17) Uani 1 1 d . . . H17 H 0.1240 0.6399 -0.1617 0.041 Uiso 1 1 calc R . . C18 C 0.16220(16) 0.7015(5) -0.0669(6) 0.0328(17) Uani 1 1 d . . . H18 H 0.1788 0.6578 -0.0977 0.039 Uiso 1 1 calc R . . C20 C 0.19167(15) 0.8483(5) 0.0674(6) 0.0323(16) Uani 1 1 d . . . C21 C 0.15603(16) 1.3432(5) 0.1912(7) 0.0400(19) Uani 1 1 d . . . H21 H 0.1366 1.3807 0.2182 0.048 Uiso 1 1 calc R . . C22 C 0.18093(18) 1.3850(6) 0.2854(8) 0.060(3) Uani 1 1 d . . . H22A H 0.2010 1.3555 0.2609 0.090 Uiso 1 1 calc R . . H22B H 0.1758 1.3577 0.3687 0.090 Uiso 1 1 calc R . . H22C H 0.1815 1.4679 0.2856 0.090 Uiso 1 1 calc R . . C23 C 0.1608(2) 1.3816(7) 0.0586(9) 0.074(3) Uani 1 1 d . . . H23A H 0.1781 1.3405 0.0224 0.111 Uiso 1 1 calc R . . H23B H 0.1651 1.4630 0.0574 0.111 Uiso 1 1 calc R . . H23C H 0.1423 1.3662 0.0103 0.111 Uiso 1 1 calc R . . C24 C 0.05167(19) 0.9603(6) 0.5069(7) 0.051(2) Uani 1 1 d . . . H24 H 0.0423 0.8830 0.5052 0.061 Uiso 1 1 calc R . . C25 C 0.0714(3) 0.9650(9) 0.6258(8) 0.106(4) Uani 1 1 d . . . H25A H 0.0857 0.9012 0.6263 0.159 Uiso 1 1 calc R . . H25B H 0.0580 0.9605 0.6986 0.159 Uiso 1 1 calc R . . H25C H 0.0829 1.0362 0.6277 0.159 Uiso 1 1 calc R . . C27 C 0.06324(16) 0.6964(5) -0.0998(6) 0.0375(17) Uani 1 1 d . . . H27 H 0.0762 0.6900 -0.1759 0.045 Uiso 1 1 calc R . . C30 C 0.22397(15) 0.7930(5) 0.0537(7) 0.0377(18) Uani 1 1 d . . . H30 H 0.2383 0.8392 0.1055 0.045 Uiso 1 1 calc R . . C32 C 0.23669(16) 0.7969(7) -0.0809(7) 0.050(2) Uani 1 1 d . . . H32A H 0.2570 0.7618 -0.0831 0.075 Uiso 1 1 calc R . . H32B H 0.2382 0.8758 -0.1081 0.075 Uiso 1 1 calc R . . H32C H 0.2228 0.7557 -0.1362 0.075 Uiso 1 1 calc R . . C31 C 0.22457(17) 0.6709(6) 0.1085(7) 0.053(2) Uani 1 1 d . . . H31A H 0.2103 0.6228 0.0624 0.079 Uiso 1 1 calc R . . H31B H 0.2185 0.6734 0.1959 0.079 Uiso 1 1 calc R . . H31C H 0.2453 0.6399 0.1018 0.079 Uiso 1 1 calc R . . C33 C 0.13552(15) 0.7429(5) 0.3347(6) 0.0285(15) Uani 1 1 d . . . C39 C 0.16507(16) 0.8034(6) 0.4909(6) 0.0326(16) Uani 1 1 d . . . C34 C 0.15922(14) 0.8932(5) 0.4077(6) 0.0258(15) Uani 1 1 d . . . C38 C 0.18270(16) 0.8152(6) 0.6004(6) 0.0401(18) Uani 1 1 d . . . H38 H 0.1859 0.7538 0.6557 0.048 Uiso 1 1 calc R . . C37 C 0.19522(16) 0.9227(7) 0.6227(6) 0.048(2) Uani 1 1 d . . . H37 H 0.2072 0.9354 0.6949 0.057 Uiso 1 1 calc R . . C35 C 0.17265(16) 1.0017(6) 0.4341(6) 0.0369(17) Uani 1 1 d . . . H35 H 0.1694 1.0641 0.3803 0.044 Uiso 1 1 calc R . . C36 C 0.19007(16) 1.0130(6) 0.5373(7) 0.0391(17) Uani 1 1 d . . . H36 H 0.1993 1.0843 0.5537 0.047 Uiso 1 1 calc R . . C40 C 0.11790(16) 0.6563(6) 0.2624(7) 0.0409(18) Uani 1 1 d . . . H40A H 0.1261 0.6517 0.1781 0.061 Uiso 1 1 calc R . . H40B H 0.0963 0.6783 0.2590 0.061 Uiso 1 1 calc R . . H40C H 0.1198 0.5824 0.3028 0.061 Uiso 1 1 calc R . . C41 C 0.12139(14) 1.0811(5) -0.0860(6) 0.0255(14) Uani 1 1 d . . . C47 C 0.07948(15) 1.1904(5) -0.0812(7) 0.0310(16) Uani 1 1 d . . . C42 C 0.07942(14) 1.1192(5) 0.0199(6) 0.0277(16) Uani 1 1 d . . . C43 C 0.05492(15) 1.1242(5) 0.1064(7) 0.0382(18) Uani 1 1 d . . . H43 H 0.0542 1.0765 0.1772 0.046 Uiso 1 1 calc R . . C44 C 0.03193(16) 1.2036(6) 0.0812(7) 0.0442(19) Uani 1 1 d . . . H44 H 0.0151 1.2090 0.1366 0.053 Uiso 1 1 calc R . . C45 C 0.03260(18) 1.2749(6) -0.0213(8) 0.053(2) Uani 1 1 d . . . H45 H 0.0166 1.3287 -0.0316 0.063 Uiso 1 1 calc R . . N1 N 0.16373(10) 1.0181(4) 0.1399(5) 0.0246(12) Uani 1 1 d . . . N2 N 0.11232(11) 1.0683(4) 0.2756(5) 0.0223(12) Uani 1 1 d . . . N3 N 0.08351(11) 0.8824(4) 0.1854(5) 0.0233(12) Uani 1 1 d . . . N4 N 0.13484(11) 0.8323(4) 0.0466(5) 0.0240(12) Uani 1 1 d . . . N5 N 0.14954(13) 0.7111(4) 0.4410(5) 0.0349(14) Uani 1 1 d . . . H5 H 0.1489 0.6429 0.4734 0.042 Uiso 1 1 calc R . . N6 N 0.14074(11) 0.8553(4) 0.3092(5) 0.0272(13) Uani 1 1 d . . . N8 N 0.10688(12) 1.0501(4) 0.0162(5) 0.0268(13) Uani 1 1 d . . . N7 N 0.10611(13) 1.1656(5) -0.1501(5) 0.0348(14) Uani 1 1 d . . . H7A H 0.1119 1.1974 -0.2199 0.042 Uiso 1 1 calc R . . C48 C 0.15022(16) 1.0348(6) -0.1449(7) 0.0447(19) Uani 1 1 d . . . H48A H 0.1680 1.0556 -0.0943 0.067 Uiso 1 1 calc R . . H48B H 0.1526 1.0665 -0.2282 0.067 Uiso 1 1 calc R . . H48C H 0.1488 0.9522 -0.1502 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.13365(4) 0.43259(15) 0.6520(2) 0.0447(4) Uani 1 1 d . . . O4 O 0.14317(13) 0.3151(4) 0.6535(6) 0.0686(15) Uani 1 1 d . . . O1 O 0.12991(12) 0.4732(4) 0.5292(5) 0.0510(14) Uani 1 1 d . . . O3 O 0.15636(13) 0.5002(5) 0.7165(6) 0.079(2) Uani 1 1 d . . . O2 O 0.10452(14) 0.4465(7) 0.7196(6) 0.097(3) Uani 1 1 d . . . C49 C 0.05204(19) 0.4958(7) 0.4983(9) 0.064(3) Uani 1 1 d . . . H49 H 0.0716 0.4536 0.5121 0.077 Uiso 1 1 calc R . . Cl2 Cl 0.02481(7) 0.4442(3) 0.6059(3) 0.1255(14) Uani 1 1 d . . . Cl3 Cl 0.05914(6) 0.64115(19) 0.5307(3) 0.0827(8) Uani 1 1 d . . . Cl4 Cl 0.04120(7) 0.4747(3) 0.3467(3) 0.1015(9) Uani 1 1 d . . . C29 C 0.03274(17) 0.7516(7) -0.1420(7) 0.054(2) Uani 1 1 d . . . H29A H 0.0181 0.7506 -0.0733 0.081 Uiso 1 1 calc R . . H29B H 0.0243 0.7090 -0.2121 0.081 Uiso 1 1 calc R . . H29C H 0.0366 0.8299 -0.1674 0.081 Uiso 1 1 calc R . . C28 C 0.05797(18) 0.5719(6) -0.0527(8) 0.055(2) Uani 1 1 d . . . H28A H 0.0778 0.5359 -0.0366 0.083 Uiso 1 1 calc R . . H28B H 0.0469 0.5287 -0.1160 0.083 Uiso 1 1 calc R . . H28C H 0.0459 0.5734 0.0239 0.083 Uiso 1 1 calc R . . C26 C 0.0249(2) 1.0430(7) 0.5141(12) 0.095(4) Uani 1 1 d . . . H26A H 0.0322 1.1163 0.5442 0.143 Uiso 1 1 calc R . . H26B H 0.0094 1.0134 0.5712 0.143 Uiso 1 1 calc R . . H26C H 0.0159 1.0522 0.4316 0.143 Uiso 1 1 calc R . . C46 C 0.05582(17) 1.2700(6) -0.1091(7) 0.047(2) Uani 1 1 d . . . H46 H 0.0560 1.3157 -0.1814 0.057 Uiso 1 1 calc R . . C50 C 0.21570(17) 0.3530(7) 0.7433(8) 0.052(2) Uani 1 1 d . . . H50 H 0.1928 0.3572 0.7445 0.062 Uiso 1 1 calc R . . Cl6 Cl 0.23126(5) 0.46789(19) 0.8312(2) 0.0682(6) Uani 1 1 d . . . Cl7 Cl 0.22862(6) 0.3583(2) 0.5901(2) 0.0774(7) Uani 1 1 d . . . Cl5 Cl 0.22799(5) 0.22160(19) 0.8138(2) 0.0702(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0174(4) 0.0130(3) 0.0368(5) -0.0017(5) 0.0028(5) -0.0028(3) C4 0.027(3) 0.025(3) 0.041(4) -0.003(4) 0.009(4) -0.011(3) C1 0.021(3) 0.023(3) 0.040(4) -0.004(3) 0.004(3) 0.000(3) C2 0.017(4) 0.038(4) 0.070(5) 0.003(4) -0.001(3) -0.006(3) C3 0.022(4) 0.026(4) 0.057(5) 0.002(3) 0.000(3) -0.013(3) C6 0.021(4) 0.027(4) 0.042(4) -0.002(3) -0.005(3) 0.001(3) C5 0.030(4) 0.013(3) 0.038(4) 0.001(3) -0.002(3) -0.004(3) C8 0.034(5) 0.037(4) 0.053(5) -0.021(4) 0.013(4) -0.004(3) C7 0.040(4) 0.024(4) 0.064(5) -0.017(4) 0.012(4) -0.010(3) C9 0.032(4) 0.017(3) 0.035(4) -0.006(3) 0.004(3) 0.000(3) C10 0.028(4) 0.023(4) 0.046(4) 0.003(3) 0.006(3) 0.000(3) C14 0.020(3) 0.017(3) 0.038(4) 0.002(3) 0.003(3) -0.003(3) C13 0.023(3) 0.030(3) 0.050(4) -0.003(4) 0.006(4) -0.010(3) C11 0.027(4) 0.010(3) 0.036(4) 0.005(3) 0.003(3) -0.001(3) C12 0.021(4) 0.023(4) 0.061(5) 0.009(4) 0.010(3) -0.003(3) C15 0.028(4) 0.018(3) 0.046(4) 0.000(3) -0.001(3) 0.000(3) C16 0.022(4) 0.016(3) 0.042(4) -0.005(3) -0.002(3) -0.005(3) C19 0.020(4) 0.019(3) 0.043(4) -0.003(3) 0.008(3) 0.001(3) C17 0.032(4) 0.029(4) 0.043(4) -0.015(3) -0.004(3) 0.004(3) C18 0.034(4) 0.021(4) 0.044(4) -0.012(3) 0.005(3) 0.006(3) C20 0.027(4) 0.026(4) 0.044(4) -0.009(3) -0.005(3) 0.010(3) C21 0.039(4) 0.019(3) 0.062(6) -0.007(3) 0.002(4) -0.005(3) C22 0.046(5) 0.033(4) 0.101(7) -0.026(5) 0.003(5) -0.018(4) C23 0.095(8) 0.032(5) 0.095(8) 0.009(5) 0.010(6) -0.002(5) C24 0.064(6) 0.032(4) 0.057(5) -0.012(4) 0.023(4) -0.019(4) C25 0.166(12) 0.108(9) 0.043(6) 0.002(5) 0.014(6) -0.074(8) C27 0.041(5) 0.032(4) 0.040(4) -0.010(3) -0.007(3) -0.008(3) C30 0.028(4) 0.028(4) 0.058(5) -0.007(4) -0.010(3) 0.010(3) C32 0.023(4) 0.066(5) 0.060(5) -0.002(4) 0.012(4) 0.018(4) C31 0.048(5) 0.040(4) 0.070(6) 0.003(4) -0.014(4) 0.022(4) C33 0.027(4) 0.021(3) 0.037(4) -0.001(3) 0.005(3) -0.003(3) C39 0.037(4) 0.028(4) 0.033(4) 0.000(3) 0.003(3) 0.000(3) C34 0.024(4) 0.026(3) 0.028(4) -0.001(3) 0.001(3) 0.005(3) C38 0.045(5) 0.042(4) 0.033(4) 0.008(3) 0.006(4) 0.015(4) C37 0.033(4) 0.075(6) 0.035(5) 0.000(4) -0.008(3) 0.002(4) C35 0.030(4) 0.043(4) 0.037(4) -0.003(3) -0.005(3) -0.005(3) C36 0.040(4) 0.036(4) 0.041(4) -0.005(4) -0.004(4) -0.004(3) C40 0.035(4) 0.023(4) 0.064(5) 0.003(4) -0.002(4) -0.007(3) C41 0.024(4) 0.015(3) 0.037(4) 0.000(3) -0.001(3) 0.002(3) C47 0.029(4) 0.019(3) 0.045(4) -0.003(3) -0.005(3) 0.001(3) C42 0.020(4) 0.017(3) 0.046(4) 0.000(3) -0.010(3) -0.004(3) C43 0.031(4) 0.027(4) 0.057(5) -0.003(3) 0.005(4) -0.002(3) C44 0.024(4) 0.033(4) 0.076(6) 0.006(4) 0.011(4) 0.003(3) C45 0.035(5) 0.036(4) 0.087(7) 0.004(4) 0.003(4) 0.014(4) N1 0.016(3) 0.015(2) 0.042(3) 0.003(2) 0.007(2) -0.0032(18) N2 0.019(3) 0.019(3) 0.030(3) -0.003(2) 0.002(2) -0.006(2) N3 0.016(3) 0.018(2) 0.036(3) 0.001(2) -0.002(2) -0.003(2) N4 0.019(3) 0.019(3) 0.034(3) -0.002(2) 0.011(2) -0.002(2) N5 0.034(4) 0.022(3) 0.049(4) 0.010(3) 0.003(3) -0.001(3) N6 0.023(3) 0.022(3) 0.036(3) -0.006(3) 0.003(3) -0.004(2) N8 0.028(3) 0.016(3) 0.036(3) -0.009(3) 0.003(3) -0.005(2) N7 0.036(4) 0.035(3) 0.033(3) 0.003(3) -0.001(3) 0.002(3) C48 0.041(5) 0.053(5) 0.040(4) -0.002(4) 0.006(3) 0.008(4) Cl1 0.0357(10) 0.0514(11) 0.0470(10) -0.0026(11) -0.0013(10) 0.0040(8) O4 0.070(4) 0.045(3) 0.090(4) 0.013(4) -0.022(4) -0.005(3) O1 0.070(4) 0.037(3) 0.046(3) 0.002(2) 0.000(3) 0.000(3) O3 0.048(4) 0.065(4) 0.124(5) -0.057(4) -0.026(3) 0.023(3) O2 0.043(4) 0.156(7) 0.092(5) 0.026(4) 0.035(3) 0.024(4) C49 0.045(5) 0.045(5) 0.102(7) 0.022(5) -0.011(5) 0.002(4) Cl2 0.082(2) 0.176(3) 0.119(2) 0.064(2) -0.0343(17) -0.079(2) Cl3 0.092(2) 0.0488(13) 0.108(2) 0.0042(14) -0.0037(16) 0.0064(12) Cl4 0.099(2) 0.108(2) 0.097(2) -0.0107(18) -0.0134(17) -0.0209(18) C29 0.044(5) 0.051(5) 0.067(6) -0.008(4) -0.011(4) 0.003(4) C28 0.051(5) 0.025(4) 0.090(6) -0.011(4) -0.004(4) -0.007(4) C26 0.070(7) 0.041(5) 0.174(11) -0.012(6) 0.080(7) -0.009(4) C46 0.048(5) 0.029(4) 0.066(6) 0.011(4) -0.015(4) 0.008(3) C50 0.024(4) 0.073(6) 0.059(5) -0.004(5) -0.009(4) 0.009(4) Cl6 0.0626(15) 0.0589(13) 0.0831(16) -0.0095(13) -0.0084(12) 0.0008(11) Cl7 0.0804(18) 0.104(2) 0.0480(12) 0.0062(13) 0.0083(13) 0.0229(15) Cl5 0.0769(17) 0.0552(13) 0.0786(16) 0.0096(12) 0.0073(13) 0.0027(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 N4 1.905(5) . ? Fe1 N2 1.910(5) . ? Fe1 N1 1.916(4) . ? Fe1 N3 1.927(5) . ? Fe1 N6 2.064(5) . ? Fe1 N8 2.075(5) . ? C4 N1 1.389(7) . ? C4 C5 1.405(8) . ? C4 C3 1.459(8) . ? C1 N1 1.371(7) . ? C1 C20 1.387(8) . ? C1 C2 1.459(8) . ? C2 C3 1.359(9) . ? C2 H2 0.9400 . ? C3 H3 0.9400 . ? C6 N2 1.400(8) . ? C6 C5 1.406(8) . ? C6 C7 1.436(9) . ? C5 C21 1.538(8) . ? C8 C7 1.331(9) . ? C8 C9 1.455(9) . ? C8 H8 0.9400 . ? C7 H7 0.9400 . ? C9 N2 1.359(7) . ? C9 C10 1.423(9) . ? C10 C11 1.390(9) . ? C10 C24 1.512(10) . ? C14 N3 1.387(7) . ? C14 C15 1.400(8) . ? C14 C13 1.433(8) . ? C13 C12 1.350(9) . ? C13 H13 0.9400 . ? C11 N3 1.370(7) . ? C11 C12 1.465(8) . ? C12 H12 0.9400 . ? C15 C16 1.415(8) . ? C15 C27 1.523(9) . ? C16 N4 1.394(7) . ? C16 C17 1.433(9) . ? C19 N4 1.389(7) . ? C19 C18 1.424(8) . ? C19 C20 1.436(8) . ? C17 C18 1.364(9) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C20 C30 1.545(9) . ? C21 C23 1.501(11) . ? C21 C22 1.552(10) . ? C21 H21 0.9900 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C26 1.510(12) . ? C24 C25 1.529(12) . ? C24 H24 0.9900 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C27 C29 1.535(10) . ? C27 C28 1.559(9) . ? C27 H27 0.9900 . ? C30 C32 1.540(10) . ? C30 C31 1.543(9) . ? C30 H30 0.9900 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C33 N5 1.339(8) . ? C33 N6 1.362(7) . ? C33 C40 1.484(9) . ? C39 N5 1.379(8) . ? C39 C34 1.399(9) . ? C39 C38 1.402(9) . ? C34 N6 1.393(8) . ? C34 C35 1.424(9) . ? C38 C37 1.389(10) . ? C38 H38 0.9400 . ? C37 C36 1.413(10) . ? C37 H37 0.9400 . ? C35 C36 1.342(9) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 N8 1.310(8) . ? C41 N7 1.372(8) . ? C41 C48 1.497(9) . ? C47 C42 1.364(9) . ? C47 N7 1.396(8) . ? C47 C46 1.415(9) . ? C42 C43 1.406(9) . ? C42 N8 1.437(8) . ? C43 C44 1.386(9) . ? C43 H43 0.9400 . ? C44 C45 1.376(10) . ? C44 H44 0.9400 . ? C45 C46 1.374(10) . ? C45 H45 0.9400 . ? N5 H5 0.8700 . ? N7 H7A 0.8700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? Cl1 O1 1.405(5) . ? Cl1 O4 1.435(5) . ? Cl1 O3 1.436(6) . ? Cl1 O2 1.460(6) . ? C49 Cl4 1.704(10) . ? C49 Cl2 1.752(9) . ? C49 Cl3 1.762(8) . ? C49 H49 0.9900 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C46 H46 0.9400 . ? C50 Cl7 1.730(8) . ? C50 Cl6 1.773(9) . ? C50 Cl5 1.792(9) . ? C50 H50 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 N4 Fe1 N2 179.5(2) . . ? N4 Fe1 N1 89.8(2) . . ? N2 Fe1 N1 90.5(2) . . ? N4 Fe1 N3 90.9(2) . . ? N2 Fe1 N3 88.8(2) . . ? N1 Fe1 N3 179.2(2) . . ? N4 Fe1 N6 90.9(2) . . ? N2 Fe1 N6 89.5(2) . . ? N1 Fe1 N6 89.7(2) . . ? N3 Fe1 N6 89.9(2) . . ? N4 Fe1 N8 90.9(2) . . ? N2 Fe1 N8 88.74(19) . . ? N1 Fe1 N8 89.6(2) . . ? N3 Fe1 N8 90.8(2) . . ? N6 Fe1 N8 178.1(2) . . ? N1 C4 C5 123.7(5) . . ? N1 C4 C3 106.7(5) . . ? C5 C4 C3 128.7(5) . . ? N1 C1 C20 125.4(6) . . ? N1 C1 C2 108.1(5) . . ? C20 C1 C2 125.4(6) . . ? C3 C2 C1 107.1(6) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 108.5(5) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? N2 C6 C5 123.9(5) . . ? N2 C6 C7 108.7(5) . . ? C5 C6 C7 126.6(6) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 C21 120.8(6) . . ? C6 C5 C21 117.4(5) . . ? C7 C8 C9 108.8(6) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? C8 C7 C6 107.0(6) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? N2 C9 C10 123.3(5) . . ? N2 C9 C8 108.0(5) . . ? C10 C9 C8 127.3(6) . . ? C11 C10 C9 119.4(6) . . ? C11 C10 C24 119.5(6) . . ? C9 C10 C24 120.8(6) . . ? N3 C14 C15 123.9(5) . . ? N3 C14 C13 107.5(5) . . ? C15 C14 C13 127.2(6) . . ? C12 C13 C14 108.2(6) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? N3 C11 C10 126.6(5) . . ? N3 C11 C12 106.5(5) . . ? C10 C11 C12 126.1(6) . . ? C13 C12 C11 108.0(6) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C14 C15 C16 122.5(6) . . ? C14 C15 C27 121.0(6) . . ? C16 C15 C27 116.0(6) . . ? N4 C16 C15 123.6(5) . . ? N4 C16 C17 108.5(6) . . ? C15 C16 C17 126.6(6) . . ? N4 C19 C18 108.5(5) . . ? N4 C19 C20 122.1(5) . . ? C18 C19 C20 128.3(6) . . ? C18 C17 C16 107.3(6) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 108.4(6) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? C1 C20 C19 120.9(6) . . ? C1 C20 C30 117.7(6) . . ? C19 C20 C30 120.9(5) . . ? C23 C21 C5 112.3(5) . . ? C23 C21 C22 115.0(6) . . ? C5 C21 C22 113.4(6) . . ? C23 C21 H21 105.0 . . ? C5 C21 H21 105.0 . . ? C22 C21 H21 105.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C10 114.9(7) . . ? C26 C24 C25 111.2(8) . . ? C10 C24 C25 112.2(7) . . ? C26 C24 H24 105.9 . . ? C10 C24 H24 105.9 . . ? C25 C24 H24 105.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C15 C27 C29 114.8(6) . . ? C15 C27 C28 112.0(6) . . ? C29 C27 C28 111.3(6) . . ? C15 C27 H27 106.0 . . ? C29 C27 H27 106.0 . . ? C28 C27 H27 106.0 . . ? C32 C30 C31 112.1(6) . . ? C32 C30 C20 113.4(5) . . ? C31 C30 C20 111.5(6) . . ? C32 C30 H30 106.4 . . ? C31 C30 H30 106.4 . . ? C20 C30 H30 106.4 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C33 N6 111.3(6) . . ? N5 C33 C40 118.9(6) . . ? N6 C33 C40 129.8(6) . . ? N5 C39 C34 104.8(6) . . ? N5 C39 C38 131.6(6) . . ? C34 C39 C38 123.6(6) . . ? N6 C34 C39 110.1(5) . . ? N6 C34 C35 131.8(6) . . ? C39 C34 C35 118.1(6) . . ? C37 C38 C39 116.3(6) . . ? C37 C38 H38 121.8 . . ? C39 C38 H38 121.8 . . ? C38 C37 C36 120.3(6) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C36 C35 C34 118.6(7) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C35 C36 C37 123.0(7) . . ? C35 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N8 C41 N7 112.6(6) . . ? N8 C41 C48 130.4(6) . . ? N7 C41 C48 116.9(6) . . ? C42 C47 N7 107.0(5) . . ? C42 C47 C46 124.5(7) . . ? N7 C47 C46 128.4(7) . . ? C47 C42 C43 119.8(6) . . ? C47 C42 N8 108.7(6) . . ? C43 C42 N8 131.5(6) . . ? C44 C43 C42 116.0(6) . . ? C44 C43 H43 122.0 . . ? C42 C43 H43 122.0 . . ? C45 C44 C43 123.1(7) . . ? C45 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C46 C45 C44 122.2(7) . . ? C46 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? C1 N1 C4 109.4(5) . . ? C1 N1 Fe1 125.3(4) . . ? C4 N1 Fe1 125.3(4) . . ? C9 N2 C6 107.3(5) . . ? C9 N2 Fe1 127.9(4) . . ? C6 N2 Fe1 124.8(4) . . ? C11 N3 C14 109.6(5) . . ? C11 N3 Fe1 124.7(4) . . ? C14 N3 Fe1 125.6(4) . . ? C19 N4 C16 107.2(5) . . ? C19 N4 Fe1 126.9(4) . . ? C16 N4 Fe1 125.9(4) . . ? C33 N5 C39 109.3(5) . . ? C33 N5 H5 125.4 . . ? C39 N5 H5 125.4 . . ? C33 N6 C34 104.6(5) . . ? C33 N6 Fe1 127.8(4) . . ? C34 N6 Fe1 127.6(4) . . ? C41 N8 C42 105.2(5) . . ? C41 N8 Fe1 127.7(4) . . ? C42 N8 Fe1 125.9(4) . . ? C41 N7 C47 106.5(5) . . ? C41 N7 H7A 126.8 . . ? C47 N7 H7A 126.8 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O1 Cl1 O4 111.6(4) . . ? O1 Cl1 O3 109.9(4) . . ? O4 Cl1 O3 109.0(3) . . ? O1 Cl1 O2 109.0(4) . . ? O4 Cl1 O2 110.4(4) . . ? O3 Cl1 O2 106.9(4) . . ? Cl4 C49 Cl2 112.9(5) . . ? Cl4 C49 Cl3 112.0(5) . . ? Cl2 C49 Cl3 108.7(5) . . ? Cl4 C49 H49 107.7 . . ? Cl2 C49 H49 107.7 . . ? Cl3 C49 H49 107.7 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C45 C46 C47 114.3(7) . . ? C45 C46 H46 122.9 . . ? C47 C46 H46 122.9 . . ? Cl7 C50 Cl6 110.6(5) . . ? Cl7 C50 Cl5 109.4(5) . . ? Cl6 C50 Cl5 108.4(4) . . ? Cl7 C50 H50 109.5 . . ? Cl6 C50 H50 109.5 . . ? Cl5 C50 H50 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.645 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.080 # Attachment '- TiPrPFeHIm2.cif' data_tiprpfehim2 _database_code_depnum_ccdc_archive 'CCDC 807918' #TrackingRef '- TiPrPFeHIm2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(5,10,15,20-tetraisopropylporphyrinato)iron(III) (imidazole)2]perchlorate ; _chemical_name_common '[Fe(TiPrP)(HIm)2]ClO4' _chemical_melting_point ? _chemical_formula_moiety 'C38 H44 Fe N8, Cl O4, C1 H1 Cl3, C6 H12' _chemical_formula_sum 'C45 H57 Cl4 Fe N8 O4' _chemical_formula_weight 971.64 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)/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 9.4670(19) _cell_length_b 40.940(8) _cell_length_c 12.708(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.23(3) _cell_angle_gamma 90.00 _cell_volume 4874.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223 _cell_measurement_reflns_used 5216 _cell_measurement_theta_min 4.354 _cell_measurement_theta_max 49.207 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7649 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details ; XPREP Bruker AXS 2000 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27016 _diffrn_reflns_av_R_equivalents 0.1470 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.69 _reflns_number_total 9256 _reflns_number_gt 5715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^+0.7207P] 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 9256 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2139 _refine_ls_wR_factor_gt 0.1952 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.72355(7) 0.846106(13) 0.24438(4) 0.03016(19) Uani 1 1 d . . . N1 N 0.6344(4) 0.83530(8) 0.3676(2) 0.0317(8) Uani 1 1 d . . . N2 N 0.7302(4) 0.89156(8) 0.2876(2) 0.0346(8) Uani 1 1 d . . . N3 N 0.8108(4) 0.85716(9) 0.1199(2) 0.0392(9) Uani 1 1 d . . . N4 N 0.7181(4) 0.80044(8) 0.2028(2) 0.0352(8) Uani 1 1 d . . . C1 C 0.5477(4) 0.80844(9) 0.3792(3) 0.0333(9) Uani 1 1 d . . . C2 C 0.5007(5) 0.81037(11) 0.4811(3) 0.0424(11) Uani 1 1 d . . . H2 H 0.4379 0.7958 0.5078 0.051 Uiso 1 1 calc R . . C3 C 0.5618(5) 0.83654(11) 0.5319(3) 0.0436(11) Uani 1 1 d . . . H3 H 0.5529 0.8429 0.6017 0.052 Uiso 1 1 calc R . . C4 C 0.6429(5) 0.85327(10) 0.4616(3) 0.0351(10) Uani 1 1 d . . . C5 C 0.7082(5) 0.88387(10) 0.4766(3) 0.0376(10) Uani 1 1 d . . . C6 C 0.7367(5) 0.90252(10) 0.3908(3) 0.0398(10) Uani 1 1 d . . . C7 C 0.7555(7) 0.93733(12) 0.3899(4) 0.0625(15) Uani 1 1 d . . . H7 H 0.7677 0.9510 0.4499 0.075 Uiso 1 1 calc R . . C8 C 0.7527(6) 0.94697(12) 0.2882(4) 0.0604(14) Uani 1 1 d . . . H8 H 0.7561 0.9686 0.2643 0.073 Uiso 1 1 calc R . . C9 C 0.7434(5) 0.91810(11) 0.2228(3) 0.0445(11) Uani 1 1 d . . . C10 C 0.7631(5) 0.91655(11) 0.1161(3) 0.0461(11) Uani 1 1 d . C . C11 C 0.8070(5) 0.88741(12) 0.0722(3) 0.0455(12) Uani 1 1 d . . . C12 C 0.8759(6) 0.88451(16) -0.0211(3) 0.0641(16) Uani 1 1 d . . . H12 H 0.8850 0.9012 -0.0705 0.077 Uiso 1 1 calc R . . C13 C 0.9248(6) 0.85409(16) -0.0255(4) 0.0626(15) Uani 1 1 d . . . H13 H 0.9781 0.8460 -0.0768 0.075 Uiso 1 1 calc R . . C14 C 0.8827(5) 0.83549(13) 0.0615(3) 0.0465(12) Uani 1 1 d . . . C15 C 0.8888(5) 0.80182(13) 0.0752(3) 0.0528(13) Uani 1 1 d . D . C16 C 0.8014(5) 0.78548(11) 0.1366(3) 0.0427(11) Uani 1 1 d . . . C17 C 0.7606(6) 0.75156(12) 0.1301(4) 0.0583(14) Uani 1 1 d . . . H17 H 0.8047 0.7353 0.0942 0.070 Uiso 1 1 calc R . . C18 C 0.6515(6) 0.74688(11) 0.1827(3) 0.0508(12) Uani 1 1 d . . . H18 H 0.6011 0.7272 0.1869 0.061 Uiso 1 1 calc R . . C19 C 0.6238(5) 0.77748(10) 0.2323(3) 0.0386(10) Uani 1 1 d . . . C20 C 0.5323(5) 0.78193(10) 0.3080(3) 0.0387(10) Uani 1 1 d . . . C21 C 0.7399(6) 0.89840(13) 0.5878(3) 0.0590(14) Uani 1 1 d . . . H21 H 0.8023 0.9175 0.5812 0.071 Uiso 1 1 calc R . . C22 C 0.6072(8) 0.91198(16) 0.6292(5) 0.090(2) Uani 1 1 d . . . H22A H 0.5429 0.8942 0.6393 0.136 Uiso 1 1 calc R . . H22B H 0.5592 0.9273 0.5780 0.136 Uiso 1 1 calc R . . H22C H 0.6356 0.9230 0.6964 0.136 Uiso 1 1 calc R . . C23 C 0.8266(8) 0.87539(17) 0.6650(4) 0.091(2) Uani 1 1 d . . . H23A H 0.7643 0.8589 0.6880 0.137 Uiso 1 1 calc R . . H23B H 0.8715 0.8876 0.7262 0.137 Uiso 1 1 calc R . . H23C H 0.8995 0.8650 0.6302 0.137 Uiso 1 1 calc R . . C24 C 0.7480(8) 0.94723(16) 0.0485(5) 0.082(2) Uani 1 1 d . . . H24 H 0.7401 0.9376 -0.0236 0.098 Uiso 1 1 calc R A 1 C26 C 0.8796(8) 0.96764(15) 0.0499(5) 0.090(2) Uani 1 1 d . C . H26A H 0.8636 0.9840 -0.0058 0.135 Uiso 1 1 calc R . . H26B H 0.9589 0.9538 0.0381 0.135 Uiso 1 1 calc R . . H26C H 0.9014 0.9784 0.1183 0.135 Uiso 1 1 calc R . . C27 C 0.9839(6) 0.78273(19) 0.0081(4) 0.082(2) Uani 1 1 d . . . H27 H 0.9849 0.7615 0.0457 0.098 Uiso 1 1 calc R B 3 C28 C 0.9047(6) 0.77190(15) -0.0990(4) 0.0724(17) Uani 1 1 d . D . H28A H 0.9694 0.7600 -0.1377 0.109 Uiso 1 1 calc R . . H28B H 0.8686 0.7909 -0.1396 0.109 Uiso 1 1 calc R . . H28C H 0.8256 0.7579 -0.0878 0.109 Uiso 1 1 calc R . . C30 C 0.4215(6) 0.75554(11) 0.3175(4) 0.0494(12) Uani 1 1 d . . . H30 H 0.4145 0.7426 0.2511 0.059 Uiso 1 1 calc R . . C31 C 0.2721(7) 0.76925(15) 0.3214(5) 0.0779(18) Uani 1 1 d . . . H31A H 0.2665 0.7777 0.3919 0.117 Uiso 1 1 calc R . . H31B H 0.2020 0.7520 0.3049 0.117 Uiso 1 1 calc R . . H31C H 0.2529 0.7867 0.2697 0.117 Uiso 1 1 calc R . . C32 C 0.4666(6) 0.73100(12) 0.4095(4) 0.0663(16) Uani 1 1 d . . . H32A H 0.5587 0.7216 0.4017 0.099 Uiso 1 1 calc R . . H32B H 0.3960 0.7137 0.4070 0.099 Uiso 1 1 calc R . . H32C H 0.4732 0.7423 0.4771 0.099 Uiso 1 1 calc R . . C33 C 0.4986(5) 0.84693(11) 0.0560(3) 0.0421(10) Uani 1 1 d . . . H33 H 0.5617 0.8386 0.0118 0.050 Uiso 1 1 calc R . . C34 C 0.4130(5) 0.86519(14) 0.1921(4) 0.0569(14) Uani 1 1 d . . . H34 H 0.4052 0.8717 0.2619 0.068 Uiso 1 1 calc R . . C35 C 0.3081(6) 0.86649(17) 0.1097(4) 0.0741(18) Uani 1 1 d . . . H35 H 0.2149 0.8743 0.1105 0.089 Uiso 1 1 calc R . . C36 C 0.9477(5) 0.82247(11) 0.4161(3) 0.0437(11) Uani 1 1 d . . . H36 H 0.8865 0.8071 0.4409 0.052 Uiso 1 1 calc R . . C37 C 1.0339(6) 0.85963(14) 0.3238(4) 0.0605(14) Uani 1 1 d . . . H37 H 1.0422 0.8751 0.2705 0.073 Uiso 1 1 calc R . . C38 C 1.1356(6) 0.85274(15) 0.4055(4) 0.0683(16) Uani 1 1 d . . . H38 H 1.2267 0.8622 0.4201 0.082 Uiso 1 1 calc R . . N5 N 0.5323(4) 0.85300(8) 0.1593(2) 0.0343(8) Uani 1 1 d . . . N6 N 0.3623(4) 0.85436(11) 0.0246(3) 0.0576(11) Uani 1 1 d . . . H6 H 0.3162 0.8519 -0.0392 0.069 Uiso 1 1 calc R . . N7 N 0.9156(4) 0.84065(8) 0.3298(2) 0.0362(8) Uani 1 1 d . . . N8 N 1.0803(4) 0.82930(10) 0.4628(3) 0.0525(11) Uani 1 1 d . . . H8A H 1.1237 0.8202 0.5203 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.27597(15) 0.84043(3) 0.72926(8) 0.0577(4) Uani 1 1 d . . . O1 O 0.2399(5) 0.81093(9) 0.6703(3) 0.0849(13) Uani 1 1 d . . . O2 O 0.2498(5) 0.86732(10) 0.6569(3) 0.0883(14) Uani 1 1 d . . . O3 O 0.4231(4) 0.83976(12) 0.7721(3) 0.0882(14) Uani 1 1 d . . . O4 O 0.1962(5) 0.84305(14) 0.8138(3) 0.1026(18) Uani 1 1 d . . . C39 C 0.1981(11) 0.93573(17) 0.7689(7) 0.128(4) Uani 1 1 d . . . H39 H 0.1977 0.9143 0.7327 0.154 Uiso 1 1 calc R . . Cl2 Cl 0.3379(4) 0.95837(7) 0.7447(3) 0.1706(13) Uani 1 1 d . . . Cl3 Cl 0.2036(5) 0.93065(9) 0.9059(3) 0.2045(16) Uani 1 1 d . . . Cl4 Cl 0.0348(5) 0.95560(9) 0.7352(4) 0.273(3) Uani 1 1 d . . . C40 C 0.234(3) 0.9773(5) 0.4236(13) 0.351(16) Uani 1 1 d . . . H40A H 0.1400 0.9865 0.3974 0.421 Uiso 1 1 calc R . . H40B H 0.2512 0.9794 0.5012 0.421 Uiso 1 1 calc R . . C41 C 0.343(3) 0.9940(4) 0.3768(13) 0.279(13) Uani 1 1 d . . . H41A H 0.3367 1.0175 0.3901 0.335 Uiso 1 1 calc R . . H41B H 0.4371 0.9865 0.4105 0.335 Uiso 1 1 calc R . . C42 C 0.331(2) 0.9889(5) 0.2741(16) 0.264(9) Uani 1 1 d . . . H42A H 0.4150 0.9981 0.2481 0.317 Uiso 1 1 calc R . . H42B H 0.2473 1.0008 0.2396 0.317 Uiso 1 1 calc R . . C43 C 0.318(2) 0.9563(4) 0.2420(17) 0.297(13) Uani 1 1 d . . . H43A H 0.4090 0.9450 0.2635 0.356 Uiso 1 1 calc R . . H43B H 0.2965 0.9553 0.1643 0.356 Uiso 1 1 calc R . . C44 C 0.1984(17) 0.9385(3) 0.2915(18) 0.244(9) Uani 1 1 d . . . H44A H 0.1050 0.9485 0.2689 0.293 Uiso 1 1 calc R . . H44B H 0.1940 0.9153 0.2731 0.293 Uiso 1 1 calc R . . C45 C 0.240(3) 0.9429(5) 0.3929(14) 0.349(18) Uani 1 1 d . . . H45A H 0.3382 0.9350 0.4110 0.419 Uiso 1 1 calc R . . H45B H 0.1792 0.9300 0.4335 0.419 Uiso 1 1 calc R . . C25 C 0.6140(16) 0.9634(3) 0.0422(13) 0.089(5) Uani 0.58(2) 1 d P C 1 H25A H 0.5994 0.9770 -0.0210 0.134 Uiso 0.58(2) 1 calc PR C 1 H25B H 0.6130 0.9769 0.1047 0.134 Uiso 0.58(2) 1 calc PR C 1 H25C H 0.5383 0.9473 0.0386 0.134 Uiso 0.58(2) 1 calc PR C 1 C25B C 0.630(2) 0.9471(5) -0.0391(19) 0.111(10) Uani 0.42(2) 1 d P C 2 H25D H 0.5414 0.9426 -0.0117 0.167 Uiso 0.42(2) 1 calc PR C 2 H25E H 0.6462 0.9303 -0.0899 0.167 Uiso 0.42(2) 1 calc PR C 2 H25F H 0.6238 0.9683 -0.0738 0.167 Uiso 0.42(2) 1 calc PR C 2 C29 C 1.1327(13) 0.7889(4) 0.0244(9) 0.078(5) Uani 0.543(17) 1 d P D 3 H29A H 1.1573 0.8017 0.0885 0.117 Uiso 0.543(17) 1 calc PR D 3 H29B H 1.1587 0.8008 -0.0359 0.117 Uiso 0.543(17) 1 calc PR D 3 H29C H 1.1840 0.7683 0.0318 0.117 Uiso 0.543(17) 1 calc PR D 3 C29B C 1.0851(17) 0.7617(5) 0.0592(10) 0.074(6) Uani 0.457(17) 1 d P D 4 H29D H 1.1522 0.7558 0.0114 0.111 Uiso 0.457(17) 1 calc PR D 4 H29E H 1.0385 0.7421 0.0803 0.111 Uiso 0.457(17) 1 calc PR D 4 H29F H 1.1356 0.7723 0.1217 0.111 Uiso 0.457(17) 1 calc PR D 4 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 0.0427(4) 0.0298(3) 0.0171(3) -0.0017(2) 0.0011(2) -0.0026(3) N1 0.043(2) 0.0310(18) 0.0195(16) -0.0026(12) -0.0001(14) 0.0010(16) N2 0.051(2) 0.0260(18) 0.0245(16) 0.0008(13) -0.0015(15) -0.0018(16) N3 0.046(2) 0.054(2) 0.0170(16) 0.0029(14) 0.0018(14) -0.0013(18) N4 0.047(2) 0.0313(19) 0.0245(16) -0.0073(13) -0.0036(14) 0.0042(16) C1 0.042(3) 0.030(2) 0.028(2) 0.0028(16) 0.0021(17) -0.0001(19) C2 0.054(3) 0.042(3) 0.033(2) 0.0076(18) 0.012(2) -0.004(2) C3 0.067(3) 0.043(3) 0.022(2) 0.0018(17) 0.011(2) 0.002(2) C4 0.048(3) 0.036(2) 0.0201(19) -0.0033(16) 0.0034(17) 0.0002(19) C5 0.051(3) 0.035(2) 0.027(2) -0.0081(17) 0.0044(18) -0.004(2) C6 0.057(3) 0.031(2) 0.031(2) -0.0095(17) 0.0029(19) -0.005(2) C7 0.101(5) 0.034(3) 0.054(3) -0.011(2) 0.015(3) -0.018(3) C8 0.093(4) 0.030(3) 0.056(3) 0.003(2) 0.003(3) -0.011(3) C9 0.059(3) 0.034(2) 0.039(2) 0.0024(18) 0.002(2) -0.010(2) C10 0.056(3) 0.041(3) 0.039(2) 0.016(2) -0.001(2) -0.011(2) C11 0.048(3) 0.062(3) 0.025(2) 0.006(2) -0.0014(19) -0.016(2) C12 0.075(4) 0.092(4) 0.026(2) 0.012(3) 0.008(2) -0.025(3) C13 0.059(4) 0.099(5) 0.031(3) -0.007(3) 0.011(2) -0.012(3) C14 0.044(3) 0.078(4) 0.018(2) -0.008(2) 0.0059(18) -0.006(3) C15 0.056(3) 0.070(4) 0.029(2) -0.018(2) -0.003(2) 0.014(3) C16 0.050(3) 0.050(3) 0.026(2) -0.0128(19) -0.0021(19) 0.006(2) C17 0.083(4) 0.044(3) 0.044(3) -0.019(2) -0.004(3) 0.014(3) C18 0.072(4) 0.038(3) 0.038(3) -0.0112(19) -0.003(2) 0.001(2) C19 0.058(3) 0.027(2) 0.026(2) -0.0036(16) -0.0068(19) 0.001(2) C20 0.052(3) 0.027(2) 0.034(2) 0.0021(16) -0.0040(19) -0.004(2) C21 0.093(4) 0.055(3) 0.029(2) -0.017(2) 0.010(2) -0.015(3) C22 0.134(6) 0.074(4) 0.069(4) -0.043(3) 0.035(4) -0.007(4) C23 0.121(6) 0.102(5) 0.038(3) -0.015(3) -0.032(3) 0.000(4) C24 0.109(6) 0.074(4) 0.058(4) 0.034(3) -0.005(3) -0.025(4) C26 0.129(6) 0.062(4) 0.083(4) 0.014(3) 0.027(4) -0.031(4) C27 0.064(4) 0.122(6) 0.059(3) -0.045(3) 0.005(3) 0.016(4) C28 0.080(4) 0.096(5) 0.042(3) -0.033(3) 0.012(3) 0.008(3) C30 0.059(3) 0.038(3) 0.048(3) 0.001(2) 0.000(2) -0.015(2) C31 0.081(5) 0.074(4) 0.074(4) 0.012(3) -0.004(3) -0.025(4) C32 0.085(4) 0.042(3) 0.067(3) 0.012(2) -0.005(3) -0.024(3) C33 0.050(3) 0.045(3) 0.029(2) -0.0086(18) -0.0024(19) -0.001(2) C34 0.047(3) 0.087(4) 0.034(2) -0.015(2) -0.003(2) 0.015(3) C35 0.050(4) 0.114(5) 0.054(3) -0.016(3) -0.008(3) 0.019(3) C36 0.053(3) 0.043(3) 0.033(2) 0.0026(19) 0.000(2) 0.003(2) C37 0.052(3) 0.074(4) 0.053(3) 0.017(3) -0.002(2) -0.014(3) C38 0.047(3) 0.084(4) 0.068(4) 0.010(3) -0.014(3) -0.010(3) N5 0.045(2) 0.0324(19) 0.0246(17) -0.0042(13) 0.0006(15) -0.0033(16) N6 0.055(3) 0.081(3) 0.031(2) -0.0082(19) -0.0138(18) 0.000(2) N7 0.043(2) 0.038(2) 0.0254(17) -0.0031(14) 0.0003(14) 0.0033(17) N8 0.057(3) 0.062(3) 0.034(2) 0.0018(18) -0.0095(18) 0.012(2) Cl1 0.0694(9) 0.0752(9) 0.0260(6) 0.0000(5) -0.0016(5) 0.0048(7) O1 0.136(4) 0.059(2) 0.049(2) 0.0033(17) -0.023(2) 0.005(3) O2 0.145(4) 0.058(3) 0.052(2) 0.0009(18) -0.018(2) 0.010(3) O3 0.064(3) 0.138(4) 0.060(2) 0.019(2) -0.001(2) -0.006(3) O4 0.065(3) 0.199(6) 0.045(2) -0.023(3) 0.0109(19) -0.001(3) C39 0.196(10) 0.047(4) 0.159(8) -0.013(4) 0.084(7) -0.004(5) Cl2 0.192(3) 0.127(2) 0.215(3) -0.004(2) 0.102(3) -0.004(2) Cl3 0.254(4) 0.181(3) 0.199(3) 0.017(2) 0.102(3) -0.036(3) Cl4 0.191(4) 0.137(3) 0.443(7) -0.091(4) -0.125(4) 0.018(3) C40 0.71(5) 0.176(17) 0.204(17) -0.027(13) 0.20(2) -0.07(2) C41 0.53(4) 0.155(13) 0.159(14) -0.047(11) 0.068(19) -0.171(17) C42 0.35(3) 0.179(17) 0.28(2) 0.056(17) 0.13(2) -0.029(17) C43 0.28(2) 0.159(14) 0.49(4) -0.155(19) 0.21(2) -0.071(15) C44 0.181(13) 0.134(11) 0.40(3) -0.069(15) -0.001(16) -0.089(10) C45 0.63(5) 0.176(17) 0.204(17) 0.057(13) -0.05(2) -0.23(2) C25 0.120(11) 0.071(9) 0.073(10) 0.036(7) 0.005(7) 0.014(8) C25B 0.126(17) 0.112(16) 0.081(16) 0.040(13) -0.038(12) 0.017(13) C29 0.076(9) 0.108(13) 0.051(6) -0.025(7) 0.018(5) -0.007(7) C29B 0.063(10) 0.103(14) 0.050(7) -0.019(8) -0.011(6) 0.040(9) _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 N1 1.933(3) . ? Fe1 N2 1.939(3) . ? Fe1 N3 1.940(3) . ? Fe1 N4 1.941(3) . ? Fe1 N5 1.992(4) . ? Fe1 N7 1.993(4) . ? N1 C1 1.393(5) . ? N1 C4 1.396(5) . ? N2 C6 1.378(5) . ? N2 C9 1.380(5) . ? N3 C11 1.377(6) . ? N3 C14 1.395(6) . ? N4 C16 1.377(5) . ? N4 C19 1.384(5) . ? C1 C20 1.407(5) . ? C1 C2 1.431(5) . ? C2 C3 1.338(6) . ? C2 H2 0.9400 . ? C3 C4 1.433(6) . ? C3 H3 0.9400 . ? C4 C5 1.398(6) . ? C5 C6 1.389(6) . ? C5 C21 1.523(5) . ? C6 C7 1.437(6) . ? C7 C8 1.347(7) . ? C7 H7 0.9400 . ? C8 C9 1.441(6) . ? C8 H8 0.9400 . ? C9 C10 1.396(6) . ? C10 C11 1.405(7) . ? C10 C24 1.517(7) . ? C11 C12 1.438(6) . ? C12 C13 1.333(8) . ? C12 H12 0.9400 . ? C13 C14 1.444(7) . ? C13 H13 0.9400 . ? C14 C15 1.389(7) . ? C15 C16 1.389(7) . ? C15 C27 1.538(7) . ? C16 C17 1.441(7) . ? C17 C18 1.321(7) . ? C17 H17 0.9400 . ? C18 C19 1.443(6) . ? C18 H18 0.9400 . ? C19 C20 1.396(6) . ? C20 C30 1.523(6) . ? C21 C23 1.514(8) . ? C21 C22 1.534(8) . ? C21 H21 0.9900 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.422(14) . ? C24 C25B 1.460(18) . ? C24 C26 1.498(8) . ? C24 H24 0.9900 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C29B 1.379(14) . ? C27 C29 1.417(13) . ? C27 C28 1.523(7) . ? C27 H27 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C30 C31 1.529(8) . ? C30 C32 1.554(7) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 N5 1.328(5) . ? C33 N6 1.330(6) . ? C33 H33 0.9400 . ? C34 C35 1.338(7) . ? C34 N5 1.354(6) . ? C34 H34 0.9400 . ? C35 N6 1.355(6) . ? C35 H35 0.9400 . ? C36 N7 1.324(5) . ? C36 N8 1.339(6) . ? C36 H36 0.9400 . ? C37 C38 1.341(7) . ? C37 N7 1.374(6) . ? C37 H37 0.9400 . ? C38 N8 1.354(7) . ? C38 H38 0.9400 . ? N6 H6 0.8700 . ? N8 H8A 0.8700 . ? Cl1 O4 1.402(4) . ? Cl1 O3 1.422(4) . ? Cl1 O2 1.433(4) . ? Cl1 O1 1.436(4) . ? C39 Cl2 1.680(9) . ? C39 Cl4 1.745(10) . ? C39 Cl3 1.747(9) . ? C39 H39 0.9900 . ? C40 C41 1.44(2) . ? C40 C45 1.46(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.311(18) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.396(19) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.55(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.30(2) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C25B H25D 0.9700 . ? C25B H25E 0.9700 . ? C25B H25F 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C29B H29D 0.9700 . ? C29B H29E 0.9700 . ? C29B H29F 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 89.45(14) . . ? N1 Fe1 N3 179.31(16) . . ? N2 Fe1 N3 90.39(15) . . ? N1 Fe1 N4 90.13(14) . . ? N2 Fe1 N4 179.28(14) . . ? N3 Fe1 N4 90.05(15) . . ? N1 Fe1 N5 90.23(14) . . ? N2 Fe1 N5 90.47(14) . . ? N3 Fe1 N5 89.09(14) . . ? N4 Fe1 N5 90.11(14) . . ? N1 Fe1 N7 90.18(14) . . ? N2 Fe1 N7 87.88(14) . . ? N3 Fe1 N7 90.49(15) . . ? N4 Fe1 N7 91.55(14) . . ? N5 Fe1 N7 178.30(14) . . ? C1 N1 C4 106.8(3) . . ? C1 N1 Fe1 126.8(2) . . ? C4 N1 Fe1 126.5(3) . . ? C6 N2 C9 108.4(3) . . ? C6 N2 Fe1 125.2(3) . . ? C9 N2 Fe1 126.0(3) . . ? C11 N3 C14 108.8(4) . . ? C11 N3 Fe1 125.5(3) . . ? C14 N3 Fe1 125.6(3) . . ? C16 N4 C19 108.1(3) . . ? C16 N4 Fe1 126.8(3) . . ? C19 N4 Fe1 125.0(3) . . ? N1 C1 C20 123.3(4) . . ? N1 C1 C2 108.4(3) . . ? C20 C1 C2 127.4(4) . . ? C3 C2 C1 108.2(4) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? C2 C3 C4 108.4(4) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? N1 C4 C5 124.0(4) . . ? N1 C4 C3 108.1(4) . . ? C5 C4 C3 127.6(4) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 C21 118.7(4) . . ? C4 C5 C21 120.0(4) . . ? N2 C6 C5 125.5(4) . . ? N2 C6 C7 107.7(4) . . ? C5 C6 C7 126.1(4) . . ? C8 C7 C6 108.2(4) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 107.7(4) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N2 C9 C10 125.5(4) . . ? N2 C9 C8 107.7(4) . . ? C10 C9 C8 126.3(4) . . ? C9 C10 C11 120.8(4) . . ? C9 C10 C24 119.8(5) . . ? C11 C10 C24 119.2(4) . . ? N3 C11 C10 125.4(4) . . ? N3 C11 C12 107.6(5) . . ? C10 C11 C12 126.3(5) . . ? C13 C12 C11 108.2(5) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 C14 109.0(5) . . ? C12 C13 H13 125.5 . . ? C14 C13 H13 125.5 . . ? C15 C14 N3 125.4(4) . . ? C15 C14 C13 127.4(5) . . ? N3 C14 C13 106.3(5) . . ? C16 C15 C14 122.0(4) . . ? C16 C15 C27 120.7(5) . . ? C14 C15 C27 116.9(5) . . ? N4 C16 C15 124.7(4) . . ? N4 C16 C17 106.9(4) . . ? C15 C16 C17 127.5(4) . . ? C18 C17 C16 109.5(4) . . ? C18 C17 H17 125.3 . . ? C16 C17 H17 125.3 . . ? C17 C18 C19 107.4(5) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C20 125.8(3) . . ? N4 C19 C18 107.9(4) . . ? C20 C19 C18 125.7(4) . . ? C19 C20 C1 121.8(4) . . ? C19 C20 C30 117.7(4) . . ? C1 C20 C30 120.4(4) . . ? C23 C21 C5 112.0(4) . . ? C23 C21 C22 113.4(5) . . ? C5 C21 C22 113.5(5) . . ? C23 C21 H21 105.7 . . ? C5 C21 H21 105.7 . . ? C22 C21 H21 105.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C25B 51.7(10) . . ? C25 C24 C26 118.3(8) . . ? C25B C24 C26 123.7(9) . . ? C25 C24 C10 115.4(6) . . ? C25B C24 C10 115.4(9) . . ? C26 C24 C10 116.4(6) . . ? C25 C24 H24 100.6 . . ? C25B C24 H24 49.1 . . ? C26 C24 H24 100.6 . . ? C10 C24 H24 100.6 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29B C27 C29 55.5(8) . . ? C29B C27 C28 117.3(7) . . ? C29 C27 C28 122.3(6) . . ? C29B C27 C15 118.6(7) . . ? C29 C27 C15 118.5(6) . . ? C28 C27 C15 113.0(5) . . ? C29B C27 H27 42.9 . . ? C29 C27 H27 98.3 . . ? C28 C27 H27 98.3 . . ? C15 C27 H27 98.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 C30 C31 113.2(4) . . ? C20 C30 C32 113.6(4) . . ? C31 C30 C32 111.7(4) . . ? C20 C30 H30 105.9 . . ? C31 C30 H30 105.9 . . ? C32 C30 H30 105.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 N6 109.8(4) . . ? N5 C33 H33 125.1 . . ? N6 C33 H33 125.1 . . ? C35 C34 N5 109.4(4) . . ? C35 C34 H34 125.3 . . ? N5 C34 H34 125.3 . . ? C34 C35 N6 106.6(5) . . ? C34 C35 H35 126.7 . . ? N6 C35 H35 126.7 . . ? N7 C36 N8 109.8(4) . . ? N7 C36 H36 125.1 . . ? N8 C36 H36 125.1 . . ? C38 C37 N7 109.8(5) . . ? C38 C37 H37 125.1 . . ? N7 C37 H37 125.1 . . ? C37 C38 N8 106.0(5) . . ? C37 C38 H38 127.0 . . ? N8 C38 H38 127.0 . . ? C33 N5 C34 106.3(4) . . ? C33 N5 Fe1 125.5(3) . . ? C34 N5 Fe1 128.2(3) . . ? C33 N6 C35 107.9(4) . . ? C33 N6 H6 126.1 . . ? C35 N6 H6 126.1 . . ? C36 N7 C37 105.8(4) . . ? C36 N7 Fe1 126.7(3) . . ? C37 N7 Fe1 126.4(3) . . ? C36 N8 C38 108.7(4) . . ? C36 N8 H8A 125.7 . . ? C38 N8 H8A 125.7 . . ? O4 Cl1 O3 108.3(3) . . ? O4 Cl1 O2 111.7(3) . . ? O3 Cl1 O2 109.3(3) . . ? O4 Cl1 O1 110.5(3) . . ? O3 Cl1 O1 109.3(3) . . ? O2 Cl1 O1 107.8(2) . . ? Cl2 C39 Cl4 113.0(5) . . ? Cl2 C39 Cl3 109.7(6) . . ? Cl4 C39 Cl3 101.5(5) . . ? Cl2 C39 H39 110.8 . . ? Cl4 C39 H39 110.8 . . ? Cl3 C39 H39 110.8 . . ? C41 C40 C45 106.8(19) . . ? C41 C40 H40A 110.4 . . ? C45 C40 H40A 110.4 . . ? C41 C40 H40B 110.4 . . ? C45 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C42 C41 C40 111.7(18) . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41B 109.3 . . ? C40 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? C41 C42 C43 115.8(17) . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C42 C43 C44 111.6(13) . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 101.6(15) . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44B 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.3 . . ? C44 C45 C40 112.1(18) . . ? C44 C45 H45A 109.2 . . ? C40 C45 H45A 109.2 . . ? C44 C45 H45B 109.2 . . ? C40 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? C24 C25B H25D 109.5 . . ? C24 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? C27 C29B H29D 109.5 . . ? C27 C29B H29E 109.5 . . ? C27 C29B H29F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.767 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.087