# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr. Ohgo, Yoshiki' _publ_contact_author_address ; Department of Chemistry Toho University 5-21-16 Omorinishi Ota-ku Tokyo 143-8540 Japan ; _publ_contact_author_email yohgo@med.toho-u.ac.jp _publ_contact_author_fax '81 3 5493 5430' _publ_contact_author_phone '81 3 3762 4151 x2551' _publ_contact_letter ; Please consider this CIF submission for publication as a New manuscript in Chem. Commun ; # TITLE AND AUTHOR LIST _publ_section_title ; An Isocyanide Probe for Heme Electronic Structure: Bis(tert-butyIisocyanide) Complex of Diazaporphyrin Showing a Unique (dxy)2(dxz dyz)3 Ground State ; loop_ _publ_author_name _publ_author_address 'Yoshiki Ohgo' ; Department of Chemistry, School of Medicine, Toho University, Ota-ku, Tokyo 143-8540, Japan. ; 'Saburo Neya' ; Department of Physical Chemistry, Graduate School of Pharmaceutical Sciences, Chiba University, Chiba 263-8522, Japan. ; 'Hidehiro Uekusa' ; Department of Chemistry and Materials Science, Tokyo Institute of Technology, Tokyo152-8551, Japan. ; 'Mikio Nakamura' ; Department of Chemistry, School of Medicine, Toho University, Ota-ku, Tokyo 143-8540, Japan. ; data_[Fe(TBTMDAzP)(4-CNPy)]ClO4 _database_code_depnum_ccdc_archive 'CCDC 606379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [bis(4-cyanopyridine)(2,8,12,18-tetrabutyl- 3,7,13,17-tetramethyl- 5,15-diazaporphyrinate-\/Yk^4^N)]iron(III)perchlorate dichloromethane solvate ; _chemical_name_common ; (bis(4-cyanopyridine)(2,8,12,18-tetrabutyl-3,7,13,17- tetramethyl-5,15-diazaporphyrinate-\/Yk$4!N))iron(iii)perchlorate dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C50 H58 Fe N10, Cl O4, C H2 Cl2' _chemical_formula_sum 'C51 H60 Cl3 Fe N10 O4' _chemical_formula_weight 1039.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.935(4) _cell_length_b 14.355(6) _cell_length_c 15.946(6) _cell_angle_alpha 94.668(8) _cell_angle_beta 109.913(9) _cell_angle_gamma 109.878(9) _cell_volume 2552.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 80 _cell_measurement_reflns_used 31961 _cell_measurement_theta_min 6.1 _cell_measurement_theta_max 54.8 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details ; ABSCOR(Higashi et al., 1968) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 80 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 35216 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.43 _reflns_number_total 11471 _reflns_number_gt 9286 _reflns_threshold_expression >2\s(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992a) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software ; _computing_data_reduction ; MSC/AFC Diffractometer Control Software. Data Reduction: TEXSAN (Molecular Structure Corporation, 1992b) ; _computing_structure_solution SIR-2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SV (Nemoto & Ohashi, 1993)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1749P)^2^+5.0201P] 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 11471 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2634 _refine_ls_wR_factor_gt 0.2436 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max <0.001 _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 0.86618(4) 0.30723(3) 0.21982(3) 0.01119(16) Uani 1 1 d . . . Cl1 Cl 0.38780(8) 0.29363(7) 0.26682(6) 0.0262(2) Uani 1 1 d . . . Cl2 Cl 0.8919(2) 0.06392(16) 0.47270(15) 0.0837(6) Uani 1 1 d . . . Cl3 Cl 1.11356(19) 0.18821(14) 0.45765(14) 0.0782(5) Uani 1 1 d . . . O1 O 0.3442(3) 0.1841(2) 0.2380(2) 0.0314(6) Uani 1 1 d . . . O2 O 0.2867(3) 0.3212(2) 0.2500(2) 0.0383(7) Uani 1 1 d . . . O3 O 0.4642(3) 0.3256(3) 0.3616(3) 0.0557(10) Uani 1 1 d . . . O4 O 0.4524(3) 0.3402(3) 0.2132(3) 0.0478(9) Uani 1 1 d . . . N1 N 1.0223(2) 0.3882(2) 0.31548(19) 0.0153(5) Uani 1 1 d . . . N2 N 0.9282(2) 0.3410(2) 0.12570(19) 0.0135(5) Uani 1 1 d . . . N3 N 0.7096(2) 0.22538(19) 0.12385(18) 0.0122(5) Uani 1 1 d . . . N4 N 0.8040(2) 0.2733(2) 0.31376(18) 0.0142(5) Uani 1 1 d . . . N5 N 0.7522(2) 0.2456(2) -0.01291(18) 0.0140(5) Uani 1 1 d . . . N6 N 0.9817(3) 0.3627(2) 0.4522(2) 0.0201(6) Uani 1 1 d . . . N7 N 0.9115(2) 0.1848(2) 0.22271(18) 0.0139(5) Uani 1 1 d . . . N8 N 1.0298(3) -0.1380(3) 0.2594(3) 0.0411(10) Uani 1 1 d . . . N9 N 0.8222(2) 0.4302(2) 0.21975(18) 0.0130(5) Uani 1 1 d . . . N10 N 0.7302(3) 0.7671(3) 0.2396(3) 0.0374(9) Uani 1 1 d . . . C1 C 1.0524(3) 0.4010(3) 0.4089(2) 0.0192(7) Uani 1 1 d . . . C2 C 1.1796(3) 0.4613(3) 0.4584(3) 0.0260(8) Uani 1 1 d . . . C3 C 1.2269(3) 0.4831(3) 0.3947(3) 0.0260(8) Uani 1 1 d . . . C4 C 1.1283(3) 0.4403(3) 0.3059(2) 0.0181(7) Uani 1 1 d . . . C5 C 1.1361(3) 0.4479(3) 0.2218(2) 0.0185(7) Uani 1 1 d . . . H5 H 1.2103 0.4874 0.2224 0.022 Uiso 1 1 calc R . . C6 C 1.0440(3) 0.4024(2) 0.1380(2) 0.0161(6) Uani 1 1 d . . . C7 C 1.0531(3) 0.4065(2) 0.0497(2) 0.0171(6) Uani 1 1 d . . . C8 C 0.9440(3) 0.3437(2) -0.0151(2) 0.0165(6) Uani 1 1 d . . . C9 C 0.8669(3) 0.3050(2) 0.0329(2) 0.0142(6) Uani 1 1 d . . . C10 C 0.6798(3) 0.2109(2) 0.0306(2) 0.0138(6) Uani 1 1 d . . . C11 C 0.5535(3) 0.1503(2) -0.0193(2) 0.0148(6) Uani 1 1 d . . . C12 C 0.5066(3) 0.1261(2) 0.0447(2) 0.0154(6) Uani 1 1 d . . . C13 C 0.6039(3) 0.1730(2) 0.1334(2) 0.0136(6) Uani 1 1 d . . . C14 C 0.5947(3) 0.1673(2) 0.2173(2) 0.0147(6) Uani 1 1 d . . . H14 H 0.5198 0.1307 0.2169 0.018 Uiso 1 1 calc R . . C15 C 0.6889(3) 0.2121(2) 0.3012(2) 0.0157(6) Uani 1 1 d . . . C16 C 0.6810(3) 0.2010(3) 0.3897(2) 0.0199(7) Uani 1 1 d . . . C17 C 0.7907(3) 0.2576(3) 0.4543(2) 0.0239(7) Uani 1 1 d . . . C18 C 0.8676(3) 0.3029(3) 0.4073(2) 0.0187(7) Uani 1 1 d . . . C19 C 1.2390(4) 0.4865(4) 0.5600(3) 0.0371(10) Uani 1 1 d . . . H19A H 1.2471 0.4275 0.5807 0.056 Uiso 1 1 calc R . . H19B H 1.1916 0.5083 0.5856 0.056 Uiso 1 1 calc R . . H19C H 1.3167 0.5401 0.5791 0.056 Uiso 1 1 calc R . . C20 C 1.3567(4) 0.5332(4) 0.4096(3) 0.0382(10) Uani 1 1 d . . . H20A H 1.3705 0.4964 0.3636 0.046 Uiso 1 1 calc R . . H20B H 1.4049 0.5267 0.4689 0.046 Uiso 1 1 calc R . . C21 C 1.4001(5) 0.6445(5) 0.4062(6) 0.074(2) Uani 1 1 d . . . H21A H 1.4011 0.6848 0.4585 0.089 Uiso 1 1 calc R . . H21B H 1.3469 0.6542 0.3510 0.089 Uiso 1 1 calc R . . C22 C 1.5324(6) 0.6795(7) 0.4073(9) 0.136(5) Uani 1 1 d . . . H22A H 1.5856 0.6749 0.4652 0.163 Uiso 1 1 calc R . . H22B H 1.5315 0.6329 0.3592 0.163 Uiso 1 1 calc R . . C23 C 1.5797(10) 0.7824(8) 0.3945(9) 0.124(4) Uani 1 1 d . . . H23A H 1.5369 0.7846 0.3328 0.185 Uiso 1 1 calc R . . H23B H 1.6629 0.8025 0.4061 0.185 Uiso 1 1 calc R . . H23C H 1.5704 0.8280 0.4362 0.185 Uiso 1 1 calc R . . C24 C 1.1625(3) 0.4698(3) 0.0360(3) 0.0194(7) Uani 1 1 d . . . H24A H 1.2023 0.5337 0.0809 0.023 Uiso 1 1 calc R . . H24B H 1.1379 0.4850 -0.0240 0.023 Uiso 1 1 calc R . . C25 C 1.2522(3) 0.4209(3) 0.0438(3) 0.0263(8) Uani 1 1 d . . . H25A H 1.2129 0.3569 -0.0010 0.032 Uiso 1 1 calc R . . H25B H 1.2779 0.4061 0.1040 0.032 Uiso 1 1 calc R . . C26 C 1.3619(4) 0.4878(3) 0.0290(3) 0.0337(9) Uani 1 1 d . . . H26A H 1.4139 0.4515 0.0335 0.040 Uiso 1 1 calc R . . H26B H 1.3361 0.4990 -0.0326 0.040 Uiso 1 1 calc R . . C27 C 1.4327(4) 0.5892(4) 0.0952(4) 0.0486(13) Uani 1 1 d . . . H27A H 1.3817 0.6253 0.0925 0.073 Uiso 1 1 calc R . . H27B H 1.4973 0.6279 0.0794 0.073 Uiso 1 1 calc R . . H27C H 1.4643 0.5793 0.1561 0.073 Uiso 1 1 calc R . . C28 C 0.9041(3) 0.3177(3) -0.1166(2) 0.0230(7) Uani 1 1 d . . . H28A H 0.9333 0.3782 -0.1377 0.034 Uiso 1 1 calc R . . H28B H 0.8184 0.2879 -0.1446 0.034 Uiso 1 1 calc R . . H28C H 0.9351 0.2701 -0.1329 0.034 Uiso 1 1 calc R . . C29 C 0.4928(3) 0.1216(3) -0.1212(2) 0.0197(7) Uani 1 1 d . . . H29A H 0.4439 0.0501 -0.1405 0.030 Uiso 1 1 calc R . . H29B H 0.5519 0.1370 -0.1473 0.030 Uiso 1 1 calc R . . H29C H 0.4437 0.1592 -0.1414 0.030 Uiso 1 1 calc R . . C30 C 0.3782(3) 0.0660(3) 0.0284(2) 0.0183(6) Uani 1 1 d . . . H30A H 0.3754 0.0346 0.0796 0.022 Uiso 1 1 calc R . . H30B H 0.3425 0.0122 -0.0261 0.022 Uiso 1 1 calc R . . C31 C 0.3046(3) 0.1320(3) 0.0167(2) 0.0199(7) Uani 1 1 d . . . H31A H 0.3459 0.1911 0.0671 0.024 Uiso 1 1 calc R . . H31B H 0.2973 0.1555 -0.0396 0.024 Uiso 1 1 calc R . . C32 C 0.1803(3) 0.0730(3) 0.0138(3) 0.0233(7) Uani 1 1 d . . . H32A H 0.1880 0.0481 0.0694 0.028 Uiso 1 1 calc R . . H32B H 0.1388 0.0147 -0.0374 0.028 Uiso 1 1 calc R . . C33 C 0.1058(4) 0.1377(3) 0.0043(4) 0.0353(10) Uani 1 1 d . . . H33A H 0.1390 0.1886 0.0597 0.053 Uiso 1 1 calc R . . H33B H 0.0250 0.0950 -0.0067 0.053 Uiso 1 1 calc R . . H33C H 0.1068 0.1699 -0.0460 0.053 Uiso 1 1 calc R . . C34 C 0.5696(4) 0.1335(3) 0.3985(3) 0.0269(8) Uani 1 1 d . . . H34A H 0.5018 0.1441 0.3571 0.032 Uiso 1 1 calc R . . H34B H 0.5758 0.1522 0.4603 0.032 Uiso 1 1 calc R . . C35 C 0.5478(4) 0.0214(3) 0.3769(3) 0.0346(10) Uani 1 1 d . . . H35A H 0.6063 0.0079 0.4258 0.042 Uiso 1 1 calc R . . H35B H 0.5586 0.0060 0.3209 0.042 Uiso 1 1 calc R . . C36 C 0.4205(5) -0.0490(4) 0.3658(4) 0.0507(13) Uani 1 1 d . . . H36A H 0.4186 -0.1167 0.3695 0.061 Uiso 1 1 calc R . . H36B H 0.4043 -0.0243 0.4164 0.061 Uiso 1 1 calc R . . C37 C 0.3245(5) -0.0560(5) 0.2790(5) 0.0618(16) Uani 1 1 d . . . H37A H 0.3240 0.0103 0.2754 0.093 Uiso 1 1 calc R . . H37B H 0.2487 -0.1007 0.2770 0.093 Uiso 1 1 calc R . . H37C H 0.3385 -0.0821 0.2283 0.093 Uiso 1 1 calc R . . C38 C 0.8355(4) 0.2735(4) 0.5566(3) 0.0398(11) Uani 1 1 d . . . H38A H 0.7688 0.2530 0.5745 0.060 Uiso 1 1 calc R . . H38B H 0.8846 0.3441 0.5839 0.060 Uiso 1 1 calc R . . H38C H 0.8818 0.2336 0.5767 0.060 Uiso 1 1 calc R . . C39 C 1.0177(3) 0.1905(3) 0.2222(2) 0.0175(6) Uani 1 1 d . . . H39 H 1.0688 0.2509 0.2164 0.021 Uiso 1 1 calc R . . C40 C 1.0536(3) 0.1095(3) 0.2301(2) 0.0192(7) Uani 1 1 d . . . H40 H 1.1275 0.1154 0.2302 0.023 Uiso 1 1 calc R . . C41 C 0.9748(3) 0.0185(3) 0.2379(2) 0.0197(7) Uani 1 1 d . . . C42 C 0.8646(3) 0.0120(3) 0.2371(2) 0.0201(7) Uani 1 1 d . . . H42 H 0.8111 -0.0478 0.2419 0.024 Uiso 1 1 calc R . . C43 C 0.8365(3) 0.0965(2) 0.2289(2) 0.0167(6) Uani 1 1 d . . . H43 H 0.7625 0.0921 0.2277 0.020 Uiso 1 1 calc R . . C44 C 1.0078(3) -0.0680(3) 0.2495(3) 0.0278(8) Uani 1 1 d . . . C45 C 0.7128(3) 0.4236(2) 0.2134(2) 0.0149(6) Uani 1 1 d . . . H45 H 0.6549 0.3601 0.2060 0.018 Uiso 1 1 calc R . . C46 C 0.6833(3) 0.5077(2) 0.2173(2) 0.0170(6) Uani 1 1 d . . . H46 H 0.6074 0.5009 0.2127 0.020 Uiso 1 1 calc R . . C47 C 0.7707(3) 0.6029(2) 0.2283(2) 0.0165(6) Uani 1 1 d . . . C48 C 0.8832(3) 0.6107(2) 0.2343(2) 0.0165(6) Uani 1 1 d . . . H48 H 0.9425 0.6733 0.2416 0.020 Uiso 1 1 calc R . . C49 C 0.9046(3) 0.5223(2) 0.2291(2) 0.0164(6) Uani 1 1 d . . . H49 H 0.9794 0.5271 0.2323 0.020 Uiso 1 1 calc R . . C50 C 0.7467(3) 0.6941(3) 0.2349(3) 0.0245(8) Uani 1 1 d . . . C51 C 1.0448(8) 0.1635(6) 0.5233(6) 0.089(3) Uani 1 1 d . . . H51A H 1.0406 0.2256 0.5478 0.107 Uiso 1 1 calc R . . H51B H 1.0920 0.1433 0.5744 0.107 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 0.0100(2) 0.0084(2) 0.0137(2) 0.00318(17) 0.00378(19) 0.00253(18) Cl1 0.0139(4) 0.0261(5) 0.0322(5) 0.0028(4) 0.0050(4) 0.0053(3) Cl2 0.0917(14) 0.0797(13) 0.0831(13) 0.0153(10) 0.0288(11) 0.0437(11) Cl3 0.0874(13) 0.0657(11) 0.0763(11) 0.0162(9) 0.0223(10) 0.0338(10) O1 0.0268(14) 0.0239(14) 0.0367(15) 0.0043(11) 0.0091(12) 0.0060(12) O2 0.0239(15) 0.0392(18) 0.056(2) 0.0103(15) 0.0172(14) 0.0165(13) O3 0.047(2) 0.048(2) 0.0392(19) -0.0054(16) -0.0128(16) 0.0132(18) O4 0.0346(17) 0.0341(18) 0.079(3) 0.0137(17) 0.0355(19) 0.0049(14) N1 0.0138(13) 0.0099(12) 0.0170(13) 0.0017(10) 0.0038(11) 0.0012(10) N2 0.0111(12) 0.0096(12) 0.0173(13) 0.0032(10) 0.0044(10) 0.0023(10) N3 0.0103(12) 0.0087(12) 0.0150(12) 0.0024(9) 0.0048(10) 0.0008(10) N4 0.0135(13) 0.0109(12) 0.0148(12) 0.0039(10) 0.0031(11) 0.0031(10) N5 0.0140(13) 0.0127(13) 0.0160(12) 0.0041(10) 0.0070(11) 0.0050(10) N6 0.0203(14) 0.0165(14) 0.0167(13) 0.0035(11) 0.0022(12) 0.0045(12) N7 0.0120(12) 0.0111(12) 0.0159(12) 0.0034(10) 0.0035(10) 0.0031(10) N8 0.0324(19) 0.0190(17) 0.073(3) 0.0155(17) 0.019(2) 0.0127(15) N9 0.0129(12) 0.0097(12) 0.0141(12) 0.0030(9) 0.0040(10) 0.0030(10) N10 0.0245(17) 0.0173(16) 0.070(3) 0.0082(16) 0.0186(18) 0.0084(14) C1 0.0196(17) 0.0160(16) 0.0179(15) 0.0038(12) 0.0017(13) 0.0078(13) C2 0.0197(17) 0.0225(18) 0.0221(17) 0.0008(14) 0.0002(14) 0.0016(15) C3 0.0181(17) 0.0225(18) 0.0242(18) -0.0003(14) 0.0017(15) 0.0003(15) C4 0.0118(15) 0.0148(15) 0.0212(16) 0.0026(12) 0.0024(13) 0.0021(12) C5 0.0118(15) 0.0144(15) 0.0268(17) 0.0054(13) 0.0072(13) 0.0025(12) C6 0.0150(15) 0.0120(14) 0.0253(16) 0.0071(12) 0.0108(13) 0.0065(12) C7 0.0189(16) 0.0136(15) 0.0237(16) 0.0081(12) 0.0121(14) 0.0075(13) C8 0.0173(15) 0.0150(15) 0.0221(16) 0.0066(12) 0.0112(13) 0.0078(13) C9 0.0172(15) 0.0117(14) 0.0175(14) 0.0060(11) 0.0084(13) 0.0081(12) C10 0.0146(15) 0.0095(14) 0.0152(14) 0.0023(11) 0.0043(12) 0.0039(12) C11 0.0130(14) 0.0124(14) 0.0159(14) 0.0027(11) 0.0043(12) 0.0029(12) C12 0.0119(14) 0.0119(14) 0.0185(15) 0.0023(12) 0.0039(12) 0.0024(12) C13 0.0110(14) 0.0108(14) 0.0176(15) 0.0035(11) 0.0057(12) 0.0027(12) C14 0.0140(14) 0.0117(14) 0.0201(15) 0.0057(12) 0.0099(13) 0.0032(12) C15 0.0188(16) 0.0128(15) 0.0175(15) 0.0065(12) 0.0092(13) 0.0058(13) C16 0.0228(17) 0.0192(16) 0.0165(15) 0.0062(13) 0.0087(14) 0.0052(14) C17 0.0263(18) 0.0249(18) 0.0162(16) 0.0071(13) 0.0078(14) 0.0050(15) C18 0.0225(17) 0.0169(16) 0.0156(15) 0.0047(12) 0.0058(13) 0.0079(14) C19 0.024(2) 0.044(3) 0.0198(18) -0.0003(17) -0.0031(16) -0.0018(18) C20 0.0194(19) 0.043(3) 0.034(2) 0.0012(19) 0.0029(17) 0.0008(18) C21 0.037(3) 0.046(3) 0.095(5) 0.029(3) -0.004(3) -0.007(2) C22 0.031(3) 0.082(6) 0.216(12) 0.077(7) -0.012(5) -0.017(3) C23 0.089(7) 0.105(8) 0.163(11) 0.055(8) 0.038(7) 0.029(6) C24 0.0176(16) 0.0172(16) 0.0268(17) 0.0081(13) 0.0133(14) 0.0055(13) C25 0.0227(18) 0.0213(18) 0.042(2) 0.0094(16) 0.0208(17) 0.0088(15) C26 0.0219(19) 0.040(2) 0.042(2) 0.0094(19) 0.0192(18) 0.0086(17) C27 0.018(2) 0.033(2) 0.084(4) 0.009(2) 0.013(2) 0.0055(18) C28 0.0255(18) 0.0213(17) 0.0231(17) 0.0052(14) 0.0150(15) 0.0049(14) C29 0.0158(16) 0.0197(17) 0.0161(15) 0.0009(13) 0.0037(13) 0.0012(13) C30 0.0120(15) 0.0161(15) 0.0208(15) 0.0035(12) 0.0039(13) 0.0012(12) C31 0.0132(15) 0.0185(16) 0.0246(17) 0.0049(13) 0.0068(13) 0.0031(13) C32 0.0146(16) 0.0205(17) 0.0311(18) 0.0044(14) 0.0090(14) 0.0027(14) C33 0.0216(19) 0.030(2) 0.057(3) 0.0100(19) 0.020(2) 0.0093(17) C34 0.0252(19) 0.033(2) 0.0183(16) 0.0075(15) 0.0125(15) 0.0022(16) C35 0.036(2) 0.027(2) 0.029(2) 0.0096(16) 0.0117(18) -0.0030(17) C36 0.047(3) 0.038(3) 0.054(3) 0.012(2) 0.028(3) -0.006(2) C37 0.042(3) 0.049(3) 0.082(4) 0.003(3) 0.027(3) 0.003(3) C38 0.038(2) 0.051(3) 0.0152(17) 0.0100(17) 0.0077(17) 0.001(2) C39 0.0160(15) 0.0144(15) 0.0238(16) 0.0067(12) 0.0093(13) 0.0058(13) C40 0.0157(15) 0.0157(16) 0.0270(17) 0.0052(13) 0.0084(14) 0.0070(13) C41 0.0189(16) 0.0119(15) 0.0249(16) 0.0024(12) 0.0055(14) 0.0055(13) C42 0.0196(16) 0.0114(15) 0.0275(17) 0.0057(13) 0.0080(14) 0.0050(13) C43 0.0133(15) 0.0113(15) 0.0226(16) 0.0033(12) 0.0065(13) 0.0023(12) C44 0.0230(18) 0.0189(18) 0.044(2) 0.0095(16) 0.0149(17) 0.0091(15) C45 0.0132(14) 0.0114(14) 0.0173(14) 0.0037(11) 0.0049(12) 0.0025(12) C46 0.0142(15) 0.0158(16) 0.0206(15) 0.0056(12) 0.0059(13) 0.0063(13) C47 0.0171(15) 0.0110(14) 0.0197(15) 0.0026(12) 0.0058(13) 0.0050(12) C48 0.0165(15) 0.0108(14) 0.0220(15) 0.0048(12) 0.0086(13) 0.0039(12) C49 0.0150(15) 0.0130(15) 0.0213(15) 0.0053(12) 0.0079(13) 0.0044(12) C50 0.0160(16) 0.0153(17) 0.041(2) 0.0068(15) 0.0105(16) 0.0048(13) C51 0.111(7) 0.065(5) 0.073(5) 0.002(4) -0.002(5) 0.056(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 N1 1.942(3) . ? Fe1 N3 1.950(3) . ? Fe1 N4 1.950(3) . ? Fe1 N2 1.950(3) . ? Fe1 N9 2.031(3) . ? Fe1 N7 2.032(3) . ? Cl1 O3 1.426(4) . ? Cl1 O2 1.438(3) . ? Cl1 O4 1.440(4) . ? Cl1 O1 1.451(3) . ? Cl2 C51 1.846(9) . ? Cl3 C51 1.579(10) . ? N1 C1 1.384(4) . ? N1 C4 1.388(4) . ? N2 C9 1.373(4) . ? N2 C6 1.390(4) . ? N3 C10 1.382(4) . ? N3 C13 1.385(4) . ? N4 C15 1.380(4) . ? N4 C18 1.380(4) . ? N5 C9 1.327(4) . ? N5 C10 1.337(4) . ? N6 C18 1.321(5) . ? N6 C1 1.329(5) . ? N7 C43 1.344(4) . ? N7 C39 1.351(4) . ? N8 C44 1.142(5) . ? N9 C49 1.344(4) . ? N9 C45 1.353(4) . ? N10 C50 1.140(5) . ? C1 C2 1.454(5) . ? C2 C3 1.361(6) . ? C2 C19 1.487(5) . ? C3 C4 1.450(5) . ? C3 C20 1.508(6) . ? C4 C5 1.391(5) . ? C5 C6 1.369(5) . ? C5 H5 0.9300 . ? C6 C7 1.458(5) . ? C7 C8 1.364(5) . ? C7 C24 1.498(4) . ? C8 C9 1.450(4) . ? C8 C28 1.493(5) . ? C10 C11 1.447(4) . ? C11 C12 1.366(5) . ? C11 C29 1.494(4) . ? C12 C13 1.447(4) . ? C12 C30 1.506(4) . ? C13 C14 1.389(5) . ? C14 C15 1.380(5) . ? C14 H14 0.9300 . ? C15 C16 1.467(4) . ? C16 C17 1.349(5) . ? C16 C34 1.498(5) . ? C17 C18 1.456(5) . ? C17 C38 1.502(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.515(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.604(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.455(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.524(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.527(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.503(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.536(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.523(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.531(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.524(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.550(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.481(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.391(5) . ? C39 H39 0.9300 . ? C40 C41 1.403(5) . ? C40 H40 0.9300 . ? C41 C42 1.392(5) . ? C41 C44 1.450(5) . ? C42 C43 1.384(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C45 C46 1.386(4) . ? C45 H45 0.9300 . ? C46 C47 1.396(5) . ? C46 H46 0.9300 . ? C47 C48 1.390(5) . ? C47 C50 1.449(5) . ? C48 C49 1.388(4) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 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 N3 179.72(11) . . ? N1 Fe1 N4 89.19(12) . . ? N3 Fe1 N4 90.78(12) . . ? N1 Fe1 N2 90.90(12) . . ? N3 Fe1 N2 89.13(12) . . ? N4 Fe1 N2 179.91(14) . . ? N1 Fe1 N9 90.13(11) . . ? N3 Fe1 N9 90.14(11) . . ? N4 Fe1 N9 89.11(11) . . ? N2 Fe1 N9 90.88(11) . . ? N1 Fe1 N7 89.07(11) . . ? N3 Fe1 N7 90.66(11) . . ? N4 Fe1 N7 90.03(11) . . ? N2 Fe1 N7 89.98(11) . . ? N9 Fe1 N7 178.83(10) . . ? O3 Cl1 O2 110.5(2) . . ? O3 Cl1 O4 110.1(3) . . ? O2 Cl1 O4 109.0(2) . . ? O3 Cl1 O1 109.8(2) . . ? O2 Cl1 O1 108.48(19) . . ? O4 Cl1 O1 108.8(2) . . ? C1 N1 C4 105.2(3) . . ? C1 N1 Fe1 126.6(2) . . ? C4 N1 Fe1 128.1(2) . . ? C9 N2 C6 105.5(3) . . ? C9 N2 Fe1 126.7(2) . . ? C6 N2 Fe1 127.7(2) . . ? C10 N3 C13 105.1(3) . . ? C10 N3 Fe1 126.7(2) . . ? C13 N3 Fe1 128.2(2) . . ? C15 N4 C18 105.6(3) . . ? C15 N4 Fe1 127.6(2) . . ? C18 N4 Fe1 126.8(2) . . ? C9 N5 C10 121.3(3) . . ? C18 N6 C1 121.8(3) . . ? C43 N7 C39 118.6(3) . . ? C43 N7 Fe1 119.6(2) . . ? C39 N7 Fe1 121.8(2) . . ? C49 N9 C45 118.1(3) . . ? C49 N9 Fe1 119.7(2) . . ? C45 N9 Fe1 122.2(2) . . ? N6 C1 N1 127.9(3) . . ? N6 C1 C2 121.6(3) . . ? N1 C1 C2 110.5(3) . . ? C3 C2 C1 106.9(3) . . ? C3 C2 C19 130.1(4) . . ? C1 C2 C19 123.0(4) . . ? C2 C3 C4 106.7(3) . . ? C2 C3 C20 128.1(4) . . ? C4 C3 C20 124.9(4) . . ? N1 C4 C5 123.4(3) . . ? N1 C4 C3 110.6(3) . . ? C5 C4 C3 125.9(3) . . ? C6 C5 C4 125.6(3) . . ? C6 C5 H5 117.2 . . ? C4 C5 H5 117.2 . . ? C5 C6 N2 124.1(3) . . ? C5 C6 C7 125.7(3) . . ? N2 C6 C7 110.1(3) . . ? C8 C7 C6 106.5(3) . . ? C8 C7 C24 128.3(3) . . ? C6 C7 C24 125.1(3) . . ? C7 C8 C9 106.8(3) . . ? C7 C8 C28 129.3(3) . . ? C9 C8 C28 123.9(3) . . ? N5 C9 N2 128.3(3) . . ? N5 C9 C8 120.8(3) . . ? N2 C9 C8 110.9(3) . . ? N5 C10 N3 127.7(3) . . ? N5 C10 C11 121.4(3) . . ? N3 C10 C11 110.9(3) . . ? C12 C11 C10 106.6(3) . . ? C12 C11 C29 129.3(3) . . ? C10 C11 C29 124.1(3) . . ? C11 C12 C13 106.8(3) . . ? C11 C12 C30 127.6(3) . . ? C13 C12 C30 125.5(3) . . ? N3 C13 C14 123.8(3) . . ? N3 C13 C12 110.6(3) . . ? C14 C13 C12 125.5(3) . . ? C15 C14 C13 124.6(3) . . ? C15 C14 H14 117.7 . . ? C13 C14 H14 117.7 . . ? N4 C15 C14 124.9(3) . . ? N4 C15 C16 110.4(3) . . ? C14 C15 C16 124.7(3) . . ? C17 C16 C15 106.3(3) . . ? C17 C16 C34 130.5(3) . . ? C15 C16 C34 123.0(3) . . ? C16 C17 C18 107.5(3) . . ? C16 C17 C38 129.9(4) . . ? C18 C17 C38 122.6(3) . . ? N6 C18 N4 127.7(3) . . ? N6 C18 C17 122.1(3) . . ? N4 C18 C17 110.3(3) . . ? C2 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C3 C20 C21 115.6(5) . . ? C3 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? C3 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C20 C21 C22 108.4(6) . . ? C20 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? C20 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C23 C22 C21 113.9(9) . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 C25 114.9(3) . . ? C7 C24 H24A 108.5 . . ? C25 C24 H24A 108.5 . . ? C7 C24 H24B 108.5 . . ? C25 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 113.1(3) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 114.6(4) . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? C25 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C8 C28 H28A 109.5 . . ? C8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C11 C29 H29A 109.5 . . ? C11 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C11 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C12 C30 C31 112.5(3) . . ? C12 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C12 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C32 C31 C30 111.4(3) . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C33 112.6(3) . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C16 C34 C35 112.5(3) . . ? C16 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C16 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C34 C35 C36 112.2(4) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C35 114.2(4) . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C17 C38 H38A 109.5 . . ? C17 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C17 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 122.7(3) . . ? N7 C39 H39 118.7 . . ? C40 C39 H39 118.7 . . ? C39 C40 C41 117.9(3) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? C42 C41 C40 119.6(3) . . ? C42 C41 C44 119.4(3) . . ? C40 C41 C44 121.0(3) . . ? C43 C42 C41 118.5(3) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? N7 C43 C42 122.8(3) . . ? N7 C43 H43 118.6 . . ? C42 C43 H43 118.6 . . ? N8 C44 C41 177.2(4) . . ? N9 C45 C46 122.7(3) . . ? N9 C45 H45 118.6 . . ? C46 C45 H45 118.6 . . ? C45 C46 C47 118.3(3) . . ? C45 C46 H46 120.9 . . ? C47 C46 H46 120.9 . . ? C48 C47 C46 119.6(3) . . ? C48 C47 C50 119.3(3) . . ? C46 C47 C50 121.2(3) . . ? C49 C48 C47 118.2(3) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? N9 C49 C48 123.1(3) . . ? N9 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? N10 C50 C47 178.3(4) . . ? Cl3 C51 Cl2 116.7(5) . . ? Cl3 C51 H51A 108.1 . . ? Cl2 C51 H51A 108.1 . . ? Cl3 C51 H51B 108.1 . . ? Cl2 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Fe1 N1 C1 1.4(3) . . . . ? N2 Fe1 N1 C1 -178.7(3) . . . . ? N9 Fe1 N1 C1 90.5(3) . . . . ? N7 Fe1 N1 C1 -88.7(3) . . . . ? N4 Fe1 N1 C4 177.2(3) . . . . ? N2 Fe1 N1 C4 -2.8(3) . . . . ? N9 Fe1 N1 C4 -93.7(3) . . . . ? N7 Fe1 N1 C4 87.2(3) . . . . ? N1 Fe1 N2 C9 176.4(3) . . . . ? N3 Fe1 N2 C9 -3.3(3) . . . . ? N9 Fe1 N2 C9 -93.4(3) . . . . ? N7 Fe1 N2 C9 87.4(3) . . . . ? N1 Fe1 N2 C6 -0.4(3) . . . . ? N3 Fe1 N2 C6 179.9(3) . . . . ? N9 Fe1 N2 C6 89.7(3) . . . . ? N7 Fe1 N2 C6 -89.5(3) . . . . ? N4 Fe1 N3 C10 179.8(3) . . . . ? N2 Fe1 N3 C10 -0.2(3) . . . . ? N9 Fe1 N3 C10 90.7(3) . . . . ? N7 Fe1 N3 C10 -90.2(3) . . . . ? N4 Fe1 N3 C13 2.6(3) . . . . ? N2 Fe1 N3 C13 -177.4(3) . . . . ? N9 Fe1 N3 C13 -86.5(3) . . . . ? N7 Fe1 N3 C13 92.7(3) . . . . ? N1 Fe1 N4 C15 -179.4(3) . . . . ? N3 Fe1 N4 C15 0.3(3) . . . . ? N9 Fe1 N4 C15 90.5(3) . . . . ? N7 Fe1 N4 C15 -90.3(3) . . . . ? N1 Fe1 N4 C18 -2.0(3) . . . . ? N3 Fe1 N4 C18 177.7(3) . . . . ? N9 Fe1 N4 C18 -92.1(3) . . . . ? N7 Fe1 N4 C18 87.1(3) . . . . ? N1 Fe1 N7 C43 130.2(3) . . . . ? N3 Fe1 N7 C43 -49.8(3) . . . . ? N4 Fe1 N7 C43 41.0(3) . . . . ? N2 Fe1 N7 C43 -138.9(3) . . . . ? N1 Fe1 N7 C39 -47.1(3) . . . . ? N3 Fe1 N7 C39 132.9(3) . . . . ? N4 Fe1 N7 C39 -136.3(3) . . . . ? N2 Fe1 N7 C39 43.8(3) . . . . ? N1 Fe1 N9 C49 39.3(3) . . . . ? N3 Fe1 N9 C49 -140.8(2) . . . . ? N4 Fe1 N9 C49 128.5(3) . . . . ? N2 Fe1 N9 C49 -51.6(3) . . . . ? N1 Fe1 N9 C45 -138.6(3) . . . . ? N3 Fe1 N9 C45 41.3(3) . . . . ? N4 Fe1 N9 C45 -49.4(3) . . . . ? N2 Fe1 N9 C45 130.5(3) . . . . ? C18 N6 C1 N1 1.2(6) . . . . ? C18 N6 C1 C2 -175.9(3) . . . . ? C4 N1 C1 N6 -177.9(3) . . . . ? Fe1 N1 C1 N6 -1.2(5) . . . . ? C4 N1 C1 C2 -0.5(4) . . . . ? Fe1 N1 C1 C2 176.1(2) . . . . ? N6 C1 C2 C3 176.2(3) . . . . ? N1 C1 C2 C3 -1.3(4) . . . . ? N6 C1 C2 C19 -1.5(6) . . . . ? N1 C1 C2 C19 -179.0(4) . . . . ? C1 C2 C3 C4 2.5(4) . . . . ? C19 C2 C3 C4 180.0(4) . . . . ? C1 C2 C3 C20 -172.4(4) . . . . ? C19 C2 C3 C20 5.1(8) . . . . ? C1 N1 C4 C5 -178.5(3) . . . . ? Fe1 N1 C4 C5 4.9(5) . . . . ? C1 N1 C4 C3 2.1(4) . . . . ? Fe1 N1 C4 C3 -174.4(2) . . . . ? C2 C3 C4 N1 -3.0(4) . . . . ? C20 C3 C4 N1 172.1(4) . . . . ? C2 C3 C4 C5 177.7(3) . . . . ? C20 C3 C4 C5 -7.2(6) . . . . ? N1 C4 C5 C6 -3.3(5) . . . . ? C3 C4 C5 C6 176.0(3) . . . . ? C4 C5 C6 N2 -0.1(5) . . . . ? C4 C5 C6 C7 -177.0(3) . . . . ? C9 N2 C6 C5 -175.6(3) . . . . ? Fe1 N2 C6 C5 1.8(5) . . . . ? C9 N2 C6 C7 1.7(3) . . . . ? Fe1 N2 C6 C7 179.1(2) . . . . ? C5 C6 C7 C8 174.5(3) . . . . ? N2 C6 C7 C8 -2.7(4) . . . . ? C5 C6 C7 C24 -6.4(5) . . . . ? N2 C6 C7 C24 176.4(3) . . . . ? C6 C7 C8 C9 2.5(3) . . . . ? C24 C7 C8 C9 -176.6(3) . . . . ? C6 C7 C8 C28 -178.5(3) . . . . ? C24 C7 C8 C28 2.4(6) . . . . ? C10 N5 C9 N2 -1.2(5) . . . . ? C10 N5 C9 C8 -178.9(3) . . . . ? C6 N2 C9 N5 -177.9(3) . . . . ? Fe1 N2 C9 N5 4.7(5) . . . . ? C6 N2 C9 C8 -0.1(3) . . . . ? Fe1 N2 C9 C8 -177.5(2) . . . . ? C7 C8 C9 N5 176.4(3) . . . . ? C28 C8 C9 N5 -2.6(5) . . . . ? C7 C8 C9 N2 -1.6(4) . . . . ? C28 C8 C9 N2 179.4(3) . . . . ? C9 N5 C10 N3 -3.0(5) . . . . ? C9 N5 C10 C11 176.9(3) . . . . ? C13 N3 C10 N5 -179.0(3) . . . . ? Fe1 N3 C10 N5 3.3(5) . . . . ? C13 N3 C10 C11 1.1(3) . . . . ? Fe1 N3 C10 C11 -176.6(2) . . . . ? N5 C10 C11 C12 179.0(3) . . . . ? N3 C10 C11 C12 -1.2(4) . . . . ? N5 C10 C11 C29 -0.3(5) . . . . ? N3 C10 C11 C29 179.6(3) . . . . ? C10 C11 C12 C13 0.7(3) . . . . ? C29 C11 C12 C13 179.9(3) . . . . ? C10 C11 C12 C30 178.5(3) . . . . ? C29 C11 C12 C30 -2.3(6) . . . . ? C10 N3 C13 C14 179.4(3) . . . . ? Fe1 N3 C13 C14 -3.0(4) . . . . ? C10 N3 C13 C12 -0.7(3) . . . . ? Fe1 N3 C13 C12 177.0(2) . . . . ? C11 C12 C13 N3 0.0(4) . . . . ? C30 C12 C13 N3 -177.9(3) . . . . ? C11 C12 C13 C14 179.9(3) . . . . ? C30 C12 C13 C14 2.0(5) . . . . ? N3 C13 C14 C15 -0.4(5) . . . . ? C12 C13 C14 C15 179.6(3) . . . . ? C18 N4 C15 C14 178.9(3) . . . . ? Fe1 N4 C15 C14 -3.3(5) . . . . ? C18 N4 C15 C16 -1.4(4) . . . . ? Fe1 N4 C15 C16 176.4(2) . . . . ? C13 C14 C15 N4 3.7(5) . . . . ? C13 C14 C15 C16 -176.0(3) . . . . ? N4 C15 C16 C17 1.4(4) . . . . ? C14 C15 C16 C17 -178.9(3) . . . . ? N4 C15 C16 C34 -175.8(3) . . . . ? C14 C15 C16 C34 3.9(5) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C34 C16 C17 C18 176.2(4) . . . . ? C15 C16 C17 C38 -179.0(4) . . . . ? C34 C16 C17 C38 -2.1(7) . . . . ? C1 N6 C18 N4 -1.9(6) . . . . ? C1 N6 C18 C17 177.6(3) . . . . ? C15 N4 C18 N6 -179.4(3) . . . . ? Fe1 N4 C18 N6 2.7(5) . . . . ? C15 N4 C18 C17 1.0(4) . . . . ? Fe1 N4 C18 C17 -176.9(2) . . . . ? C16 C17 C18 N6 -179.7(3) . . . . ? C38 C17 C18 N6 -1.3(6) . . . . ? C16 C17 C18 N4 -0.1(4) . . . . ? C38 C17 C18 N4 178.3(4) . . . . ? C2 C3 C20 C21 -101.7(6) . . . . ? C4 C3 C20 C21 84.3(6) . . . . ? C3 C20 C21 C22 -171.0(6) . . . . ? C20 C21 C22 C23 173.9(10) . . . . ? C8 C7 C24 C25 -96.0(4) . . . . ? C6 C7 C24 C25 85.1(4) . . . . ? C7 C24 C25 C26 179.7(3) . . . . ? C24 C25 C26 C27 59.6(5) . . . . ? C11 C12 C30 C31 -84.7(4) . . . . ? C13 C12 C30 C31 92.7(4) . . . . ? C12 C30 C31 C32 -172.0(3) . . . . ? C30 C31 C32 C33 178.7(3) . . . . ? C17 C16 C34 C35 -100.9(5) . . . . ? C15 C16 C34 C35 75.5(4) . . . . ? C16 C34 C35 C36 -167.8(3) . . . . ? C34 C35 C36 C37 74.3(6) . . . . ? C43 N7 C39 C40 -1.6(5) . . . . ? Fe1 N7 C39 C40 175.8(3) . . . . ? N7 C39 C40 C41 0.6(5) . . . . ? C39 C40 C41 C42 0.3(5) . . . . ? C39 C40 C41 C44 -177.9(3) . . . . ? C40 C41 C42 C43 -0.3(5) . . . . ? C44 C41 C42 C43 178.0(3) . . . . ? C39 N7 C43 C42 1.6(5) . . . . ? Fe1 N7 C43 C42 -175.8(3) . . . . ? C41 C42 C43 N7 -0.7(5) . . . . ? C49 N9 C45 C46 -0.9(5) . . . . ? Fe1 N9 C45 C46 177.1(2) . . . . ? N9 C45 C46 C47 0.0(5) . . . . ? C45 C46 C47 C48 0.4(5) . . . . ? C45 C46 C47 C50 -178.7(3) . . . . ? C46 C47 C48 C49 0.0(5) . . . . ? C50 C47 C48 C49 179.1(3) . . . . ? C45 N9 C49 C48 1.3(5) . . . . ? Fe1 N9 C49 C48 -176.7(2) . . . . ? C47 C48 C49 N9 -0.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.248 _refine_diff_density_min -1.950 _refine_diff_density_rms 0.157