# 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 _publ_contact_author_name 'Sankar Rath' _publ_contact_author_email SPRATH@IITK.AC.IN _publ_section_title ; Effects of Axial Pyridine Coordination on Geometry and Electronic Structure: Stabilization of Hexa-coordinated High-Spin Fe(III) and Air-stable Low-Spin Iron(II) Complexes in a Highly Saddle-distorted Porphyrin ; loop_ _publ_author_name 'Sankar Rath' 'Sudip Kumar Ghosh' 'Ranjan Patra' # Attachment '12augb.cif' data_12augb _database_code_depnum_ccdc_archive 'CCDC 755822' #TrackingRef '12augb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(tn-OEP)(pyridine)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H50 Fe N10 O8' _chemical_formula_weight 926.81 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.4183(11) _cell_length_b 25.469(2) _cell_length_c 26.501(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9056.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.4 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9246 _exptl_absorpt_correction_T_max 0.9575 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46993 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15904 _reflns_number_gt 12674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0565P)^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 0.471(13) _refine_ls_number_reflns 15904 _refine_ls_number_parameters 1188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.58431(4) 0.62451(2) 0.12038(2) 0.01726(13) Uani 1 1 d . . . O1 O 0.9094(3) 0.70592(12) 0.03064(11) 0.0403(8) Uani 1 1 d . . . O2 O 0.9759(2) 0.68912(11) 0.10378(12) 0.0353(8) Uani 1 1 d . . . O3 O 0.7492(2) 0.45053(12) 0.20501(11) 0.0355(8) Uani 1 1 d . . . O4 O 0.7024(2) 0.41894(11) 0.13286(11) 0.0352(8) Uani 1 1 d . . . O5 O 0.2539(2) 0.53360(12) 0.04712(12) 0.0385(8) Uani 1 1 d . . . O6 O 0.1920(2) 0.55809(12) 0.11852(13) 0.0363(8) Uani 1 1 d . . . O7 O 0.4732(3) 0.83148(12) 0.10207(12) 0.0405(8) Uani 1 1 d . . . O8 O 0.4179(2) 0.80998(12) 0.17573(12) 0.0397(8) Uani 1 1 d . . . N1 N 0.6440(2) 0.69439(12) 0.11576(12) 0.0173(7) Uani 1 1 d . . . N2 N 0.7178(2) 0.59251(11) 0.11926(13) 0.0192(7) Uani 1 1 d . . . N3 N 0.5237(2) 0.55520(12) 0.12957(11) 0.0183(7) Uani 1 1 d . . . N4 N 0.4513(2) 0.65595(12) 0.11508(12) 0.0192(7) Uani 1 1 d . . . N5 N 0.5868(2) 0.63327(13) 0.19590(11) 0.0194(7) Uani 1 1 d . . . N6 N 0.5825(2) 0.61695(12) 0.04562(11) 0.0185(7) Uani 1 1 d . . . N7 N 0.9062(3) 0.68879(13) 0.07403(14) 0.0278(9) Uani 1 1 d . . . N8 N 0.7107(3) 0.45505(13) 0.16352(14) 0.0264(8) Uani 1 1 d . . . N9 N 0.2609(3) 0.55441(14) 0.08821(14) 0.0267(8) Uani 1 1 d . . . N10 N 0.4600(3) 0.80039(14) 0.13638(15) 0.0308(9) Uani 1 1 d . . . C1 C 0.5995(3) 0.74067(15) 0.13110(14) 0.0205(9) Uani 1 1 d . . . C2 C 0.6740(3) 0.78164(16) 0.13855(15) 0.0224(10) Uani 1 1 d . . . C3 C 0.7605(3) 0.76130(15) 0.12089(16) 0.0230(9) Uani 1 1 d . . . C4 C 0.7428(3) 0.70689(15) 0.10822(15) 0.0214(9) Uani 1 1 d . . . C5 C 0.8100(3) 0.66832(16) 0.09235(15) 0.0208(9) Uani 1 1 d . . . C6 C 0.8002(3) 0.61416(15) 0.09682(14) 0.0195(9) Uani 1 1 d . . . C7 C 0.8763(3) 0.57384(16) 0.08773(15) 0.0222(9) Uani 1 1 d . . . C8 C 0.8422(3) 0.52934(16) 0.11006(14) 0.0214(9) Uani 1 1 d . . . C9 C 0.7428(3) 0.54127(15) 0.12856(15) 0.0207(9) Uani 1 1 d . . . C10 C 0.6724(3) 0.50672(15) 0.14910(15) 0.0220(9) Uani 1 1 d . . . C11 C 0.5691(3) 0.51174(14) 0.15064(14) 0.0176(9) Uani 1 1 d . . . C12 C 0.4961(3) 0.47169(15) 0.16372(14) 0.0203(9) Uani 1 1 d . . . C13 C 0.4074(3) 0.48873(15) 0.14374(15) 0.0217(9) Uani 1 1 d . . . C14 C 0.4256(3) 0.54175(14) 0.12390(15) 0.0183(9) Uani 1 1 d . . . C15 C 0.3582(3) 0.57666(16) 0.10232(15) 0.0221(9) Uani 1 1 d . . . C16 C 0.3669(3) 0.63047(16) 0.09763(14) 0.0196(9) Uani 1 1 d . . . C17 C 0.2925(3) 0.66860(17) 0.08124(15) 0.0240(10) Uani 1 1 d . . . C18 C 0.3274(3) 0.71679(16) 0.09495(15) 0.0231(10) Uani 1 1 d . . . C19 C 0.4269(3) 0.70833(15) 0.11570(15) 0.0187(9) Uani 1 1 d . . . C20 C 0.4979(3) 0.74616(14) 0.12923(14) 0.0187(9) Uani 1 1 d . . . C21 C 0.6638(3) 0.83249(16) 0.16584(16) 0.0285(10) Uani 1 1 d . . . H21A H 0.6039 0.8512 0.1535 0.034 Uiso 1 1 calc R . . H21B H 0.7227 0.8548 0.1587 0.034 Uiso 1 1 calc R . . C22 C 0.6550(4) 0.82374(18) 0.22307(17) 0.0370(12) Uani 1 1 d . . . H22A H 0.6527 0.8578 0.2403 0.056 Uiso 1 1 calc R . . H22B H 0.7127 0.8038 0.2350 0.056 Uiso 1 1 calc R . . H22C H 0.5938 0.8041 0.2304 0.056 Uiso 1 1 calc R . . C23 C 0.8582(3) 0.79084(16) 0.11933(18) 0.0320(10) Uani 1 1 d . . . H23A H 0.8999 0.7764 0.0918 0.038 Uiso 1 1 calc R . . H23B H 0.8447 0.8281 0.1114 0.038 Uiso 1 1 calc R . . C24 C 0.9160(4) 0.7878(2) 0.16822(18) 0.0447(13) Uani 1 1 d . . . H24A H 0.9791 0.8068 0.1646 0.067 Uiso 1 1 calc R . . H24B H 0.9296 0.7510 0.1764 0.067 Uiso 1 1 calc R . . H24C H 0.8767 0.8037 0.1954 0.067 Uiso 1 1 calc R . . C25 C 0.9659(3) 0.57835(17) 0.05444(16) 0.0279(10) Uani 1 1 d . . . H25A H 1.0106 0.5481 0.0606 0.034 Uiso 1 1 calc R . . H25B H 1.0029 0.6108 0.0631 0.034 Uiso 1 1 calc R . . C26 C 0.9374(3) 0.57980(18) -0.00177(16) 0.0375(12) Uani 1 1 d . . . H26A H 0.9975 0.5851 -0.0222 0.056 Uiso 1 1 calc R . . H26B H 0.8907 0.6087 -0.0077 0.056 Uiso 1 1 calc R . . H26C H 0.9059 0.5465 -0.0112 0.056 Uiso 1 1 calc R . . C27 C 0.8981(3) 0.47765(16) 0.11028(16) 0.0277(10) Uani 1 1 d . . . H27A H 0.9704 0.4848 0.1130 0.033 Uiso 1 1 calc R . . H27B H 0.8780 0.4572 0.1403 0.033 Uiso 1 1 calc R . . C28 C 0.8791(4) 0.44522(19) 0.06353(17) 0.0414(12) Uani 1 1 d . . . H28A H 0.9122 0.4111 0.0669 0.062 Uiso 1 1 calc R . . H28B H 0.9056 0.4636 0.0339 0.062 Uiso 1 1 calc R . . H28C H 0.8073 0.4399 0.0594 0.062 Uiso 1 1 calc R . . C29 C 0.5090(3) 0.42451(16) 0.19664(14) 0.0257(10) Uani 1 1 d . . . H29A H 0.5689 0.4049 0.1857 0.031 Uiso 1 1 calc R . . H29B H 0.4506 0.4011 0.1926 0.031 Uiso 1 1 calc R . . C30 C 0.5199(4) 0.43906(19) 0.25194(16) 0.0380(12) Uani 1 1 d . . . H30A H 0.5299 0.4071 0.2720 0.057 Uiso 1 1 calc R . . H30B H 0.4594 0.4571 0.2634 0.057 Uiso 1 1 calc R . . H30C H 0.5774 0.4624 0.2561 0.057 Uiso 1 1 calc R . . C31 C 0.3114(3) 0.45787(18) 0.14581(17) 0.0325(11) Uani 1 1 d . . . H31A H 0.3272 0.4200 0.1429 0.039 Uiso 1 1 calc R . . H31B H 0.2699 0.4676 0.1164 0.039 Uiso 1 1 calc R . . C32 C 0.2506(4) 0.4666(2) 0.1940(2) 0.0507(14) Uani 1 1 d . . . H32A H 0.1895 0.4456 0.1925 0.076 Uiso 1 1 calc R . . H32B H 0.2333 0.5038 0.1969 0.076 Uiso 1 1 calc R . . H32C H 0.2901 0.4559 0.2233 0.076 Uiso 1 1 calc R . . C33 C 0.2007(3) 0.65977(17) 0.05002(16) 0.0278(10) Uani 1 1 d . . . H33A H 0.1512 0.6875 0.0576 0.033 Uiso 1 1 calc R . . H33B H 0.1709 0.6255 0.0590 0.033 Uiso 1 1 calc R . . C34 C 0.2247(4) 0.6606(2) -0.00641(18) 0.0499(14) Uani 1 1 d . . . H34A H 0.1635 0.6546 -0.0258 0.075 Uiso 1 1 calc R . . H34B H 0.2729 0.6328 -0.0141 0.075 Uiso 1 1 calc R . . H34C H 0.2530 0.6948 -0.0155 0.075 Uiso 1 1 calc R . . C35 C 0.2693(3) 0.76703(16) 0.08926(16) 0.0277(10) Uani 1 1 d . . . H35A H 0.2287 0.7654 0.0581 0.033 Uiso 1 1 calc R . . H35B H 0.3160 0.7969 0.0861 0.033 Uiso 1 1 calc R . . C36 C 0.2007(4) 0.77594(19) 0.13492(18) 0.0390(12) Uani 1 1 d . . . H36A H 0.1657 0.8095 0.1311 0.058 Uiso 1 1 calc R . . H36B H 0.2407 0.7767 0.1658 0.058 Uiso 1 1 calc R . . H36C H 0.1520 0.7474 0.1370 0.058 Uiso 1 1 calc R . . C37 C 0.5067(3) 0.62354(16) 0.22422(15) 0.0260(10) Uani 1 1 d . . . H37A H 0.4489 0.6101 0.2081 0.031 Uiso 1 1 calc R . . C38 C 0.5030(4) 0.63187(17) 0.27518(15) 0.0311(11) Uani 1 1 d . . . H38A H 0.4448 0.6233 0.2939 0.037 Uiso 1 1 calc R . . C39 C 0.5857(4) 0.65300(19) 0.29898(17) 0.0381(12) Uani 1 1 d . . . H39A H 0.5848 0.6602 0.3341 0.046 Uiso 1 1 calc R . . C40 C 0.6691(3) 0.66322(18) 0.27063(16) 0.0315(11) Uani 1 1 d . . . H40A H 0.7273 0.6774 0.2859 0.038 Uiso 1 1 calc R . . C41 C 0.6668(3) 0.65263(16) 0.21972(15) 0.0253(10) Uani 1 1 d . . . H41A H 0.7251 0.6594 0.2004 0.030 Uiso 1 1 calc R . . C42 C 0.6025(3) 0.57079(16) 0.02270(15) 0.0226(9) Uani 1 1 d . . . H42A H 0.6188 0.5413 0.0431 0.027 Uiso 1 1 calc R . . C43 C 0.6005(3) 0.56452(18) -0.02891(16) 0.0326(11) Uani 1 1 d . . . H43A H 0.6147 0.5313 -0.0436 0.039 Uiso 1 1 calc R . . C44 C 0.5778(3) 0.60652(18) -0.05883(15) 0.0322(11) Uani 1 1 d . . . H44A H 0.5760 0.6029 -0.0945 0.039 Uiso 1 1 calc R . . C45 C 0.5575(3) 0.65424(18) -0.03650(15) 0.0289(11) Uani 1 1 d . . . H45A H 0.5411 0.6839 -0.0565 0.035 Uiso 1 1 calc R . . C46 C 0.5613(3) 0.65816(16) 0.01509(15) 0.0249(10) Uani 1 1 d . . . H46A H 0.5484 0.6913 0.0301 0.030 Uiso 1 1 calc R . . Fe51 Fe 0.02943(4) 0.62983(2) 0.38140(2) 0.01727(14) Uani 1 1 d . . . O51 O 0.3702(2) 0.71222(11) 0.45811(11) 0.0332(7) Uani 1 1 d . . . O52 O 0.4282(2) 0.67989(12) 0.38825(12) 0.0343(7) Uani 1 1 d . . . O53 O -0.1333(3) 0.81277(12) 0.31738(12) 0.0395(8) Uani 1 1 d . . . O54 O -0.0573(2) 0.84117(11) 0.38408(13) 0.0429(8) Uani 1 1 d . . . O55 O -0.3756(2) 0.57948(12) 0.38793(12) 0.0396(8) Uani 1 1 d . . . O56 O -0.3001(3) 0.53465(13) 0.44561(13) 0.0453(9) Uani 1 1 d . . . O57 O 0.2073(3) 0.45206(12) 0.31614(12) 0.0397(8) Uani 1 1 d . . . O58 O 0.1143(2) 0.41863(12) 0.37459(14) 0.0467(9) Uani 1 1 d . . . N51 N 0.1587(2) 0.59493(12) 0.38710(12) 0.0205(8) Uani 1 1 d . . . N52 N 0.0952(2) 0.69834(11) 0.38082(12) 0.0188(7) Uani 1 1 d . . . N53 N -0.1024(2) 0.66440(12) 0.38281(12) 0.0199(7) Uani 1 1 d . . . N54 N -0.0363(2) 0.56154(12) 0.37516(12) 0.0183(7) Uani 1 1 d . . . N55 N 0.0362(2) 0.63019(12) 0.30538(12) 0.0199(7) Uani 1 1 d . . . N56 N 0.0220(2) 0.62713(12) 0.45669(11) 0.0169(7) Uani 1 1 d . . . N57 N 0.3598(3) 0.68886(13) 0.41834(14) 0.0253(8) Uani 1 1 d . . . N58 N -0.0824(3) 0.80633(14) 0.35442(15) 0.0308(9) Uani 1 1 d . . . N59 N -0.3011(3) 0.56609(13) 0.41116(14) 0.0265(8) Uani 1 1 d . . . N60 N 0.1456(3) 0.45579(14) 0.34995(14) 0.0279(9) Uani 1 1 d . . . C51 C 0.1789(3) 0.54248(14) 0.38399(15) 0.0190(9) Uani 1 1 d . . . C52 C 0.2732(3) 0.52974(15) 0.40812(15) 0.0218(9) Uani 1 1 d . . . C53 C 0.3116(3) 0.57611(15) 0.42506(15) 0.0217(9) Uani 1 1 d . . . C54 C 0.2431(3) 0.61657(15) 0.40832(14) 0.0196(9) Uani 1 1 d . . . C55 C 0.2593(3) 0.67035(16) 0.40447(15) 0.0224(9) Uani 1 1 d . . . C56 C 0.1956(3) 0.70840(14) 0.38481(15) 0.0187(9) Uani 1 1 d . . . C57 C 0.2194(3) 0.76012(15) 0.36448(15) 0.0220(10) Uani 1 1 d . . . C58 C 0.1320(3) 0.78083(16) 0.34912(15) 0.0235(10) Uani 1 1 d . . . C59 C 0.0533(3) 0.74397(15) 0.36295(14) 0.0198(9) Uani 1 1 d . . . C60 C -0.0492(3) 0.75219(15) 0.36524(14) 0.0203(9) Uani 1 1 d . . . C61 C -0.1215(3) 0.71692(14) 0.38155(15) 0.0189(9) Uani 1 1 d . . . C62 C -0.2195(3) 0.72874(16) 0.40278(15) 0.0238(10) Uani 1 1 d . . . C63 C -0.2574(3) 0.68150(16) 0.41908(15) 0.0233(9) Uani 1 1 d . . . C64 C -0.1883(3) 0.64157(16) 0.40219(15) 0.0220(10) Uani 1 1 d . . . C65 C -0.2024(3) 0.58846(16) 0.39626(14) 0.0223(10) Uani 1 1 d . . . C66 C -0.1358(3) 0.55185(15) 0.37496(15) 0.0194(9) Uani 1 1 d . . . C67 C -0.1584(3) 0.50325(16) 0.34917(14) 0.0218(9) Uani 1 1 d . . . C68 C -0.0691(3) 0.48257(15) 0.33535(15) 0.0223(9) Uani 1 1 d . . . C69 C 0.0075(3) 0.51742(15) 0.35541(15) 0.0211(9) Uani 1 1 d . . . C70 C 0.1085(3) 0.50887(15) 0.36215(15) 0.0221(10) Uani 1 1 d . . . C71 C 0.3232(3) 0.47741(15) 0.41608(16) 0.0246(10) Uani 1 1 d . . . H71A H 0.2742 0.4490 0.4102 0.030 Uiso 1 1 calc R . . H71B H 0.3459 0.4749 0.4516 0.030 Uiso 1 1 calc R . . C72 C 0.4113(3) 0.46947(16) 0.38154(17) 0.0315(10) Uani 1 1 d . . . H72A H 0.4442 0.4362 0.3898 0.047 Uiso 1 1 calc R . . H72B H 0.4585 0.4985 0.3859 0.047 Uiso 1 1 calc R . . H72C H 0.3884 0.4686 0.3464 0.047 Uiso 1 1 calc R . . C73 C 0.3971(3) 0.58180(17) 0.46139(15) 0.0294(10) Uani 1 1 d . . . H73A H 0.4406 0.6111 0.4505 0.035 Uiso 1 1 calc R . . H73B H 0.4374 0.5492 0.4614 0.035 Uiso 1 1 calc R . . C74 C 0.3585(4) 0.5925(2) 0.51471(16) 0.0406(12) Uani 1 1 d . . . H74A H 0.4151 0.5971 0.5377 0.061 Uiso 1 1 calc R . . H74B H 0.3179 0.5628 0.5260 0.061 Uiso 1 1 calc R . . H74C H 0.3179 0.6245 0.5146 0.061 Uiso 1 1 calc R . . C75 C 0.3216(3) 0.78398(17) 0.35566(17) 0.0310(11) Uani 1 1 d . . . H75A H 0.3671 0.7724 0.3829 0.037 Uiso 1 1 calc R . . H75B H 0.3163 0.8227 0.3574 0.037 Uiso 1 1 calc R . . C76 C 0.3657(4) 0.7686(2) 0.30498(18) 0.0462(13) Uani 1 1 d . . . H76A H 0.4331 0.7831 0.3020 0.069 Uiso 1 1 calc R . . H76B H 0.3239 0.7825 0.2778 0.069 Uiso 1 1 calc R . . H76C H 0.3687 0.7302 0.3025 0.069 Uiso 1 1 calc R . . C77 C 0.1225(3) 0.82776(16) 0.31477(16) 0.0291(10) Uani 1 1 d . . . H77A H 0.1862 0.8473 0.3140 0.035 Uiso 1 1 calc R . . H77B H 0.0700 0.8516 0.3276 0.035 Uiso 1 1 calc R . . C78 C 0.0957(4) 0.80937(18) 0.26175(16) 0.0392(12) Uani 1 1 d . . . H78A H 0.0950 0.8395 0.2388 0.059 Uiso 1 1 calc R . . H78B H 0.0297 0.7929 0.2622 0.059 Uiso 1 1 calc R . . H78C H 0.1453 0.7838 0.2502 0.059 Uiso 1 1 calc R . . C79 C -0.2732(3) 0.78039(16) 0.40731(15) 0.0269(10) Uani 1 1 d . . . H79A H -0.2238 0.8093 0.4071 0.032 Uiso 1 1 calc R . . H79B H -0.3089 0.7816 0.4400 0.032 Uiso 1 1 calc R . . C80 C -0.3473(4) 0.78880(18) 0.36472(16) 0.0347(11) Uani 1 1 d . . . H80A H -0.3786 0.8234 0.3684 0.052 Uiso 1 1 calc R . . H80B H -0.3987 0.7615 0.3660 0.052 Uiso 1 1 calc R . . H80C H -0.3125 0.7870 0.3323 0.052 Uiso 1 1 calc R . . C81 C -0.3464(3) 0.67731(17) 0.45341(16) 0.0288(10) Uani 1 1 d . . . H81A H -0.3763 0.6419 0.4500 0.035 Uiso 1 1 calc R . . H81B H -0.3971 0.7035 0.4432 0.035 Uiso 1 1 calc R . . C82 C -0.3178(4) 0.68657(19) 0.50773(17) 0.0384(12) Uani 1 1 d . . . H82A H -0.3778 0.6866 0.5288 0.058 Uiso 1 1 calc R . . H82B H -0.2840 0.7205 0.5107 0.058 Uiso 1 1 calc R . . H82C H -0.2729 0.6586 0.5190 0.058 Uiso 1 1 calc R . . C83 C -0.2591(3) 0.48123(17) 0.33488(16) 0.0288(10) Uani 1 1 d . . . H83A H -0.2568 0.4702 0.2991 0.035 Uiso 1 1 calc R . . H83B H -0.3092 0.5096 0.3377 0.035 Uiso 1 1 calc R . . C84 C -0.2937(4) 0.43506(18) 0.36629(18) 0.0395(12) Uani 1 1 d . . . H84A H -0.3601 0.4241 0.3551 0.059 Uiso 1 1 calc R . . H84B H -0.2965 0.4454 0.4019 0.059 Uiso 1 1 calc R . . H84C H -0.2468 0.4058 0.3623 0.059 Uiso 1 1 calc R . . C85 C -0.0549(3) 0.43809(17) 0.29853(16) 0.0294(11) Uani 1 1 d . . . H85A H -0.1198 0.4206 0.2925 0.035 Uiso 1 1 calc R . . H85B H -0.0089 0.4118 0.3132 0.035 Uiso 1 1 calc R . . C86 C -0.0127(4) 0.45764(19) 0.24821(16) 0.0375(12) Uani 1 1 d . . . H86A H -0.0080 0.4282 0.2245 0.056 Uiso 1 1 calc R . . H86B H 0.0538 0.4726 0.2537 0.056 Uiso 1 1 calc R . . H86C H -0.0568 0.4846 0.2342 0.056 Uiso 1 1 calc R . . C87 C -0.0450(3) 0.62135(16) 0.27652(15) 0.0274(10) Uani 1 1 d . . . H87A H -0.1078 0.6178 0.2927 0.033 Uiso 1 1 calc R . . C88 C -0.0409(4) 0.61727(19) 0.22461(16) 0.0394(13) Uani 1 1 d . . . H88A H -0.0996 0.6108 0.2056 0.047 Uiso 1 1 calc R . . C89 C 0.0494(4) 0.6227(2) 0.20103(18) 0.0484(14) Uani 1 1 d . . . H89A H 0.0538 0.6197 0.1654 0.058 Uiso 1 1 calc R . . C90 C 0.1326(4) 0.6323(2) 0.22876(16) 0.0417(13) Uani 1 1 d . . . H90A H 0.1955 0.6366 0.2128 0.050 Uiso 1 1 calc R . . C91 C 0.1240(3) 0.63590(17) 0.28111(15) 0.0277(10) Uani 1 1 d . . . H91A H 0.1823 0.6426 0.3005 0.033 Uiso 1 1 calc R . . C92 C 0.0267(3) 0.58122(16) 0.48160(15) 0.0240(9) Uani 1 1 d . . . H92A H 0.0398 0.5501 0.4629 0.029 Uiso 1 1 calc R . . C93 C 0.0133(4) 0.57725(17) 0.53285(15) 0.0313(11) Uani 1 1 d . . . H93A H 0.0182 0.5441 0.5491 0.038 Uiso 1 1 calc R . . C94 C -0.0072(3) 0.62192(18) 0.56048(16) 0.0323(11) Uani 1 1 d . . . H94A H -0.0187 0.6200 0.5958 0.039 Uiso 1 1 calc R . . C95 C -0.0107(3) 0.66921(17) 0.53558(15) 0.0274(10) Uani 1 1 d . . . H95A H -0.0226 0.7008 0.5537 0.033 Uiso 1 1 calc R . . C96 C 0.0034(3) 0.67048(15) 0.48414(14) 0.0209(9) Uani 1 1 d . . . H96A H -0.0002 0.7034 0.4673 0.025 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 0.0151(3) 0.0163(3) 0.0203(3) -0.0017(3) 0.0004(2) -0.0005(2) O1 0.048(2) 0.040(2) 0.0322(18) 0.0039(15) 0.0117(16) -0.0133(17) O2 0.0191(17) 0.0325(18) 0.054(2) -0.0083(15) -0.0031(15) -0.0052(14) O3 0.0370(19) 0.0365(19) 0.0330(19) 0.0054(14) -0.0039(16) 0.0054(16) O4 0.042(2) 0.0230(17) 0.0407(19) -0.0041(14) 0.0013(15) 0.0024(15) O5 0.039(2) 0.040(2) 0.0358(19) -0.0052(16) -0.0119(16) -0.0060(17) O6 0.0194(16) 0.0418(19) 0.0478(19) 0.0071(17) 0.0042(17) -0.0043(14) O7 0.040(2) 0.0270(18) 0.055(2) 0.0130(16) -0.0108(17) 0.0015(16) O8 0.035(2) 0.038(2) 0.046(2) -0.0136(16) 0.0020(17) 0.0072(16) N1 0.0183(17) 0.0142(17) 0.0195(17) 0.0003(14) -0.0011(15) 0.0000(14) N2 0.0181(18) 0.0155(17) 0.0240(18) -0.0048(15) -0.0031(16) -0.0001(14) N3 0.0160(17) 0.0187(17) 0.0200(18) -0.0033(14) 0.0002(14) -0.0004(15) N4 0.0184(18) 0.0195(18) 0.0197(17) -0.0021(15) 0.0011(15) -0.0035(14) N5 0.0186(18) 0.0186(18) 0.0209(17) 0.0033(14) -0.0004(15) 0.0022(16) N6 0.0158(18) 0.0195(18) 0.0201(17) 0.0007(14) 0.0018(14) -0.0050(15) N7 0.022(2) 0.024(2) 0.037(2) -0.0065(17) 0.0034(18) -0.0050(16) N8 0.029(2) 0.020(2) 0.030(2) 0.0030(17) 0.0025(18) -0.0009(17) N9 0.019(2) 0.026(2) 0.036(2) 0.0062(17) -0.0023(18) -0.0025(16) N10 0.023(2) 0.027(2) 0.043(2) -0.0033(19) -0.0043(18) 0.0025(17) C1 0.026(2) 0.017(2) 0.019(2) -0.0001(16) 0.0001(18) -0.0029(18) C2 0.025(3) 0.018(2) 0.024(2) 0.0058(17) 0.0005(18) 0.0011(19) C3 0.024(2) 0.018(2) 0.027(2) 0.0038(19) -0.004(2) -0.0063(17) C4 0.021(2) 0.016(2) 0.028(2) 0.0015(17) -0.0022(18) 0.0015(18) C5 0.014(2) 0.027(2) 0.022(2) -0.0001(18) 0.0000(17) -0.0029(19) C6 0.019(2) 0.021(2) 0.019(2) -0.0013(17) -0.0020(17) -0.0022(18) C7 0.016(2) 0.025(2) 0.026(2) -0.0047(19) -0.0028(18) -0.0042(18) C8 0.016(2) 0.025(2) 0.023(2) -0.0044(18) -0.0052(18) 0.0008(18) C9 0.018(2) 0.020(2) 0.024(2) -0.0015(17) -0.0049(18) -0.0001(17) C10 0.026(2) 0.016(2) 0.024(2) -0.0012(17) -0.0013(18) 0.0012(18) C11 0.022(2) 0.015(2) 0.016(2) -0.0016(16) -0.0019(17) -0.0009(17) C12 0.026(2) 0.018(2) 0.017(2) -0.0017(17) 0.0033(18) -0.0034(18) C13 0.026(2) 0.018(2) 0.021(2) -0.0051(17) 0.0031(18) -0.0056(19) C14 0.016(2) 0.020(2) 0.019(2) -0.0053(17) 0.0020(18) 0.0010(17) C15 0.019(2) 0.022(2) 0.025(2) -0.0026(17) 0.0025(18) -0.0078(19) C16 0.009(2) 0.024(2) 0.026(2) 0.0015(18) 0.0012(16) 0.0010(18) C17 0.017(2) 0.032(3) 0.023(2) -0.0007(19) 0.0008(18) -0.0029(19) C18 0.017(2) 0.025(2) 0.028(2) 0.0034(18) 0.0011(18) 0.0006(19) C19 0.015(2) 0.022(2) 0.020(2) 0.0000(18) 0.0007(18) 0.0043(17) C20 0.023(2) 0.013(2) 0.020(2) 0.0001(16) 0.0036(18) 0.0052(18) C21 0.024(2) 0.015(2) 0.047(3) -0.0005(19) -0.003(2) 0.0006(19) C22 0.035(3) 0.035(3) 0.041(3) -0.015(2) -0.006(2) 0.007(2) C23 0.026(2) 0.016(2) 0.055(3) -0.004(2) -0.002(2) -0.0057(18) C24 0.029(3) 0.051(3) 0.054(3) -0.021(3) -0.004(2) -0.006(3) C25 0.023(2) 0.022(2) 0.039(3) -0.003(2) 0.004(2) 0.0012(19) C26 0.035(3) 0.038(3) 0.039(3) -0.001(2) 0.012(2) -0.005(2) C27 0.025(2) 0.024(2) 0.034(3) 0.0011(19) 0.001(2) 0.0023(19) C28 0.041(3) 0.037(3) 0.046(3) -0.001(2) 0.009(2) 0.010(2) C29 0.028(3) 0.025(2) 0.025(2) 0.0046(18) -0.0018(19) -0.003(2) C30 0.047(3) 0.038(3) 0.029(3) 0.005(2) -0.004(2) -0.003(2) C31 0.029(3) 0.028(3) 0.040(3) 0.008(2) 0.005(2) -0.004(2) C32 0.031(3) 0.066(4) 0.055(3) 0.011(3) 0.012(3) 0.001(3) C33 0.017(2) 0.032(3) 0.035(3) 0.003(2) -0.004(2) -0.001(2) C34 0.045(3) 0.066(4) 0.039(3) 0.003(3) -0.012(3) -0.014(3) C35 0.022(2) 0.027(2) 0.035(3) 0.002(2) -0.002(2) 0.0019(19) C36 0.030(3) 0.034(3) 0.053(3) -0.005(2) 0.003(2) 0.008(2) C37 0.027(2) 0.023(2) 0.028(2) 0.0001(19) 0.0018(19) 0.000(2) C38 0.036(3) 0.035(3) 0.023(2) -0.003(2) 0.007(2) 0.001(2) C39 0.048(3) 0.044(3) 0.022(2) -0.006(2) 0.002(2) 0.015(3) C40 0.027(3) 0.036(3) 0.032(3) -0.003(2) -0.006(2) 0.002(2) C41 0.024(2) 0.028(2) 0.024(2) -0.0025(18) 0.0002(19) 0.0052(19) C42 0.025(2) 0.020(2) 0.024(2) -0.0009(17) 0.0029(18) -0.0060(19) C43 0.036(3) 0.032(3) 0.029(2) -0.007(2) 0.004(2) -0.004(2) C44 0.033(3) 0.048(3) 0.016(2) -0.007(2) 0.0000(19) -0.004(2) C45 0.025(3) 0.037(3) 0.024(2) 0.005(2) -0.0020(19) 0.003(2) C46 0.022(2) 0.023(2) 0.030(2) -0.0032(19) -0.0021(19) 0.0009(19) Fe51 0.0184(3) 0.0150(3) 0.0185(3) 0.0004(3) -0.0013(2) 0.0001(2) O51 0.0353(19) 0.0286(18) 0.0356(18) -0.0051(14) -0.0108(15) -0.0020(15) O52 0.0252(17) 0.0351(18) 0.0426(19) 0.0055(15) 0.0067(16) -0.0011(14) O53 0.039(2) 0.037(2) 0.042(2) 0.0136(16) -0.0052(17) 0.0077(16) O54 0.045(2) 0.0226(17) 0.061(2) -0.0158(17) 0.0014(19) 0.0000(15) O55 0.0222(17) 0.044(2) 0.053(2) -0.0022(17) -0.0082(16) -0.0042(15) O56 0.045(2) 0.045(2) 0.046(2) 0.0161(18) 0.0144(17) -0.0023(18) O57 0.047(2) 0.036(2) 0.0359(19) -0.0095(15) 0.0019(17) 0.0138(17) O58 0.040(2) 0.0202(17) 0.080(3) 0.0090(18) -0.0028(19) 0.0022(15) N51 0.0160(18) 0.0194(18) 0.0261(19) -0.0035(15) -0.0023(15) -0.0017(14) N52 0.0195(18) 0.0161(17) 0.0208(17) -0.0008(15) -0.0004(15) 0.0007(14) N53 0.0210(18) 0.0182(17) 0.0205(17) 0.0000(15) 0.0002(16) 0.0012(14) N54 0.0190(18) 0.0174(17) 0.0186(17) 0.0008(14) -0.0003(15) -0.0005(14) N55 0.0234(19) 0.0145(18) 0.0220(17) 0.0013(14) -0.0015(15) 0.0039(16) N56 0.0137(17) 0.0159(17) 0.0210(17) 0.0007(14) -0.0015(13) -0.0047(15) N57 0.028(2) 0.0175(19) 0.030(2) 0.0045(16) -0.0029(18) 0.0030(16) N58 0.025(2) 0.025(2) 0.042(2) 0.0043(18) 0.0066(19) 0.0041(18) N59 0.024(2) 0.023(2) 0.032(2) -0.0022(17) 0.0064(18) -0.0013(17) N60 0.029(2) 0.020(2) 0.035(2) -0.0004(17) -0.0101(18) -0.0033(17) C51 0.019(2) 0.016(2) 0.023(2) 0.0011(18) -0.0008(19) 0.0002(16) C52 0.022(2) 0.019(2) 0.025(2) 0.0001(18) 0.0018(18) 0.0043(18) C53 0.020(2) 0.019(2) 0.026(2) 0.0015(17) 0.0020(18) 0.0027(18) C54 0.017(2) 0.018(2) 0.024(2) -0.0004(17) 0.0032(17) 0.0034(18) C55 0.019(2) 0.024(2) 0.024(2) -0.0038(18) -0.0003(18) -0.0037(19) C56 0.022(2) 0.015(2) 0.018(2) -0.0017(17) -0.0019(18) 0.0008(17) C57 0.026(2) 0.018(2) 0.023(2) -0.0027(17) -0.0025(18) -0.0015(18) C58 0.025(2) 0.016(2) 0.029(2) -0.0042(18) 0.0002(19) 0.0003(19) C59 0.029(2) 0.013(2) 0.018(2) 0.0023(16) 0.0005(18) -0.0022(18) C60 0.024(2) 0.015(2) 0.022(2) 0.0009(16) -0.0011(18) 0.0024(18) C61 0.021(2) 0.015(2) 0.021(2) -0.0026(18) -0.0052(19) 0.0035(16) C62 0.027(3) 0.026(2) 0.018(2) -0.0026(18) -0.0032(18) 0.006(2) C63 0.020(2) 0.024(2) 0.026(2) -0.0055(19) -0.0050(19) -0.0034(19) C64 0.019(2) 0.024(2) 0.023(2) 0.0073(17) -0.0013(18) -0.0025(18) C65 0.014(2) 0.031(3) 0.022(2) 0.0012(18) -0.0041(17) -0.0021(19) C66 0.021(2) 0.020(2) 0.018(2) 0.0001(17) -0.0016(18) -0.0010(17) C67 0.026(2) 0.020(2) 0.020(2) 0.0018(17) -0.0019(18) -0.0056(19) C68 0.026(2) 0.018(2) 0.023(2) 0.0019(17) 0.0019(18) -0.0017(19) C69 0.024(2) 0.019(2) 0.021(2) 0.0019(17) -0.0034(18) -0.0038(18) C70 0.032(3) 0.013(2) 0.022(2) -0.0004(16) 0.0008(18) 0.0042(19) C71 0.025(2) 0.018(2) 0.030(2) 0.0017(18) -0.0095(19) 0.0015(18) C72 0.034(3) 0.028(2) 0.032(2) -0.006(2) -0.004(2) 0.006(2) C73 0.029(3) 0.022(2) 0.037(3) 0.0008(19) -0.007(2) 0.006(2) C74 0.042(3) 0.049(3) 0.032(3) -0.001(2) -0.012(2) -0.001(2) C75 0.029(3) 0.023(2) 0.041(3) 0.005(2) -0.004(2) -0.003(2) C76 0.026(3) 0.059(4) 0.053(3) 0.013(3) 0.009(2) -0.003(3) C77 0.028(3) 0.017(2) 0.042(3) 0.0067(19) -0.004(2) -0.0022(19) C78 0.057(3) 0.029(3) 0.031(3) 0.010(2) -0.005(2) -0.001(2) C79 0.027(3) 0.026(2) 0.028(2) 0.0007(19) 0.0036(19) 0.004(2) C80 0.036(3) 0.039(3) 0.029(2) 0.000(2) 0.000(2) 0.016(2) C81 0.020(2) 0.025(2) 0.041(3) -0.008(2) 0.001(2) -0.0001(19) C82 0.032(3) 0.048(3) 0.034(3) 0.001(2) 0.010(2) -0.004(2) C83 0.026(2) 0.033(3) 0.027(2) -0.005(2) -0.002(2) -0.003(2) C84 0.033(3) 0.036(3) 0.049(3) 0.000(2) -0.002(2) -0.011(2) C85 0.024(2) 0.031(3) 0.034(3) -0.009(2) 0.001(2) -0.004(2) C86 0.038(3) 0.045(3) 0.029(2) -0.011(2) -0.003(2) -0.008(2) C87 0.030(3) 0.028(2) 0.024(2) 0.0016(19) -0.0046(19) 0.006(2) C88 0.046(3) 0.047(3) 0.026(2) -0.005(2) -0.012(2) 0.017(3) C89 0.062(4) 0.060(4) 0.023(2) -0.003(2) 0.001(3) 0.028(3) C90 0.040(3) 0.060(3) 0.026(2) 0.006(2) 0.011(2) 0.011(3) C91 0.027(3) 0.029(3) 0.027(2) -0.0002(19) 0.000(2) 0.003(2) C92 0.028(2) 0.019(2) 0.025(2) -0.0001(18) -0.0022(19) -0.0001(19) C93 0.044(3) 0.028(3) 0.021(2) 0.0051(19) -0.004(2) -0.010(2) C94 0.032(3) 0.041(3) 0.024(2) 0.000(2) -0.001(2) -0.007(2) C95 0.030(3) 0.026(2) 0.026(2) -0.0046(18) -0.0011(19) 0.000(2) C96 0.024(2) 0.019(2) 0.019(2) -0.0016(17) -0.0019(18) -0.0024(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.956(3) . ? Fe1 N3 1.959(3) . ? Fe1 N4 1.961(3) . ? Fe1 N2 1.969(3) . ? Fe1 N6 1.991(3) . ? Fe1 N5 2.014(3) . ? O1 N7 1.231(4) . ? O2 N7 1.223(4) . ? O3 N8 1.220(4) . ? O4 N8 1.232(4) . ? O5 N9 1.215(4) . ? O6 N9 1.228(4) . ? O7 N10 1.219(4) . ? O8 N10 1.211(4) . ? N1 C4 1.378(5) . ? N1 C1 1.382(5) . ? N2 C9 1.370(5) . ? N2 C6 1.371(5) . ? N3 C14 1.368(5) . ? N3 C11 1.381(5) . ? N4 C19 1.374(5) . ? N4 C16 1.384(5) . ? N5 C37 1.334(5) . ? N5 C41 1.340(5) . ? N6 C42 1.350(5) . ? N6 C46 1.355(5) . ? N7 C5 1.475(5) . ? N8 C10 1.464(5) . ? N9 C15 1.472(5) . ? N10 C20 1.484(5) . ? C1 C20 1.372(6) . ? C1 C2 1.458(6) . ? C2 C3 1.354(6) . ? C2 C21 1.490(6) . ? C3 C4 1.445(5) . ? C3 C23 1.512(5) . ? C4 C5 1.398(5) . ? C5 C6 1.391(5) . ? C6 C7 1.468(6) . ? C7 C8 1.358(6) . ? C7 C25 1.496(6) . ? C8 C9 1.452(5) . ? C8 C27 1.516(6) . ? C9 C10 1.402(6) . ? C10 C11 1.392(6) . ? C11 C12 1.456(5) . ? C12 C13 1.373(6) . ? C12 C29 1.495(5) . ? C13 C14 1.469(5) . ? C13 C31 1.510(6) . ? C14 C15 1.391(5) . ? C15 C16 1.381(5) . ? C16 C17 1.459(6) . ? C17 C18 1.363(6) . ? C17 C33 1.501(6) . ? C18 C19 1.460(5) . ? C18 C35 1.506(6) . ? C19 C20 1.401(5) . ? C21 C22 1.538(6) . ? C23 C24 1.511(6) . ? C25 C26 1.538(6) . ? C27 C28 1.511(6) . ? C29 C30 1.519(6) . ? C31 C32 1.531(6) . ? C33 C34 1.530(6) . ? C35 C36 1.537(6) . ? C37 C38 1.368(5) . ? C38 C39 1.386(7) . ? C39 C40 1.372(6) . ? C40 C41 1.376(6) . ? C42 C43 1.377(6) . ? C43 C44 1.366(6) . ? C44 C45 1.379(6) . ? C45 C46 1.372(6) . ? Fe51 N51 1.955(3) . ? Fe51 N52 1.955(3) . ? Fe51 N54 1.957(3) . ? Fe51 N53 1.976(3) . ? Fe51 N56 1.999(3) . ? Fe51 N55 2.017(3) . ? O51 N57 1.218(4) . ? O52 N57 1.238(4) . ? O53 N58 1.207(4) . ? O54 N58 1.232(4) . ? O55 N59 1.223(4) . ? O56 N59 1.214(4) . ? O57 N60 1.223(5) . ? O58 N60 1.224(4) . ? N51 C51 1.366(5) . ? N51 C54 1.379(5) . ? N52 C56 1.375(5) . ? N52 C59 1.375(5) . ? N53 C61 1.362(5) . ? N53 C64 1.390(5) . ? N54 C66 1.357(5) . ? N54 C69 1.372(5) . ? N55 C87 1.349(5) . ? N55 C91 1.351(5) . ? N56 C92 1.344(5) . ? N56 C96 1.346(5) . ? N57 C55 1.475(5) . ? N58 C60 1.477(5) . ? N59 C65 1.495(5) . ? N60 C70 1.477(5) . ? C51 C70 1.400(5) . ? C51 C52 1.454(6) . ? C52 C53 1.364(6) . ? C52 C71 1.507(5) . ? C53 C54 1.451(5) . ? C53 C73 1.505(6) . ? C54 C55 1.391(5) . ? C55 C56 1.394(5) . ? C56 C57 1.459(5) . ? C57 C58 1.349(6) . ? C57 C75 1.518(6) . ? C58 C59 1.459(6) . ? C58 C77 1.508(6) . ? C59 C60 1.393(6) . ? C60 C61 1.391(5) . ? C61 C62 1.462(6) . ? C62 C63 1.376(6) . ? C62 C79 1.505(6) . ? C63 C64 1.447(6) . ? C63 C81 1.505(6) . ? C64 C65 1.375(6) . ? C65 C66 1.410(5) . ? C66 C67 1.446(5) . ? C67 C68 1.360(6) . ? C67 C83 1.511(6) . ? C68 C69 1.458(6) . ? C68 C85 1.507(6) . ? C69 C70 1.384(6) . ? C71 C72 1.508(6) . ? C73 C74 1.529(6) . ? C75 C76 1.519(6) . ? C77 C78 1.524(6) . ? C79 C80 1.520(6) . ? C81 C82 1.509(6) . ? C83 C84 1.514(6) . ? C85 C86 1.532(6) . ? C87 C88 1.381(6) . ? C88 C89 1.370(7) . ? C89 C90 1.359(7) . ? C90 C91 1.395(6) . ? C92 C93 1.374(5) . ? C93 C94 1.381(6) . ? C94 C95 1.374(6) . ? C95 C96 1.376(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N3 176.42(13) . . ? N1 Fe1 N4 89.82(13) . . ? N3 Fe1 N4 89.94(13) . . ? N1 Fe1 N2 90.16(13) . . ? N3 Fe1 N2 90.39(13) . . ? N4 Fe1 N2 175.02(14) . . ? N1 Fe1 N6 91.75(13) . . ? N3 Fe1 N6 91.81(13) . . ? N4 Fe1 N6 87.55(13) . . ? N2 Fe1 N6 87.47(14) . . ? N1 Fe1 N5 87.40(13) . . ? N3 Fe1 N5 89.04(13) . . ? N4 Fe1 N5 92.35(13) . . ? N2 Fe1 N5 92.63(14) . . ? N6 Fe1 N5 179.15(13) . . ? C4 N1 C1 105.1(3) . . ? C4 N1 Fe1 127.9(3) . . ? C1 N1 Fe1 125.5(3) . . ? C9 N2 C6 105.3(3) . . ? C9 N2 Fe1 127.9(3) . . ? C6 N2 Fe1 125.0(3) . . ? C14 N3 C11 105.5(3) . . ? C14 N3 Fe1 127.7(3) . . ? C11 N3 Fe1 126.1(3) . . ? C19 N4 C16 105.4(3) . . ? C19 N4 Fe1 127.7(3) . . ? C16 N4 Fe1 125.2(3) . . ? C37 N5 C41 116.7(3) . . ? C37 N5 Fe1 121.7(3) . . ? C41 N5 Fe1 121.5(3) . . ? C42 N6 C46 116.6(3) . . ? C42 N6 Fe1 122.0(3) . . ? C46 N6 Fe1 121.4(3) . . ? O2 N7 O1 125.0(4) . . ? O2 N7 C5 117.4(3) . . ? O1 N7 C5 117.6(4) . . ? O3 N8 O4 124.2(4) . . ? O3 N8 C10 118.0(3) . . ? O4 N8 C10 117.8(4) . . ? O5 N9 O6 124.1(4) . . ? O5 N9 C15 117.7(4) . . ? O6 N9 C15 118.2(4) . . ? O8 N10 O7 125.4(4) . . ? O8 N10 C20 117.2(4) . . ? O7 N10 C20 117.4(4) . . ? C20 C1 N1 120.4(4) . . ? C20 C1 C2 127.8(4) . . ? N1 C1 C2 110.7(4) . . ? C3 C2 C1 105.5(3) . . ? C3 C2 C21 125.4(4) . . ? C1 C2 C21 128.7(4) . . ? C2 C3 C4 107.8(4) . . ? C2 C3 C23 124.2(4) . . ? C4 C3 C23 127.8(4) . . ? N1 C4 C5 120.1(3) . . ? N1 C4 C3 110.2(3) . . ? C5 C4 C3 129.6(4) . . ? C6 C5 C4 127.6(4) . . ? C6 C5 N7 117.5(4) . . ? C4 C5 N7 114.5(3) . . ? N2 C6 C5 120.8(4) . . ? N2 C6 C7 110.5(3) . . ? C5 C6 C7 127.9(4) . . ? C8 C7 C6 106.1(3) . . ? C8 C7 C25 126.3(4) . . ? C6 C7 C25 127.0(4) . . ? C7 C8 C9 106.4(4) . . ? C7 C8 C27 124.0(4) . . ? C9 C8 C27 129.4(4) . . ? N2 C9 C10 120.2(4) . . ? N2 C9 C8 111.3(3) . . ? C10 C9 C8 128.2(4) . . ? C11 C10 C9 128.7(4) . . ? C11 C10 N8 115.1(4) . . ? C9 C10 N8 115.4(4) . . ? N3 C11 C10 120.0(4) . . ? N3 C11 C12 111.2(3) . . ? C10 C11 C12 127.7(4) . . ? C13 C12 C11 105.6(3) . . ? C13 C12 C29 125.4(4) . . ? C11 C12 C29 128.6(4) . . ? C12 C13 C14 106.6(4) . . ? C12 C13 C31 124.1(4) . . ? C14 C13 C31 129.2(4) . . ? N3 C14 C15 120.7(3) . . ? N3 C14 C13 110.5(3) . . ? C15 C14 C13 128.8(4) . . ? C16 C15 C14 128.1(4) . . ? C16 C15 N9 115.7(4) . . ? C14 C15 N9 115.8(3) . . ? C15 C16 N4 120.3(4) . . ? C15 C16 C17 129.0(4) . . ? N4 C16 C17 110.3(3) . . ? C18 C17 C16 106.5(4) . . ? C18 C17 C33 124.3(4) . . ? C16 C17 C33 128.8(4) . . ? C17 C18 C19 106.4(4) . . ? C17 C18 C35 124.1(4) . . ? C19 C18 C35 129.6(4) . . ? N4 C19 C20 120.6(3) . . ? N4 C19 C18 110.9(3) . . ? C20 C19 C18 128.0(4) . . ? C1 C20 C19 127.9(4) . . ? C1 C20 N10 115.5(3) . . ? C19 C20 N10 116.1(3) . . ? C2 C21 C22 111.1(3) . . ? C24 C23 C3 113.3(4) . . ? C7 C25 C26 111.9(4) . . ? C28 C27 C8 112.9(4) . . ? C12 C29 C30 112.2(4) . . ? C13 C31 C32 114.2(4) . . ? C17 C33 C34 111.3(4) . . ? C18 C35 C36 110.9(4) . . ? N5 C37 C38 123.7(4) . . ? C37 C38 C39 118.7(4) . . ? C40 C39 C38 118.5(4) . . ? C39 C40 C41 118.8(4) . . ? N5 C41 C40 123.5(4) . . ? N6 C42 C43 122.9(4) . . ? C44 C43 C42 119.3(4) . . ? C43 C44 C45 119.0(4) . . ? C46 C45 C44 119.0(4) . . ? N6 C46 C45 123.1(4) . . ? N51 Fe51 N52 90.32(13) . . ? N51 Fe51 N54 90.15(13) . . ? N52 Fe51 N54 174.69(13) . . ? N51 Fe51 N53 174.45(14) . . ? N52 Fe51 N53 90.37(13) . . ? N54 Fe51 N53 89.67(13) . . ? N51 Fe51 N56 87.24(13) . . ? N52 Fe51 N56 93.51(13) . . ? N54 Fe51 N56 91.79(13) . . ? N53 Fe51 N56 87.23(13) . . ? N51 Fe51 N55 92.26(13) . . ? N52 Fe51 N55 88.15(13) . . ? N54 Fe51 N55 86.55(13) . . ? N53 Fe51 N55 93.26(13) . . ? N56 Fe51 N55 178.27(12) . . ? C51 N51 C54 104.6(3) . . ? C51 N51 Fe51 128.0(3) . . ? C54 N51 Fe51 125.3(3) . . ? C56 N52 C59 105.6(3) . . ? C56 N52 Fe51 127.4(2) . . ? C59 N52 Fe51 124.9(3) . . ? C61 N53 C64 105.3(3) . . ? C61 N53 Fe51 127.3(3) . . ? C64 N53 Fe51 124.3(3) . . ? C66 N54 C69 105.7(3) . . ? C66 N54 Fe51 127.2(3) . . ? C69 N54 Fe51 124.5(3) . . ? C87 N55 C91 116.9(3) . . ? C87 N55 Fe51 122.0(3) . . ? C91 N55 Fe51 121.0(3) . . ? C92 N56 C96 117.2(3) . . ? C92 N56 Fe51 121.2(3) . . ? C96 N56 Fe51 121.4(3) . . ? O51 N57 O52 124.3(4) . . ? O51 N57 C55 118.4(4) . . ? O52 N57 C55 117.3(3) . . ? O53 N58 O54 125.1(4) . . ? O53 N58 C60 117.1(4) . . ? O54 N58 C60 117.8(4) . . ? O56 N59 O55 124.9(4) . . ? O56 N59 C65 116.1(4) . . ? O55 N59 C65 119.0(3) . . ? O57 N60 O58 124.3(4) . . ? O57 N60 C70 117.4(4) . . ? O58 N60 C70 118.4(4) . . ? N51 C51 C70 119.3(3) . . ? N51 C51 C52 111.4(3) . . ? C70 C51 C52 129.2(3) . . ? C53 C52 C51 106.3(3) . . ? C53 C52 C71 123.4(4) . . ? C51 C52 C71 130.3(4) . . ? C52 C53 C54 105.9(4) . . ? C52 C53 C73 125.6(4) . . ? C54 C53 C73 127.6(4) . . ? N51 C54 C55 119.5(4) . . ? N51 C54 C53 111.2(3) . . ? C55 C54 C53 128.5(4) . . ? C54 C55 C56 128.1(4) . . ? C54 C55 N57 116.1(4) . . ? C56 C55 N57 115.6(3) . . ? N52 C56 C55 120.0(3) . . ? N52 C56 C57 110.8(3) . . ? C55 C56 C57 129.2(4) . . ? C58 C57 C56 105.9(4) . . ? C58 C57 C75 125.6(4) . . ? C56 C57 C75 128.1(4) . . ? C57 C58 C59 107.6(4) . . ? C57 C58 C77 124.4(4) . . ? C59 C58 C77 126.9(4) . . ? N52 C59 C60 121.1(4) . . ? N52 C59 C58 109.5(4) . . ? C60 C59 C58 128.9(4) . . ? C61 C60 C59 127.2(4) . . ? C61 C60 N58 116.9(3) . . ? C59 C60 N58 115.5(4) . . ? N53 C61 C60 120.7(4) . . ? N53 C61 C62 111.2(3) . . ? C60 C61 C62 127.9(4) . . ? C63 C62 C61 105.9(4) . . ? C63 C62 C79 124.2(4) . . ? C61 C62 C79 129.9(4) . . ? C62 C63 C64 106.3(4) . . ? C62 C63 C81 123.0(4) . . ? C64 C63 C81 130.2(4) . . ? C65 C64 N53 118.9(4) . . ? C65 C64 C63 129.7(4) . . ? N53 C64 C63 110.6(3) . . ? C64 C65 C66 127.5(4) . . ? C64 C65 N59 117.8(4) . . ? C66 C65 N59 114.6(3) . . ? N54 C66 C65 120.1(3) . . ? N54 C66 C67 111.4(3) . . ? C65 C66 C67 128.5(4) . . ? C68 C67 C66 105.9(4) . . ? C68 C67 C83 125.2(4) . . ? C66 C67 C83 128.6(4) . . ? C67 C68 C69 106.7(4) . . ? C67 C68 C85 125.2(4) . . ? C69 C68 C85 127.2(4) . . ? N54 C69 C70 120.0(4) . . ? N54 C69 C68 109.6(4) . . ? C70 C69 C68 129.9(4) . . ? C69 C70 C51 128.2(4) . . ? C69 C70 N60 116.5(4) . . ? C51 C70 N60 115.0(4) . . ? C52 C71 C72 112.5(3) . . ? C53 C73 C74 110.5(4) . . ? C57 C75 C76 112.6(4) . . ? C58 C77 C78 109.4(3) . . ? C62 C79 C80 112.2(3) . . ? C63 C81 C82 111.3(4) . . ? C67 C83 C84 115.1(4) . . ? C68 C85 C86 111.5(4) . . ? N55 C87 C88 123.0(4) . . ? C89 C88 C87 118.8(5) . . ? C90 C89 C88 119.9(4) . . ? C89 C90 C91 118.8(5) . . ? N55 C91 C90 122.6(4) . . ? N56 C92 C93 122.9(4) . . ? C92 C93 C94 119.3(4) . . ? C95 C94 C93 118.3(4) . . ? C94 C95 C96 119.4(4) . . ? N56 C96 C95 122.8(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.788 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.106 # Attachment '25junc.cif' data_25junc _database_code_depnum_ccdc_archive 'CCDC 755823' #TrackingRef '25junc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(tn-OEP)(4-CNpy)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Fe N12 O8' _chemical_formula_weight 976.83 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 19.4563(17) _cell_length_b 14.1225(12) _cell_length_c 16.7267(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.694(2) _cell_angle_gamma 90.00 _cell_volume 4586.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.2 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9688 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8767 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.75 _reflns_number_total 8767 _reflns_number_gt 6303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0562P)^2^+2.1677P] 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 8767 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 0.262235(18) 0.52808(2) 1.02679(2) 0.01386(11) Uani 1 1 d . . . O1 O 0.53191(9) 0.60021(13) 0.97599(11) 0.0227(4) Uani 1 1 d . . . O2 O 0.51792(9) 0.69699(13) 1.07417(11) 0.0220(4) Uani 1 1 d . . . O3 O 0.28670(10) 0.60095(14) 1.35275(11) 0.0263(5) Uani 1 1 d . . . O4 O 0.26458(10) 0.45067(14) 1.34690(11) 0.0263(5) Uani 1 1 d . . . O5 O 0.04504(11) 0.29522(14) 1.07316(12) 0.0332(5) Uani 1 1 d . . . O6 O -0.00499(10) 0.39414(14) 0.98888(12) 0.0277(5) Uani 1 1 d . . . O7 O 0.18283(10) 0.61102(14) 0.71715(11) 0.0266(5) Uani 1 1 d . . . O8 O 0.27134(10) 0.52238(14) 0.69635(11) 0.0246(4) Uani 1 1 d . . . N1 N 0.32176(10) 0.57349(14) 0.94281(12) 0.0144(5) Uani 1 1 d . . . N2 N 0.33597(11) 0.55832(14) 1.11135(12) 0.0145(5) Uani 1 1 d . . . N3 N 0.19878(11) 0.49506(15) 1.11044(12) 0.0152(5) Uani 1 1 d . . . N4 N 0.19229(11) 0.48507(15) 0.94305(12) 0.0153(5) Uani 1 1 d . . . N5 N 0.49704(11) 0.63648(15) 1.02506(13) 0.0163(5) Uani 1 1 d . . . N6 N 0.27495(11) 0.52821(16) 1.31633(13) 0.0190(5) Uani 1 1 d . . . N7 N 0.04498(12) 0.36536(16) 1.03036(13) 0.0211(5) Uani 1 1 d . . . N8 N 0.23209(11) 0.56157(16) 0.74014(13) 0.0199(5) Uani 1 1 d . . . N9 N 0.22435(11) 0.66085(15) 1.02769(12) 0.0154(5) Uani 1 1 d . . . N10 N 0.12298(17) 1.01415(19) 1.03709(16) 0.0430(8) Uani 1 1 d . . . N11 N 0.29849(11) 0.39457(15) 1.02576(12) 0.0158(5) Uani 1 1 d . . . N12 N 0.37332(16) 0.02776(18) 1.02844(17) 0.0406(7) Uani 1 1 d . . . C1 C 0.30026(13) 0.59409(18) 0.86432(15) 0.0156(5) Uani 1 1 d . . . C2 C 0.34636(13) 0.66180(17) 0.82982(15) 0.0154(5) Uani 1 1 d . . . C3 C 0.39816(13) 0.67861(18) 0.88726(15) 0.0160(6) Uani 1 1 d . . . C4 C 0.38377(13) 0.61967(17) 0.95564(15) 0.0139(5) Uani 1 1 d . . . C5 C 0.42443(13) 0.60727(17) 1.02674(15) 0.0143(5) Uani 1 1 d . . . C6 C 0.40436(13) 0.57174(17) 1.09911(15) 0.0139(5) Uani 1 1 d . . . C7 C 0.44731(13) 0.54714(17) 1.17095(15) 0.0152(6) Uani 1 1 d . . . C8 C 0.40334(13) 0.52658(17) 1.22835(15) 0.0157(5) Uani 1 1 d . . . C9 C 0.33402(13) 0.53747(17) 1.19184(15) 0.0147(5) Uani 1 1 d . . . C10 C 0.27180(13) 0.53203(17) 1.22694(15) 0.0163(6) Uani 1 1 d . . . C11 C 0.20626(13) 0.52053(17) 1.19010(15) 0.0157(5) Uani 1 1 d . . . C12 C 0.14038(13) 0.51852(18) 1.22597(16) 0.0167(6) Uani 1 1 d . . . C13 C 0.09399(14) 0.48209(18) 1.17007(16) 0.0183(6) Uani 1 1 d . . . C14 C 0.13200(13) 0.46381(17) 1.09927(15) 0.0159(6) Uani 1 1 d . . . C15 C 0.11020(13) 0.41877(18) 1.02825(16) 0.0173(6) Uani 1 1 d . . . C16 C 0.14021(13) 0.42170(18) 0.95504(15) 0.0156(6) Uani 1 1 d . . . C17 C 0.11840(13) 0.37354(18) 0.88111(16) 0.0175(6) Uani 1 1 d . . . C18 C 0.15127(13) 0.41727(18) 0.82191(16) 0.0179(6) Uani 1 1 d . . . C19 C 0.19754(13) 0.48687(18) 0.86147(15) 0.0166(6) Uani 1 1 d . . . C20 C 0.24398(13) 0.54751(18) 0.82765(15) 0.0155(5) Uani 1 1 d . . . C21 C 0.34063(14) 0.71010(19) 0.74940(15) 0.0189(6) Uani 1 1 d . . . H21A H 0.3486 0.7788 0.7571 0.023 Uiso 1 1 calc R . . H21B H 0.2933 0.7017 0.7251 0.023 Uiso 1 1 calc R . . C22 C 0.39183(14) 0.6719(2) 0.69161(16) 0.0232(6) Uani 1 1 d . . . H22A H 0.3875 0.7079 0.6415 0.035 Uiso 1 1 calc R . . H22B H 0.3820 0.6049 0.6805 0.035 Uiso 1 1 calc R . . H22C H 0.4388 0.6783 0.7159 0.035 Uiso 1 1 calc R . . C23 C 0.45251(14) 0.75430(18) 0.88369(16) 0.0200(6) Uani 1 1 d . . . H23A H 0.4510 0.7812 0.8290 0.024 Uiso 1 1 calc R . . H23B H 0.4985 0.7255 0.8950 0.024 Uiso 1 1 calc R . . C24 C 0.44230(15) 0.83404(19) 0.94410(17) 0.0251(7) Uani 1 1 d . . . H24A H 0.4785 0.8817 0.9399 0.038 Uiso 1 1 calc R . . H24B H 0.4448 0.8078 0.9985 0.038 Uiso 1 1 calc R . . H24C H 0.3971 0.8634 0.9325 0.038 Uiso 1 1 calc R . . C25 C 0.52441(13) 0.53224(18) 1.18014(16) 0.0168(6) Uani 1 1 d . . . H25A H 0.5427 0.5341 1.1263 0.020 Uiso 1 1 calc R . . H25B H 0.5334 0.4681 1.2023 0.020 Uiso 1 1 calc R . . C26 C 0.56446(14) 0.6041(2) 1.23379(16) 0.0228(6) Uani 1 1 d . . . H26A H 0.6135 0.5879 1.2370 0.034 Uiso 1 1 calc R . . H26B H 0.5473 0.6027 1.2876 0.034 Uiso 1 1 calc R . . H26C H 0.5581 0.6677 1.2111 0.034 Uiso 1 1 calc R . . C27 C 0.42404(14) 0.47696(19) 1.30590(16) 0.0194(6) Uani 1 1 d . . . H27A H 0.3952 0.4999 1.3486 0.023 Uiso 1 1 calc R . . H27B H 0.4727 0.4915 1.3220 0.023 Uiso 1 1 calc R . . C28 C 0.41500(15) 0.37002(19) 1.29594(17) 0.0238(6) Uani 1 1 d . . . H28A H 0.4312 0.3381 1.3457 0.036 Uiso 1 1 calc R . . H28B H 0.4418 0.3479 1.2520 0.036 Uiso 1 1 calc R . . H28C H 0.3662 0.3554 1.2838 0.036 Uiso 1 1 calc R . . C29 C 0.12243(15) 0.5643(2) 1.30343(16) 0.0252(6) Uani 1 1 d . . . H29A H 0.1558 0.5438 1.3472 0.030 Uiso 1 1 calc R . . H29B H 0.0759 0.5436 1.3169 0.030 Uiso 1 1 calc R . . C30 C 0.12391(18) 0.6722(2) 1.29639(19) 0.0375(8) Uani 1 1 d . . . H30A H 0.1102 0.7005 1.3465 0.056 Uiso 1 1 calc R . . H30B H 0.0918 0.6923 1.2521 0.056 Uiso 1 1 calc R . . H30C H 0.1706 0.6929 1.2861 0.056 Uiso 1 1 calc R . . C31 C 0.01761(13) 0.4748(2) 1.17815(16) 0.0204(6) Uani 1 1 d . . . H31A H -0.0055 0.4683 1.1240 0.024 Uiso 1 1 calc R . . H31B H 0.0015 0.5347 1.2014 0.024 Uiso 1 1 calc R . . C32 C -0.00495(15) 0.3927(2) 1.22969(18) 0.0299(7) Uani 1 1 d . . . H32A H -0.0553 0.3912 1.2289 0.045 Uiso 1 1 calc R . . H32B H 0.0142 0.4012 1.2849 0.045 Uiso 1 1 calc R . . H32C H 0.0118 0.3330 1.2084 0.045 Uiso 1 1 calc R . . C33 C 0.07638(15) 0.28405(19) 0.87157(17) 0.0236(6) Uani 1 1 d . . . H33A H 0.0666 0.2708 0.8138 0.028 Uiso 1 1 calc R . . H33B H 0.0319 0.2931 0.8961 0.028 Uiso 1 1 calc R . . C34 C 0.11437(18) 0.1993(2) 0.9112(2) 0.0380(8) Uani 1 1 d . . . H34A H 0.0843 0.1436 0.9081 0.057 Uiso 1 1 calc R . . H34B H 0.1270 0.2140 0.9675 0.057 Uiso 1 1 calc R . . H34C H 0.1561 0.1861 0.8834 0.057 Uiso 1 1 calc R . . C35 C 0.14424(15) 0.3891(2) 0.73469(16) 0.0259(7) Uani 1 1 d . . . H35A H 0.1518 0.4455 0.7013 0.031 Uiso 1 1 calc R . . H35B H 0.0967 0.3663 0.7215 0.031 Uiso 1 1 calc R . . C36 C 0.19480(18) 0.3122(3) 0.7142(2) 0.0426(9) Uani 1 1 d . . . H36A H 0.1887 0.2974 0.6569 0.064 Uiso 1 1 calc R . . H36B H 0.1864 0.2552 0.7455 0.064 Uiso 1 1 calc R . . H36C H 0.2420 0.3344 0.7269 0.064 Uiso 1 1 calc R . . C37 C 0.15607(14) 0.67731(19) 1.01709(16) 0.0205(6) Uani 1 1 d . . . H37A H 0.1259 0.6249 1.0085 0.025 Uiso 1 1 calc R . . C38 C 0.12820(15) 0.7672(2) 1.01825(17) 0.0235(6) Uani 1 1 d . . . H38A H 0.0798 0.7762 1.0109 0.028 Uiso 1 1 calc R . . C39 C 0.17201(15) 0.84403(19) 1.03025(16) 0.0211(6) Uani 1 1 d . . . C40 C 0.24282(14) 0.82834(19) 1.03938(16) 0.0218(6) Uani 1 1 d . . . H40A H 0.2742 0.8797 1.0462 0.026 Uiso 1 1 calc R . . C41 C 0.26600(14) 0.73627(19) 1.03824(15) 0.0185(6) Uani 1 1 d . . . H41A H 0.3142 0.7255 1.0453 0.022 Uiso 1 1 calc R . . C42 C 0.14473(16) 0.9395(2) 1.03320(17) 0.0284(7) Uani 1 1 d . . . C43 C 0.30929(14) 0.34524(18) 1.09372(16) 0.0186(6) Uani 1 1 d . . . H43A H 0.3022 0.3761 1.1430 0.022 Uiso 1 1 calc R . . C44 C 0.33030(14) 0.25118(19) 1.09582(17) 0.0212(6) Uani 1 1 d . . . H44A H 0.3393 0.2195 1.1455 0.025 Uiso 1 1 calc R . . C45 C 0.33777(14) 0.20453(18) 1.02416(17) 0.0203(6) Uani 1 1 d . . . C46 C 0.32623(14) 0.2546(2) 0.95297(16) 0.0221(6) Uani 1 1 d . . . H46A H 0.3305 0.2242 0.9028 0.026 Uiso 1 1 calc R . . C47 C 0.30849(13) 0.34895(19) 0.95640(16) 0.0184(6) Uani 1 1 d . . . H47A H 0.3030 0.3836 0.9077 0.022 Uiso 1 1 calc R . . C48 C 0.35750(16) 0.1053(2) 1.02468(18) 0.0281(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 0.0132(2) 0.01477(19) 0.0136(2) -0.00009(15) 0.00089(14) -0.00087(15) O1 0.0185(10) 0.0265(10) 0.0238(11) -0.0021(9) 0.0065(8) 0.0003(8) O2 0.0228(11) 0.0205(10) 0.0222(11) -0.0034(8) -0.0029(8) -0.0039(8) O3 0.0289(12) 0.0311(11) 0.0191(11) -0.0069(9) 0.0031(8) -0.0023(9) O4 0.0260(11) 0.0311(11) 0.0217(11) 0.0085(9) 0.0019(8) -0.0010(9) O5 0.0378(13) 0.0281(11) 0.0338(13) 0.0084(10) 0.0019(10) -0.0102(10) O6 0.0156(10) 0.0377(12) 0.0294(12) 0.0010(9) -0.0015(9) -0.0010(9) O7 0.0223(11) 0.0341(11) 0.0226(11) 0.0064(9) -0.0049(8) 0.0020(9) O8 0.0222(11) 0.0342(11) 0.0179(10) -0.0045(9) 0.0043(8) -0.0007(9) N1 0.0141(11) 0.0145(11) 0.0144(12) -0.0021(9) 0.0005(9) 0.0000(9) N2 0.0152(11) 0.0135(10) 0.0149(11) -0.0008(9) 0.0018(9) -0.0003(9) N3 0.0148(11) 0.0152(11) 0.0159(12) -0.0008(9) 0.0025(9) 0.0017(9) N4 0.0121(11) 0.0181(11) 0.0156(12) -0.0004(9) -0.0001(9) -0.0007(9) N5 0.0195(12) 0.0164(11) 0.0129(11) 0.0024(9) -0.0001(9) -0.0031(10) N6 0.0134(12) 0.0265(13) 0.0171(12) 0.0036(10) 0.0008(9) 0.0019(10) N7 0.0206(13) 0.0230(12) 0.0195(13) 0.0006(10) -0.0006(10) -0.0031(10) N8 0.0164(12) 0.0281(13) 0.0151(12) 0.0021(10) 0.0010(10) -0.0078(10) N9 0.0172(12) 0.0177(11) 0.0113(11) 0.0005(9) 0.0020(9) -0.0015(9) N10 0.068(2) 0.0269(15) 0.0330(16) 0.0003(12) -0.0034(14) 0.0155(15) N11 0.0154(12) 0.0193(11) 0.0127(11) -0.0007(9) 0.0010(9) -0.0059(9) N12 0.055(2) 0.0242(15) 0.0425(18) -0.0034(12) 0.0020(14) 0.0080(13) C1 0.0153(13) 0.0171(13) 0.0145(14) 0.0000(11) 0.0022(10) 0.0029(11) C2 0.0170(14) 0.0139(12) 0.0154(14) -0.0012(10) 0.0030(11) 0.0032(11) C3 0.0158(14) 0.0156(13) 0.0168(14) 0.0001(11) 0.0024(11) 0.0004(11) C4 0.0152(13) 0.0131(12) 0.0138(13) -0.0016(10) 0.0045(10) 0.0003(10) C5 0.0127(13) 0.0132(12) 0.0174(14) -0.0012(10) 0.0025(10) -0.0013(10) C6 0.0148(13) 0.0116(12) 0.0151(14) -0.0028(10) 0.0004(10) 0.0003(10) C7 0.0176(14) 0.0123(12) 0.0155(14) -0.0027(10) -0.0019(11) 0.0000(10) C8 0.0190(14) 0.0115(12) 0.0162(14) -0.0010(10) -0.0005(11) -0.0009(11) C9 0.0186(14) 0.0133(12) 0.0122(13) -0.0013(10) 0.0001(10) -0.0023(11) C10 0.0196(14) 0.0154(13) 0.0138(13) 0.0009(11) 0.0009(10) 0.0007(11) C11 0.0176(14) 0.0139(13) 0.0157(14) -0.0007(11) 0.0026(10) 0.0004(11) C12 0.0156(13) 0.0171(13) 0.0178(14) 0.0042(11) 0.0048(11) 0.0014(11) C13 0.0179(14) 0.0186(14) 0.0183(14) 0.0048(11) 0.0013(11) 0.0042(11) C14 0.0143(13) 0.0150(13) 0.0182(14) 0.0057(11) 0.0004(10) 0.0005(11) C15 0.0134(13) 0.0170(13) 0.0212(15) 0.0030(11) -0.0013(11) -0.0041(11) C16 0.0135(13) 0.0157(13) 0.0175(14) 0.0013(11) 0.0004(10) 0.0026(11) C17 0.0166(14) 0.0175(13) 0.0179(14) 0.0010(11) -0.0023(11) 0.0006(11) C18 0.0167(14) 0.0190(14) 0.0179(14) -0.0037(11) -0.0004(11) 0.0004(11) C19 0.0156(14) 0.0197(13) 0.0140(14) -0.0007(11) -0.0016(10) 0.0024(11) C20 0.0133(13) 0.0208(13) 0.0125(13) -0.0012(11) 0.0002(10) 0.0016(11) C21 0.0179(14) 0.0222(14) 0.0166(14) 0.0036(11) 0.0003(11) 0.0002(11) C22 0.0219(15) 0.0307(16) 0.0172(15) 0.0080(12) 0.0028(11) -0.0002(12) C23 0.0212(15) 0.0188(13) 0.0197(15) 0.0055(11) -0.0009(11) -0.0026(12) C24 0.0295(17) 0.0191(14) 0.0260(16) 0.0027(12) -0.0046(13) -0.0056(12) C25 0.0159(14) 0.0173(13) 0.0172(14) 0.0018(11) 0.0005(10) 0.0033(11) C26 0.0184(15) 0.0260(15) 0.0235(16) -0.0010(12) -0.0013(12) -0.0020(12) C27 0.0188(14) 0.0239(14) 0.0154(14) 0.0011(11) 0.0014(11) -0.0008(12) C28 0.0241(16) 0.0235(15) 0.0236(16) 0.0071(12) 0.0005(12) 0.0007(12) C29 0.0246(16) 0.0315(16) 0.0199(15) -0.0023(13) 0.0047(12) 0.0037(13) C30 0.051(2) 0.0355(18) 0.0261(18) -0.0072(14) 0.0049(15) 0.0152(16) C31 0.0162(14) 0.0279(15) 0.0173(14) 0.0038(12) 0.0026(11) 0.0018(12) C32 0.0210(16) 0.0385(18) 0.0305(18) 0.0115(14) 0.0044(13) -0.0034(14) C33 0.0278(16) 0.0222(14) 0.0204(15) -0.0025(12) 0.0003(12) -0.0058(12) C34 0.053(2) 0.0227(16) 0.037(2) -0.0003(14) -0.0083(16) -0.0062(15) C35 0.0274(16) 0.0326(16) 0.0178(15) -0.0065(12) 0.0021(12) -0.0082(13) C36 0.040(2) 0.052(2) 0.036(2) -0.0217(17) 0.0085(16) 0.0008(17) C37 0.0185(15) 0.0228(14) 0.0199(15) -0.0016(12) -0.0002(11) -0.0008(12) C38 0.0188(15) 0.0272(15) 0.0242(16) 0.0024(12) -0.0008(12) 0.0048(12) C39 0.0298(16) 0.0187(14) 0.0148(14) -0.0020(11) 0.0012(12) 0.0046(12) C40 0.0257(16) 0.0215(14) 0.0180(15) 0.0006(12) 0.0013(12) -0.0032(12) C41 0.0175(14) 0.0239(14) 0.0142(14) -0.0014(11) 0.0005(11) -0.0007(12) C42 0.0369(18) 0.0266(16) 0.0211(16) -0.0008(13) -0.0028(13) 0.0023(14) C43 0.0221(15) 0.0173(13) 0.0165(14) -0.0006(11) 0.0014(11) -0.0009(11) C44 0.0235(15) 0.0191(14) 0.0211(15) 0.0009(12) 0.0010(12) 0.0028(12) C45 0.0178(14) 0.0164(13) 0.0268(16) -0.0003(12) 0.0031(11) 0.0004(11) C46 0.0185(15) 0.0273(15) 0.0205(15) -0.0054(12) 0.0013(11) 0.0005(12) C47 0.0157(14) 0.0241(14) 0.0154(14) -0.0017(11) -0.0002(11) 0.0017(11) C48 0.0322(17) 0.0256(16) 0.0265(17) -0.0028(13) 0.0024(13) 0.0043(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.980(2) . ? Fe1 N1 1.984(2) . ? Fe1 N4 1.984(2) . ? Fe1 N2 1.995(2) . ? Fe1 N11 2.014(2) . ? Fe1 N9 2.015(2) . ? O1 N5 1.212(3) . ? O2 N5 1.236(3) . ? O3 N6 1.209(3) . ? O4 N6 1.231(3) . ? O5 N7 1.222(3) . ? O6 N7 1.227(3) . ? O7 N8 1.227(3) . ? O8 N8 1.224(3) . ? N1 C4 1.376(3) . ? N1 C1 1.383(3) . ? N2 C6 1.372(3) . ? N2 C9 1.381(3) . ? N3 C14 1.374(3) . ? N3 C11 1.379(3) . ? N4 C19 1.375(3) . ? N4 C16 1.376(3) . ? N5 C5 1.474(3) . ? N6 C10 1.493(3) . ? N7 C15 1.479(3) . ? N8 C20 1.481(3) . ? N9 C41 1.343(3) . ? N9 C37 1.349(3) . ? N10 C42 1.139(4) . ? N11 C43 1.338(3) . ? N11 C47 1.352(3) . ? N12 C48 1.138(4) . ? C1 C20 1.386(4) . ? C1 C2 1.456(4) . ? C2 C3 1.368(3) . ? C2 C21 1.506(3) . ? C3 C4 1.456(4) . ? C3 C23 1.507(4) . ? C4 C5 1.396(3) . ? C5 C6 1.389(4) . ? C6 C7 1.461(3) . ? C7 C8 1.358(4) . ? C7 C25 1.513(4) . ? C8 C9 1.452(4) . ? C8 C27 1.506(4) . ? C9 C10 1.381(4) . ? C10 C11 1.390(4) . ? C11 C12 1.450(4) . ? C12 C13 1.358(4) . ? C12 C29 1.509(4) . ? C13 C14 1.459(4) . ? C13 C31 1.504(4) . ? C14 C15 1.389(4) . ? C15 C16 1.391(4) . ? C16 C17 1.451(4) . ? C17 C18 1.361(4) . ? C17 C33 1.508(4) . ? C18 C19 1.462(4) . ? C18 C35 1.510(4) . ? C19 C20 1.391(4) . ? C21 C22 1.530(4) . ? C23 C24 1.534(4) . ? C25 C26 1.534(4) . ? C27 C28 1.528(4) . ? C29 C30 1.529(4) . ? C31 C32 1.526(4) . ? C33 C34 1.535(4) . ? C35 C36 1.519(4) . ? C37 C38 1.380(4) . ? C38 C39 1.387(4) . ? C39 C40 1.394(4) . ? C39 C42 1.451(4) . ? C40 C41 1.377(4) . ? C43 C44 1.390(4) . ? C44 C45 1.384(4) . ? C45 C46 1.390(4) . ? C45 C48 1.453(4) . ? C46 C47 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N1 174.48(8) . . ? N3 Fe1 N4 89.79(9) . . ? N1 Fe1 N4 90.24(9) . . ? N3 Fe1 N2 90.12(9) . . ? N1 Fe1 N2 90.39(9) . . ? N4 Fe1 N2 174.39(8) . . ? N3 Fe1 N11 91.16(9) . . ? N1 Fe1 N11 94.35(9) . . ? N4 Fe1 N11 86.10(8) . . ? N2 Fe1 N11 88.29(8) . . ? N3 Fe1 N9 88.21(9) . . ? N1 Fe1 N9 86.27(8) . . ? N4 Fe1 N9 93.18(9) . . ? N2 Fe1 N9 92.42(8) . . ? N11 Fe1 N9 179.06(9) . . ? C4 N1 C1 104.9(2) . . ? C4 N1 Fe1 126.06(16) . . ? C1 N1 Fe1 125.84(17) . . ? C6 N2 C9 105.2(2) . . ? C6 N2 Fe1 125.71(17) . . ? C9 N2 Fe1 125.58(17) . . ? C14 N3 C11 104.8(2) . . ? C14 N3 Fe1 127.36(17) . . ? C11 N3 Fe1 126.13(17) . . ? C19 N4 C16 105.0(2) . . ? C19 N4 Fe1 127.12(17) . . ? C16 N4 Fe1 125.03(17) . . ? O1 N5 O2 124.6(2) . . ? O1 N5 C5 118.3(2) . . ? O2 N5 C5 117.1(2) . . ? O3 N6 O4 125.3(2) . . ? O3 N6 C10 117.9(2) . . ? O4 N6 C10 116.8(2) . . ? O5 N7 O6 124.8(2) . . ? O5 N7 C15 117.3(2) . . ? O6 N7 C15 117.9(2) . . ? O8 N8 O7 125.1(2) . . ? O8 N8 C20 117.9(2) . . ? O7 N8 C20 117.1(2) . . ? C41 N9 C37 117.5(2) . . ? C41 N9 Fe1 121.40(18) . . ? C37 N9 Fe1 121.13(17) . . ? C43 N11 C47 117.2(2) . . ? C43 N11 Fe1 121.07(17) . . ? C47 N11 Fe1 121.56(17) . . ? N1 C1 C20 120.2(2) . . ? N1 C1 C2 111.0(2) . . ? C20 C1 C2 128.7(2) . . ? C3 C2 C1 106.3(2) . . ? C3 C2 C21 123.9(2) . . ? C1 C2 C21 129.8(2) . . ? C2 C3 C4 106.4(2) . . ? C2 C3 C23 125.6(2) . . ? C4 C3 C23 127.4(2) . . ? N1 C4 C5 121.1(2) . . ? N1 C4 C3 111.1(2) . . ? C5 C4 C3 127.8(2) . . ? C6 C5 C4 127.7(2) . . ? C6 C5 N5 116.2(2) . . ? C4 C5 N5 116.1(2) . . ? N2 C6 C5 120.6(2) . . ? N2 C6 C7 110.7(2) . . ? C5 C6 C7 128.7(2) . . ? C8 C7 C6 106.2(2) . . ? C8 C7 C25 124.4(2) . . ? C6 C7 C25 128.9(2) . . ? C7 C8 C9 106.9(2) . . ? C7 C8 C27 124.2(2) . . ? C9 C8 C27 126.9(2) . . ? N2 C9 C10 120.4(2) . . ? N2 C9 C8 110.4(2) . . ? C10 C9 C8 129.1(2) . . ? C9 C10 C11 128.5(2) . . ? C9 C10 N6 116.6(2) . . ? C11 C10 N6 114.7(2) . . ? N3 C11 C10 119.7(2) . . ? N3 C11 C12 110.7(2) . . ? C10 C11 C12 129.0(2) . . ? C13 C12 C11 106.8(2) . . ? C13 C12 C29 125.0(2) . . ? C11 C12 C29 127.3(2) . . ? C12 C13 C14 106.1(2) . . ? C12 C13 C31 125.5(2) . . ? C14 C13 C31 128.0(2) . . ? N3 C14 C15 119.8(2) . . ? N3 C14 C13 110.9(2) . . ? C15 C14 C13 129.2(2) . . ? C14 C15 C16 128.1(2) . . ? C14 C15 N7 115.4(2) . . ? C16 C15 N7 116.5(2) . . ? N4 C16 C15 120.2(2) . . ? N4 C16 C17 111.0(2) . . ? C15 C16 C17 128.3(2) . . ? C18 C17 C16 106.4(2) . . ? C18 C17 C33 125.5(2) . . ? C16 C17 C33 127.6(2) . . ? C17 C18 C19 106.3(2) . . ? C17 C18 C35 124.5(2) . . ? C19 C18 C35 129.0(2) . . ? N4 C19 C20 120.4(2) . . ? N4 C19 C18 110.7(2) . . ? C20 C19 C18 128.8(2) . . ? C1 C20 C19 128.9(2) . . ? C1 C20 N8 116.3(2) . . ? C19 C20 N8 114.9(2) . . ? C2 C21 C22 113.0(2) . . ? C3 C23 C24 111.9(2) . . ? C7 C25 C26 115.5(2) . . ? C8 C27 C28 110.1(2) . . ? C12 C29 C30 110.8(2) . . ? C13 C31 C32 115.1(2) . . ? C17 C33 C34 111.4(2) . . ? C18 C35 C36 112.8(2) . . ? N9 C37 C38 122.7(3) . . ? C37 C38 C39 118.9(3) . . ? C38 C39 C40 119.0(2) . . ? C38 C39 C42 120.6(3) . . ? C40 C39 C42 120.3(3) . . ? C41 C40 C39 118.1(3) . . ? N9 C41 C40 123.7(3) . . ? N10 C42 C39 178.6(3) . . ? N11 C43 C44 123.3(2) . . ? C45 C44 C43 118.7(3) . . ? C44 C45 C46 118.7(2) . . ? C44 C45 C48 119.8(2) . . ? C46 C45 C48 121.6(3) . . ? C47 C46 C45 118.9(2) . . ? N11 C47 C46 123.1(2) . . ? N12 C48 C45 177.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.596 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.072 # Attachment '2octa.cif' data_2octa _database_code_depnum_ccdc_archive 'CCDC 755824' #TrackingRef '2octa.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(tn-OEP)(3-Cl-pyridine)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H48 Cl2 Fe N10 O8' _chemical_formula_weight 995.69 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.3561(10) _cell_length_b 25.439(2) _cell_length_c 27.699(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9411.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.0 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8649 _exptl_absorpt_correction_T_max 0.9290 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51053 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9247 _reflns_number_gt 6266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0618P)^2^+3.5508P] 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 9247 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 -0.55309(3) 0.142010(15) 0.878755(15) 0.02309(12) Uani 1 1 d . . . Cl1 Cl -0.76289(12) 0.19903(7) 0.71447(5) 0.0594(4) Uani 0.65 1 d P . . Cl1A Cl -0.3927(3) 0.11119(12) 0.69640(10) 0.0632(9) Uani 0.35 1 d P . . Cl2 Cl -0.59011(8) 0.01875(4) 1.04298(3) 0.0542(3) Uani 1 1 d . . . O1 O -0.7085(2) -0.03433(10) 0.79766(9) 0.0504(7) Uani 1 1 d . . . O2 O -0.6391(2) -0.06824(9) 0.86105(10) 0.0558(7) Uani 1 1 d . . . O3 O -0.20886(19) 0.05631(11) 0.93846(11) 0.0583(8) Uani 1 1 d . . . O4 O -0.14768(19) 0.09346(11) 0.87515(10) 0.0568(7) Uani 1 1 d . . . O5 O -0.4005(2) 0.33087(10) 0.82536(10) 0.0524(7) Uani 1 1 d . . . O6 O -0.46958(19) 0.35391(9) 0.89335(10) 0.0502(7) Uani 1 1 d . . . O7 O -0.95399(18) 0.19159(10) 0.89075(10) 0.0508(7) Uani 1 1 d . . . O8 O -0.89378(18) 0.21399(9) 0.96048(10) 0.0459(6) Uani 1 1 d . . . N1 N -0.68246(18) 0.10567(9) 0.88056(9) 0.0249(5) Uani 1 1 d . . . N2 N -0.48436(19) 0.07502(9) 0.86814(9) 0.0251(6) Uani 1 1 d . . . N3 N -0.42275(18) 0.17783(9) 0.88278(9) 0.0254(6) Uani 1 1 d . . . N4 N -0.62111(18) 0.21013(9) 0.88340(9) 0.0240(5) Uani 1 1 d . . . N5 N -0.6611(2) -0.03084(10) 0.83513(11) 0.0399(7) Uani 1 1 d . . . N6 N -0.2170(2) 0.08197(11) 0.90205(11) 0.0368(7) Uani 1 1 d . . . N7 N -0.4469(2) 0.32139(10) 0.86237(12) 0.0398(7) Uani 1 1 d . . . N8 N -0.8853(2) 0.19585(10) 0.91996(12) 0.0372(7) Uani 1 1 d . . . N9 N -0.56022(19) 0.14986(9) 0.80666(9) 0.0268(6) Uani 1 1 d . . . N10 N -0.54741(17) 0.13412(9) 0.95015(8) 0.0234(5) Uani 1 1 d . . . C1 C -0.7680(2) 0.12472(12) 0.90244(11) 0.0285(7) Uani 1 1 d . . . C2 C -0.8367(2) 0.08200(12) 0.91344(12) 0.0321(7) Uani 1 1 d . . . C3 C -0.7977(2) 0.03808(12) 0.89228(12) 0.0339(8) Uani 1 1 d . . . C4 C -0.7012(2) 0.05320(11) 0.87259(11) 0.0284(7) Uani 1 1 d . . . C5 C -0.6278(2) 0.02177(11) 0.85087(11) 0.0294(7) Uani 1 1 d . . . C6 C -0.5259(2) 0.03139(11) 0.84630(11) 0.0302(7) Uani 1 1 d . . . C7 C -0.4475(3) -0.00208(12) 0.82635(12) 0.0352(8) Uani 1 1 d . . . C8 C -0.3592(3) 0.01865(12) 0.84111(11) 0.0328(7) Uani 1 1 d . . . C9 C -0.3827(2) 0.06602(12) 0.86793(11) 0.0300(7) Uani 1 1 d . . . C10 C -0.3182(2) 0.10216(12) 0.88994(11) 0.0280(7) Uani 1 1 d . . . C11 C -0.3352(2) 0.15474(12) 0.89906(11) 0.0280(7) Uani 1 1 d . . . C12 C -0.2657(2) 0.19464(12) 0.91606(11) 0.0315(7) Uani 1 1 d . . . C13 C -0.3060(2) 0.24167(13) 0.90366(12) 0.0326(7) Uani 1 1 d . . . C14 C -0.4045(2) 0.23096(11) 0.88354(11) 0.0283(7) Uani 1 1 d . . . C15 C -0.4794(2) 0.26607(11) 0.86997(11) 0.0290(7) Uani 1 1 d . . . C16 C -0.5814(2) 0.25750(11) 0.86778(10) 0.0272(7) Uani 1 1 d . . . C17 C -0.6613(2) 0.29462(11) 0.85702(11) 0.0291(7) Uani 1 1 d . . . C18 C -0.7477(2) 0.27196(11) 0.87236(11) 0.0299(7) Uani 1 1 d . . . C19 C -0.7217(2) 0.21900(11) 0.88841(11) 0.0261(7) Uani 1 1 d . . . C20 C -0.7844(2) 0.17868(12) 0.90462(11) 0.0271(7) Uani 1 1 d . . . C21 C -0.9259(3) 0.08347(13) 0.94633(14) 0.0431(9) Uani 1 1 d . . . H21A H -0.9662 0.0512 0.9415 0.052 Uiso 1 1 calc R . . H21B H -0.9683 0.1140 0.9378 0.052 Uiso 1 1 calc R . . C22 C -0.8956(3) 0.08739(16) 0.99910(14) 0.0550(11) Uani 1 1 d . . . H22A H -0.9557 0.0883 1.0194 0.082 Uiso 1 1 calc R . . H22B H -0.8567 0.1196 1.0042 0.082 Uiso 1 1 calc R . . H22C H -0.8547 0.0568 1.0078 0.082 Uiso 1 1 calc R . . C23 C -0.8462(3) -0.01539(13) 0.89343(13) 0.0441(9) Uani 1 1 d . . . H23A H -0.8277 -0.0348 0.8637 0.053 Uiso 1 1 calc R . . H23B H -0.9198 -0.0110 0.8935 0.053 Uiso 1 1 calc R . . C24 C -0.8155(3) -0.04801(15) 0.93748(16) 0.0643(12) Uani 1 1 d . . . H24A H -0.8461 -0.0829 0.9354 0.096 Uiso 1 1 calc R . . H24B H -0.8383 -0.0304 0.9670 0.096 Uiso 1 1 calc R . . H24C H -0.7425 -0.0516 0.9383 0.096 Uiso 1 1 calc R . . C25 C -0.4592(3) -0.04689(14) 0.79123(14) 0.0497(10) Uani 1 1 d . . . H25A H -0.5137 -0.0703 0.8024 0.060 Uiso 1 1 calc R . . H25B H -0.3966 -0.0676 0.7905 0.060 Uiso 1 1 calc R . . C26 C -0.4832(3) -0.02756(17) 0.74043(14) 0.0613(12) Uani 1 1 d . . . H26A H -0.4926 -0.0578 0.7190 0.092 Uiso 1 1 calc R . . H26B H -0.4276 -0.0060 0.7285 0.092 Uiso 1 1 calc R . . H26C H -0.5446 -0.0065 0.7411 0.092 Uiso 1 1 calc R . . C27 C -0.2563(3) -0.00259(14) 0.82734(13) 0.0452(9) Uani 1 1 d . . . H27A H -0.2076 0.0268 0.8273 0.054 Uiso 1 1 calc R . . H27B H -0.2594 -0.0170 0.7942 0.054 Uiso 1 1 calc R . . C28 C -0.2187(3) -0.04542(16) 0.86148(16) 0.0631(12) Uani 1 1 d . . . H28A H -0.1541 -0.0587 0.8500 0.095 Uiso 1 1 calc R . . H28B H -0.2673 -0.0743 0.8624 0.095 Uiso 1 1 calc R . . H28C H -0.2107 -0.0308 0.8940 0.095 Uiso 1 1 calc R . . C29 C -0.1738(2) 0.18803(14) 0.94701(13) 0.0418(9) Uani 1 1 d . . . H29A H -0.1279 0.2179 0.9413 0.050 Uiso 1 1 calc R . . H29B H -0.1386 0.1554 0.9375 0.050 Uiso 1 1 calc R . . C30 C -0.1992(3) 0.18539(17) 1.00021(14) 0.0550(11) Uani 1 1 d . . . H30A H -0.1374 0.1824 1.0191 0.082 Uiso 1 1 calc R . . H30B H -0.2416 0.1546 1.0063 0.082 Uiso 1 1 calc R . . H30C H -0.2351 0.2174 1.0097 0.082 Uiso 1 1 calc R . . C31 C -0.2535(3) 0.29422(13) 0.90966(13) 0.0392(8) Uani 1 1 d . . . H31A H -0.2169 0.2947 0.9407 0.047 Uiso 1 1 calc R . . H31B H -0.3038 0.3228 0.9103 0.047 Uiso 1 1 calc R . . C32 C -0.1798(3) 0.30354(15) 0.86809(15) 0.0543(11) Uani 1 1 d . . . H32A H -0.1492 0.3383 0.8716 0.082 Uiso 1 1 calc R . . H32B H -0.2157 0.3017 0.8373 0.082 Uiso 1 1 calc R . . H32C H -0.1275 0.2765 0.8688 0.082 Uiso 1 1 calc R . . C33 C -0.6542(3) 0.34378(12) 0.82735(13) 0.0379(8) Uani 1 1 d . . . H33A H -0.5998 0.3663 0.8401 0.046 Uiso 1 1 calc R . . H33B H -0.7178 0.3636 0.8297 0.046 Uiso 1 1 calc R . . C34 C -0.6331(3) 0.33056(14) 0.77462(13) 0.0513(10) Uani 1 1 d . . . H34A H -0.6354 0.3628 0.7553 0.077 Uiso 1 1 calc R . . H34B H -0.6838 0.3058 0.7628 0.077 Uiso 1 1 calc R . . H34C H -0.5666 0.3145 0.7719 0.077 Uiso 1 1 calc R . . C35 C -0.8494(3) 0.29662(13) 0.86726(14) 0.0427(9) Uani 1 1 d . . . H35A H -0.8434 0.3349 0.8728 0.051 Uiso 1 1 calc R . . H35B H -0.8941 0.2822 0.8925 0.051 Uiso 1 1 calc R . . C36 C -0.8977(3) 0.28743(18) 0.81758(16) 0.0623(12) Uani 1 1 d . . . H36A H -0.9649 0.3029 0.8172 0.094 Uiso 1 1 calc R . . H36B H -0.9025 0.2496 0.8114 0.094 Uiso 1 1 calc R . . H36C H -0.8565 0.3039 0.7925 0.094 Uiso 1 1 calc R . . C37 C -0.6446(3) 0.16708(12) 0.78532(12) 0.0333(8) Uani 1 1 d . . . H37A H -0.7013 0.1742 0.8049 0.040 Uiso 1 1 calc R . . C38 C -0.6521(3) 0.17488(14) 0.73621(12) 0.0409(9) Uani 1 1 d . . . H38A H -0.7133 0.1885 0.7225 0.049 Uiso 0.35 1 d P A 1 C39 C -0.5721(3) 0.16333(16) 0.70659(13) 0.0508(10) Uani 1 1 d . . . H39A H -0.5756 0.1683 0.6726 0.061 Uiso 1 1 calc R . . C40 C -0.4871(3) 0.14428(17) 0.72837(13) 0.0550(11) Uani 1 1 d . . . H40A H -0.4297 0.1347 0.7088 0.066 Uiso 0.65 1 d P B 2 C41 C -0.4830(3) 0.13872(13) 0.77783(12) 0.0387(8) Uani 1 1 d . . . H41A H -0.4226 0.1264 0.7920 0.046 Uiso 1 1 calc R . . C42 C -0.5663(2) 0.08726(11) 0.97097(12) 0.0295(7) Uani 1 1 d . . . H42A H -0.5847 0.0584 0.9511 0.035 Uiso 1 1 calc R . . C43 C -0.5597(2) 0.07977(12) 1.02003(12) 0.0337(8) Uani 1 1 d . . . C44 C -0.5312(3) 0.11999(14) 1.04977(12) 0.0407(9) Uani 1 1 d . . . H44A H -0.5236 0.1149 1.0836 0.049 Uiso 1 1 calc R . . C45 C -0.5139(3) 0.16811(14) 1.02871(12) 0.0403(8) Uani 1 1 d . . . H45A H -0.4958 0.1973 1.0482 0.048 Uiso 1 1 calc R . . C46 C -0.5228(2) 0.17420(12) 0.97974(11) 0.0315(7) Uani 1 1 d . . . H46A H -0.5111 0.2079 0.9661 0.038 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 0.0270(2) 0.0148(2) 0.0274(2) 0.00130(17) 0.00156(18) -0.00036(17) Cl1 0.0539(10) 0.0817(12) 0.0426(9) 0.0140(8) -0.0190(7) -0.0077(8) Cl1A 0.079(2) 0.0641(19) 0.0463(17) 0.0003(14) 0.0347(15) 0.0182(16) Cl2 0.0772(7) 0.0378(5) 0.0475(6) 0.0175(4) 0.0172(5) 0.0067(5) O1 0.0619(18) 0.0424(15) 0.0469(16) -0.0105(12) -0.0106(13) -0.0082(13) O2 0.0681(19) 0.0201(13) 0.079(2) 0.0062(13) -0.0139(15) -0.0021(12) O3 0.0437(17) 0.0581(18) 0.073(2) 0.0253(16) -0.0116(14) 0.0027(13) O4 0.0368(16) 0.0684(19) 0.0653(19) -0.0026(15) 0.0181(13) 0.0051(13) O5 0.0555(17) 0.0425(15) 0.0591(18) 0.0167(13) 0.0046(14) -0.0164(13) O6 0.0569(18) 0.0221(12) 0.0716(18) -0.0122(12) -0.0102(13) -0.0046(11) O7 0.0305(15) 0.0522(16) 0.0698(19) 0.0140(13) -0.0046(13) 0.0031(12) O8 0.0470(16) 0.0356(14) 0.0551(17) -0.0008(12) 0.0175(12) 0.0059(11) N1 0.0296(15) 0.0155(12) 0.0296(14) 0.0012(10) 0.0000(11) -0.0013(10) N2 0.0291(14) 0.0181(12) 0.0281(14) 0.0016(10) 0.0026(11) 0.0021(10) N3 0.0269(14) 0.0211(13) 0.0283(14) 0.0014(11) 0.0029(11) 0.0007(10) N4 0.0267(14) 0.0152(12) 0.0302(14) 0.0020(10) 0.0015(11) -0.0026(10) N5 0.0470(19) 0.0219(15) 0.051(2) -0.0043(13) -0.0022(15) 0.0010(13) N6 0.0331(17) 0.0311(16) 0.0463(18) -0.0009(14) 0.0035(14) 0.0018(12) N7 0.0402(17) 0.0217(14) 0.058(2) 0.0065(14) -0.0089(15) -0.0091(13) N8 0.0361(18) 0.0242(14) 0.051(2) 0.0086(14) 0.0077(15) 0.0016(12) N9 0.0338(15) 0.0165(12) 0.0300(14) -0.0016(10) 0.0024(11) -0.0021(11) N10 0.0211(13) 0.0194(12) 0.0297(14) 0.0012(10) 0.0031(10) 0.0014(10) C1 0.0326(19) 0.0227(15) 0.0302(17) 0.0030(13) 0.0005(14) -0.0019(13) C2 0.0281(18) 0.0277(17) 0.041(2) 0.0073(14) 0.0010(14) -0.0049(14) C3 0.037(2) 0.0226(17) 0.042(2) 0.0075(14) -0.0032(15) -0.0052(14) C4 0.0344(19) 0.0183(15) 0.0323(18) 0.0051(13) -0.0016(14) -0.0012(13) C5 0.042(2) 0.0132(14) 0.0330(18) 0.0007(13) -0.0045(14) -0.0033(13) C6 0.040(2) 0.0216(16) 0.0288(17) 0.0003(13) -0.0012(14) 0.0042(14) C7 0.047(2) 0.0238(16) 0.0347(19) -0.0038(14) -0.0002(15) 0.0115(15) C8 0.041(2) 0.0249(17) 0.0326(18) 0.0030(14) 0.0009(15) 0.0065(14) C9 0.0350(19) 0.0250(16) 0.0299(18) 0.0047(13) 0.0041(14) 0.0061(14) C10 0.0255(18) 0.0299(17) 0.0288(18) 0.0034(13) 0.0053(13) 0.0045(13) C11 0.0222(17) 0.0285(17) 0.0334(18) 0.0079(13) 0.0035(13) -0.0021(13) C12 0.0266(18) 0.0322(18) 0.0357(19) -0.0011(14) 0.0023(14) -0.0020(14) C13 0.0286(18) 0.0310(18) 0.0382(19) -0.0001(15) 0.0026(14) -0.0080(14) C14 0.0320(18) 0.0206(15) 0.0324(18) -0.0012(13) 0.0060(14) -0.0055(13) C15 0.0371(19) 0.0181(15) 0.0317(18) 0.0013(13) -0.0006(14) -0.0063(13) C16 0.0340(18) 0.0174(15) 0.0301(17) -0.0013(13) 0.0011(13) -0.0014(12) C17 0.040(2) 0.0186(15) 0.0287(17) 0.0005(13) -0.0023(14) 0.0021(13) C18 0.0365(19) 0.0179(15) 0.0353(18) -0.0005(13) 0.0024(14) 0.0017(13) C19 0.0299(18) 0.0198(15) 0.0287(17) -0.0019(12) 0.0014(13) 0.0024(12) C20 0.0247(17) 0.0243(16) 0.0323(18) 0.0011(13) 0.0024(13) 0.0013(12) C21 0.037(2) 0.0307(19) 0.062(3) 0.0088(17) 0.0110(17) -0.0049(15) C22 0.060(3) 0.051(2) 0.054(3) 0.0023(19) 0.023(2) -0.003(2) C23 0.051(2) 0.0249(18) 0.057(2) 0.0034(16) 0.0025(18) -0.0138(16) C24 0.089(3) 0.038(2) 0.066(3) 0.014(2) -0.001(2) -0.017(2) C25 0.053(3) 0.036(2) 0.060(3) -0.0168(18) -0.0011(19) 0.0149(18) C26 0.070(3) 0.068(3) 0.046(2) -0.023(2) -0.004(2) 0.010(2) C27 0.044(2) 0.041(2) 0.050(2) -0.0051(18) 0.0075(17) 0.0117(17) C28 0.061(3) 0.050(3) 0.079(3) 0.004(2) 0.010(2) 0.024(2) C29 0.031(2) 0.037(2) 0.057(2) -0.0036(17) -0.0047(16) 0.0008(15) C30 0.048(3) 0.065(3) 0.052(3) 0.012(2) -0.0123(19) 0.000(2) C31 0.036(2) 0.0309(18) 0.050(2) -0.0001(16) -0.0033(16) -0.0101(15) C32 0.054(3) 0.046(2) 0.063(3) 0.006(2) -0.002(2) -0.0199(19) C33 0.042(2) 0.0198(16) 0.052(2) 0.0064(15) -0.0028(16) 0.0003(14) C34 0.071(3) 0.037(2) 0.046(2) 0.0172(18) -0.0020(19) -0.0113(19) C35 0.038(2) 0.0269(18) 0.063(3) 0.0133(17) 0.0073(18) 0.0093(15) C36 0.039(2) 0.076(3) 0.072(3) 0.025(2) -0.007(2) 0.004(2) C37 0.036(2) 0.0267(17) 0.037(2) -0.0004(14) -0.0002(15) -0.0048(14) C38 0.043(2) 0.044(2) 0.036(2) 0.0053(16) -0.0068(16) -0.0107(17) C39 0.058(3) 0.064(3) 0.030(2) 0.0046(18) -0.0019(18) -0.009(2) C40 0.058(3) 0.073(3) 0.033(2) -0.001(2) 0.0101(18) 0.008(2) C41 0.046(2) 0.0346(19) 0.036(2) 0.0015(15) 0.0022(16) 0.0046(16) C42 0.0293(18) 0.0233(16) 0.0359(19) 0.0054(14) 0.0033(14) 0.0004(13) C43 0.0363(19) 0.0294(17) 0.0354(19) 0.0098(15) 0.0069(15) 0.0067(14) C44 0.047(2) 0.047(2) 0.0274(19) 0.0041(16) 0.0022(15) 0.0051(17) C45 0.049(2) 0.038(2) 0.034(2) -0.0052(16) -0.0070(16) -0.0015(16) C46 0.0350(19) 0.0225(16) 0.0370(19) -0.0003(14) -0.0001(14) -0.0021(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.958(2) . ? Fe1 N1 1.960(2) . ? Fe1 N4 1.961(2) . ? Fe1 N3 1.968(2) . ? Fe1 N10 1.989(2) . ? Fe1 N9 2.009(2) . ? Cl1 C38 1.712(4) . ? Cl1 H38A 0.7482 . ? Cl1A C40 1.756(5) . ? Cl1A H40A 0.8494 . ? Cl2 C43 1.726(3) . ? O1 N5 1.219(3) . ? O2 N5 1.228(3) . ? O3 N6 1.206(4) . ? O4 N6 1.224(3) . ? O5 N7 1.222(4) . ? O6 N7 1.230(4) . ? O7 N8 1.228(4) . ? O8 N8 1.219(3) . ? N1 C4 1.376(4) . ? N1 C1 1.381(4) . ? N2 C9 1.377(4) . ? N2 C6 1.380(4) . ? N3 C14 1.373(4) . ? N3 C11 1.384(4) . ? N4 C19 1.369(4) . ? N4 C16 1.386(4) . ? N5 C5 1.476(4) . ? N6 C10 1.484(4) . ? N7 C15 1.488(4) . ? N8 C20 1.480(4) . ? N9 C41 1.335(4) . ? N9 C37 1.346(4) . ? N10 C42 1.348(4) . ? N10 C46 1.349(4) . ? C1 C20 1.391(4) . ? C1 C2 1.455(4) . ? C2 C3 1.365(4) . ? C2 C21 1.500(4) . ? C3 C4 1.452(4) . ? C3 C23 1.507(4) . ? C4 C5 1.400(4) . ? C5 C6 1.389(4) . ? C6 C7 1.458(4) . ? C7 C8 1.355(5) . ? C7 C25 1.507(4) . ? C8 C9 1.450(4) . ? C8 C27 1.526(5) . ? C9 C10 1.399(4) . ? C10 C11 1.380(4) . ? C11 C12 1.453(4) . ? C12 C13 1.356(4) . ? C12 C29 1.506(4) . ? C13 C14 1.455(4) . ? C13 C31 1.519(4) . ? C14 C15 1.393(4) . ? C15 C16 1.381(4) . ? C16 C17 1.456(4) . ? C17 C18 1.358(4) . ? C17 C33 1.499(4) . ? C18 C19 1.460(4) . ? C18 C35 1.504(4) . ? C19 C20 1.398(4) . ? C21 C22 1.520(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.531(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.524(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.527(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.514(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.533(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.525(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.537(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.378(4) . ? C37 H37A 0.9500 . ? C38 C39 1.379(5) . ? C38 H38A 0.9656 . ? C39 C40 1.373(5) . ? C39 H39A 0.9500 . ? C40 C41 1.378(5) . ? C40 H40A 0.9697 . ? C41 H41A 0.9500 . ? C42 C43 1.375(4) . ? C42 H42A 0.9500 . ? C43 C44 1.368(5) . ? C44 C45 1.375(5) . ? C44 H44A 0.9500 . ? C45 C46 1.370(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 90.38(10) . . ? N2 Fe1 N4 175.08(10) . . ? N1 Fe1 N4 90.38(10) . . ? N2 Fe1 N3 89.82(10) . . ? N1 Fe1 N3 175.27(10) . . ? N4 Fe1 N3 89.82(10) . . ? N2 Fe1 N10 92.50(10) . . ? N1 Fe1 N10 87.75(10) . . ? N4 Fe1 N10 92.39(10) . . ? N3 Fe1 N10 87.52(10) . . ? N2 Fe1 N9 87.68(10) . . ? N1 Fe1 N9 91.74(10) . . ? N4 Fe1 N9 87.44(10) . . ? N3 Fe1 N9 92.99(10) . . ? N10 Fe1 N9 179.46(10) . . ? C38 Cl1 H38A 3.3 . . ? C40 Cl1A H40A 16.1 . . ? C4 N1 C1 105.1(2) . . ? C4 N1 Fe1 127.8(2) . . ? C1 N1 Fe1 125.09(19) . . ? C9 N2 C6 105.1(2) . . ? C9 N2 Fe1 127.4(2) . . ? C6 N2 Fe1 125.3(2) . . ? C14 N3 C11 105.3(2) . . ? C14 N3 Fe1 127.8(2) . . ? C11 N3 Fe1 124.70(19) . . ? C19 N4 C16 105.3(2) . . ? C19 N4 Fe1 127.37(19) . . ? C16 N4 Fe1 124.8(2) . . ? O1 N5 O2 124.5(3) . . ? O1 N5 C5 118.3(3) . . ? O2 N5 C5 117.2(3) . . ? O3 N6 O4 124.7(3) . . ? O3 N6 C10 117.3(3) . . ? O4 N6 C10 118.0(3) . . ? O5 N7 O6 125.3(3) . . ? O5 N7 C15 116.9(3) . . ? O6 N7 C15 117.8(3) . . ? O8 N8 O7 124.8(3) . . ? O8 N8 C20 117.4(3) . . ? O7 N8 C20 117.7(3) . . ? C41 N9 C37 116.9(3) . . ? C41 N9 Fe1 122.5(2) . . ? C37 N9 Fe1 120.6(2) . . ? C42 N10 C46 117.0(3) . . ? C42 N10 Fe1 120.5(2) . . ? C46 N10 Fe1 122.5(2) . . ? N1 C1 C20 119.7(3) . . ? N1 C1 C2 110.6(3) . . ? C20 C1 C2 128.9(3) . . ? C3 C2 C1 106.3(3) . . ? C3 C2 C21 125.8(3) . . ? C1 C2 C21 127.6(3) . . ? C2 C3 C4 106.5(3) . . ? C2 C3 C23 124.4(3) . . ? C4 C3 C23 129.0(3) . . ? N1 C4 C5 119.7(3) . . ? N1 C4 C3 111.0(3) . . ? C5 C4 C3 129.1(3) . . ? C6 C5 C4 128.6(3) . . ? C6 C5 N5 115.3(3) . . ? C4 C5 N5 115.7(3) . . ? N2 C6 C5 119.7(3) . . ? N2 C6 C7 110.3(3) . . ? C5 C6 C7 129.5(3) . . ? C8 C7 C6 106.5(3) . . ? C8 C7 C25 125.5(3) . . ? C6 C7 C25 127.7(3) . . ? C7 C8 C9 106.8(3) . . ? C7 C8 C27 124.8(3) . . ? C9 C8 C27 128.1(3) . . ? N2 C9 C10 119.7(3) . . ? N2 C9 C8 110.7(3) . . ? C10 C9 C8 129.5(3) . . ? C11 C10 C9 128.0(3) . . ? C11 C10 N6 116.3(3) . . ? C9 C10 N6 115.6(3) . . ? C10 C11 N3 119.4(3) . . ? C10 C11 C12 129.2(3) . . ? N3 C11 C12 110.4(3) . . ? C13 C12 C11 106.3(3) . . ? C13 C12 C29 124.5(3) . . ? C11 C12 C29 128.8(3) . . ? C12 C13 C14 106.9(3) . . ? C12 C13 C31 124.4(3) . . ? C14 C13 C31 128.7(3) . . ? N3 C14 C15 120.0(3) . . ? N3 C14 C13 110.5(3) . . ? C15 C14 C13 129.3(3) . . ? C16 C15 C14 128.2(3) . . ? C16 C15 N7 115.5(3) . . ? C14 C15 N7 115.8(3) . . ? C15 C16 N4 120.1(3) . . ? C15 C16 C17 129.0(3) . . ? N4 C16 C17 110.3(3) . . ? C18 C17 C16 106.5(3) . . ? C18 C17 C33 125.4(3) . . ? C16 C17 C33 127.3(3) . . ? C17 C18 C19 106.6(3) . . ? C17 C18 C35 124.1(3) . . ? C19 C18 C35 128.9(3) . . ? N4 C19 C20 119.9(3) . . ? N4 C19 C18 110.8(3) . . ? C20 C19 C18 129.2(3) . . ? C1 C20 C19 128.0(3) . . ? C1 C20 N8 116.6(3) . . ? C19 C20 N8 114.9(3) . . ? C2 C21 C22 111.9(3) . . ? C2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? 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 . . ? C3 C23 C24 113.0(3) . . ? C3 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C3 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 111.9(3) . . ? C7 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? C7 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 113.2(3) . . ? C8 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C8 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.8 . . ? 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 . . ? C12 C29 C30 112.1(3) . . ? C12 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C12 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 110.5(3) . . ? C13 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? C13 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C34 110.7(3) . . ? C17 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C17 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 113.6(3) . . ? C18 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C18 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 C38 122.8(3) . . ? N9 C37 H37A 118.6 . . ? C38 C37 H37A 118.6 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 Cl1 117.5(3) . . ? C39 C38 Cl1 122.5(3) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? Cl1 C38 H38A 2.5 . . ? C40 C39 C38 117.0(3) . . ? C40 C39 H39A 121.5 . . ? C38 C39 H39A 121.5 . . ? C39 C40 C41 120.4(4) . . ? C39 C40 Cl1A 122.8(3) . . ? C41 C40 Cl1A 115.0(3) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? Cl1A C40 H40A 14.1 . . ? N9 C41 C40 122.8(3) . . ? N9 C41 H41A 118.6 . . ? C40 C41 H41A 118.6 . . ? N10 C42 C43 122.2(3) . . ? N10 C42 H42A 118.9 . . ? C43 C42 H42A 118.9 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 Cl2 121.1(3) . . ? C42 C43 Cl2 118.3(3) . . ? C43 C44 C45 117.2(3) . . ? C43 C44 H44A 121.4 . . ? C45 C44 H44A 121.4 . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? N10 C46 C45 122.5(3) . . ? N10 C46 H46A 118.8 . . ? C45 C46 H46A 118.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.577 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.076