# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Andreas A. Danopoulos' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ United Kingdom ; _publ_contact_author_email ad1@soton.ac.uk _publ_contact_author_phone '+44 (0)2380 594116' loop_ _publ_author_name _publ_author_address 'Danopoulos, Andreas A.' ;Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ United Kingdom ; 'Wright, Joseph A.' ;Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ United Kingdom ; 'Motherwell, Willam B.' ;Department of Chemistry University College London Christopher Ingold Laboratories 20 Gordon Street London WC1H 0AJ United Kingdom ; _publ_section_title ; Molecular N2 complexes of iron stabilised by N-heterocyclic 'pincer' dicarbene ligands ; _publ_requested_category FM data_1 _database_code_depnum_ccdc_archive 'CCDC 252527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Fe N9, C5 H12' _chemical_formula_sum 'C40 H53 Fe N9' _chemical_formula_weight 715.76 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7070(17) _cell_length_b 15.226(3) _cell_length_c 15.788(5) _cell_angle_alpha 73.78(2) _cell_angle_beta 79.44(2) _cell_angle_gamma 76.978(16) _cell_volume 1941.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8713 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7412 _exptl_absorpt_correction_T_max 0.9957 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34076 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.66 _reflns_number_total 8972 _reflns_number_gt 6153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SIR-92 (Altamore, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 2004) ; _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^)+(0.0377P)^2^+1.8532P] 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 8972 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.8124(3) 0.05730(17) 0.33350(18) 0.0209(6) Uani 1 1 d . . . C2 C 0.9230(3) 0.15496(17) 0.20365(16) 0.0170(5) Uani 1 1 d . . . C3 C 0.8342(3) 0.10783(18) 0.09907(18) 0.0227(6) Uani 1 1 d . . . H3 H 0.8156 0.1050 0.0425 0.027 Uiso 1 1 calc R . . C4 C 0.7823(3) 0.05537(18) 0.17780(18) 0.0242(6) Uani 1 1 d . . . H4 H 0.7201 0.0087 0.1879 0.029 Uiso 1 1 calc R . . C5 C 0.9849(3) 0.23920(17) 0.04643(16) 0.0172(5) Uani 1 1 d . . . C6 C 1.1468(3) 0.22336(18) 0.01533(16) 0.0197(5) Uani 1 1 d . . . C7 C 1.2059(3) 0.29407(19) -0.05003(18) 0.0268(6) Uani 1 1 d . . . H7 H 1.3156 0.2853 -0.0726 0.032 Uiso 1 1 calc R . . C8 C 1.1072(3) 0.3773(2) -0.08281(18) 0.0300(7) Uani 1 1 d . . . H8 H 1.1496 0.4248 -0.1278 0.036 Uiso 1 1 calc R . . C9 C 0.9475(3) 0.39157(19) -0.05042(18) 0.0269(6) Uani 1 1 d . . . H9 H 0.8811 0.4492 -0.0730 0.032 Uiso 1 1 calc R . . C10 C 0.8829(3) 0.32241(18) 0.01497(17) 0.0215(6) Uani 1 1 d . . . C11 C 0.7074(3) 0.34027(18) 0.05021(18) 0.0249(6) Uani 1 1 d . . . H11 H 0.6852 0.2849 0.0991 0.030 Uiso 1 1 calc R . . C12 C 0.6062(3) 0.3506(2) -0.0224(2) 0.0394(8) Uani 1 1 d . . . H12A H 0.6225 0.4061 -0.0701 0.059 Uiso 1 1 calc R . . H12B H 0.4938 0.3570 0.0027 0.059 Uiso 1 1 calc R . . H12C H 0.6372 0.2955 -0.0464 0.059 Uiso 1 1 calc R . . C13 C 0.6632(4) 0.4251(2) 0.0890(2) 0.0407(8) Uani 1 1 d . . . H13A H 0.7284 0.4163 0.1362 0.061 Uiso 1 1 calc R . . H13B H 0.5506 0.4329 0.1137 0.061 Uiso 1 1 calc R . . H13C H 0.6821 0.4806 0.0420 0.061 Uiso 1 1 calc R . . C14 C 1.2524(3) 0.13054(18) 0.04922(18) 0.0238(6) Uani 1 1 d . . . H14 H 1.2028 0.1015 0.1100 0.029 Uiso 1 1 calc R . . C15 C 1.2583(4) 0.0660(2) -0.0106(2) 0.0360(7) Uani 1 1 d . . . H15A H 1.1503 0.0580 -0.0120 0.054 Uiso 1 1 calc R . . H15B H 1.3233 0.0054 0.0128 0.054 Uiso 1 1 calc R . . H15C H 1.3052 0.0934 -0.0710 0.054 Uiso 1 1 calc R . . C16 C 1.4201(3) 0.1398(2) 0.0569(2) 0.0338(7) Uani 1 1 d . . . H16A H 1.4778 0.1582 -0.0028 0.051 Uiso 1 1 calc R . . H16B H 1.4762 0.0800 0.0892 0.051 Uiso 1 1 calc R . . H16C H 1.4139 0.1872 0.0891 0.051 Uiso 1 1 calc R . . C17 C 0.7285(3) -0.00808(18) 0.38862(19) 0.0269(6) Uani 1 1 d . . . H17 H 0.6813 -0.0450 0.3649 0.032 Uiso 1 1 calc R . . C18 C 0.7144(3) -0.01870(19) 0.48030(19) 0.0285(7) Uani 1 1 d . . . H18 H 0.6592 -0.0643 0.5199 0.034 Uiso 1 1 calc R . . C19 C 0.7812(3) 0.03729(18) 0.51360(18) 0.0253(6) Uani 1 1 d . . . H19 H 0.7716 0.0312 0.5758 0.030 Uiso 1 1 calc R . . C20 C 0.8615(3) 0.10171(17) 0.45426(17) 0.0204(6) Uani 1 1 d . . . C21 C 0.9961(3) 0.22761(17) 0.39721(17) 0.0193(5) Uani 1 1 d . . . C22 C 0.9996(3) 0.2670(2) 0.52637(17) 0.0274(6) Uani 1 1 d . . . H22 H 1.0175 0.2998 0.5657 0.033 Uiso 1 1 calc R . . C23 C 0.9314(3) 0.19160(19) 0.54963(18) 0.0267(6) Uani 1 1 d . . . H23 H 0.8927 0.1606 0.6081 0.032 Uiso 1 1 calc R . . C24 C 1.0954(3) 0.37194(18) 0.38264(16) 0.0197(5) Uani 1 1 d . . . C25 C 1.2562(3) 0.36602(18) 0.34831(17) 0.0209(6) Uani 1 1 d . . . C26 C 1.3051(3) 0.44801(19) 0.29694(18) 0.0242(6) Uani 1 1 d . . . H26 H 1.4136 0.4467 0.2728 0.029 Uiso 1 1 calc R . . C27 C 1.1983(3) 0.53107(19) 0.28068(18) 0.0276(6) Uani 1 1 d . . . H27 H 1.2341 0.5862 0.2457 0.033 Uiso 1 1 calc R . . C28 C 1.0394(3) 0.53473(19) 0.31487(18) 0.0247(6) Uani 1 1 d . . . H28 H 0.9673 0.5924 0.3030 0.030 Uiso 1 1 calc R . . C29 C 0.9839(3) 0.45487(18) 0.36658(17) 0.0212(6) Uani 1 1 d . . . C30 C 0.8084(3) 0.45960(19) 0.40188(18) 0.0252(6) Uani 1 1 d . . . H30 H 0.7924 0.3956 0.4361 0.030 Uiso 1 1 calc R . . C31 C 0.7069(3) 0.4910(3) 0.3261(2) 0.0422(8) Uani 1 1 d . . . H31A H 0.7192 0.5541 0.2922 0.063 Uiso 1 1 calc R . . H31B H 0.5951 0.4905 0.3505 0.063 Uiso 1 1 calc R . . H31C H 0.7412 0.4485 0.2869 0.063 Uiso 1 1 calc R . . C32 C 0.7544(3) 0.5237(3) 0.4647(2) 0.0440(9) Uani 1 1 d . . . H32A H 0.7683 0.5870 0.4324 0.066 Uiso 1 1 calc R . . H32B H 0.8182 0.5016 0.5142 0.066 Uiso 1 1 calc R . . H32C H 0.6421 0.5237 0.4879 0.066 Uiso 1 1 calc R . . C33 C 1.3726(3) 0.27471(19) 0.36655(18) 0.0253(6) Uani 1 1 d . . . H33 H 1.3102 0.2237 0.3798 0.030 Uiso 1 1 calc R . . C34 C 1.4971(3) 0.2632(2) 0.2865(2) 0.0383(8) Uani 1 1 d . . . H34A H 1.4446 0.2800 0.2328 0.057 Uiso 1 1 calc R . . H34B H 1.5528 0.1984 0.2964 0.057 Uiso 1 1 calc R . . H34C H 1.5737 0.3040 0.2789 0.057 Uiso 1 1 calc R . . C35 C 1.4522(4) 0.2626(2) 0.4486(2) 0.0461(9) Uani 1 1 d . . . H35A H 1.5135 0.3121 0.4381 0.069 Uiso 1 1 calc R . . H35B H 1.5235 0.2019 0.4603 0.069 Uiso 1 1 calc R . . H35C H 1.3707 0.2659 0.5000 0.069 Uiso 1 1 calc R . . C36 C 0.3229(6) 0.7959(3) 0.2338(3) 0.0837(16) Uani 1 1 d . . . H36A H 0.2889 0.7558 0.2923 0.100 Uiso 1 1 calc R . . H36B H 0.3803 0.7547 0.1950 0.100 Uiso 1 1 calc R . . C37 C 0.1641(7) 0.8592(3) 0.1901(3) 0.0987(19) Uani 1 1 d . . . H37A H 0.1213 0.9107 0.2195 0.118 Uiso 1 1 calc R . . H37B H 0.1948 0.8870 0.1262 0.118 Uiso 1 1 calc R . . C38 C 0.0372(5) 0.8048(3) 0.1988(3) 0.0782(13) Uani 1 1 d . . . H38A H 0.0755 0.7573 0.1651 0.117 Uiso 1 1 calc R . . H38B H -0.0571 0.8467 0.1754 0.117 Uiso 1 1 calc R . . H38C H 0.0096 0.7748 0.2617 0.117 Uiso 1 1 calc R . . C39 C 0.4296(9) 0.8489(4) 0.2455(4) 0.130(3) Uani 1 1 d . . . H39A H 0.3745 0.8878 0.2868 0.155 Uiso 1 1 calc R . . H39B H 0.4606 0.8911 0.1876 0.155 Uiso 1 1 calc R . . C40 C 0.5769(7) 0.7883(4) 0.2817(4) 0.0996(18) Uani 1 1 d . . . H40A H 0.5469 0.7465 0.3391 0.149 Uiso 1 1 calc R . . H40B H 0.6456 0.8275 0.2897 0.149 Uiso 1 1 calc R . . H40C H 0.6341 0.7514 0.2399 0.149 Uiso 1 1 calc R . . Fe1 Fe 1.00642(4) 0.19621(3) 0.28692(2) 0.01723(11) Uani 1 1 d . . . N1 N 1.2127(3) 0.13114(15) 0.27742(14) 0.0214(5) Uani 1 1 d . . . N2 N 1.3332(3) 0.08651(17) 0.27585(15) 0.0291(5) Uani 1 1 d . . . N3 N 1.0391(3) 0.30818(15) 0.21413(14) 0.0219(5) Uani 1 1 d . . . N4 N 1.0608(3) 0.37637(17) 0.16973(16) 0.0345(6) Uani 1 1 d . . . N5 N 0.8828(2) 0.11178(14) 0.36454(14) 0.0179(5) Uani 1 1 d . . . N6 N 0.8373(2) 0.08271(14) 0.24197(14) 0.0191(5) Uani 1 1 d . . . N7 N 0.9203(2) 0.16714(14) 0.11458(13) 0.0172(4) Uani 1 1 d . . . N8 N 0.9286(2) 0.16798(15) 0.47164(14) 0.0202(5) Uani 1 1 d . . . N9 N 1.0395(2) 0.28864(15) 0.43460(14) 0.0207(5) 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 C1 0.0171(13) 0.0168(13) 0.0267(15) -0.0025(11) -0.0026(11) -0.0026(10) C2 0.0141(12) 0.0146(12) 0.0198(13) -0.0030(10) -0.0022(10) 0.0006(10) C3 0.0248(14) 0.0209(14) 0.0266(15) -0.0088(12) -0.0077(11) -0.0056(11) C4 0.0242(14) 0.0200(14) 0.0326(16) -0.0069(12) -0.0096(12) -0.0072(11) C5 0.0230(13) 0.0161(13) 0.0147(13) -0.0049(10) -0.0033(10) -0.0057(10) C6 0.0217(13) 0.0239(14) 0.0157(13) -0.0076(11) -0.0032(10) -0.0044(11) C7 0.0245(14) 0.0348(17) 0.0237(15) -0.0104(13) 0.0012(11) -0.0102(13) C8 0.0386(17) 0.0304(16) 0.0221(15) -0.0011(12) -0.0025(13) -0.0165(14) C9 0.0324(15) 0.0212(15) 0.0255(15) -0.0012(12) -0.0078(12) -0.0041(12) C10 0.0259(14) 0.0211(14) 0.0194(14) -0.0064(11) -0.0043(11) -0.0056(11) C11 0.0236(14) 0.0184(14) 0.0279(15) -0.0019(12) -0.0040(11) 0.0012(11) C12 0.0271(16) 0.043(2) 0.047(2) -0.0082(16) -0.0095(14) -0.0035(14) C13 0.0376(18) 0.0354(18) 0.047(2) -0.0173(16) 0.0014(15) -0.0003(14) C14 0.0238(14) 0.0242(15) 0.0227(15) -0.0075(12) -0.0026(11) -0.0013(11) C15 0.0395(17) 0.0306(17) 0.0380(18) -0.0141(14) -0.0042(14) -0.0002(14) C16 0.0222(15) 0.0401(18) 0.0363(18) -0.0089(14) -0.0042(13) -0.0005(13) C17 0.0235(14) 0.0211(14) 0.0349(17) -0.0024(12) -0.0028(12) -0.0082(11) C18 0.0231(14) 0.0225(15) 0.0315(16) 0.0042(12) 0.0029(12) -0.0064(12) C19 0.0220(14) 0.0245(15) 0.0230(15) 0.0023(12) 0.0008(11) -0.0046(11) C20 0.0171(13) 0.0201(14) 0.0197(14) -0.0007(11) -0.0007(10) -0.0017(10) C21 0.0162(12) 0.0211(14) 0.0185(13) -0.0027(11) -0.0013(10) -0.0029(10) C22 0.0342(16) 0.0332(16) 0.0157(14) -0.0087(12) -0.0003(11) -0.0070(13) C23 0.0320(15) 0.0316(16) 0.0143(13) -0.0041(12) 0.0011(11) -0.0065(13) C24 0.0240(14) 0.0217(14) 0.0161(13) -0.0071(11) -0.0018(10) -0.0073(11) C25 0.0217(13) 0.0238(14) 0.0203(14) -0.0086(11) -0.0054(11) -0.0041(11) C26 0.0206(13) 0.0307(16) 0.0260(15) -0.0125(12) -0.0013(11) -0.0085(12) C27 0.0314(15) 0.0264(16) 0.0275(16) -0.0060(12) -0.0029(12) -0.0118(13) C28 0.0267(14) 0.0215(14) 0.0271(15) -0.0074(12) -0.0081(12) -0.0014(11) C29 0.0226(13) 0.0265(15) 0.0185(14) -0.0111(11) -0.0033(11) -0.0051(11) C30 0.0212(14) 0.0261(15) 0.0276(15) -0.0082(12) -0.0011(11) -0.0028(11) C31 0.0276(16) 0.069(2) 0.0375(19) -0.0228(17) -0.0048(14) -0.0119(16) C32 0.0252(16) 0.070(2) 0.047(2) -0.0381(19) 0.0018(14) -0.0052(16) C33 0.0224(14) 0.0241(15) 0.0300(16) -0.0085(12) -0.0024(11) -0.0040(11) C34 0.0297(16) 0.0330(18) 0.048(2) -0.0144(15) 0.0062(14) -0.0008(13) C35 0.045(2) 0.041(2) 0.055(2) -0.0157(17) -0.0261(17) 0.0083(16) C36 0.139(4) 0.056(3) 0.049(3) -0.028(2) 0.041(3) -0.029(3) C37 0.130(5) 0.038(3) 0.080(4) 0.010(2) 0.020(3) 0.023(3) C38 0.081(3) 0.058(3) 0.084(3) -0.001(2) -0.020(3) -0.003(3) C39 0.193(7) 0.080(4) 0.111(5) -0.053(4) 0.085(5) -0.063(5) C40 0.134(5) 0.099(4) 0.083(4) -0.034(3) -0.028(4) -0.031(4) Fe1 0.01851(19) 0.0172(2) 0.01565(19) -0.00270(15) -0.00073(14) -0.00551(14) N1 0.0250(12) 0.0221(12) 0.0179(12) -0.0047(9) -0.0009(9) -0.0077(10) N2 0.0264(13) 0.0303(14) 0.0287(14) -0.0076(11) -0.0030(10) -0.0013(11) N3 0.0298(12) 0.0216(12) 0.0178(12) -0.0078(10) -0.0038(10) -0.0077(10) N4 0.0577(17) 0.0243(14) 0.0248(14) -0.0005(11) -0.0105(12) -0.0171(12) N5 0.0167(10) 0.0160(11) 0.0198(11) -0.0033(9) -0.0005(8) -0.0033(9) N6 0.0189(11) 0.0167(11) 0.0223(12) -0.0035(9) -0.0027(9) -0.0058(9) N7 0.0201(11) 0.0157(11) 0.0185(11) -0.0065(9) -0.0046(9) -0.0041(9) N8 0.0198(11) 0.0225(12) 0.0162(11) -0.0024(9) 0.0001(9) -0.0046(9) N9 0.0227(11) 0.0212(12) 0.0177(11) -0.0042(9) 0.0002(9) -0.0061(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N5 1.367(3) . ? C1 C17 1.376(3) . ? C1 N6 1.377(3) . ? C2 N7 1.370(3) . ? C2 N6 1.402(3) . ? C2 Fe1 1.915(3) . ? C3 C4 1.338(4) . ? C3 N7 1.390(3) . ? C3 H3 0.9500 . ? C4 N6 1.390(3) . ? C4 H4 0.9500 . ? C5 C10 1.394(4) . ? C5 C6 1.395(3) . ? C5 N7 1.440(3) . ? C6 C7 1.387(4) . ? C6 C14 1.517(4) . ? C7 C8 1.385(4) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C8 H8 0.9500 . ? C9 C10 1.392(4) . ? C9 H9 0.9500 . ? C10 C11 1.518(4) . ? C11 C12 1.523(4) . ? C11 C13 1.524(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.528(4) . ? C14 C15 1.529(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.396(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 C20 1.373(3) . ? C19 H19 0.9500 . ? C20 N5 1.364(3) . ? C20 N8 1.383(3) . ? C21 N9 1.379(3) . ? C21 N8 1.394(3) . ? C21 Fe1 1.912(3) . ? C22 C23 1.340(4) . ? C22 N9 1.389(3) . ? C22 H22 0.9500 . ? C23 N8 1.382(3) . ? C23 H23 0.9500 . ? C24 C25 1.398(3) . ? C24 C29 1.400(4) . ? C24 N9 1.438(3) . ? C25 C26 1.394(4) . ? C25 C33 1.513(4) . ? C26 C27 1.381(4) . ? C26 H26 0.9500 . ? C27 C28 1.385(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(4) . ? C28 H28 0.9500 . ? C29 C30 1.521(3) . ? C30 C31 1.522(4) . ? C30 C32 1.523(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.526(4) . ? C33 C34 1.529(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C39 1.426(7) . ? C36 C37 1.641(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.489(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.505(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? Fe1 N3 1.820(2) . ? Fe1 N1 1.847(2) . ? Fe1 N5 1.890(2) . ? N1 N2 1.115(3) . ? N3 N4 1.113(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 C1 C17 123.0(2) . . ? N5 C1 N6 108.1(2) . . ? C17 C1 N6 128.9(2) . . ? N7 C2 N6 102.3(2) . . ? N7 C2 Fe1 142.92(18) . . ? N6 C2 Fe1 114.66(17) . . ? C4 C3 N7 108.0(2) . . ? C4 C3 H3 126.0 . . ? N7 C3 H3 126.0 . . ? C3 C4 N6 106.4(2) . . ? C3 C4 H4 126.8 . . ? N6 C4 H4 126.8 . . ? C10 C5 C6 122.7(2) . . ? C10 C5 N7 118.5(2) . . ? C6 C5 N7 118.8(2) . . ? C7 C6 C5 117.6(2) . . ? C7 C6 C14 121.4(2) . . ? C5 C6 C14 121.0(2) . . ? C8 C7 C6 121.0(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.7(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 117.7(2) . . ? C9 C10 C11 119.6(2) . . ? C5 C10 C11 122.7(2) . . ? C10 C11 C12 110.5(2) . . ? C10 C11 C13 111.5(2) . . ? C12 C11 C13 111.0(2) . . ? C10 C11 H11 107.9 . . ? C12 C11 H11 107.9 . . ? C13 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C16 113.1(2) . . ? C6 C14 C15 109.7(2) . . ? C16 C14 C15 110.6(2) . . ? C6 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? C15 C14 H14 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 C18 118.2(3) . . ? C1 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C19 C18 C17 120.1(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 118.2(3) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? N5 C20 C19 123.4(2) . . ? N5 C20 N8 108.3(2) . . ? C19 C20 N8 128.2(2) . . ? N9 C21 N8 102.0(2) . . ? N9 C21 Fe1 142.84(19) . . ? N8 C21 Fe1 115.05(18) . . ? C23 C22 N9 107.9(2) . . ? C23 C22 H22 126.1 . . ? N9 C22 H22 126.1 . . ? C22 C23 N8 106.3(2) . . ? C22 C23 H23 126.8 . . ? N8 C23 H23 126.8 . . ? C25 C24 C29 123.2(2) . . ? C25 C24 N9 118.9(2) . . ? C29 C24 N9 117.9(2) . . ? C26 C25 C24 117.1(2) . . ? C26 C25 C33 121.4(2) . . ? C24 C25 C33 121.5(2) . . ? C27 C26 C25 121.1(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.6(3) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 120.8(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C24 117.2(2) . . ? C28 C29 C30 120.2(2) . . ? C24 C29 C30 122.6(2) . . ? C29 C30 C31 111.1(2) . . ? C29 C30 C32 111.4(2) . . ? C31 C30 C32 110.2(2) . . ? C29 C30 H30 108.0 . . ? C31 C30 H30 108.0 . . ? C32 C30 H30 108.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 C35 111.1(2) . . ? C25 C33 C34 112.8(2) . . ? C35 C33 C34 110.7(2) . . ? C25 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? C34 C33 H33 107.3 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C37 114.1(5) . . ? C39 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? C39 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C36 113.0(3) . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 C40 112.3(5) . . ? C36 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? C36 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 Fe1 N1 98.88(10) . . ? N3 Fe1 N5 154.90(9) . . ? N1 Fe1 N5 106.22(9) . . ? N3 Fe1 C21 97.10(10) . . ? N1 Fe1 C21 99.93(10) . . ? N5 Fe1 C21 78.82(10) . . ? N3 Fe1 C2 97.02(10) . . ? N1 Fe1 C2 99.77(10) . . ? N5 Fe1 C2 78.94(10) . . ? C21 Fe1 C2 153.61(10) . . ? N2 N1 Fe1 175.0(2) . . ? N4 N3 Fe1 179.2(2) . . ? C20 N5 C1 117.0(2) . . ? C20 N5 Fe1 121.34(17) . . ? C1 N5 Fe1 121.61(17) . . ? C1 N6 C4 132.1(2) . . ? C1 N6 C2 116.1(2) . . ? C4 N6 C2 111.6(2) . . ? C2 N7 C3 111.7(2) . . ? C2 N7 C5 123.7(2) . . ? C3 N7 C5 124.3(2) . . ? C23 N8 C20 131.9(2) . . ? C23 N8 C21 112.3(2) . . ? C20 N8 C21 115.6(2) . . ? C21 N9 C22 111.5(2) . . ? C21 N9 C24 123.0(2) . . ? C22 N9 C24 124.8(2) . . ? 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 N7 C3 C4 N6 -0.1(3) . . . . ? C10 C5 C6 C7 -0.5(4) . . . . ? N7 C5 C6 C7 -179.7(2) . . . . ? C10 C5 C6 C14 -177.9(2) . . . . ? N7 C5 C6 C14 2.8(3) . . . . ? C5 C6 C7 C8 0.2(4) . . . . ? C14 C6 C7 C8 177.6(2) . . . . ? C6 C7 C8 C9 0.4(4) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C5 0.3(4) . . . . ? C8 C9 C10 C11 179.3(2) . . . . ? C6 C5 C10 C9 0.2(4) . . . . ? N7 C5 C10 C9 179.5(2) . . . . ? C6 C5 C10 C11 -178.7(2) . . . . ? N7 C5 C10 C11 0.6(4) . . . . ? C9 C10 C11 C12 66.1(3) . . . . ? C5 C10 C11 C12 -114.9(3) . . . . ? C9 C10 C11 C13 -57.9(3) . . . . ? C5 C10 C11 C13 121.1(3) . . . . ? C7 C6 C14 C16 37.9(3) . . . . ? C5 C6 C14 C16 -144.8(2) . . . . ? C7 C6 C14 C15 -86.1(3) . . . . ? C5 C6 C14 C15 91.3(3) . . . . ? N5 C1 C17 C18 0.2(4) . . . . ? N6 C1 C17 C18 -177.3(2) . . . . ? C1 C17 C18 C19 1.4(4) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? C18 C19 C20 N5 -1.8(4) . . . . ? C18 C19 C20 N8 175.7(2) . . . . ? N9 C22 C23 N8 -0.6(3) . . . . ? C29 C24 C25 C26 1.0(4) . . . . ? N9 C24 C25 C26 178.9(2) . . . . ? C29 C24 C25 C33 -179.4(2) . . . . ? N9 C24 C25 C33 -1.5(4) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C33 C25 C26 C27 -179.9(2) . . . . ? C25 C26 C27 C28 -0.3(4) . . . . ? C26 C27 C28 C29 0.2(4) . . . . ? C27 C28 C29 C24 0.5(4) . . . . ? C27 C28 C29 C30 -178.6(2) . . . . ? C25 C24 C29 C28 -1.1(4) . . . . ? N9 C24 C29 C28 -179.0(2) . . . . ? C25 C24 C29 C30 178.0(2) . . . . ? N9 C24 C29 C30 0.1(4) . . . . ? C28 C29 C30 C31 60.7(3) . . . . ? C24 C29 C30 C31 -118.3(3) . . . . ? C28 C29 C30 C32 -62.5(3) . . . . ? C24 C29 C30 C32 118.5(3) . . . . ? C26 C25 C33 C35 87.2(3) . . . . ? C24 C25 C33 C35 -92.4(3) . . . . ? C26 C25 C33 C34 -37.8(3) . . . . ? C24 C25 C33 C34 142.6(3) . . . . ? C39 C36 C37 C38 -165.9(4) . . . . ? C37 C36 C39 C40 -177.3(4) . . . . ? N9 C21 Fe1 N3 -21.5(3) . . . . ? N8 C21 Fe1 N3 163.02(18) . . . . ? N9 C21 Fe1 N1 78.8(3) . . . . ? N8 C21 Fe1 N1 -96.62(18) . . . . ? N9 C21 Fe1 N5 -176.4(3) . . . . ? N8 C21 Fe1 N5 8.12(17) . . . . ? N9 C21 Fe1 C2 -143.4(3) . . . . ? N8 C21 Fe1 C2 41.1(3) . . . . ? N7 C2 Fe1 N3 22.9(3) . . . . ? N6 C2 Fe1 N3 -161.32(17) . . . . ? N7 C2 Fe1 N1 -77.4(3) . . . . ? N6 C2 Fe1 N1 98.37(18) . . . . ? N7 C2 Fe1 N5 177.8(3) . . . . ? N6 C2 Fe1 N5 -6.42(16) . . . . ? N7 C2 Fe1 C21 144.8(3) . . . . ? N6 C2 Fe1 C21 -39.4(3) . . . . ? C19 C20 N5 C1 3.4(4) . . . . ? N8 C20 N5 C1 -174.6(2) . . . . ? C19 C20 N5 Fe1 -175.81(19) . . . . ? N8 C20 N5 Fe1 6.2(3) . . . . ? C17 C1 N5 C20 -2.5(4) . . . . ? N6 C1 N5 C20 175.4(2) . . . . ? C17 C1 N5 Fe1 176.65(19) . . . . ? N6 C1 N5 Fe1 -5.4(3) . . . . ? N3 Fe1 N5 C20 -91.1(3) . . . . ? N1 Fe1 N5 C20 88.9(2) . . . . ? C21 Fe1 N5 C20 -8.27(19) . . . . ? C2 Fe1 N5 C20 -174.0(2) . . . . ? N3 Fe1 N5 C1 89.7(3) . . . . ? N1 Fe1 N5 C1 -90.2(2) . . . . ? C21 Fe1 N5 C1 172.6(2) . . . . ? C2 Fe1 N5 C1 6.86(19) . . . . ? N5 C1 N6 C4 -174.4(2) . . . . ? C17 C1 N6 C4 3.4(5) . . . . ? N5 C1 N6 C2 -0.5(3) . . . . ? C17 C1 N6 C2 177.3(2) . . . . ? C3 C4 N6 C1 175.3(3) . . . . ? C3 C4 N6 C2 1.2(3) . . . . ? N7 C2 N6 C1 -176.9(2) . . . . ? Fe1 C2 N6 C1 5.7(3) . . . . ? N7 C2 N6 C4 -1.7(3) . . . . ? Fe1 C2 N6 C4 -179.13(17) . . . . ? N6 C2 N7 C3 1.7(3) . . . . ? Fe1 C2 N7 C3 177.7(2) . . . . ? N6 C2 N7 C5 175.7(2) . . . . ? Fe1 C2 N7 C5 -8.3(4) . . . . ? C4 C3 N7 C2 -1.0(3) . . . . ? C4 C3 N7 C5 -175.0(2) . . . . ? C10 C5 N7 C2 -94.6(3) . . . . ? C6 C5 N7 C2 84.7(3) . . . . ? C10 C5 N7 C3 78.6(3) . . . . ? C6 C5 N7 C3 -102.1(3) . . . . ? C22 C23 N8 C20 -174.0(3) . . . . ? C22 C23 N8 C21 0.4(3) . . . . ? N5 C20 N8 C23 175.4(2) . . . . ? C19 C20 N8 C23 -2.5(5) . . . . ? N5 C20 N8 C21 1.1(3) . . . . ? C19 C20 N8 C21 -176.8(2) . . . . ? N9 C21 N8 C23 -0.1(3) . . . . ? Fe1 C21 N8 C23 177.07(17) . . . . ? N9 C21 N8 C20 175.3(2) . . . . ? Fe1 C21 N8 C20 -7.5(3) . . . . ? N8 C21 N9 C22 -0.2(3) . . . . ? Fe1 C21 N9 C22 -176.0(2) . . . . ? N8 C21 N9 C24 -171.1(2) . . . . ? Fe1 C21 N9 C24 13.1(4) . . . . ? C23 C22 N9 C21 0.5(3) . . . . ? C23 C22 N9 C24 171.2(2) . . . . ? C25 C24 N9 C21 -84.4(3) . . . . ? C29 C24 N9 C21 93.5(3) . . . . ? C25 C24 N9 C22 106.0(3) . . . . ? C29 C24 N9 C22 -76.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.058 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.069 data_2 _database_code_depnum_ccdc_archive 'CCDC 252528' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H41 Fe N5 O2, 1.5(C6 H6)' _chemical_formula_sum 'C46 H50 Fe N5 O2' _chemical_formula_weight 760.76 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' 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 17.343(3) _cell_length_b 16.989(2) _cell_length_c 27.436(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8084(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6775 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 24.71 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4310708662 _exptl_absorpt_correction_T_max 0.9958 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23527 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 24.65 _reflns_number_total 6816 _reflns_number_gt 4723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 2004) ; _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^)+(0.0333P)^2^+7.0684P] 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 6816 _refine_ls_number_parameters 495 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _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 C1 C 0.31279(19) -0.01991(17) 0.37685(11) 0.0218(7) Uani 1 1 d . . . C2 C 0.24830(18) 0.08872(16) 0.41189(11) 0.0189(7) Uani 1 1 d . . . C3 C 0.17834(19) 0.02441(17) 0.47065(11) 0.0235(8) Uani 1 1 d . . . H3 H 0.1438 0.0160 0.4970 0.028 Uiso 1 1 calc R . . C4 C 0.21831(19) -0.03112(18) 0.44734(11) 0.0247(8) Uani 1 1 d . . . H4 H 0.2178 -0.0860 0.4539 0.030 Uiso 1 1 calc R . . C5 C 0.16155(18) 0.17162(17) 0.46299(11) 0.0192(7) Uani 1 1 d . . . C6 C 0.09077(18) 0.19216(17) 0.44189(11) 0.0210(7) Uani 1 1 d . . . C7 C 0.06019(19) 0.26591(18) 0.45337(11) 0.0251(8) Uani 1 1 d . . . H7 H 0.0131 0.2822 0.4388 0.030 Uiso 1 1 calc R . . C8 C 0.0975(2) 0.31572(18) 0.48563(12) 0.0288(8) Uani 1 1 d . . . H8 H 0.0761 0.3658 0.4929 0.035 Uiso 1 1 calc R . . C9 C 0.16597(19) 0.29274(18) 0.50733(11) 0.0252(8) Uani 1 1 d . . . H9 H 0.1902 0.3270 0.5300 0.030 Uiso 1 1 calc R . . C10 C 0.20013(18) 0.22072(17) 0.49669(10) 0.0212(7) Uani 1 1 d . . . C11 C 0.27370(19) 0.19401(18) 0.52137(11) 0.0255(8) Uani 1 1 d . . . H11 H 0.3037 0.1622 0.4973 0.031 Uiso 1 1 calc R . . C12 C 0.3254(2) 0.2610(2) 0.53867(13) 0.0402(10) Uani 1 1 d . . . H12A H 0.3351 0.2972 0.5115 0.060 Uiso 1 1 calc R . . H12B H 0.3744 0.2395 0.5504 0.060 Uiso 1 1 calc R . . H12C H 0.2998 0.2895 0.5652 0.060 Uiso 1 1 calc R . . C13 C 0.2545(2) 0.1404(2) 0.56473(12) 0.0362(9) Uani 1 1 d . . . H13A H 0.2250 0.1701 0.5890 0.054 Uiso 1 1 calc R . . H13B H 0.3024 0.1212 0.5795 0.054 Uiso 1 1 calc R . . H13C H 0.2238 0.0955 0.5534 0.054 Uiso 1 1 calc R . . C14 C 0.04685(19) 0.13439(19) 0.40978(11) 0.0269(8) Uani 1 1 d . . . H14 H 0.0849 0.0969 0.3953 0.032 Uiso 1 1 calc R . . C15 C -0.0103(2) 0.08663(19) 0.44097(12) 0.0303(8) Uani 1 1 d . . . H15A H 0.0180 0.0577 0.4661 0.045 Uiso 1 1 calc R . . H15B H -0.0382 0.0494 0.4201 0.045 Uiso 1 1 calc R . . H15C H -0.0472 0.1225 0.4565 0.045 Uiso 1 1 calc R . . C16 C 0.0031(2) 0.1737(2) 0.36813(12) 0.0356(9) Uani 1 1 d . . . H16A H -0.0384 0.2064 0.3815 0.053 Uiso 1 1 calc R . . H16B H -0.0190 0.1332 0.3469 0.053 Uiso 1 1 calc R . . H16C H 0.0386 0.2067 0.3493 0.053 Uiso 1 1 calc R . . C17 C 0.33565(19) -0.09618(18) 0.36762(12) 0.0273(8) Uani 1 1 d . . . H17 H 0.3139 -0.1391 0.3850 0.033 Uiso 1 1 calc R . . C18 C 0.3915(2) -0.10828(18) 0.33211(12) 0.0312(9) Uani 1 1 d . . . H18 H 0.4077 -0.1603 0.3246 0.037 Uiso 1 1 calc R . . C19 C 0.4242(2) -0.04457(17) 0.30740(12) 0.0273(8) Uani 1 1 d . . . H19 H 0.4630 -0.0523 0.2835 0.033 Uiso 1 1 calc R . . C20 C 0.39826(18) 0.02972(17) 0.31880(11) 0.0219(7) Uani 1 1 d . . . C21 C 0.38558(19) 0.16854(17) 0.31917(11) 0.0209(7) Uani 1 1 d . . . C22 C 0.48180(19) 0.20024(18) 0.26517(11) 0.0240(8) Uani 1 1 d . . . H22 H 0.5154 0.2312 0.2457 0.029 Uiso 1 1 calc R . . C23 C 0.48091(19) 0.12134(18) 0.26768(11) 0.0255(8) Uani 1 1 d . . . H23 H 0.5134 0.0859 0.2505 0.031 Uiso 1 1 calc R . . C24 C 0.40879(18) 0.31245(17) 0.30351(11) 0.0212(7) Uani 1 1 d . . . C25 C 0.36171(19) 0.35077(18) 0.26986(11) 0.0261(8) Uani 1 1 d . . . C26 C 0.3479(2) 0.43083(18) 0.27716(12) 0.0320(9) Uani 1 1 d . . . H26 H 0.3163 0.4587 0.2548 0.038 Uiso 1 1 calc R . . C27 C 0.3795(2) 0.47015(19) 0.31632(12) 0.0313(9) Uani 1 1 d . . . H27 H 0.3693 0.5246 0.3209 0.038 Uiso 1 1 calc R . . C28 C 0.4259(2) 0.43037(18) 0.34891(12) 0.0284(8) Uani 1 1 d . . . H28 H 0.4472 0.4581 0.3758 0.034 Uiso 1 1 calc R . . C29 C 0.44251(18) 0.35103(18) 0.34347(11) 0.0227(7) Uani 1 1 d . . . C30 C 0.49621(19) 0.30769(19) 0.37823(11) 0.0277(8) Uani 1 1 d . . . H30 H 0.4760 0.2529 0.3822 0.033 Uiso 1 1 calc R . . C31 C 0.5771(2) 0.3018(2) 0.35678(13) 0.0410(10) Uani 1 1 d . . . H31A H 0.5749 0.2742 0.3255 0.062 Uiso 1 1 calc R . . H31B H 0.6105 0.2727 0.3793 0.062 Uiso 1 1 calc R . . H31C H 0.5980 0.3548 0.3518 0.062 Uiso 1 1 calc R . . C32 C 0.5012(2) 0.3451(2) 0.42926(12) 0.0341(9) Uani 1 1 d . . . H32A H 0.5262 0.3967 0.4269 0.051 Uiso 1 1 calc R . . H32B H 0.5314 0.3109 0.4508 0.051 Uiso 1 1 calc R . . H32C H 0.4491 0.3515 0.4426 0.051 Uiso 1 1 calc R . . C33 C 0.3294(2) 0.3098(2) 0.22499(12) 0.0360(9) Uani 1 1 d . . . H33 H 0.3352 0.2518 0.2299 0.043 Uiso 1 1 calc R . . C34 C 0.3760(2) 0.3325(2) 0.17960(13) 0.0493(11) Uani 1 1 d . . . H34A H 0.3694 0.3888 0.1730 0.074 Uiso 1 1 calc R . . H34B H 0.3577 0.3021 0.1516 0.074 Uiso 1 1 calc R . . H34C H 0.4307 0.3212 0.1852 0.074 Uiso 1 1 calc R . . C35 C 0.2439(2) 0.3269(2) 0.21707(13) 0.0422(10) Uani 1 1 d . . . H35A H 0.2153 0.3153 0.2470 0.063 Uiso 1 1 calc R . . H35B H 0.2243 0.2940 0.1905 0.063 Uiso 1 1 calc R . . H35C H 0.2371 0.3826 0.2086 0.063 Uiso 1 1 calc R . . C36 C 0.2230(2) 0.17642(19) 0.32766(12) 0.0265(8) Uani 1 1 d . . . C37 C 0.31396(19) 0.23276(18) 0.39855(11) 0.0241(8) Uani 1 1 d . . . C38 C 0.2667(2) 0.0900(2) 0.20995(14) 0.0388(10) Uani 1 1 d . . . H38 H 0.2817 0.1020 0.2424 0.047 Uiso 1 1 calc R . . C39 C 0.3166(2) 0.0499(2) 0.17956(15) 0.0494(11) Uani 1 1 d . . . H39 H 0.3657 0.0341 0.1914 0.059 Uiso 1 1 calc R . . C40 C 0.2960(3) 0.0328(2) 0.13261(15) 0.0525(11) Uani 1 1 d . . . H40 H 0.3308 0.0056 0.1118 0.063 Uiso 1 1 calc R . . C41 C 0.2243(3) 0.0554(2) 0.11568(14) 0.0533(13) Uani 1 1 d . . . H41 H 0.2098 0.0439 0.0831 0.064 Uiso 1 1 calc R . . C42 C 0.1733(3) 0.0949(2) 0.14614(16) 0.0584(13) Uani 1 1 d . . . H42 H 0.1237 0.1098 0.1347 0.070 Uiso 1 1 calc R . . C43 C 0.1959(3) 0.1122(2) 0.19341(14) 0.0455(10) Uani 1 1 d . . . H43 H 0.1617 0.1398 0.2144 0.055 Uiso 1 1 calc R . . C44 C 0.0086(4) 0.0013(3) 0.04888(16) 0.0685(16) Uani 1 1 d D . . H44 H 0.0152 0.0022 0.0832 0.082 Uiso 1 1 calc R . . C45 C 0.0604(3) -0.0372(3) 0.0205(3) 0.0675(16) Uani 1 1 d D . . H45 H 0.1028 -0.0636 0.0350 0.081 Uiso 1 1 calc R . . C46 C -0.0517(3) 0.0380(2) 0.0287(2) 0.0644(15) Uani 1 1 d D . . H46 H -0.0882 0.0644 0.0486 0.077 Uiso 1 1 calc R . . Fe1 Fe 0.30270(3) 0.14763(2) 0.363609(15) 0.01982(14) Uani 1 1 d . . . N1 N 0.34156(15) 0.04309(14) 0.35233(9) 0.0211(6) Uani 1 1 d . . . N2 N 0.26090(15) 0.00735(14) 0.41149(9) 0.0200(6) Uani 1 1 d . . . N3 N 0.19607(15) 0.09722(13) 0.44964(8) 0.0192(6) Uani 1 1 d . . . N4 N 0.42268(15) 0.10192(14) 0.30063(9) 0.0212(6) Uani 1 1 d . . . N5 N 0.42443(15) 0.22870(13) 0.29638(9) 0.0199(6) Uani 1 1 d . . . O1 O 0.16969(14) 0.19843(14) 0.30600(8) 0.0360(6) Uani 1 1 d . . . O2 O 0.31798(14) 0.29119(12) 0.42060(8) 0.0345(6) 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 C1 0.0249(19) 0.0181(16) 0.0225(18) -0.0005(13) -0.0031(15) 0.0009(15) C2 0.0153(17) 0.0173(16) 0.0240(18) -0.0036(13) -0.0069(15) 0.0044(14) C3 0.0242(19) 0.0231(17) 0.0233(18) 0.0042(14) 0.0018(15) -0.0055(15) C4 0.026(2) 0.0184(16) 0.030(2) 0.0015(14) 0.0029(16) -0.0046(16) C5 0.0191(17) 0.0176(15) 0.0209(17) 0.0030(13) 0.0064(15) 0.0005(14) C6 0.0212(18) 0.0252(17) 0.0164(17) 0.0054(13) 0.0022(14) -0.0009(15) C7 0.0205(19) 0.0271(18) 0.0276(19) 0.0045(14) 0.0004(16) 0.0069(16) C8 0.033(2) 0.0196(17) 0.034(2) -0.0031(15) 0.0086(17) 0.0062(16) C9 0.027(2) 0.0221(17) 0.0265(19) -0.0043(14) 0.0020(16) -0.0032(16) C10 0.0192(18) 0.0256(17) 0.0188(17) 0.0018(13) 0.0021(15) -0.0021(15) C11 0.0228(19) 0.0292(18) 0.0245(19) -0.0065(14) 0.0021(15) 0.0024(16) C12 0.029(2) 0.049(2) 0.042(2) -0.0019(18) -0.0090(18) -0.0053(19) C13 0.038(2) 0.038(2) 0.033(2) 0.0037(16) -0.0097(18) 0.0017(19) C14 0.0224(19) 0.0317(18) 0.0266(19) -0.0049(14) -0.0029(16) 0.0004(16) C15 0.028(2) 0.0288(18) 0.034(2) -0.0025(15) -0.0011(17) -0.0020(17) C16 0.031(2) 0.048(2) 0.027(2) 0.0024(16) -0.0050(17) -0.0052(18) C17 0.0246(19) 0.0224(17) 0.035(2) 0.0016(15) 0.0009(17) -0.0014(15) C18 0.035(2) 0.0189(17) 0.040(2) -0.0055(15) 0.0033(18) 0.0070(16) C19 0.025(2) 0.0256(18) 0.032(2) -0.0043(14) 0.0079(16) 0.0045(16) C20 0.0226(19) 0.0214(16) 0.0217(18) 0.0004(14) -0.0023(15) 0.0009(15) C21 0.0237(18) 0.0190(16) 0.0200(17) -0.0009(13) -0.0053(15) 0.0014(15) C22 0.0245(19) 0.0294(18) 0.0180(17) 0.0011(14) 0.0034(15) 0.0030(16) C23 0.0233(19) 0.0289(18) 0.0243(19) -0.0022(14) 0.0039(16) 0.0064(16) C24 0.0227(19) 0.0219(16) 0.0189(17) 0.0007(13) 0.0045(15) 0.0008(15) C25 0.029(2) 0.0261(17) 0.0229(18) 0.0045(14) -0.0012(16) 0.0034(16) C26 0.040(2) 0.0264(18) 0.030(2) 0.0038(15) -0.0073(18) 0.0084(17) C27 0.042(2) 0.0204(17) 0.031(2) -0.0024(15) -0.0016(18) 0.0050(17) C28 0.032(2) 0.0252(17) 0.028(2) -0.0055(14) -0.0016(17) -0.0014(17) C29 0.0220(18) 0.0269(17) 0.0192(17) 0.0003(14) 0.0022(14) 0.0026(15) C30 0.027(2) 0.0253(17) 0.031(2) -0.0033(14) -0.0083(16) -0.0012(16) C31 0.029(2) 0.050(2) 0.044(2) -0.0111(18) -0.0115(19) 0.0073(19) C32 0.037(2) 0.037(2) 0.029(2) 0.0006(15) -0.0079(17) 0.0022(18) C33 0.048(2) 0.0257(18) 0.034(2) -0.0013(15) -0.0189(19) 0.0056(18) C34 0.046(3) 0.073(3) 0.029(2) -0.013(2) -0.006(2) 0.014(2) C35 0.042(2) 0.048(2) 0.037(2) 0.0031(18) -0.0092(19) -0.008(2) C36 0.029(2) 0.0270(18) 0.0233(19) 0.0017(15) 0.0089(17) 0.0029(17) C37 0.024(2) 0.0235(18) 0.0247(19) 0.0036(14) 0.0060(15) 0.0003(15) C38 0.043(3) 0.040(2) 0.034(2) -0.0044(17) 0.003(2) -0.009(2) C39 0.035(3) 0.055(3) 0.058(3) -0.012(2) 0.000(2) -0.014(2) C40 0.055(3) 0.057(3) 0.046(3) -0.011(2) 0.013(2) -0.017(2) C41 0.098(4) 0.029(2) 0.032(2) -0.0017(17) -0.011(3) -0.012(2) C42 0.074(3) 0.034(2) 0.067(3) -0.005(2) -0.029(3) 0.008(2) C43 0.052(3) 0.037(2) 0.048(3) -0.0065(18) 0.000(2) 0.004(2) C44 0.127(5) 0.037(3) 0.042(3) 0.006(2) -0.014(3) -0.036(3) C45 0.036(3) 0.037(3) 0.129(5) 0.015(3) -0.036(3) 0.003(2) C46 0.058(4) 0.033(2) 0.102(5) -0.015(3) 0.051(3) -0.013(3) Fe1 0.0214(3) 0.0169(2) 0.0211(3) -0.00070(18) 0.0024(2) 0.0024(2) N1 0.0231(15) 0.0199(13) 0.0202(15) -0.0023(11) 0.0016(12) 0.0009(12) N2 0.0210(15) 0.0190(13) 0.0199(14) 0.0001(11) 0.0020(12) 0.0001(12) N3 0.0204(15) 0.0183(13) 0.0188(14) -0.0002(10) -0.0009(12) 0.0012(12) N4 0.0223(15) 0.0214(14) 0.0198(15) -0.0024(11) 0.0022(12) 0.0043(12) N5 0.0234(16) 0.0178(13) 0.0185(14) -0.0014(11) 0.0009(12) 0.0014(12) O1 0.0286(15) 0.0436(15) 0.0358(15) 0.0063(11) -0.0026(12) 0.0086(12) O2 0.0454(16) 0.0220(12) 0.0361(14) -0.0073(11) 0.0129(12) -0.0025(12) _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 C1 N1 1.359(4) . ? C1 C17 1.379(4) . ? C1 N2 1.389(4) . ? C2 N3 1.384(4) . ? C2 N2 1.400(4) . ? C2 Fe1 1.910(3) . ? C3 C4 1.334(4) . ? C3 N3 1.399(4) . ? C3 H3 0.9500 . ? C4 N2 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.401(4) . ? C5 C10 1.414(4) . ? C5 N3 1.446(4) . ? C6 C7 1.397(4) . ? C6 C14 1.523(4) . ? C7 C8 1.385(4) . ? C7 H7 0.9500 . ? C8 C9 1.384(4) . ? C8 H8 0.9500 . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.514(4) . ? C11 C12 1.525(5) . ? C11 C13 1.535(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.526(4) . ? C14 C15 1.541(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.389(5) . ? C17 H17 0.9500 . ? C18 C19 1.397(4) . ? C18 H18 0.9500 . ? C19 C20 1.376(4) . ? C19 H19 0.9500 . ? C20 N1 1.366(4) . ? C20 N4 1.390(4) . ? C21 N5 1.375(4) . ? C21 N4 1.398(4) . ? C21 Fe1 1.918(3) . ? C22 C23 1.342(4) . ? C22 N5 1.399(4) . ? C22 H22 0.9500 . ? C23 N4 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.394(4) . ? C24 C29 1.405(4) . ? C24 N5 1.462(4) . ? C25 C26 1.395(4) . ? C25 C33 1.521(4) . ? C26 C27 1.379(5) . ? C26 H26 0.9500 . ? C27 C28 1.380(5) . ? C27 H27 0.9500 . ? C28 C29 1.386(4) . ? C28 H28 0.9500 . ? C29 C30 1.523(4) . ? C30 C31 1.525(5) . ? C30 C32 1.540(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.527(5) . ? C33 C34 1.534(5) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 O1 1.161(4) . ? C36 Fe1 1.767(4) . ? C37 O2 1.165(4) . ? C37 Fe1 1.746(3) . ? C38 C43 1.363(5) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.368(5) . ? C39 H39 0.9500 . ? C40 C41 1.382(6) . ? C40 H40 0.9500 . ? C41 C42 1.389(6) . ? C41 H41 0.9500 . ? C42 C43 1.386(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C46 1.338(7) . ? C44 C45 1.357(7) . ? C44 H44 0.9500 . ? C45 C46 1.357(7) 5 ? C45 H45 0.9500 . ? C46 C45 1.357(7) 5 ? C46 H46 0.9500 . ? Fe1 N1 1.925(2) . ? 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 C1 C17 122.9(3) . . ? N1 C1 N2 108.3(2) . . ? C17 C1 N2 128.7(3) . . ? N3 C2 N2 102.2(2) . . ? N3 C2 Fe1 142.0(2) . . ? N2 C2 Fe1 115.8(2) . . ? C4 C3 N3 108.3(3) . . ? C4 C3 H3 125.9 . . ? N3 C3 H3 125.9 . . ? C3 C4 N2 106.4(3) . . ? C3 C4 H4 126.8 . . ? N2 C4 H4 126.8 . . ? C6 C5 C10 122.5(3) . . ? C6 C5 N3 118.4(3) . . ? C10 C5 N3 119.1(3) . . ? C7 C6 C5 117.6(3) . . ? C7 C6 C14 121.3(3) . . ? C5 C6 C14 121.1(3) . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 120.2(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C5 117.1(3) . . ? C9 C10 C11 121.9(3) . . ? C5 C10 C11 121.0(3) . . ? C10 C11 C12 114.2(3) . . ? C10 C11 C13 110.0(3) . . ? C12 C11 C13 109.2(3) . . ? C10 C11 H11 107.7 . . ? C12 C11 H11 107.7 . . ? C13 C11 H11 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C16 113.6(3) . . ? C6 C14 C15 109.9(3) . . ? C16 C14 C15 109.0(3) . . ? C6 C14 H14 108.1 . . ? C16 C14 H14 108.1 . . ? C15 C14 H14 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 C18 117.9(3) . . ? C1 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 117.9(3) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? N1 C20 C19 122.8(3) . . ? N1 C20 N4 108.3(2) . . ? C19 C20 N4 128.9(3) . . ? N5 C21 N4 102.2(3) . . ? N5 C21 Fe1 142.6(2) . . ? N4 C21 Fe1 115.2(2) . . ? C23 C22 N5 107.8(3) . . ? C23 C22 H22 126.1 . . ? N5 C22 H22 126.1 . . ? C22 C23 N4 106.1(3) . . ? C22 C23 H23 126.9 . . ? N4 C23 H23 126.9 . . ? C25 C24 C29 122.9(3) . . ? C25 C24 N5 118.3(3) . . ? C29 C24 N5 118.8(3) . . ? C24 C25 C26 117.4(3) . . ? C24 C25 C33 122.6(3) . . ? C26 C25 C33 119.9(3) . . ? C27 C26 C25 121.1(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.0(3) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 121.8(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C24 116.8(3) . . ? C28 C29 C30 122.0(3) . . ? C24 C29 C30 121.2(3) . . ? C29 C30 C31 110.6(3) . . ? C29 C30 C32 113.8(3) . . ? C31 C30 C32 109.0(3) . . ? C29 C30 H30 107.7 . . ? C31 C30 H30 107.7 . . ? C32 C30 H30 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 C35 112.7(3) . . ? C25 C33 C34 110.4(3) . . ? C35 C33 C34 110.4(3) . . ? C25 C33 H33 107.7 . . ? C35 C33 H33 107.7 . . ? C34 C33 H33 107.7 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 Fe1 176.2(3) . . ? O2 C37 Fe1 176.3(3) . . ? C43 C38 C39 120.0(4) . . ? C43 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.6(4) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.5(4) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 119.1(4) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C38 C43 C42 120.5(4) . . ? C38 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C46 C44 C45 120.3(4) . . ? C46 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.1(4) 5 . ? C46 C45 H45 119.9 5 . ? C44 C45 H45 119.9 . . ? C44 C46 C45 119.6(4) . 5 ? C44 C46 H46 120.2 . . ? C45 C46 H46 120.2 5 . ? C37 Fe1 C36 99.48(15) . . ? C37 Fe1 C2 96.23(13) . . ? C36 Fe1 C2 98.38(14) . . ? C37 Fe1 C21 96.43(13) . . ? C36 Fe1 C21 100.38(13) . . ? C2 Fe1 C21 155.27(12) . . ? C37 Fe1 N1 144.43(13) . . ? C36 Fe1 N1 116.07(13) . . ? C2 Fe1 N1 78.51(11) . . ? C21 Fe1 N1 78.83(11) . . ? C1 N1 C20 117.8(3) . . ? C1 N1 Fe1 121.2(2) . . ? C20 N1 Fe1 120.9(2) . . ? C1 N2 C4 132.1(2) . . ? C1 N2 C2 115.8(2) . . ? C4 N2 C2 112.0(2) . . ? C2 N3 C3 111.1(2) . . ? C2 N3 C5 123.5(2) . . ? C3 N3 C5 125.3(3) . . ? C20 N4 C23 131.4(3) . . ? C20 N4 C21 116.3(3) . . ? C23 N4 C21 112.2(2) . . ? C21 N5 C22 111.7(2) . . ? C21 N5 C24 124.9(3) . . ? C22 N5 C24 123.4(2) . . ? 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 N3 C3 C4 N2 -0.2(3) . . . . ? C10 C5 C6 C7 3.2(4) . . . . ? N3 C5 C6 C7 -176.9(3) . . . . ? C10 C5 C6 C14 -173.7(3) . . . . ? N3 C5 C6 C14 6.3(4) . . . . ? C5 C6 C7 C8 -1.9(4) . . . . ? C14 C6 C7 C8 174.9(3) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C7 C8 C9 C10 1.6(5) . . . . ? C8 C9 C10 C5 -0.5(4) . . . . ? C8 C9 C10 C11 -178.1(3) . . . . ? C6 C5 C10 C9 -2.0(4) . . . . ? N3 C5 C10 C9 178.1(3) . . . . ? C6 C5 C10 C11 175.7(3) . . . . ? N3 C5 C10 C11 -4.2(4) . . . . ? C9 C10 C11 C12 -27.0(4) . . . . ? C5 C10 C11 C12 155.5(3) . . . . ? C9 C10 C11 C13 96.2(3) . . . . ? C5 C10 C11 C13 -81.3(3) . . . . ? C7 C6 C14 C16 37.7(4) . . . . ? C5 C6 C14 C16 -145.6(3) . . . . ? C7 C6 C14 C15 -84.7(3) . . . . ? C5 C6 C14 C15 92.0(3) . . . . ? N1 C1 C17 C18 1.0(5) . . . . ? N2 C1 C17 C18 -177.1(3) . . . . ? C1 C17 C18 C19 1.2(5) . . . . ? C17 C18 C19 C20 -1.1(5) . . . . ? C18 C19 C20 N1 -1.2(5) . . . . ? C18 C19 C20 N4 178.0(3) . . . . ? N5 C22 C23 N4 0.0(3) . . . . ? C29 C24 C25 C26 -0.4(5) . . . . ? N5 C24 C25 C26 -179.6(3) . . . . ? C29 C24 C25 C33 176.2(3) . . . . ? N5 C24 C25 C33 -3.0(5) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C33 C25 C26 C27 -177.0(3) . . . . ? C25 C26 C27 C28 0.4(5) . . . . ? C26 C27 C28 C29 0.2(5) . . . . ? C27 C28 C29 C24 -0.9(5) . . . . ? C27 C28 C29 C30 177.6(3) . . . . ? C25 C24 C29 C28 1.0(5) . . . . ? N5 C24 C29 C28 -179.8(3) . . . . ? C25 C24 C29 C30 -177.5(3) . . . . ? N5 C24 C29 C30 1.6(4) . . . . ? C28 C29 C30 C31 -97.9(4) . . . . ? C24 C29 C30 C31 80.6(4) . . . . ? C28 C29 C30 C32 25.3(4) . . . . ? C24 C29 C30 C32 -156.2(3) . . . . ? C24 C25 C33 C35 134.4(3) . . . . ? C26 C25 C33 C35 -49.0(4) . . . . ? C24 C25 C33 C34 -101.6(4) . . . . ? C26 C25 C33 C34 74.9(4) . . . . ? C43 C38 C39 C40 0.6(6) . . . . ? C38 C39 C40 C41 -0.4(6) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C40 C41 C42 C43 0.9(6) . . . . ? C39 C38 C43 C42 0.1(6) . . . . ? C41 C42 C43 C38 -0.8(6) . . . . ? C46 C44 C45 C46 0.7(7) . . . 5 ? C45 C44 C46 C45 -0.7(7) . . . 5 ? N3 C2 Fe1 C37 33.6(4) . . . . ? N2 C2 Fe1 C37 -147.8(2) . . . . ? N3 C2 Fe1 C36 -67.0(4) . . . . ? N2 C2 Fe1 C36 111.6(2) . . . . ? N3 C2 Fe1 C21 154.0(3) . . . . ? N2 C2 Fe1 C21 -27.4(4) . . . . ? N3 C2 Fe1 N1 178.0(4) . . . . ? N2 C2 Fe1 N1 -3.5(2) . . . . ? N5 C21 Fe1 C37 -32.4(4) . . . . ? N4 C21 Fe1 C37 149.1(2) . . . . ? N5 C21 Fe1 C36 68.5(4) . . . . ? N4 C21 Fe1 C36 -110.0(2) . . . . ? N5 C21 Fe1 C2 -152.8(3) . . . . ? N4 C21 Fe1 C2 28.7(4) . . . . ? N5 C21 Fe1 N1 -176.7(4) . . . . ? N4 C21 Fe1 N1 4.8(2) . . . . ? C17 C1 N1 C20 -3.2(4) . . . . ? N2 C1 N1 C20 175.3(2) . . . . ? C17 C1 N1 Fe1 175.8(2) . . . . ? N2 C1 N1 Fe1 -5.7(3) . . . . ? C19 C20 N1 C1 3.3(4) . . . . ? N4 C20 N1 C1 -176.1(3) . . . . ? C19 C20 N1 Fe1 -175.7(2) . . . . ? N4 C20 N1 Fe1 4.9(3) . . . . ? C37 Fe1 N1 C1 90.0(3) . . . . ? C36 Fe1 N1 C1 -88.4(3) . . . . ? C2 Fe1 N1 C1 5.4(2) . . . . ? C21 Fe1 N1 C1 175.4(3) . . . . ? C37 Fe1 N1 C20 -91.1(3) . . . . ? C36 Fe1 N1 C20 90.5(3) . . . . ? C2 Fe1 N1 C20 -175.7(3) . . . . ? C21 Fe1 N1 C20 -5.6(2) . . . . ? N1 C1 N2 C4 -176.7(3) . . . . ? C17 C1 N2 C4 1.7(5) . . . . ? N1 C1 N2 C2 2.4(4) . . . . ? C17 C1 N2 C2 -179.2(3) . . . . ? C3 C4 N2 C1 179.3(3) . . . . ? C3 C4 N2 C2 0.2(4) . . . . ? N3 C2 N2 C1 -179.4(2) . . . . ? Fe1 C2 N2 C1 1.5(3) . . . . ? N3 C2 N2 C4 -0.1(3) . . . . ? Fe1 C2 N2 C4 -179.2(2) . . . . ? N2 C2 N3 C3 -0.1(3) . . . . ? Fe1 C2 N3 C3 178.6(3) . . . . ? N2 C2 N3 C5 -176.6(3) . . . . ? Fe1 C2 N3 C5 2.1(5) . . . . ? C4 C3 N3 C2 0.2(4) . . . . ? C4 C3 N3 C5 176.6(3) . . . . ? C6 C5 N3 C2 92.2(3) . . . . ? C10 C5 N3 C2 -87.9(3) . . . . ? C6 C5 N3 C3 -83.8(4) . . . . ? C10 C5 N3 C3 96.1(4) . . . . ? N1 C20 N4 C23 176.7(3) . . . . ? C19 C20 N4 C23 -2.6(5) . . . . ? N1 C20 N4 C21 -0.6(4) . . . . ? C19 C20 N4 C21 -179.9(3) . . . . ? C22 C23 N4 C20 -176.9(3) . . . . ? C22 C23 N4 C21 0.4(3) . . . . ? N5 C21 N4 C20 177.2(2) . . . . ? Fe1 C21 N4 C20 -3.8(3) . . . . ? N5 C21 N4 C23 -0.6(3) . . . . ? Fe1 C21 N4 C23 178.5(2) . . . . ? N4 C21 N5 C22 0.5(3) . . . . ? Fe1 C21 N5 C22 -178.0(3) . . . . ? N4 C21 N5 C24 -179.2(3) . . . . ? Fe1 C21 N5 C24 2.2(5) . . . . ? C23 C22 N5 C21 -0.3(3) . . . . ? C23 C22 N5 C24 179.4(3) . . . . ? C25 C24 N5 C21 -97.2(4) . . . . ? C29 C24 N5 C21 83.7(4) . . . . ? C25 C24 N5 C22 83.1(4) . . . . ? C29 C24 N5 C22 -96.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.65 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.356 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.062 data_3 _database_code_depnum_ccdc_archive 'CCDC 252529' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H45 Fe N7' _chemical_formula_sum 'C37 H45 Fe N7' _chemical_formula_weight 643.65 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.84(5) _cell_length_b 8.911(12) _cell_length_c 23.56(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.3(2) _cell_angle_gamma 90.00 _cell_volume 6679(20) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6990 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.73 _exptl_crystal_description plate _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7105 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32549 _diffrn_reflns_av_R_equivalents 0.1619 _diffrn_reflns_av_sigmaI/netI 0.1732 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.83 _reflns_number_total 7073 _reflns_number_gt 3678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'Sir92 (Altamore, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 2004) ; _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^)+(0.0395P)^2^+14.4751P] 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 7073 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1771 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 C1 C 0.29728(13) 0.1149(4) -0.03973(19) 0.0231(10) Uani 1 1 d . . . C2 C 0.35868(13) 0.2623(5) -0.04697(19) 0.0245(10) Uani 1 1 d . . . C3 C 0.36497(13) 0.2521(5) -0.14350(18) 0.0299(11) Uani 1 1 d . . . H3 H 0.3756 0.2708 -0.1799 0.036 Uiso 1 1 calc R . . C4 C 0.33162(14) 0.1673(5) -0.1331(2) 0.0293(11) Uani 1 1 d . . . H4 H 0.3144 0.1132 -0.1599 0.035 Uiso 1 1 calc R . . C5 C 0.41518(14) 0.4184(5) -0.09078(18) 0.0254(11) Uani 1 1 d . . . C6 C 0.40379(14) 0.5701(5) -0.09179(19) 0.0286(11) Uani 1 1 d . . . C7 C 0.43662(15) 0.6731(5) -0.0951(2) 0.0370(13) Uani 1 1 d . . . H7 H 0.4304 0.7774 -0.0963 0.044 Uiso 1 1 calc R . . C8 C 0.47761(15) 0.6272(6) -0.0967(2) 0.0434(14) Uani 1 1 d . . . H8 H 0.4993 0.6997 -0.0994 0.052 Uiso 1 1 calc R . . C9 C 0.48764(15) 0.4772(6) -0.0946(2) 0.0391(13) Uani 1 1 d . . . H9 H 0.5163 0.4474 -0.0952 0.047 Uiso 1 1 calc R . . C10 C 0.45668(14) 0.3690(5) -0.09161(19) 0.0287(11) Uani 1 1 d . . . C11 C 0.46778(15) 0.2036(5) -0.0895(2) 0.0391(13) Uani 1 1 d . . . H11 H 0.4442 0.1492 -0.0716 0.047 Uiso 1 1 calc R . . C12 C 0.50820(16) 0.1707(6) -0.0541(2) 0.0528(16) Uani 1 1 d . . . H12A H 0.5323 0.2133 -0.0731 0.079 Uiso 1 1 calc R . . H12B H 0.5119 0.0619 -0.0503 0.079 Uiso 1 1 calc R . . H12C H 0.5063 0.2158 -0.0164 0.079 Uiso 1 1 calc R . . C13 C 0.47174(16) 0.1420(6) -0.1499(2) 0.0506(15) Uani 1 1 d . . . H13A H 0.4455 0.1600 -0.1720 0.076 Uiso 1 1 calc R . . H13B H 0.4774 0.0339 -0.1481 0.076 Uiso 1 1 calc R . . H13C H 0.4949 0.1928 -0.1682 0.076 Uiso 1 1 calc R . . C14 C 0.35813(14) 0.6193(5) -0.0909(2) 0.0312(12) Uani 1 1 d . . . H14 H 0.3432 0.5467 -0.0664 0.037 Uiso 1 1 calc R . . C15 C 0.33633(15) 0.6146(6) -0.1499(2) 0.0441(14) Uani 1 1 d . . . H15A H 0.3517 0.6779 -0.1760 0.066 Uiso 1 1 calc R . . H15B H 0.3075 0.6517 -0.1476 0.066 Uiso 1 1 calc R . . H15C H 0.3358 0.5110 -0.1639 0.066 Uiso 1 1 calc R . . C16 C 0.35318(16) 0.7758(5) -0.0649(2) 0.0510(15) Uani 1 1 d . . . H16A H 0.3689 0.7805 -0.0283 0.076 Uiso 1 1 calc R . . H16B H 0.3234 0.7954 -0.0591 0.076 Uiso 1 1 calc R . . H16C H 0.3641 0.8514 -0.0906 0.076 Uiso 1 1 calc R . . C17 C 0.26374(13) 0.0236(5) -0.0555(2) 0.0284(11) Uani 1 1 d . . . H17 H 0.2588 -0.0060 -0.0939 0.034 Uiso 1 1 calc R . . C18 C 0.23730(14) -0.0238(5) -0.0131(2) 0.0304(12) Uani 1 1 d . . . H18 H 0.2138 -0.0862 -0.0224 0.036 Uiso 1 1 calc R . . C19 C 0.24554(13) 0.0212(5) 0.0431(2) 0.0276(11) Uani 1 1 d . . . H19 H 0.2282 -0.0119 0.0725 0.033 Uiso 1 1 calc R . . C20 C 0.27904(13) 0.1137(5) 0.05484(19) 0.0232(10) Uani 1 1 d . . . C21 C 0.32939(13) 0.2589(4) 0.10696(17) 0.0224(10) Uani 1 1 d . . . C22 C 0.29817(13) 0.2572(5) 0.1939(2) 0.0309(11) Uani 1 1 d . . . H22 H 0.2934 0.2784 0.2326 0.037 Uiso 1 1 calc R . . C23 C 0.27380(14) 0.1734(5) 0.1594(2) 0.0287(11) Uani 1 1 d . . . H23 H 0.2487 0.1230 0.1687 0.034 Uiso 1 1 calc R . . C24 C 0.36656(14) 0.3939(5) 0.18816(18) 0.0256(11) Uani 1 1 d . . . C25 C 0.40082(15) 0.3161(5) 0.2121(2) 0.0315(12) Uani 1 1 d . . . C26 C 0.43351(15) 0.3994(6) 0.2373(2) 0.0412(14) Uani 1 1 d . . . H26 H 0.4570 0.3493 0.2546 0.049 Uiso 1 1 calc R . . C27 C 0.43210(16) 0.5526(6) 0.2374(2) 0.0422(14) Uani 1 1 d . . . H27 H 0.4546 0.6078 0.2549 0.051 Uiso 1 1 calc R . . C28 C 0.39801(16) 0.6287(6) 0.2122(2) 0.0402(13) Uani 1 1 d . . . H28 H 0.3980 0.7354 0.2117 0.048 Uiso 1 1 calc R . . C29 C 0.36379(14) 0.5509(5) 0.18753(19) 0.0296(11) Uani 1 1 d . . . C30 C 0.32567(15) 0.6313(5) 0.1623(2) 0.0343(12) Uani 1 1 d . . . H30 H 0.3136 0.5679 0.1306 0.041 Uiso 1 1 calc R . . C31 C 0.29160(16) 0.6494(6) 0.2063(2) 0.0481(15) Uani 1 1 d . . . H31A H 0.2817 0.5502 0.2177 0.072 Uiso 1 1 calc R . . H31B H 0.2680 0.7071 0.1896 0.072 Uiso 1 1 calc R . . H31C H 0.3034 0.7026 0.2397 0.072 Uiso 1 1 calc R . . C32 C 0.33542(18) 0.7857(5) 0.1377(2) 0.0550(16) Uani 1 1 d . . . H32A H 0.3432 0.8549 0.1687 0.083 Uiso 1 1 calc R . . H32B H 0.3105 0.8241 0.1166 0.083 Uiso 1 1 calc R . . H32C H 0.3588 0.7770 0.1120 0.083 Uiso 1 1 calc R . . C33 C 0.40246(15) 0.1453(5) 0.2108(2) 0.0345(12) Uani 1 1 d . . . H33 H 0.3852 0.1111 0.1769 0.041 Uiso 1 1 calc R . . C34 C 0.38297(16) 0.0768(5) 0.2638(2) 0.0435(14) Uani 1 1 d . . . H34A H 0.3995 0.1070 0.2979 0.065 Uiso 1 1 calc R . . H34B H 0.3830 -0.0329 0.2607 0.065 Uiso 1 1 calc R . . H34C H 0.3540 0.1127 0.2665 0.065 Uiso 1 1 calc R . . C35 C 0.44659(16) 0.0821(6) 0.2057(2) 0.0527(16) Uani 1 1 d . . . H35A H 0.4598 0.1283 0.1732 0.079 Uiso 1 1 calc R . . H35B H 0.4450 -0.0268 0.2002 0.079 Uiso 1 1 calc R . . H35C H 0.4634 0.1041 0.2405 0.079 Uiso 1 1 calc R . . C36 C 0.39582(14) 0.0891(5) 0.0475(2) 0.0371(13) Uani 1 1 d . . . H36A H 0.3911 0.0257 0.0812 0.045 Uiso 1 1 calc R . . H36B H 0.4029 0.0311 0.0133 0.045 Uiso 1 1 calc R . . C37 C 0.41758(15) 0.2212(6) 0.0570(2) 0.0415(13) Uani 1 1 d . . . H37A H 0.4387 0.2478 0.0290 0.050 Uiso 1 1 calc R . . H37B H 0.4269 0.2424 0.0968 0.050 Uiso 1 1 calc R . . Fe1 Fe 0.355457(19) 0.27101(7) 0.03471(3) 0.02403(19) Uani 1 1 d . . . N1 N 0.37353(13) 0.4638(5) 0.04322(16) 0.0361(10) Uani 1 1 d . . . N2 N 0.38736(15) 0.5788(5) 0.04892(18) 0.0501(13) Uani 1 1 d . . . N3 N 0.30560(11) 0.1619(4) 0.01471(16) 0.0229(9) Uani 1 1 d . . . N4 N 0.32733(11) 0.1748(4) -0.07437(15) 0.0246(9) Uani 1 1 d . . . N5 N 0.38160(11) 0.3090(4) -0.09217(15) 0.0248(9) Uani 1 1 d . . . N6 N 0.29235(11) 0.1740(4) 0.10676(15) 0.0239(9) Uani 1 1 d . . . N7 N 0.33215(10) 0.3089(4) 0.16321(15) 0.0239(9) 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 C1 0.023(3) 0.024(2) 0.022(3) 0.000(2) 0.000(2) 0.005(2) C2 0.022(2) 0.027(2) 0.025(3) -0.001(2) 0.002(2) 0.004(2) C3 0.034(3) 0.043(3) 0.013(2) 0.000(2) 0.005(2) -0.005(2) C4 0.033(3) 0.036(3) 0.019(3) -0.008(2) 0.004(2) 0.003(2) C5 0.027(3) 0.038(3) 0.011(2) 0.001(2) 0.003(2) -0.007(2) C6 0.029(3) 0.034(3) 0.022(3) 0.003(2) -0.001(2) -0.004(2) C7 0.043(3) 0.038(3) 0.030(3) 0.004(2) -0.002(2) -0.005(3) C8 0.027(3) 0.062(4) 0.042(4) 0.001(3) -0.001(3) -0.017(3) C9 0.023(3) 0.061(4) 0.033(3) -0.001(3) 0.004(2) -0.001(3) C10 0.025(3) 0.041(3) 0.020(3) -0.001(2) 0.005(2) 0.000(2) C11 0.032(3) 0.051(3) 0.035(3) 0.002(3) 0.009(2) 0.011(2) C12 0.048(4) 0.068(4) 0.042(4) 0.008(3) -0.004(3) 0.021(3) C13 0.047(3) 0.055(3) 0.050(4) -0.005(3) -0.001(3) 0.016(3) C14 0.032(3) 0.030(3) 0.031(3) 0.006(2) 0.003(2) -0.001(2) C15 0.035(3) 0.054(3) 0.044(4) 0.016(3) -0.001(3) 0.003(3) C16 0.058(4) 0.039(3) 0.056(4) 0.006(3) 0.012(3) 0.010(3) C17 0.029(3) 0.030(3) 0.026(3) -0.005(2) -0.005(2) 0.000(2) C18 0.021(3) 0.032(3) 0.038(3) 0.002(2) -0.001(2) -0.008(2) C19 0.022(3) 0.029(3) 0.031(3) 0.005(2) -0.002(2) -0.003(2) C20 0.020(2) 0.026(2) 0.025(3) 0.000(2) 0.004(2) 0.002(2) C21 0.028(2) 0.021(2) 0.018(2) -0.0012(19) -0.0017(19) 0.001(2) C22 0.028(3) 0.040(3) 0.025(3) 0.006(2) 0.010(2) 0.005(2) C23 0.022(3) 0.041(3) 0.024(3) 0.003(2) 0.006(2) -0.004(2) C24 0.029(3) 0.035(3) 0.014(3) -0.002(2) 0.006(2) -0.006(2) C25 0.033(3) 0.044(3) 0.017(3) -0.001(2) 0.001(2) 0.003(2) C26 0.029(3) 0.059(4) 0.036(3) -0.014(3) -0.004(2) 0.004(3) C27 0.035(3) 0.054(4) 0.038(4) -0.020(3) 0.003(3) -0.017(3) C28 0.042(3) 0.040(3) 0.038(3) -0.015(3) 0.003(3) -0.006(3) C29 0.034(3) 0.035(3) 0.020(3) -0.005(2) 0.008(2) -0.001(2) C30 0.048(3) 0.032(3) 0.023(3) -0.004(2) -0.003(2) 0.005(2) C31 0.047(3) 0.055(3) 0.042(4) -0.002(3) 0.001(3) 0.015(3) C32 0.080(4) 0.037(3) 0.048(4) 0.003(3) 0.007(3) 0.012(3) C33 0.038(3) 0.037(3) 0.029(3) 0.004(2) 0.003(2) 0.007(2) C34 0.055(4) 0.040(3) 0.035(3) 0.001(2) 0.007(3) 0.006(3) C35 0.049(4) 0.057(4) 0.053(4) 0.016(3) 0.011(3) 0.025(3) C36 0.032(3) 0.039(3) 0.040(3) 0.003(2) 0.003(3) 0.008(2) C37 0.034(3) 0.068(4) 0.023(3) 0.000(3) 0.002(2) 0.005(3) Fe1 0.0254(4) 0.0274(4) 0.0192(4) -0.0006(3) 0.0007(3) -0.0024(3) N1 0.044(3) 0.041(3) 0.023(3) -0.002(2) 0.010(2) -0.005(2) N2 0.077(4) 0.042(3) 0.032(3) -0.008(2) 0.012(2) -0.021(3) N3 0.026(2) 0.024(2) 0.020(2) -0.0022(16) 0.0031(17) 0.0007(16) N4 0.027(2) 0.030(2) 0.017(2) 0.0002(17) 0.0001(17) 0.0007(17) N5 0.024(2) 0.031(2) 0.019(2) -0.0034(17) 0.0021(17) 0.0007(17) N6 0.022(2) 0.031(2) 0.018(2) 0.0030(17) 0.0006(17) 0.0005(17) N7 0.021(2) 0.031(2) 0.019(2) 0.0015(17) 0.0013(17) -0.0013(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.365(6) . ? C1 C17 1.382(6) . ? C1 N4 1.389(6) . ? C2 N5 1.380(6) . ? C2 N4 1.403(6) . ? C2 Fe1 1.933(6) . ? C3 C4 1.334(6) . ? C3 N5 1.396(6) . ? C3 H3 0.9500 . ? C4 N4 1.396(6) . ? C4 H4 0.9500 . ? C5 C10 1.394(6) . ? C5 C6 1.399(6) . ? C5 N5 1.446(5) . ? C6 C7 1.396(6) . ? C6 C14 1.519(6) . ? C7 C8 1.370(7) . ? C7 H7 0.9500 . ? C8 C9 1.375(7) . ? C8 H8 0.9500 . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.516(7) . ? C11 C12 1.533(7) . ? C11 C13 1.536(7) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.529(7) . ? C14 C16 1.534(6) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.398(6) . ? C17 H17 0.9500 . ? C18 C19 1.398(7) . ? C18 H18 0.9500 . ? C19 C20 1.368(6) . ? C19 H19 0.9500 . ? C20 N3 1.363(6) . ? C20 N6 1.387(6) . ? C21 N7 1.397(6) . ? C21 N6 1.401(5) . ? C21 Fe1 1.927(6) . ? C22 C23 1.330(6) . ? C22 N7 1.403(6) . ? C22 H22 0.9500 . ? C23 N6 1.394(6) . ? C23 H23 0.9500 . ? C24 C25 1.393(6) . ? C24 C29 1.402(6) . ? C24 N7 1.438(6) . ? C25 C26 1.393(7) . ? C25 C33 1.523(7) . ? C26 C27 1.365(7) . ? C26 H26 0.9500 . ? C27 C28 1.393(7) . ? C27 H27 0.9500 . ? C28 C29 1.398(7) . ? C28 H28 0.9500 . ? C29 C30 1.511(7) . ? C30 C32 1.529(6) . ? C30 C31 1.539(7) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.523(6) . ? C33 C34 1.542(7) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.379(6) . ? C36 Fe1 2.083(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 Fe1 2.074(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? Fe1 N1 1.820(5) . ? Fe1 N3 1.905(4) . ? N1 N2 1.121(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 N3 C1 C17 123.5(4) . . ? N3 C1 N4 108.8(4) . . ? C17 C1 N4 127.7(4) . . ? N5 C2 N4 101.6(4) . . ? N5 C2 Fe1 143.8(3) . . ? N4 C2 Fe1 114.5(3) . . ? C4 C3 N5 108.9(4) . . ? C4 C3 H3 125.6 . . ? N5 C3 H3 125.6 . . ? C3 C4 N4 105.4(4) . . ? C3 C4 H4 127.3 . . ? N4 C4 H4 127.3 . . ? C10 C5 C6 123.4(4) . . ? C10 C5 N5 119.1(4) . . ? C6 C5 N5 117.4(4) . . ? C5 C6 C7 116.2(4) . . ? C5 C6 C14 121.7(4) . . ? C7 C6 C14 122.0(4) . . ? C8 C7 C6 121.4(5) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 121.0(5) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C5 117.3(4) . . ? C9 C10 C11 120.9(4) . . ? C5 C10 C11 121.8(4) . . ? C10 C11 C12 113.2(4) . . ? C10 C11 C13 110.2(4) . . ? C12 C11 C13 109.7(4) . . ? C10 C11 H11 107.9 . . ? C12 C11 H11 107.9 . . ? C13 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C15 112.3(4) . . ? C6 C14 C16 112.4(4) . . ? C15 C14 C16 109.8(4) . . ? C6 C14 H14 107.4 . . ? C15 C14 H14 107.4 . . ? C16 C14 H14 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 C18 117.9(5) . . ? C1 C17 H17 121.1 . . ? C18 C17 H17 121.1 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 118.7(4) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N3 C20 C19 123.4(4) . . ? N3 C20 N6 108.3(4) . . ? C19 C20 N6 128.3(4) . . ? N7 C21 N6 101.3(4) . . ? N7 C21 Fe1 143.8(3) . . ? N6 C21 Fe1 114.8(3) . . ? C23 C22 N7 108.2(4) . . ? C23 C22 H22 125.9 . . ? N7 C22 H22 125.9 . . ? C22 C23 N6 106.5(4) . . ? C22 C23 H23 126.8 . . ? N6 C23 H23 126.8 . . ? C25 C24 C29 123.3(4) . . ? C25 C24 N7 118.3(4) . . ? C29 C24 N7 118.3(4) . . ? C24 C25 C26 117.8(5) . . ? C24 C25 C33 121.1(4) . . ? C26 C25 C33 121.0(5) . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.8(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 121.1(5) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C24 116.3(4) . . ? C28 C29 C30 121.9(4) . . ? C24 C29 C30 121.8(4) . . ? C29 C30 C32 113.8(4) . . ? C29 C30 C31 111.2(4) . . ? C32 C30 C31 108.7(4) . . ? C29 C30 H30 107.7 . . ? C32 C30 H30 107.7 . . ? C31 C30 H30 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 C35 113.8(4) . . ? C25 C33 C34 111.4(4) . . ? C35 C33 C34 108.7(4) . . ? C25 C33 H33 107.6 . . ? C35 C33 H33 107.6 . . ? C34 C33 H33 107.6 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 Fe1 70.3(3) . . ? C37 C36 H36A 116.6 . . ? Fe1 C36 H36A 116.6 . . ? C37 C36 H36B 116.6 . . ? Fe1 C36 H36B 116.6 . . ? H36A C36 H36B 113.6 . . ? C36 C37 Fe1 71.0(3) . . ? C36 C37 H37A 116.5 . . ? Fe1 C37 H37A 116.5 . . ? C36 C37 H37B 116.5 . . ? Fe1 C37 H37B 116.5 . . ? H37A C37 H37B 113.5 . . ? N1 Fe1 N3 139.96(17) . . ? N1 Fe1 C21 95.79(18) . . ? N3 Fe1 C21 78.8(2) . . ? N1 Fe1 C2 96.81(19) . . ? N3 Fe1 C2 79.1(2) . . ? C21 Fe1 C2 156.84(19) . . ? N1 Fe1 C37 83.1(2) . . ? N3 Fe1 C37 136.9(2) . . ? C21 Fe1 C37 101.8(2) . . ? C2 Fe1 C37 98.9(3) . . ? N1 Fe1 C36 121.9(2) . . ? N3 Fe1 C36 98.2(2) . . ? C21 Fe1 C36 96.5(2) . . ? C2 Fe1 C36 93.2(2) . . ? C37 Fe1 C36 38.75(17) . . ? N2 N1 Fe1 175.3(4) . . ? C20 N3 C1 116.9(4) . . ? C20 N3 Fe1 121.6(3) . . ? C1 N3 Fe1 121.2(3) . . ? C1 N4 C4 131.3(4) . . ? C1 N4 C2 115.9(4) . . ? C4 N4 C2 112.7(4) . . ? C2 N5 C3 111.4(4) . . ? C2 N5 C5 126.8(4) . . ? C3 N5 C5 121.3(4) . . ? C20 N6 C23 131.1(4) . . ? C20 N6 C21 116.1(4) . . ? C23 N6 C21 112.7(4) . . ? C21 N7 C22 111.3(4) . . ? C21 N7 C24 125.0(4) . . ? C22 N7 C24 123.6(4) . . ? 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 N5 C3 C4 N4 1.1(5) . . . . ? C10 C5 C6 C7 1.5(7) . . . . ? N5 C5 C6 C7 -174.9(4) . . . . ? C10 C5 C6 C14 179.9(4) . . . . ? N5 C5 C6 C14 3.5(6) . . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? C14 C6 C7 C8 -179.0(5) . . . . ? C6 C7 C8 C9 -0.6(8) . . . . ? C7 C8 C9 C10 1.0(8) . . . . ? C8 C9 C10 C5 -0.1(7) . . . . ? C8 C9 C10 C11 179.8(5) . . . . ? C6 C5 C10 C9 -1.2(7) . . . . ? N5 C5 C10 C9 175.2(4) . . . . ? C6 C5 C10 C11 179.0(4) . . . . ? N5 C5 C10 C11 -4.7(6) . . . . ? C9 C10 C11 C12 37.5(6) . . . . ? C5 C10 C11 C12 -142.7(5) . . . . ? C9 C10 C11 C13 -85.7(6) . . . . ? C5 C10 C11 C13 94.2(5) . . . . ? C5 C6 C14 C15 -82.5(5) . . . . ? C7 C6 C14 C15 95.8(5) . . . . ? C5 C6 C14 C16 153.1(4) . . . . ? C7 C6 C14 C16 -28.6(6) . . . . ? N3 C1 C17 C18 -0.6(6) . . . . ? N4 C1 C17 C18 180.0(4) . . . . ? C1 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 1.4(6) . . . . ? C18 C19 C20 N3 -1.7(6) . . . . ? C18 C19 C20 N6 178.6(4) . . . . ? N7 C22 C23 N6 -0.6(5) . . . . ? C29 C24 C25 C26 1.0(7) . . . . ? N7 C24 C25 C26 -178.5(4) . . . . ? C29 C24 C25 C33 -179.1(4) . . . . ? N7 C24 C25 C33 1.3(6) . . . . ? C24 C25 C26 C27 -1.2(7) . . . . ? C33 C25 C26 C27 178.9(4) . . . . ? C25 C26 C27 C28 -0.2(8) . . . . ? C26 C27 C28 C29 1.9(8) . . . . ? C27 C28 C29 C24 -2.0(7) . . . . ? C27 C28 C29 C30 177.2(4) . . . . ? C25 C24 C29 C28 0.6(7) . . . . ? N7 C24 C29 C28 -179.9(4) . . . . ? C25 C24 C29 C30 -178.7(4) . . . . ? N7 C24 C29 C30 0.9(6) . . . . ? C28 C29 C30 C32 30.5(6) . . . . ? C24 C29 C30 C32 -150.3(4) . . . . ? C28 C29 C30 C31 -92.6(5) . . . . ? C24 C29 C30 C31 86.6(5) . . . . ? C24 C25 C33 C35 146.6(5) . . . . ? C26 C25 C33 C35 -33.6(7) . . . . ? C24 C25 C33 C34 -90.1(6) . . . . ? C26 C25 C33 C34 89.7(6) . . . . ? N7 C21 Fe1 N1 -32.7(5) . . . . ? N6 C21 Fe1 N1 144.0(3) . . . . ? N7 C21 Fe1 N3 -172.6(5) . . . . ? N6 C21 Fe1 N3 4.1(3) . . . . ? N7 C21 Fe1 C2 -155.4(5) . . . . ? N6 C21 Fe1 C2 21.3(6) . . . . ? N7 C21 Fe1 C37 51.5(5) . . . . ? N6 C21 Fe1 C37 -131.9(3) . . . . ? N7 C21 Fe1 C36 90.4(5) . . . . ? N6 C21 Fe1 C36 -93.0(3) . . . . ? N5 C2 Fe1 N1 36.6(5) . . . . ? N4 C2 Fe1 N1 -145.2(3) . . . . ? N5 C2 Fe1 N3 176.3(5) . . . . ? N4 C2 Fe1 N3 -5.5(3) . . . . ? N5 C2 Fe1 C21 159.1(4) . . . . ? N4 C2 Fe1 C21 -22.7(6) . . . . ? N5 C2 Fe1 C37 -47.5(5) . . . . ? N4 C2 Fe1 C37 130.8(3) . . . . ? N5 C2 Fe1 C36 -86.0(5) . . . . ? N4 C2 Fe1 C36 92.2(3) . . . . ? C36 C37 Fe1 N1 -179.8(3) . . . . ? C36 C37 Fe1 N3 -0.4(4) . . . . ? C36 C37 Fe1 C21 85.7(3) . . . . ? C36 C37 Fe1 C2 -83.9(3) . . . . ? C37 C36 Fe1 N1 0.3(4) . . . . ? C37 C36 Fe1 N3 179.7(3) . . . . ? C37 C36 Fe1 C21 -100.7(3) . . . . ? C37 C36 Fe1 C2 100.3(3) . . . . ? C19 C20 N3 C1 0.8(6) . . . . ? N6 C20 N3 C1 -179.4(3) . . . . ? C19 C20 N3 Fe1 -172.5(3) . . . . ? N6 C20 N3 Fe1 7.4(4) . . . . ? C17 C1 N3 C20 0.4(6) . . . . ? N4 C1 N3 C20 179.9(3) . . . . ? C17 C1 N3 Fe1 173.6(3) . . . . ? N4 C1 N3 Fe1 -6.8(4) . . . . ? N1 Fe1 N3 C20 -92.3(4) . . . . ? C21 Fe1 N3 C20 -6.7(3) . . . . ? C2 Fe1 N3 C20 -179.9(3) . . . . ? C37 Fe1 N3 C20 88.7(4) . . . . ? C36 Fe1 N3 C20 88.4(3) . . . . ? N1 Fe1 N3 C1 94.7(4) . . . . ? C21 Fe1 N3 C1 -179.6(3) . . . . ? C2 Fe1 N3 C1 7.2(3) . . . . ? C37 Fe1 N3 C1 -84.2(4) . . . . ? C36 Fe1 N3 C1 -84.5(3) . . . . ? N3 C1 N4 C4 -176.3(4) . . . . ? C17 C1 N4 C4 3.2(7) . . . . ? N3 C1 N4 C2 1.7(5) . . . . ? C17 C1 N4 C2 -178.8(4) . . . . ? C3 C4 N4 C1 176.7(4) . . . . ? C3 C4 N4 C2 -1.4(5) . . . . ? N5 C2 N4 C1 -177.4(3) . . . . ? Fe1 C2 N4 C1 3.7(4) . . . . ? N5 C2 N4 C4 1.0(4) . . . . ? Fe1 C2 N4 C4 -178.0(3) . . . . ? N4 C2 N5 C3 -0.2(4) . . . . ? Fe1 C2 N5 C3 178.1(4) . . . . ? N4 C2 N5 C5 171.7(4) . . . . ? Fe1 C2 N5 C5 -9.9(8) . . . . ? C4 C3 N5 C2 -0.6(5) . . . . ? C4 C3 N5 C5 -173.1(4) . . . . ? C10 C5 N5 C2 102.8(5) . . . . ? C6 C5 N5 C2 -80.6(6) . . . . ? C10 C5 N5 C3 -86.0(5) . . . . ? C6 C5 N5 C3 90.6(5) . . . . ? N3 C20 N6 C23 171.9(4) . . . . ? C19 C20 N6 C23 -8.3(7) . . . . ? N3 C20 N6 C21 -3.4(5) . . . . ? C19 C20 N6 C21 176.4(4) . . . . ? C22 C23 N6 C20 -175.2(4) . . . . ? C22 C23 N6 C21 0.2(5) . . . . ? N7 C21 N6 C20 176.5(3) . . . . ? Fe1 C21 N6 C20 -1.5(4) . . . . ? N7 C21 N6 C23 0.3(4) . . . . ? Fe1 C21 N6 C23 -177.7(3) . . . . ? N6 C21 N7 C22 -0.7(4) . . . . ? Fe1 C21 N7 C22 176.2(4) . . . . ? N6 C21 N7 C24 175.4(4) . . . . ? Fe1 C21 N7 C24 -7.7(7) . . . . ? C23 C22 N7 C21 0.9(5) . . . . ? C23 C22 N7 C24 -175.2(4) . . . . ? C25 C24 N7 C21 -87.7(5) . . . . ? C29 C24 N7 C21 92.7(5) . . . . ? C25 C24 N7 C22 87.9(5) . . . . ? C29 C24 N7 C22 -91.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.333 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.081 data_4a _database_code_depnum_ccdc_archive 'CCDC 252530' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H50 Fe N7 P, C4 H10 O' _chemical_formula_sum 'C42 H60 Fe N7 O P' _chemical_formula_weight 765.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.2286(17) _cell_length_b 17.4745(18) _cell_length_c 13.7220(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4370.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5229 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.9752 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24392 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.57 _reflns_number_total 9009 _reflns_number_gt 6933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 2004) ; _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^)+(0.0628P)^2^+1.1939P] 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 0.036(16) _refine_ls_number_reflns 9009 _refine_ls_number_parameters 487 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.022 _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 C1 C 0.2381(2) 0.5317(2) 0.2985(3) 0.0449(11) Uani 1 1 d . . . H1A H 0.1964 0.5310 0.2533 0.067 Uiso 1 1 calc R . . H1B H 0.2820 0.5495 0.2641 0.067 Uiso 1 1 calc R . . H1C H 0.2273 0.5664 0.3528 0.067 Uiso 1 1 calc R . . C2 C 0.3268(2) 0.4537(3) 0.4338(3) 0.0476(11) Uani 1 1 d . . . H2A H 0.3171 0.5021 0.4673 0.071 Uiso 1 1 calc R . . H2B H 0.3740 0.4569 0.3998 0.071 Uiso 1 1 calc R . . H2C H 0.3284 0.4120 0.4815 0.071 Uiso 1 1 calc R . . C3 C 0.1746(2) 0.4280(3) 0.4258(3) 0.0505(12) Uani 1 1 d . . . H3A H 0.1719 0.4737 0.4671 0.076 Uiso 1 1 calc R . . H3B H 0.1793 0.3824 0.4669 0.076 Uiso 1 1 calc R . . H3C H 0.1298 0.4241 0.3866 0.076 Uiso 1 1 calc R . . C4 C 0.15945(17) 0.4151(2) 0.1121(3) 0.0248(8) Uani 1 1 d . . . C5 C 0.10885(15) 0.32884(18) 0.2234(3) 0.0237(8) Uani 1 1 d . . . C6 C 0.20756(18) 0.26908(19) 0.3022(2) 0.0240(7) Uani 1 1 d . . . C7 C 0.14374(18) 0.1809(2) 0.3921(3) 0.0302(8) Uani 1 1 d . . . H7 H 0.1344 0.1392 0.4349 0.036 Uiso 1 1 calc R . . C8 C 0.09324(18) 0.2220(2) 0.3462(3) 0.0292(8) Uani 1 1 d . . . H8 H 0.0415 0.2162 0.3505 0.035 Uiso 1 1 calc R . . C9 C 0.28066(18) 0.1656(2) 0.3772(3) 0.0289(8) Uani 1 1 d . . . C10 C 0.29790(18) 0.1126(2) 0.3052(3) 0.0298(8) Uani 1 1 d . . . C11 C 0.24514(17) 0.0925(2) 0.2224(3) 0.0326(9) Uani 1 1 d . . . H11 H 0.1975 0.1189 0.2354 0.039 Uiso 1 1 calc R . . C12 C 0.2747(2) 0.1218(3) 0.1256(3) 0.0451(11) Uani 1 1 d . . . H12A H 0.2830 0.1771 0.1299 0.068 Uiso 1 1 calc R . . H12B H 0.2391 0.1111 0.0738 0.068 Uiso 1 1 calc R . . H12C H 0.3211 0.0960 0.1107 0.068 Uiso 1 1 calc R . . C13 C 0.2304(2) 0.0062(2) 0.2186(3) 0.0406(10) Uani 1 1 d . . . H13A H 0.2757 -0.0207 0.2012 0.061 Uiso 1 1 calc R . . H13B H 0.1927 -0.0045 0.1695 0.061 Uiso 1 1 calc R . . H13C H 0.2134 -0.0114 0.2825 0.061 Uiso 1 1 calc R . . C14 C 0.36548(18) 0.0768(2) 0.3103(3) 0.0341(9) Uani 1 1 d . . . H14 H 0.3787 0.0405 0.2618 0.041 Uiso 1 1 calc R . . C15 C 0.41402(19) 0.0931(2) 0.3846(3) 0.0391(10) Uani 1 1 d . . . H15 H 0.4609 0.0693 0.3858 0.047 Uiso 1 1 calc R . . C16 C 0.3949(2) 0.1434(2) 0.4565(3) 0.0409(10) Uani 1 1 d . . . H16 H 0.4275 0.1520 0.5093 0.049 Uiso 1 1 calc R . . C17 C 0.32831(19) 0.1821(2) 0.4533(3) 0.0334(9) Uani 1 1 d . . . C18 C 0.3079(3) 0.2386(2) 0.5329(3) 0.0483(11) Uani 1 1 d . . . H18 H 0.2743 0.2776 0.5037 0.058 Uiso 1 1 calc R . . C19 C 0.3731(3) 0.2806(3) 0.5750(4) 0.0629(14) Uani 1 1 d . . . H19A H 0.3559 0.3208 0.6192 0.094 Uiso 1 1 calc R . . H19B H 0.4016 0.3037 0.5220 0.094 Uiso 1 1 calc R . . H19C H 0.4041 0.2445 0.6109 0.094 Uiso 1 1 calc R . . C20 C 0.2661(3) 0.1977(4) 0.6139(4) 0.0749(17) Uani 1 1 d . . . H20A H 0.2962 0.1558 0.6397 0.112 Uiso 1 1 calc R . . H20B H 0.2202 0.1768 0.5877 0.112 Uiso 1 1 calc R . . H20C H 0.2550 0.2340 0.6662 0.112 Uiso 1 1 calc R . . C21 C 0.03851(17) 0.3479(2) 0.1934(3) 0.0289(8) Uani 1 1 d . . . H21 H -0.0032 0.3237 0.2213 0.035 Uiso 1 1 calc R . . C22 C 0.03091(18) 0.4029(2) 0.1221(3) 0.0314(8) Uani 1 1 d . . . H22 H -0.0168 0.4172 0.1011 0.038 Uiso 1 1 calc R . . C23 C 0.09210(18) 0.4379(2) 0.0801(3) 0.0272(8) Uani 1 1 d . . . H23 H 0.0870 0.4760 0.0313 0.033 Uiso 1 1 calc R . . C24 C 0.24973(19) 0.4843(2) 0.0022(3) 0.0299(8) Uani 1 1 d . . . H24 H 0.2186 0.5128 -0.0398 0.036 Uiso 1 1 calc R . . C25 C 0.3226(2) 0.4797(2) -0.0016(3) 0.0300(8) Uani 1 1 d . . . H25 H 0.3530 0.5045 -0.0481 0.036 Uiso 1 1 calc R . . C26 C 0.28842(18) 0.40417(19) 0.1278(3) 0.0231(7) Uani 1 1 d . . . C27 C 0.42063(17) 0.4035(2) 0.0793(3) 0.0264(8) Uani 1 1 d . . . C28 C 0.4388(2) 0.3392(2) 0.0263(3) 0.0335(9) Uani 1 1 d . . . C29 C 0.3825(2) 0.2962(2) -0.0356(3) 0.0346(9) Uani 1 1 d . . . H29 H 0.3327 0.3078 -0.0090 0.042 Uiso 1 1 calc R . . C30 C 0.3935(2) 0.2104(2) -0.0317(4) 0.0531(12) Uani 1 1 d . . . H30A H 0.4375 0.1966 -0.0688 0.080 Uiso 1 1 calc R . . H30B H 0.3506 0.1848 -0.0600 0.080 Uiso 1 1 calc R . . H30C H 0.3994 0.1943 0.0362 0.080 Uiso 1 1 calc R . . C31 C 0.3840(3) 0.3217(3) -0.1422(3) 0.0516(12) Uani 1 1 d . . . H31A H 0.3734 0.3766 -0.1460 0.077 Uiso 1 1 calc R . . H31B H 0.3468 0.2933 -0.1790 0.077 Uiso 1 1 calc R . . H31C H 0.4326 0.3116 -0.1699 0.077 Uiso 1 1 calc R . . C32 C 0.5102(2) 0.3119(2) 0.0319(3) 0.0426(10) Uani 1 1 d . . . H32 H 0.5237 0.2675 -0.0037 0.051 Uiso 1 1 calc R . . C33 C 0.5616(2) 0.3485(3) 0.0883(4) 0.0484(11) Uani 1 1 d . . . H33 H 0.6107 0.3302 0.0899 0.058 Uiso 1 1 calc R . . C34 C 0.5423(2) 0.4113(3) 0.1419(3) 0.0442(10) Uani 1 1 d . . . H34 H 0.5780 0.4353 0.1821 0.053 Uiso 1 1 calc R . . C35 C 0.47200(19) 0.4403(2) 0.1389(3) 0.0377(9) Uani 1 1 d . . . C36 C 0.4505(2) 0.5091(3) 0.2003(4) 0.0563(13) Uani 1 1 d . . . H36 H 0.3971 0.5041 0.2162 0.068 Uiso 1 1 calc R . . C37 C 0.4928(3) 0.5133(3) 0.2971(4) 0.0711(16) Uani 1 1 d . . . H37A H 0.4883 0.4644 0.3316 0.107 Uiso 1 1 calc R . . H37B H 0.4724 0.5544 0.3375 0.107 Uiso 1 1 calc R . . H37C H 0.5447 0.5238 0.2838 0.107 Uiso 1 1 calc R . . C38 C 0.4605(4) 0.5825(3) 0.1433(5) 0.092(2) Uani 1 1 d . . . H38A H 0.5127 0.5903 0.1297 0.137 Uiso 1 1 calc R . . H38B H 0.4418 0.6257 0.1816 0.137 Uiso 1 1 calc R . . H38C H 0.4334 0.5791 0.0818 0.137 Uiso 1 1 calc R . . C39 C -0.1836(3) 0.7299(4) 0.4203(5) 0.098(2) Uani 1 1 d D . . H39A H -0.2207 0.6893 0.4174 0.147 Uiso 1 1 calc R . . H39B H -0.2078 0.7799 0.4185 0.147 Uiso 1 1 calc R . . H39C H -0.1556 0.7251 0.4810 0.147 Uiso 1 1 calc R . . C40 C -0.1355(4) 0.7230(6) 0.3395(5) 0.149(4) Uani 1 1 d D A . H40A H -0.1060 0.7706 0.3387 0.179 Uiso 1 1 calc R . . H40B H -0.1670 0.7249 0.2808 0.179 Uiso 1 1 calc R . . C41 C -0.0354(4) 0.6508(5) 0.2349(6) 0.160(4) Uani 0.558(6) 1 d PD A 1 H41A H -0.0663 0.6367 0.1784 0.193 Uiso 0.558(6) 1 calc PR A 1 H41B H -0.0114 0.7002 0.2196 0.193 Uiso 0.558(6) 1 calc PR A 1 C42 C 0.0214(3) 0.5924(4) 0.2472(6) 0.0366(13) Uani 0.558(6) 1 d PD A 1 H42A H 0.0478 0.6015 0.3084 0.055 Uiso 0.558(6) 1 calc PR A 1 H42B H 0.0559 0.5950 0.1925 0.055 Uiso 0.558(6) 1 calc PR A 1 H42C H -0.0014 0.5417 0.2491 0.055 Uiso 0.558(6) 1 calc PR A 1 C43 C -0.0354(4) 0.6508(5) 0.2349(6) 0.160(4) Uani 0.442(6) 1 d PD A 2 H43A H 0.0040 0.6898 0.2354 0.193 Uiso 0.442(6) 1 calc PR A 2 H43B H -0.0121 0.5996 0.2376 0.193 Uiso 0.442(6) 1 calc PR A 2 C44 C -0.0790(4) 0.6579(5) 0.1442(6) 0.0366(13) Uani 0.442(6) 1 d PD A 2 H44A H -0.1019 0.6086 0.1290 0.055 Uiso 0.442(6) 1 calc PR A 2 H44B H -0.0467 0.6731 0.0904 0.055 Uiso 0.442(6) 1 calc PR A 2 H44C H -0.1172 0.6967 0.1532 0.055 Uiso 0.442(6) 1 calc PR A 2 Fe1 Fe 0.26342(2) 0.34403(2) 0.23654(4) 0.02032(11) Uani 1 1 d . . . N1 N 0.34687(14) 0.43272(16) 0.0734(2) 0.0254(6) Uani 1 1 d . . . N2 N 0.22850(14) 0.43872(16) 0.0800(2) 0.0233(6) Uani 1 1 d . . . N3 N 0.16989(14) 0.36286(15) 0.1840(2) 0.0216(6) Uani 1 1 d . . . N4 N 0.13140(14) 0.27574(15) 0.2903(2) 0.0236(6) Uani 1 1 d . . . N5 N 0.21312(15) 0.20903(17) 0.3671(2) 0.0257(7) Uani 1 1 d . . . N6 N 0.35275(15) 0.30842(16) 0.2626(2) 0.0263(7) Uani 1 1 d . . . N7 N 0.40966(15) 0.28718(18) 0.2806(2) 0.0367(8) Uani 1 1 d . . . P1 P 0.25388(5) 0.43510(6) 0.34543(8) 0.0283(2) Uani 1 1 d . . . O1 O -0.0845(4) 0.6616(5) 0.3233(6) 0.183(3) Uani 1 1 d 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 C1 0.053(2) 0.032(2) 0.049(3) -0.002(2) 0.002(2) 0.0111(18) C2 0.057(3) 0.048(3) 0.038(2) -0.010(2) -0.017(2) 0.001(2) C3 0.056(3) 0.046(3) 0.049(3) -0.010(2) 0.018(2) -0.005(2) C4 0.0234(16) 0.0241(18) 0.0270(19) -0.0007(16) 0.0052(14) 0.0035(14) C5 0.0187(14) 0.0262(18) 0.026(2) 0.0013(16) 0.0014(14) 0.0002(11) C6 0.0262(16) 0.0235(19) 0.0224(18) 0.0014(16) 0.0013(13) 0.0018(13) C7 0.0252(18) 0.034(2) 0.031(2) 0.0131(18) 0.0051(15) -0.0032(15) C8 0.0253(17) 0.0253(19) 0.037(2) 0.0071(18) 0.0066(16) -0.0032(14) C9 0.0198(17) 0.035(2) 0.032(2) 0.0147(18) 0.0008(14) 0.0022(14) C10 0.0278(18) 0.034(2) 0.0276(19) 0.0109(17) 0.0047(15) 0.0022(15) C11 0.0296(18) 0.046(2) 0.023(2) 0.0015(19) -0.0014(15) 0.0087(14) C12 0.061(3) 0.047(3) 0.027(2) 0.006(2) 0.001(2) 0.008(2) C13 0.043(2) 0.043(2) 0.036(3) 0.006(2) -0.0004(18) -0.0019(17) C14 0.0273(18) 0.042(2) 0.033(2) 0.0128(19) 0.0077(15) 0.0072(16) C15 0.0224(18) 0.049(3) 0.046(2) 0.020(2) 0.0039(17) 0.0021(16) C16 0.034(2) 0.047(3) 0.041(2) 0.022(2) -0.0109(18) -0.0086(17) C17 0.033(2) 0.035(2) 0.032(2) 0.0118(19) -0.0036(16) -0.0072(16) C18 0.058(3) 0.040(3) 0.048(3) 0.003(2) -0.018(2) -0.003(2) C19 0.078(4) 0.056(3) 0.054(3) 0.000(3) -0.036(3) -0.008(3) C20 0.084(4) 0.087(4) 0.053(3) -0.016(3) 0.017(3) -0.012(3) C21 0.0176(16) 0.030(2) 0.039(2) -0.0013(18) 0.0023(14) 0.0013(14) C22 0.0202(17) 0.030(2) 0.044(2) 0.0016(18) -0.0034(15) 0.0052(14) C23 0.0270(17) 0.027(2) 0.0274(19) 0.0058(17) -0.0024(14) 0.0045(14) C24 0.037(2) 0.0226(19) 0.030(2) 0.0094(16) 0.0004(14) 0.0004(15) C25 0.034(2) 0.023(2) 0.033(2) 0.0143(17) 0.0085(15) -0.0006(15) C26 0.0245(16) 0.0184(18) 0.0263(19) -0.0022(15) 0.0009(14) -0.0020(13) C27 0.0230(17) 0.027(2) 0.0296(19) 0.0085(17) 0.0045(14) -0.0031(13) C28 0.0262(18) 0.040(2) 0.034(2) 0.0075(19) 0.0060(15) -0.0006(15) C29 0.0277(18) 0.036(2) 0.040(2) -0.0017(19) 0.0042(16) 0.0010(15) C30 0.040(2) 0.042(3) 0.077(3) -0.010(3) 0.005(2) -0.0067(19) C31 0.059(3) 0.050(3) 0.045(3) -0.003(2) -0.005(2) -0.004(2) C32 0.029(2) 0.050(3) 0.049(3) -0.001(2) 0.0068(18) 0.0066(18) C33 0.0249(19) 0.061(3) 0.059(3) 0.005(3) 0.0024(19) 0.0022(19) C34 0.028(2) 0.052(3) 0.052(3) -0.002(2) -0.0014(18) -0.0058(18) C35 0.0285(19) 0.037(2) 0.047(2) 0.003(2) 0.0090(17) -0.0063(16) C36 0.030(2) 0.055(3) 0.084(4) -0.019(3) -0.004(2) -0.0069(19) C37 0.060(3) 0.076(4) 0.077(4) -0.028(3) 0.000(3) -0.019(3) C38 0.120(5) 0.044(3) 0.111(5) -0.003(4) -0.041(4) -0.004(3) C39 0.058(4) 0.144(6) 0.091(5) -0.009(5) -0.001(3) -0.011(4) C40 0.096(5) 0.285(13) 0.068(5) -0.043(6) -0.027(4) 0.102(7) C41 0.121(6) 0.303(12) 0.057(4) -0.015(6) 0.027(5) -0.110(8) C42 0.022(2) 0.051(3) 0.037(3) -0.025(3) 0.004(2) -0.004(2) C43 0.121(6) 0.303(12) 0.057(4) -0.015(6) 0.027(5) -0.110(8) C44 0.022(2) 0.051(3) 0.037(3) -0.025(3) 0.004(2) -0.004(2) Fe1 0.01698(18) 0.0217(2) 0.0223(2) 0.0030(2) 0.0009(2) -0.00012(17) N1 0.0224(14) 0.0249(16) 0.0291(16) 0.0066(14) 0.0032(12) -0.0055(12) N2 0.0224(14) 0.0221(16) 0.0255(16) 0.0054(14) 0.0030(12) 0.0033(11) N3 0.0202(14) 0.0222(15) 0.0224(15) 0.0028(13) 0.0014(11) 0.0007(11) N4 0.0189(13) 0.0225(15) 0.0295(17) 0.0042(13) 0.0031(11) -0.0016(11) N5 0.0207(13) 0.0269(16) 0.0294(17) 0.0041(13) 0.0017(11) -0.0016(11) N6 0.0251(15) 0.0250(16) 0.0286(17) 0.0073(13) 0.0033(11) -0.0019(11) N7 0.0195(15) 0.041(2) 0.049(2) 0.0162(17) 0.0021(13) 0.0027(13) P1 0.0308(5) 0.0270(5) 0.0271(5) -0.0021(5) 0.0017(4) -0.0008(4) O1 0.131(6) 0.259(9) 0.158(7) -0.049(6) 0.020(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 C1 P1 1.830(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 P1 1.828(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 P1 1.823(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N3 1.358(4) . ? C4 C23 1.363(5) . ? C4 N2 1.396(4) . ? C5 N4 1.368(4) . ? C5 N3 1.372(4) . ? C5 C21 1.387(4) . ? C6 N5 1.380(4) . ? C6 N4 1.403(4) . ? C6 Fe1 1.888(3) . ? C7 C8 1.328(5) . ? C7 N5 1.400(4) . ? C7 H7 0.9500 . ? C8 N4 1.397(4) . ? C8 H8 0.9500 . ? C9 C17 1.388(5) . ? C9 C10 1.391(5) . ? C9 N5 1.453(4) . ? C10 C14 1.383(5) . ? C10 C11 1.529(5) . ? C11 C12 1.523(5) . ? C11 C13 1.532(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 C16 1.366(6) . ? C15 H15 0.9500 . ? C16 C17 1.390(5) . ? C16 H16 0.9500 . ? C17 C18 1.518(6) . ? C18 C19 1.511(6) . ? C18 C20 1.526(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.379(5) . ? C21 H21 0.9500 . ? C22 C23 1.396(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.331(5) . ? C24 N2 1.387(5) . ? C24 H24 0.9500 . ? C25 N1 1.389(4) . ? C25 H25 0.9500 . ? C26 N1 1.394(4) . ? C26 N2 1.410(4) . ? C26 Fe1 1.881(3) . ? C27 C28 1.379(5) . ? C27 C35 1.399(5) . ? C27 N1 1.441(4) . ? C28 C32 1.389(5) . ? C28 C29 1.529(5) . ? C29 C30 1.513(5) . ? C29 C31 1.529(6) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.373(6) . ? C32 H32 0.9500 . ? C33 C34 1.367(6) . ? C33 H33 0.9500 . ? C34 C35 1.379(5) . ? C34 H34 0.9500 . ? C35 C36 1.520(6) . ? C36 C38 1.514(7) . ? C36 C37 1.538(7) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.419(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 O1 1.436(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.463(7) . ? C41 O1 1.520(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Fe1 N6 1.779(3) . ? Fe1 N3 1.880(3) . ? Fe1 P1 2.1898(11) . ? N6 N7 1.129(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 P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C23 123.8(3) . . ? N3 C4 N2 107.5(3) . . ? C23 C4 N2 128.7(3) . . ? N4 C5 N3 108.3(3) . . ? N4 C5 C21 129.7(3) . . ? N3 C5 C21 121.9(3) . . ? N5 C6 N4 102.2(3) . . ? N5 C6 Fe1 142.7(2) . . ? N4 C6 Fe1 114.9(2) . . ? C8 C7 N5 108.6(3) . . ? C8 C7 H7 125.7 . . ? N5 C7 H7 125.7 . . ? C7 C8 N4 106.2(3) . . ? C7 C8 H8 126.9 . . ? N4 C8 H8 126.9 . . ? C17 C9 C10 122.1(3) . . ? C17 C9 N5 119.6(3) . . ? C10 C9 N5 118.1(3) . . ? C14 C10 C9 117.8(3) . . ? C14 C10 C11 119.6(3) . . ? C9 C10 C11 122.6(3) . . ? C12 C11 C10 110.4(3) . . ? C12 C11 C13 111.3(3) . . ? C10 C11 C13 111.2(3) . . ? C12 C11 H11 108.0 . . ? C10 C11 H11 108.0 . . ? C13 C11 H11 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 121.0(4) . . ? C15 C14 H14 119.5 . . ? C10 C14 H14 119.5 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C9 C17 C16 118.0(4) . . ? C9 C17 C18 121.5(3) . . ? C16 C17 C18 120.5(4) . . ? C19 C18 C17 113.5(4) . . ? C19 C18 C20 110.0(4) . . ? C17 C18 C20 110.0(4) . . ? C19 C18 H18 107.7 . . ? C17 C18 H18 107.7 . . ? C20 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C5 118.1(3) . . ? C22 C21 H21 121.0 . . ? C5 C21 H21 121.0 . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C4 C23 C22 117.3(3) . . ? C4 C23 H23 121.3 . . ? C22 C23 H23 121.3 . . ? C25 C24 N2 105.9(3) . . ? C25 C24 H24 127.0 . . ? N2 C24 H24 127.0 . . ? C24 C25 N1 108.9(3) . . ? C24 C25 H25 125.5 . . ? N1 C25 H25 125.5 . . ? N1 C26 N2 100.9(3) . . ? N1 C26 Fe1 144.1(3) . . ? N2 C26 Fe1 114.9(2) . . ? C28 C27 C35 121.5(3) . . ? C28 C27 N1 118.9(3) . . ? C35 C27 N1 119.6(3) . . ? C27 C28 C32 118.4(4) . . ? C27 C28 C29 122.2(3) . . ? C32 C28 C29 119.4(4) . . ? C30 C29 C28 112.3(3) . . ? C30 C29 C31 108.7(4) . . ? C28 C29 C31 112.1(3) . . ? C30 C29 H29 107.8 . . ? C28 C29 H29 107.8 . . ? C31 C29 H29 107.8 . . ? 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 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 120.8(4) . . ? C33 C32 H32 119.6 . . ? C28 C32 H32 119.6 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.2(4) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C27 118.1(4) . . ? C34 C35 C36 120.9(4) . . ? C27 C35 C36 121.0(3) . . ? C38 C36 C35 110.6(4) . . ? C38 C36 C37 110.2(4) . . ? C35 C36 C37 112.8(4) . . ? C38 C36 H36 107.7 . . ? C35 C36 H36 107.7 . . ? C37 C36 H36 107.7 . . ? 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 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C39 C40 O1 125.7(9) . . ? C39 C40 H40A 105.9 . . ? O1 C40 H40A 105.9 . . ? C39 C40 H40B 105.9 . . ? O1 C40 H40B 105.9 . . ? H40A C40 H40B 106.2 . . ? C42 C41 O1 114.3(7) . . ? C42 C41 H41A 108.7 . . ? O1 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? O1 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N6 Fe1 N3 165.47(13) . . ? N6 Fe1 C26 97.64(14) . . ? N3 Fe1 C26 79.50(13) . . ? N6 Fe1 C6 98.92(13) . . ? N3 Fe1 C6 79.36(13) . . ? C26 Fe1 C6 153.76(15) . . ? N6 Fe1 P1 100.95(10) . . ? N3 Fe1 P1 93.58(9) . . ? C26 Fe1 P1 98.89(11) . . ? C6 Fe1 P1 97.79(11) . . ? C25 N1 C26 111.4(3) . . ? C25 N1 C27 123.3(3) . . ? C26 N1 C27 123.8(3) . . ? C24 N2 C4 131.6(3) . . ? C24 N2 C26 112.8(3) . . ? C4 N2 C26 115.2(3) . . ? C4 N3 C5 117.6(3) . . ? C4 N3 Fe1 121.6(2) . . ? C5 N3 Fe1 120.5(2) . . ? C5 N4 C8 132.4(3) . . ? C5 N4 C6 115.6(3) . . ? C8 N4 C6 111.9(3) . . ? C6 N5 C7 111.1(3) . . ? C6 N5 C9 121.4(3) . . ? C7 N5 C9 124.0(3) . . ? N7 N6 Fe1 178.4(3) . . ? C3 P1 C2 100.8(2) . . ? C3 P1 C1 98.7(2) . . ? C2 P1 C1 100.6(2) . . ? C3 P1 Fe1 115.24(15) . . ? C2 P1 Fe1 121.59(16) . . ? C1 P1 Fe1 116.27(16) . . ? C40 O1 C41 126.7(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.716 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.062