data_Fe(TTC)(NO) _publ_contact_author_name 'Peter C. Ford' _publ_contact_author_email 'ford@chem.ucsb.edu' loop_ _publ_author_name 'Crisjoe A. Joseph' 'Matthew S. Lee' 'Alexei Iretskii' 'Guang Wu' 'Peter C. Ford' _journal_name_full 'Submitted to Inorganic Chemistry' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H35 Fe N5 O' _chemical_formula_weight 729.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6523(14) _cell_length_b 10.9229(14) _cell_length_c 15.285(2) _cell_angle_alpha 87.514(2) _cell_angle_beta 85.987(2) _cell_angle_gamma 84.216(2) _cell_volume 1763.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 118(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15172 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.15 _reflns_number_total 7541 _reflns_number_gt 5865 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0654P)^2^+0.8184P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7541 _refine_ls_number_parameters 618 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.9546(2) 0.3741(2) 0.56030(14) 0.0197(4) Uani 1 1 d . . . C2 C 1.0409(2) 0.2901(2) 0.51182(15) 0.0224(5) Uani 1 1 d . . . C3 C 1.1472(2) 0.2699(2) 0.55758(15) 0.0217(5) Uani 1 1 d . . . C4 C 1.1282(2) 0.3425(2) 0.63457(14) 0.0196(4) Uani 1 1 d . . . C5 C 1.2107(2) 0.3671(2) 0.69668(14) 0.0197(4) Uani 1 1 d . . . C6 C 1.1760(2) 0.45646(19) 0.76103(14) 0.0189(4) Uani 1 1 d . . . C7 C 1.2502(2) 0.4813(2) 0.83176(14) 0.0214(5) Uani 1 1 d . . . C8 C 1.1816(2) 0.5673(2) 0.88188(15) 0.0236(5) Uani 1 1 d . . . C9 C 1.0640(2) 0.5988(2) 0.84257(14) 0.0197(5) Uani 1 1 d . . . C10 C 0.9648(2) 0.68457(19) 0.87197(14) 0.0199(5) Uani 1 1 d . . . C11 C 0.8523(2) 0.7142(2) 0.82917(14) 0.0206(5) Uani 1 1 d . . . C12 C 0.7542(2) 0.8101(2) 0.85001(15) 0.0221(5) Uani 1 1 d . . . C13 C 0.6638(2) 0.8063(2) 0.79130(15) 0.0224(5) Uani 1 1 d . . . C14 C 0.7041(2) 0.7082(2) 0.73413(14) 0.0199(5) Uani 1 1 d . . . C15 C 0.6379(2) 0.6747(2) 0.66239(14) 0.0204(5) Uani 1 1 d . . . C16 C 0.6892(2) 0.58434(19) 0.60605(14) 0.0183(4) Uani 1 1 d . . . C17 C 0.6457(2) 0.5416(2) 0.52665(14) 0.0209(5) Uani 1 1 d . . . C18 C 0.7350(2) 0.4538(2) 0.49423(15) 0.0220(5) Uani 1 1 d . . . C19 C 0.8346(2) 0.4407(2) 0.55266(14) 0.0199(5) Uani 1 1 d . . . C20 C 1.3400(2) 0.3008(2) 0.69334(14) 0.0194(4) Uani 1 1 d . . . C21 C 1.3584(2) 0.1731(2) 0.68961(14) 0.0218(5) Uani 1 1 d . . . C22 C 1.4796(2) 0.1118(2) 0.68437(15) 0.0242(5) Uani 1 1 d . . . C23 C 1.5858(2) 0.1756(2) 0.68224(14) 0.0244(5) Uani 1 1 d . . . C24 C 1.5673(2) 0.3036(2) 0.68444(15) 0.0249(5) Uani 1 1 d . . . C25 C 1.4469(2) 0.3655(2) 0.69001(15) 0.0228(5) Uani 1 1 d . . . C26 C 1.7175(3) 0.1102(3) 0.6792(2) 0.0345(6) Uani 1 1 d . . . C27 C 0.9737(2) 0.7477(2) 0.95540(14) 0.0197(5) Uani 1 1 d . . . C28 C 1.0705(2) 0.8204(2) 0.96854(15) 0.0221(5) Uani 1 1 d . . . C29 C 1.0714(2) 0.8813(2) 1.04587(15) 0.0240(5) Uani 1 1 d . . . C30 C 0.9777(2) 0.8712(2) 1.11291(14) 0.0241(5) Uani 1 1 d . . . C31 C 0.8826(2) 0.7977(2) 1.10032(15) 0.0235(5) Uani 1 1 d . . . C32 C 0.8802(2) 0.7366(2) 1.02289(15) 0.0249(5) Uani 1 1 d . . . C33 C 0.9779(3) 0.9381(3) 1.19683(17) 0.0315(6) Uani 1 1 d . . . C34 C 0.5107(2) 0.7396(2) 0.64777(14) 0.0208(5) Uani 1 1 d . . . C35 C 0.4104(2) 0.7333(2) 0.71070(15) 0.0241(5) Uani 1 1 d . . . C36 C 0.2904(2) 0.7904(2) 0.69536(16) 0.0245(5) Uani 1 1 d . . . C37 C 0.2682(2) 0.8575(2) 0.61759(15) 0.0236(5) Uani 1 1 d . . . C38 C 0.3688(2) 0.8645(2) 0.55534(15) 0.0259(5) Uani 1 1 d . . . C39 C 0.4881(2) 0.8063(2) 0.56964(15) 0.0242(5) Uani 1 1 d . . . C40 C 0.1389(2) 0.9200(3) 0.60072(19) 0.0300(6) Uani 1 1 d . . . C41 C 0.5867(3) 0.0807(3) 0.9804(3) 0.0661(11) Uani 1 1 d . . . C42 C 0.4928(4) 0.0712(4) 0.9251(2) 0.0604(10) Uani 1 1 d . . . C43 C 0.4071(4) -0.0086(3) 0.9453(3) 0.0685(12) Uani 1 1 d . . . C44 C 0.5439(3) 0.4072(3) 0.94387(19) 0.0392(7) Uani 1 1 d . . . C45 C 0.5767(3) 0.5249(3) 0.92640(19) 0.0380(6) Uani 1 1 d . . . C46 C 0.5327(3) 0.6179(3) 0.98193(19) 0.0393(7) Uani 1 1 d . . . Fe Fe 0.90787(3) 0.50167(3) 0.716406(19) 0.01772(10) Uani 1 1 d . . . H2 H 1.028(3) 0.257(3) 0.4559(19) 0.037(8) Uiso 1 1 d . . . H3 H 1.220(2) 0.219(2) 0.5425(16) 0.025(7) Uiso 1 1 d . . . H7 H 1.332(2) 0.441(2) 0.8422(16) 0.023(6) Uiso 1 1 d . . . H8 H 1.205(3) 0.600(2) 0.9354(18) 0.033(7) Uiso 1 1 d . . . H12 H 0.756(2) 0.869(2) 0.8972(16) 0.022(6) Uiso 1 1 d . . . H13 H 0.586(2) 0.859(2) 0.7895(15) 0.018(6) Uiso 1 1 d . . . H17 H 0.570(2) 0.575(2) 0.5018(16) 0.024(6) Uiso 1 1 d . . . H18 H 0.734(2) 0.410(2) 0.4424(17) 0.026(7) Uiso 1 1 d . . . H21 H 1.285(2) 0.127(2) 0.6908(15) 0.020(6) Uiso 1 1 d . . . H22 H 1.486(2) 0.028(2) 0.6828(15) 0.021(6) Uiso 1 1 d . . . H24 H 1.637(2) 0.352(2) 0.6822(15) 0.020(6) Uiso 1 1 d . . . H25 H 1.440(2) 0.456(2) 0.6896(16) 0.024(6) Uiso 1 1 d . . . H28 H 1.132(2) 0.829(2) 0.9235(16) 0.017(6) Uiso 1 1 d . . . H29 H 1.135(2) 0.935(2) 1.0498(16) 0.026(7) Uiso 1 1 d . . . H31 H 0.819(3) 0.787(2) 1.1427(17) 0.028(7) Uiso 1 1 d . . . H32 H 0.816(2) 0.688(2) 1.0197(15) 0.020(6) Uiso 1 1 d . . . H35 H 0.423(2) 0.686(2) 0.7672(17) 0.028(7) Uiso 1 1 d . . . H36 H 0.224(2) 0.782(2) 0.7376(17) 0.023(6) Uiso 1 1 d . . . H38 H 0.357(3) 0.910(3) 0.5014(19) 0.040(8) Uiso 1 1 d . . . H39 H 0.553(2) 0.812(2) 0.5235(17) 0.024(6) Uiso 1 1 d . . . H41 H 0.645(4) 0.140(4) 0.970(3) 0.071(11) Uiso 1 1 d . . . H42 H 0.492(4) 0.125(4) 0.877(3) 0.082(13) Uiso 1 1 d . . . H43 H 0.354(4) -0.017(4) 0.902(3) 0.077(12) Uiso 1 1 d . . . H44 H 0.577(3) 0.340(3) 0.908(2) 0.057(10) Uiso 1 1 d . . . H45 H 0.631(3) 0.546(3) 0.875(2) 0.046(8) Uiso 1 1 d . . . H46 H 0.557(3) 0.697(3) 0.969(2) 0.054(9) Uiso 1 1 d . . . H26A H 1.723(3) 0.027(3) 0.6594(19) 0.041(8) Uiso 1 1 d . . . H33A H 0.899(3) 0.984(3) 1.208(2) 0.052(9) Uiso 1 1 d . . . H40A H 0.136(3) 1.008(3) 0.608(2) 0.050(9) Uiso 1 1 d . . . H26B H 1.778(3) 0.155(3) 0.645(2) 0.053(10) Uiso 1 1 d . . . H33B H 0.995(3) 0.883(3) 1.246(2) 0.043(8) Uiso 1 1 d . . . H40B H 0.077(3) 0.886(3) 0.641(2) 0.046(9) Uiso 1 1 d . . . H26C H 1.745(4) 0.099(4) 0.740(3) 0.080(12) Uiso 1 1 d . . . H33C H 1.041(3) 0.993(3) 1.1933(19) 0.043(8) Uiso 1 1 d . . . H40C H 0.117(3) 0.909(2) 0.5416(19) 0.036(8) Uiso 1 1 d . . . N1 N 0.84756(17) 0.39873(17) 0.78433(12) 0.0211(4) Uani 1 1 d . . . N2 N 1.00894(17) 0.40364(17) 0.63365(12) 0.0199(4) Uani 1 1 d . . . N3 N 1.06228(17) 0.53017(16) 0.76831(11) 0.0187(4) Uani 1 1 d . . . N4 N 0.82106(17) 0.65396(17) 0.75656(12) 0.0198(4) Uani 1 1 d . . . N5 N 0.80506(17) 0.51939(16) 0.61919(11) 0.0193(4) Uani 1 1 d . . . O O 0.80380(18) 0.32332(17) 0.82927(13) 0.0412(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 0.0190(11) 0.0237(11) 0.0172(10) -0.0025(8) -0.0021(9) -0.0039(9) C2 0.0244(12) 0.0230(11) 0.0204(11) -0.0024(9) -0.0023(9) -0.0045(9) C3 0.0194(12) 0.0229(11) 0.0228(11) -0.0024(9) -0.0002(9) -0.0021(9) C4 0.0174(11) 0.0207(10) 0.0206(11) 0.0003(8) -0.0006(9) -0.0016(9) C5 0.0171(11) 0.0210(11) 0.0209(11) 0.0028(8) -0.0023(9) -0.0029(9) C6 0.0165(11) 0.0202(10) 0.0197(11) 0.0010(8) -0.0027(8) -0.0008(8) C7 0.0186(11) 0.0247(11) 0.0209(11) -0.0001(9) -0.0040(9) 0.0002(9) C8 0.0221(12) 0.0288(12) 0.0208(11) 0.0021(9) -0.0083(9) -0.0036(10) C9 0.0196(11) 0.0217(10) 0.0186(10) 0.0007(8) -0.0051(9) -0.0039(9) C10 0.0219(11) 0.0202(10) 0.0179(11) 0.0015(8) -0.0028(9) -0.0035(9) C11 0.0215(11) 0.0223(11) 0.0187(11) 0.0006(8) -0.0047(9) -0.0040(9) C12 0.0242(12) 0.0213(11) 0.0211(11) -0.0026(9) -0.0052(9) -0.0004(9) C13 0.0217(12) 0.0228(11) 0.0222(11) 0.0010(9) -0.0042(9) 0.0009(9) C14 0.0181(11) 0.0208(10) 0.0205(11) 0.0024(8) -0.0033(9) 0.0000(9) C15 0.0161(11) 0.0252(11) 0.0199(11) 0.0046(9) -0.0032(9) -0.0028(9) C16 0.0159(10) 0.0223(11) 0.0167(10) 0.0023(8) -0.0027(8) -0.0017(9) C17 0.0182(11) 0.0263(11) 0.0190(11) 0.0007(9) -0.0049(9) -0.0044(9) C18 0.0228(12) 0.0256(11) 0.0190(11) -0.0010(9) -0.0060(9) -0.0056(9) C19 0.0226(11) 0.0212(11) 0.0169(10) -0.0015(8) -0.0037(9) -0.0043(9) C20 0.0175(11) 0.0249(11) 0.0152(10) 0.0010(8) -0.0018(8) -0.0001(9) C21 0.0207(12) 0.0253(11) 0.0202(11) -0.0004(9) -0.0045(9) -0.0035(10) C22 0.0265(13) 0.0226(12) 0.0229(12) -0.0012(9) -0.0056(9) 0.0035(10) C23 0.0204(12) 0.0329(13) 0.0191(11) 0.0020(9) -0.0046(9) 0.0029(10) C24 0.0192(12) 0.0327(13) 0.0235(12) 0.0047(10) -0.0059(9) -0.0055(10) C25 0.0231(12) 0.0244(12) 0.0210(11) 0.0022(9) -0.0042(9) -0.0018(9) C26 0.0240(14) 0.0401(16) 0.0378(15) 0.0001(13) -0.0063(12) 0.0074(12) C27 0.0190(11) 0.0221(11) 0.0179(10) -0.0007(8) -0.0053(9) 0.0017(9) C28 0.0195(11) 0.0252(11) 0.0211(11) -0.0009(9) -0.0020(9) 0.0002(9) C29 0.0221(12) 0.0247(12) 0.0261(12) -0.0046(9) -0.0072(10) -0.0013(10) C30 0.0283(13) 0.0241(11) 0.0196(11) -0.0006(9) -0.0084(10) 0.0029(10) C31 0.0254(12) 0.0272(12) 0.0174(11) 0.0004(9) -0.0003(10) -0.0009(10) C32 0.0249(12) 0.0276(12) 0.0232(12) 0.0023(9) -0.0060(10) -0.0054(10) C33 0.0344(15) 0.0378(14) 0.0225(13) -0.0060(11) -0.0069(11) 0.0004(13) C34 0.0203(11) 0.0208(11) 0.0220(11) -0.0025(9) -0.0053(9) -0.0014(9) C35 0.0249(12) 0.0265(12) 0.0208(11) 0.0008(9) -0.0033(9) -0.0008(10) C36 0.0190(12) 0.0285(12) 0.0254(12) -0.0054(10) 0.0018(10) -0.0009(10) C37 0.0210(12) 0.0235(11) 0.0272(12) -0.0080(9) -0.0074(9) -0.0003(9) C38 0.0261(12) 0.0304(12) 0.0208(12) -0.0005(10) -0.0080(10) 0.0027(10) C39 0.0227(12) 0.0295(12) 0.0198(11) 0.0004(9) -0.0026(9) 0.0011(10) C40 0.0235(13) 0.0332(14) 0.0339(14) -0.0084(11) -0.0095(11) 0.0027(11) C41 0.0283(17) 0.0444(19) 0.121(4) 0.011(2) 0.006(2) 0.0036(15) C42 0.078(3) 0.058(2) 0.0370(18) 0.0015(16) 0.0049(18) 0.023(2) C43 0.065(3) 0.046(2) 0.098(3) -0.019(2) -0.052(2) 0.0136(18) C44 0.0292(15) 0.0498(17) 0.0373(15) 0.0005(13) -0.0003(12) -0.0007(13) C45 0.0319(15) 0.0488(17) 0.0313(14) 0.0091(12) 0.0042(12) -0.0028(13) C46 0.0309(15) 0.0434(16) 0.0429(16) 0.0068(13) 0.0009(12) -0.0056(13) Fe 0.01631(17) 0.02127(17) 0.01576(16) 0.00021(11) -0.00407(12) -0.00096(12) N1 0.0178(9) 0.0240(10) 0.0209(9) -0.0001(8) -0.0039(8) 0.0030(8) N2 0.0166(9) 0.0237(9) 0.0198(9) 0.0006(7) -0.0047(7) -0.0021(8) N3 0.0198(9) 0.0205(9) 0.0156(9) -0.0024(7) -0.0018(7) -0.0004(7) N4 0.0176(9) 0.0233(9) 0.0185(9) 0.0018(7) -0.0049(7) -0.0013(8) N5 0.0187(9) 0.0227(9) 0.0170(9) 0.0000(7) -0.0040(7) -0.0022(8) O 0.0340(11) 0.0394(10) 0.0473(12) 0.0211(9) 0.0030(9) -0.0024(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 N2 1.362(3) . ? C1 C19 1.415(3) . ? C1 C2 1.425(3) . ? C2 C3 1.366(3) . ? C2 H2 0.97(3) . ? C3 C4 1.439(3) . ? C3 H3 0.93(3) . ? C4 N2 1.375(3) . ? C4 C5 1.390(3) . ? C5 C6 1.420(3) . ? C5 C20 1.489(3) . ? C6 N3 1.385(3) . ? C6 C7 1.434(3) . ? C7 C8 1.360(3) . ? C7 H7 0.96(3) . ? C8 C9 1.432(3) . ? C8 H8 0.96(3) . ? C9 N3 1.389(3) . ? C9 C10 1.403(3) . ? C10 C11 1.408(3) . ? C10 C27 1.489(3) . ? C11 N4 1.391(3) . ? C11 C12 1.432(3) . ? C12 C13 1.367(3) . ? C12 H12 0.99(2) . ? C13 C14 1.425(3) . ? C13 H13 0.96(2) . ? C14 N4 1.383(3) . ? C14 C15 1.425(3) . ? C15 C16 1.383(3) . ? C15 C34 1.491(3) . ? C16 N5 1.383(3) . ? C16 C17 1.441(3) . ? C17 C18 1.365(3) . ? C17 H17 0.95(3) . ? C18 C19 1.427(3) . ? C18 H18 0.95(3) . ? C19 N5 1.359(3) . ? C20 C21 1.392(3) . ? C20 C25 1.397(3) . ? C21 C22 1.392(3) . ? C21 H21 0.97(2) . ? C22 C23 1.384(3) . ? C22 H22 0.91(3) . ? C23 C24 1.393(3) . ? C23 C26 1.507(3) . ? C24 C25 1.388(3) . ? C24 H24 0.95(3) . ? C25 H25 0.99(2) . ? C26 H26A 0.96(3) . ? C26 H26B 0.96(3) . ? C26 H26C 0.99(4) . ? C27 C28 1.393(3) . ? C27 C32 1.394(3) . ? C28 C29 1.382(3) . ? C28 H28 0.92(3) . ? C29 C30 1.388(3) . ? C29 H29 0.94(3) . ? C30 C31 1.383(3) . ? C30 C33 1.504(3) . ? C31 C32 1.387(3) . ? C31 H31 0.92(3) . ? C32 H32 0.91(3) . ? C33 H33A 0.94(3) . ? C33 H33B 0.96(3) . ? C33 H33C 0.94(3) . ? C34 C35 1.392(3) . ? C34 C39 1.395(3) . ? C35 C36 1.395(3) . ? C35 H35 1.00(3) . ? C36 C37 1.391(3) . ? C36 H36 0.93(3) . ? C37 C38 1.388(3) . ? C37 C40 1.508(3) . ? C38 C39 1.390(3) . ? C38 H38 0.96(3) . ? C39 H39 0.96(3) . ? C40 H40A 0.97(3) . ? C40 H40B 0.96(3) . ? C40 H40C 0.96(3) . ? C41 C43 1.354(6) 2_657 ? C41 C42 1.370(6) . ? C41 H41 0.94(4) . ? C42 C43 1.336(6) . ? C42 H42 0.92(4) . ? C43 C41 1.354(6) 2_657 ? C43 H43 0.92(4) . ? C44 C45 1.375(4) . ? C44 C46 1.384(4) 2_667 ? C44 H44 0.95(3) . ? C45 C46 1.377(4) . ? C45 H45 0.98(3) . ? C46 C44 1.384(4) 2_667 ? C46 H46 0.93(3) . ? Fe N1 1.6450(19) . ? Fe N2 1.8974(19) . ? Fe N5 1.8987(17) . ? Fe N4 1.9230(19) . ? Fe N3 1.9336(18) . ? N1 O 1.162(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 N2 C1 C19 111.49(19) . . ? N2 C1 C2 108.95(19) . . ? C19 C1 C2 139.4(2) . . ? C3 C2 C1 106.9(2) . . ? C3 C2 H2 126.4(17) . . ? C1 C2 H2 126.6(17) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 H3 126.9(16) . . ? C4 C3 H3 125.0(16) . . ? N2 C4 C5 121.0(2) . . ? N2 C4 C3 107.18(18) . . ? C5 C4 C3 131.4(2) . . ? C4 C5 C6 121.6(2) . . ? C4 C5 C20 118.9(2) . . ? C6 C5 C20 119.51(19) . . ? N3 C6 C5 125.67(19) . . ? N3 C6 C7 108.61(19) . . ? C5 C6 C7 125.7(2) . . ? C8 C7 C6 108.0(2) . . ? C8 C7 H7 126.9(15) . . ? C6 C7 H7 125.1(15) . . ? C7 C8 C9 107.5(2) . . ? C7 C8 H8 127.4(16) . . ? C9 C8 H8 125.1(16) . . ? N3 C9 C10 124.08(19) . . ? N3 C9 C8 108.9(2) . . ? C10 C9 C8 127.0(2) . . ? C9 C10 C11 124.5(2) . . ? C9 C10 C27 119.46(18) . . ? C11 C10 C27 115.99(19) . . ? N4 C11 C10 123.9(2) . . ? N4 C11 C12 108.95(18) . . ? C10 C11 C12 127.2(2) . . ? C13 C12 C11 107.3(2) . . ? C13 C12 H12 128.1(14) . . ? C11 C12 H12 124.5(14) . . ? C12 C13 C14 107.7(2) . . ? C12 C13 H13 126.2(14) . . ? C14 C13 H13 126.1(14) . . ? N4 C14 C15 125.0(2) . . ? N4 C14 C13 109.29(19) . . ? C15 C14 C13 125.6(2) . . ? C16 C15 C14 121.6(2) . . ? C16 C15 C34 119.54(19) . . ? C14 C15 C34 118.9(2) . . ? N5 C16 C15 121.19(19) . . ? N5 C16 C17 107.15(18) . . ? C15 C16 C17 131.6(2) . . ? C18 C17 C16 107.88(19) . . ? C18 C17 H17 128.3(15) . . ? C16 C17 H17 123.7(15) . . ? C17 C18 C19 107.2(2) . . ? C17 C18 H18 127.5(15) . . ? C19 C18 H18 125.3(15) . . ? N5 C19 C1 111.82(18) . . ? N5 C19 C18 108.97(19) . . ? C1 C19 C18 139.2(2) . . ? C21 C20 C25 117.9(2) . . ? C21 C20 C5 121.2(2) . . ? C25 C20 C5 120.8(2) . . ? C20 C21 C22 121.0(2) . . ? C20 C21 H21 118.7(14) . . ? C22 C21 H21 120.3(14) . . ? C23 C22 C21 121.3(2) . . ? C23 C22 H22 121.7(16) . . ? C21 C22 H22 117.0(16) . . ? C22 C23 C24 117.7(2) . . ? C22 C23 C26 121.8(2) . . ? C24 C23 C26 120.4(2) . . ? C25 C24 C23 121.5(2) . . ? C25 C24 H24 117.6(15) . . ? C23 C24 H24 121.0(15) . . ? C24 C25 C20 120.6(2) . . ? C24 C25 H25 117.6(15) . . ? C20 C25 H25 121.7(15) . . ? C23 C26 H26A 113.9(18) . . ? C23 C26 H26B 112(2) . . ? H26A C26 H26B 110(3) . . ? C23 C26 H26C 108(2) . . ? H26A C26 H26C 103(3) . . ? H26B C26 H26C 109(3) . . ? C28 C27 C32 118.1(2) . . ? C28 C27 C10 122.8(2) . . ? C32 C27 C10 119.1(2) . . ? C29 C28 C27 120.5(2) . . ? C29 C28 H28 121.1(15) . . ? C27 C28 H28 118.4(15) . . ? C28 C29 C30 121.5(2) . . ? C28 C29 H29 117.3(16) . . ? C30 C29 H29 121.0(16) . . ? C31 C30 C29 118.0(2) . . ? C31 C30 C33 120.4(2) . . ? C29 C30 C33 121.6(2) . . ? C30 C31 C32 121.1(2) . . ? C30 C31 H31 121.6(16) . . ? C32 C31 H31 117.3(17) . . ? C31 C32 C27 120.8(2) . . ? C31 C32 H32 116.5(15) . . ? C27 C32 H32 122.7(15) . . ? C30 C33 H33A 110(2) . . ? C30 C33 H33B 112.3(18) . . ? H33A C33 H33B 109(3) . . ? C30 C33 H33C 111.2(19) . . ? H33A C33 H33C 108(3) . . ? H33B C33 H33C 106(3) . . ? C35 C34 C39 118.0(2) . . ? C35 C34 C15 121.14(19) . . ? C39 C34 C15 120.8(2) . . ? C34 C35 C36 120.9(2) . . ? C34 C35 H35 120.0(15) . . ? C36 C35 H35 119.1(15) . . ? C37 C36 C35 121.0(2) . . ? C37 C36 H36 119.8(15) . . ? C35 C36 H36 119.2(15) . . ? C38 C37 C36 117.9(2) . . ? C38 C37 C40 120.8(2) . . ? C36 C37 C40 121.3(2) . . ? C37 C38 C39 121.4(2) . . ? C37 C38 H38 119.8(17) . . ? C39 C38 H38 118.7(18) . . ? C38 C39 C34 120.8(2) . . ? C38 C39 H39 117.8(15) . . ? C34 C39 H39 121.4(15) . . ? C37 C40 H40A 111.0(19) . . ? C37 C40 H40B 109.1(18) . . ? H40A C40 H40B 109(3) . . ? C37 C40 H40C 112.0(17) . . ? H40A C40 H40C 106(2) . . ? H40B C40 H40C 109(2) . . ? C43 C41 C42 119.9(4) 2_657 . ? C43 C41 H41 119(2) 2_657 . ? C42 C41 H41 121(2) . . ? C43 C42 C41 119.5(3) . . ? C43 C42 H42 125(3) . . ? C41 C42 H42 116(3) . . ? C42 C43 C41 120.6(3) . 2_657 ? C42 C43 H43 114(3) . . ? C41 C43 H43 125(3) 2_657 . ? C45 C44 C46 119.8(3) . 2_667 ? C45 C44 H44 122(2) . . ? C46 C44 H44 118(2) 2_667 . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 122.0(18) . . ? C46 C45 H45 117.7(18) . . ? C45 C46 C44 119.9(3) . 2_667 ? C45 C46 H46 119(2) . . ? C44 C46 H46 121(2) 2_667 . ? N1 Fe N2 103.05(9) . . ? N1 Fe N5 106.30(8) . . ? N2 Fe N5 79.19(8) . . ? N1 Fe N4 102.63(8) . . ? N2 Fe N4 153.47(8) . . ? N5 Fe N4 87.36(8) . . ? N1 Fe N3 103.28(8) . . ? N2 Fe N3 87.65(8) . . ? N5 Fe N3 149.63(8) . . ? N4 Fe N3 92.85(8) . . ? O N1 Fe 177.11(19) . . ? C1 N2 C4 108.88(18) . . ? C1 N2 Fe 117.76(15) . . ? C4 N2 Fe 133.02(15) . . ? C6 N3 C9 107.06(17) . . ? C6 N3 Fe 126.21(15) . . ? C9 N3 Fe 122.97(15) . . ? C14 N4 C11 106.71(18) . . ? C14 N4 Fe 127.60(15) . . ? C11 N4 Fe 124.19(14) . . ? C19 N5 C16 108.78(17) . . ? C19 N5 Fe 117.52(14) . . ? C16 N5 Fe 132.72(15) . . ? 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 N2 C1 C2 C3 0.2(3) . . . . ? C19 C1 C2 C3 175.1(3) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C2 C3 C4 N2 0.9(2) . . . . ? C2 C3 C4 C5 -171.2(2) . . . . ? N2 C4 C5 C6 -0.5(3) . . . . ? C3 C4 C5 C6 170.7(2) . . . . ? N2 C4 C5 C20 -178.37(19) . . . . ? C3 C4 C5 C20 -7.2(4) . . . . ? C4 C5 C6 N3 -2.1(3) . . . . ? C20 C5 C6 N3 175.77(19) . . . . ? C4 C5 C6 C7 174.7(2) . . . . ? C20 C5 C6 C7 -7.4(3) . . . . ? N3 C6 C7 C8 0.9(3) . . . . ? C5 C6 C7 C8 -176.3(2) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C7 C8 C9 N3 0.3(3) . . . . ? C7 C8 C9 C10 -179.5(2) . . . . ? N3 C9 C10 C11 -1.6(4) . . . . ? C8 C9 C10 C11 178.2(2) . . . . ? N3 C9 C10 C27 176.47(19) . . . . ? C8 C9 C10 C27 -3.7(3) . . . . ? C9 C10 C11 N4 6.0(4) . . . . ? C27 C10 C11 N4 -172.12(19) . . . . ? C9 C10 C11 C12 -172.4(2) . . . . ? C27 C10 C11 C12 9.5(3) . . . . ? N4 C11 C12 C13 1.0(3) . . . . ? C10 C11 C12 C13 179.5(2) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 N4 -1.5(3) . . . . ? C12 C13 C14 C15 -178.7(2) . . . . ? N4 C14 C15 C16 -2.0(3) . . . . ? C13 C14 C15 C16 174.8(2) . . . . ? N4 C14 C15 C34 178.4(2) . . . . ? C13 C14 C15 C34 -4.8(3) . . . . ? C14 C15 C16 N5 2.5(3) . . . . ? C34 C15 C16 N5 -177.85(19) . . . . ? C14 C15 C16 C17 -174.7(2) . . . . ? C34 C15 C16 C17 4.9(4) . . . . ? N5 C16 C17 C18 -0.2(2) . . . . ? C15 C16 C17 C18 177.3(2) . . . . ? C16 C17 C18 C19 0.0(3) . . . . ? N2 C1 C19 N5 1.4(3) . . . . ? C2 C1 C19 N5 -173.4(3) . . . . ? N2 C1 C19 C18 178.9(3) . . . . ? C2 C1 C19 C18 4.1(5) . . . . ? C17 C18 C19 N5 0.2(3) . . . . ? C17 C18 C19 C1 -177.3(3) . . . . ? C4 C5 C20 C21 -51.3(3) . . . . ? C6 C5 C20 C21 130.8(2) . . . . ? C4 C5 C20 C25 125.9(2) . . . . ? C6 C5 C20 C25 -52.0(3) . . . . ? C25 C20 C21 C22 1.2(3) . . . . ? C5 C20 C21 C22 178.4(2) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C21 C22 C23 C26 178.2(2) . . . . ? C22 C23 C24 C25 1.0(3) . . . . ? C26 C23 C24 C25 -178.0(2) . . . . ? C23 C24 C25 C20 -0.2(3) . . . . ? C21 C20 C25 C24 -0.9(3) . . . . ? C5 C20 C25 C24 -178.2(2) . . . . ? C9 C10 C27 C28 59.6(3) . . . . ? C11 C10 C27 C28 -122.2(2) . . . . ? C9 C10 C27 C32 -122.0(2) . . . . ? C11 C10 C27 C32 56.2(3) . . . . ? C32 C27 C28 C29 -1.3(3) . . . . ? C10 C27 C28 C29 177.19(19) . . . . ? C27 C28 C29 C30 0.8(3) . . . . ? C28 C29 C30 C31 0.1(3) . . . . ? C28 C29 C30 C33 -179.5(2) . . . . ? C29 C30 C31 C32 -0.5(3) . . . . ? C33 C30 C31 C32 179.2(2) . . . . ? C30 C31 C32 C27 -0.1(3) . . . . ? C28 C27 C32 C31 0.9(3) . . . . ? C10 C27 C32 C31 -177.6(2) . . . . ? C16 C15 C34 C35 118.7(2) . . . . ? C14 C15 C34 C35 -61.7(3) . . . . ? C16 C15 C34 C39 -60.0(3) . . . . ? C14 C15 C34 C39 119.6(2) . . . . ? C39 C34 C35 C36 1.1(3) . . . . ? C15 C34 C35 C36 -177.6(2) . . . . ? C34 C35 C36 C37 -1.5(4) . . . . ? C35 C36 C37 C38 0.9(3) . . . . ? C35 C36 C37 C40 -179.7(2) . . . . ? C36 C37 C38 C39 0.1(4) . . . . ? C40 C37 C38 C39 -179.3(2) . . . . ? C37 C38 C39 C34 -0.5(4) . . . . ? C35 C34 C39 C38 -0.1(3) . . . . ? C15 C34 C39 C38 178.6(2) . . . . ? C43 C41 C42 C43 0.6(6) 2_657 . . . ? C41 C42 C43 C41 -0.6(6) . . . 2_657 ? C46 C44 C45 C46 -0.6(5) 2_667 . . . ? C44 C45 C46 C44 0.6(5) . . . 2_667 ? N2 Fe N1 O -46(4) . . . . ? N5 Fe N1 O 37(4) . . . . ? N4 Fe N1 O 128(4) . . . . ? N3 Fe N1 O -136(4) . . . . ? C19 C1 N2 C4 -176.06(18) . . . . ? C2 C1 N2 C4 0.4(2) . . . . ? C19 C1 N2 Fe 9.7(2) . . . . ? C2 C1 N2 Fe -173.84(14) . . . . ? C5 C4 N2 C1 172.3(2) . . . . ? C3 C4 N2 C1 -0.8(2) . . . . ? C5 C4 N2 Fe -14.7(3) . . . . ? C3 C4 N2 Fe 172.24(16) . . . . ? N1 Fe N2 C1 91.74(17) . . . . ? N5 Fe N2 C1 -12.69(16) . . . . ? N4 Fe N2 C1 -73.5(2) . . . . ? N3 Fe N2 C1 -165.18(16) . . . . ? N1 Fe N2 C4 -80.8(2) . . . . ? N5 Fe N2 C4 174.8(2) . . . . ? N4 Fe N2 C4 114.0(2) . . . . ? N3 Fe N2 C4 22.3(2) . . . . ? C5 C6 N3 C9 176.5(2) . . . . ? C7 C6 N3 C9 -0.7(2) . . . . ? C5 C6 N3 Fe 18.1(3) . . . . ? C7 C6 N3 Fe -159.19(15) . . . . ? C10 C9 N3 C6 -179.9(2) . . . . ? C8 C9 N3 C6 0.3(2) . . . . ? C10 C9 N3 Fe -20.6(3) . . . . ? C8 C9 N3 Fe 159.61(15) . . . . ? N1 Fe N3 C6 80.41(18) . . . . ? N2 Fe N3 C6 -22.45(18) . . . . ? N5 Fe N3 C6 -86.3(2) . . . . ? N4 Fe N3 C6 -175.90(17) . . . . ? N1 Fe N3 C9 -74.87(17) . . . . ? N2 Fe N3 C9 -177.73(17) . . . . ? N5 Fe N3 C9 118.46(19) . . . . ? N4 Fe N3 C9 28.82(17) . . . . ? C15 C14 N4 C11 179.3(2) . . . . ? C13 C14 N4 C11 2.1(2) . . . . ? C15 C14 N4 Fe -14.4(3) . . . . ? C13 C14 N4 Fe 168.41(15) . . . . ? C10 C11 N4 C14 179.5(2) . . . . ? C12 C11 N4 C14 -1.8(2) . . . . ? C10 C11 N4 Fe 12.6(3) . . . . ? C12 C11 N4 Fe -168.79(15) . . . . ? N1 Fe N4 C14 -85.03(19) . . . . ? N2 Fe N4 C14 80.2(3) . . . . ? N5 Fe N4 C14 21.09(18) . . . . ? N3 Fe N4 C14 170.68(18) . . . . ? N1 Fe N4 C11 79.12(19) . . . . ? N2 Fe N4 C11 -115.6(2) . . . . ? N5 Fe N4 C11 -174.76(18) . . . . ? N3 Fe N4 C11 -25.17(18) . . . . ? C1 C19 N5 C16 177.94(18) . . . . ? C18 C19 N5 C16 -0.3(2) . . . . ? C1 C19 N5 Fe -12.0(2) . . . . ? C18 C19 N5 Fe 169.78(15) . . . . ? C15 C16 N5 C19 -177.5(2) . . . . ? C17 C16 N5 C19 0.3(2) . . . . ? C15 C16 N5 Fe 14.5(3) . . . . ? C17 C16 N5 Fe -167.70(16) . . . . ? N1 Fe N5 C19 -87.07(17) . . . . ? N2 Fe N5 C19 13.52(16) . . . . ? N4 Fe N5 C19 170.54(17) . . . . ? N3 Fe N5 C19 79.4(2) . . . . ? N1 Fe N5 C16 80.1(2) . . . . ? N2 Fe N5 C16 -179.3(2) . . . . ? N4 Fe N5 C16 -22.3(2) . . . . ? N3 Fe N5 C16 -113.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.666 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.067 #===END data_Fe(TMOPC)NO _publ_contact_author_name 'Peter C. Ford' _publ_contact_author_email 'ford@chem.ucsb.edu' loop_ _publ_author_name 'Crisjoe A. Joseph' 'Matthew S. Lee' 'Alexei Iretskii' 'Guang Wu' 'Peter C. Ford' _journal_name_full 'Submitted to Inorganic Chemistry' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H35 Fe N5 O4' _chemical_formula_weight 777.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.547(4) _cell_length_b 11.047(5) _cell_length_c 15.916(7) _cell_angle_alpha 101.196(7) _cell_angle_beta 92.972(7) _cell_angle_gamma 90.164(7) _cell_volume 1816.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13739 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.1509 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.55 _reflns_number_total 7189 _reflns_number_gt 3705 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7189 _refine_ls_number_parameters 646 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.224 _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 0.5592(4) 0.6322(4) 0.5658(3) 0.0295(12) Uani 1 1 d . . . C2 C 0.4865(4) 0.7182(4) 0.5272(3) 0.0305(12) Uani 1 1 d . . . C3 C 0.3839(5) 0.7455(5) 0.5741(3) 0.0330(12) Uani 1 1 d . . . C4 C 0.3887(4) 0.6777(4) 0.6422(3) 0.0286(11) Uani 1 1 d . . . C5 C 0.3023(4) 0.6635(4) 0.7022(3) 0.0275(11) Uani 1 1 d . . . C6 C 0.3219(4) 0.5788(4) 0.7593(3) 0.0283(11) Uani 1 1 d . . . C7 C 0.2418(5) 0.5613(5) 0.8244(3) 0.0319(12) Uani 1 1 d . . . C8 C 0.2956(4) 0.4748(5) 0.8650(3) 0.0329(12) Uani 1 1 d . . . C9 C 0.4106(4) 0.4376(4) 0.8254(3) 0.0293(11) Uani 1 1 d . . . C10 C 0.4964(4) 0.3480(4) 0.8464(3) 0.0273(11) Uani 1 1 d . . . C11 C 0.6073(4) 0.3160(4) 0.8046(3) 0.0287(11) Uani 1 1 d . . . C12 C 0.6926(4) 0.2183(4) 0.8153(3) 0.0289(12) Uani 1 1 d . . . C13 C 0.7860(5) 0.2170(4) 0.7611(3) 0.0308(12) Uani 1 1 d . . . C14 C 0.7627(4) 0.3129(4) 0.7144(3) 0.0305(12) Uani 1 1 d . . . C15 C 0.8360(4) 0.3386(4) 0.6475(3) 0.0288(11) Uani 1 1 d . . . C16 C 0.7992(4) 0.4224(4) 0.5975(3) 0.0303(12) Uani 1 1 d . . . C17 C 0.8494(5) 0.4543(4) 0.5236(3) 0.0312(12) Uani 1 1 d . . . C18 C 0.7700(4) 0.5398(5) 0.4954(3) 0.0330(12) Uani 1 1 d . . . C19 C 0.6705(4) 0.5599(4) 0.5529(3) 0.0327(12) Uani 1 1 d . . . C20 C 0.1821(4) 0.7336(4) 0.7034(3) 0.0274(11) Uani 1 1 d . . . C21 C 0.0646(5) 0.6750(5) 0.6895(3) 0.0313(12) Uani 1 1 d . . . C22 C -0.0465(5) 0.7396(5) 0.6824(3) 0.0339(13) Uani 1 1 d . . . C23 C -0.0399(4) 0.8660(4) 0.6894(3) 0.0283(11) Uani 1 1 d . . . C24 C 0.0761(4) 0.9280(5) 0.7040(3) 0.0329(12) Uani 1 1 d . . . C25 C 0.1859(5) 0.8614(5) 0.7099(3) 0.0337(12) Uani 1 1 d . . . C26 C -0.2638(5) 0.8818(6) 0.6582(5) 0.0518(16) Uani 1 1 d . . . C27 C 0.4663(4) 0.2825(4) 0.9163(3) 0.0272(11) Uani 1 1 d . . . C28 C 0.3553(5) 0.2129(4) 0.9151(3) 0.0310(12) Uani 1 1 d . . . C29 C 0.3359(5) 0.1461(5) 0.9776(3) 0.0349(13) Uani 1 1 d . . . C30 C 0.4258(4) 0.1475(4) 1.0444(3) 0.0293(11) Uani 1 1 d . . . C31 C 0.5350(4) 0.2190(4) 1.0489(3) 0.0316(12) Uani 1 1 d . . . C32 C 0.5542(5) 0.2857(4) 0.9857(3) 0.0297(12) Uani 1 1 d . . . C33 C 0.4904(5) 0.0767(6) 1.1715(3) 0.0398(13) Uani 1 1 d . . . C34 C 0.9605(4) 0.2753(4) 0.6317(3) 0.0313(12) Uani 1 1 d . . . C35 C 1.0610(5) 0.2981(5) 0.6922(3) 0.0357(13) Uani 1 1 d . . . C36 C 1.1792(5) 0.2445(4) 0.6781(3) 0.0326(13) Uani 1 1 d . . . C37 C 1.1953(4) 0.1646(4) 0.6011(3) 0.0305(12) Uani 1 1 d . . . C38 C 1.0958(5) 0.1374(5) 0.5391(3) 0.0351(12) Uani 1 1 d . . . C39 C 0.9798(5) 0.1936(4) 0.5544(3) 0.0325(12) Uani 1 1 d . . . C40 C 1.4115(6) 0.1227(6) 0.6452(4) 0.0497(15) Uani 1 1 d . . . C41 C 0.0940(5) 0.9141(6) 1.0048(4) 0.0445(14) Uani 1 1 d . . . C42 C 0.0256(6) 0.9139(5) 0.9288(4) 0.0460(15) Uani 1 1 d . . . C43 C -0.0682(5) 0.9986(6) 0.9236(4) 0.0465(15) Uani 1 1 d . . . C44 C 0.9777(6) 0.3849(6) 0.9517(4) 0.0482(15) Uani 1 1 d . . . C45 C 0.9200(5) 0.4848(5) 0.9277(4) 0.0414(14) Uani 1 1 d . . . C46 C 0.9413(5) 0.6007(6) 0.9759(4) 0.0413(14) Uani 1 1 d . . . Fe Fe 0.58649(6) 0.51914(6) 0.70986(4) 0.0260(2) Uani 1 1 d . . . H2 H 0.507(4) 0.746(4) 0.475(3) 0.036(13) Uiso 1 1 d . . . H3 H 0.309(4) 0.811(4) 0.564(3) 0.048(14) Uiso 1 1 d . . . H7 H 0.162(5) 0.600(5) 0.842(3) 0.069(18) Uiso 1 1 d . . . H8 H 0.265(3) 0.443(3) 0.919(2) 0.011(10) Uiso 1 1 d . . . H12 H 0.679(3) 0.166(3) 0.848(2) 0.017(12) Uiso 1 1 d . . . H13 H 0.857(3) 0.169(3) 0.750(2) 0.000(9) Uiso 1 1 d . . . H17 H 0.926(4) 0.428(3) 0.498(2) 0.020(11) Uiso 1 1 d . . . H18 H 0.773(4) 0.594(3) 0.442(3) 0.034(12) Uiso 1 1 d . . . H21 H 0.058(3) 0.598(3) 0.686(2) 0.015(12) Uiso 1 1 d . . . H22 H -0.118(4) 0.703(3) 0.675(2) 0.017(12) Uiso 1 1 d . . . H24 H 0.082(3) 1.023(4) 0.705(2) 0.028(11) Uiso 1 1 d . . . H25 H 0.273(4) 0.909(4) 0.721(3) 0.041(13) Uiso 1 1 d . . . H28 H 0.301(4) 0.218(4) 0.873(3) 0.041(15) Uiso 1 1 d . . . H29 H 0.261(4) 0.104(3) 0.977(2) 0.017(11) Uiso 1 1 d . . . H31 H 0.597(3) 0.229(3) 1.093(2) 0.013(10) Uiso 1 1 d . . . H32 H 0.627(4) 0.330(4) 0.987(3) 0.051(15) Uiso 1 1 d . . . H35 H 1.055(4) 0.354(4) 0.751(3) 0.035(13) Uiso 1 1 d . . . H36 H 1.245(4) 0.266(4) 0.716(3) 0.048(15) Uiso 1 1 d . . . H38 H 1.119(4) 0.086(4) 0.481(3) 0.058(16) Uiso 1 1 d . . . H39 H 0.908(4) 0.181(3) 0.508(2) 0.027(12) Uiso 1 1 d . . . H41 H 0.162(6) 0.852(6) 1.007(4) 0.11(2) Uiso 1 1 d . . . H42 H 0.045(5) 0.852(5) 0.884(3) 0.07(2) Uiso 1 1 d . . . H43 H -0.123(6) 0.999(5) 0.874(4) 0.10(2) Uiso 1 1 d . . . H44 H 0.961(4) 0.311(4) 0.922(3) 0.027(13) Uiso 1 1 d . . . H45 H 0.874(4) 0.466(4) 0.868(3) 0.042(13) Uiso 1 1 d . . . H46 H 0.906(5) 0.664(5) 0.967(4) 0.08(2) Uiso 1 1 d . . . H26A H -0.313(5) 0.963(5) 0.659(3) 0.076(19) Uiso 1 1 d . . . H33A H 0.463(4) 0.013(4) 1.205(3) 0.038(13) Uiso 1 1 d . . . H40A H 1.384(3) 0.093(3) 0.699(2) 0.019(11) Uiso 1 1 d . . . H26B H -0.257(4) 0.825(4) 0.600(3) 0.047(15) Uiso 1 1 d . . . H33B H 0.586(5) 0.044(4) 1.144(3) 0.064(16) Uiso 1 1 d . . . H40B H 1.484(6) 0.062(6) 0.614(4) 0.10(2) Uiso 1 1 d . . . H26C H -0.283(4) 0.845(4) 0.707(3) 0.052(17) Uiso 1 1 d . . . H33C H 0.502(4) 0.162(4) 1.200(3) 0.043(15) Uiso 1 1 d . . . H40C H 1.435(4) 0.227(5) 0.652(3) 0.067(16) Uiso 1 1 d . . . N1 N 0.6719(4) 0.6243(3) 0.7837(2) 0.0253(9) Uani 1 1 d . . . N2 N 0.4996(3) 0.6106(3) 0.6366(2) 0.0253(9) Uani 1 1 d . . . N3 N 0.4271(3) 0.5021(3) 0.7600(2) 0.0263(9) Uani 1 1 d . . . N4 N 0.6502(3) 0.3715(3) 0.7396(2) 0.0239(9) Uani 1 1 d . . . N5 N 0.6877(3) 0.4880(3) 0.6145(2) 0.0284(9) Uani 1 1 d . . . O1 O 0.7374(4) 0.6836(3) 0.8273(2) 0.0524(10) Uani 1 1 d . . . O2 O -0.1422(3) 0.9402(3) 0.6821(2) 0.0380(8) Uani 1 1 d . . . O3 O 0.3983(3) 0.0750(3) 1.10233(19) 0.0353(8) Uani 1 1 d . . . O4 O 1.3067(3) 0.1023(3) 0.5806(2) 0.0428(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 0.035(3) 0.034(3) 0.018(3) 0.002(2) 0.001(2) -0.009(2) C2 0.032(3) 0.034(3) 0.028(3) 0.013(2) -0.001(2) -0.002(2) C3 0.031(3) 0.038(3) 0.031(3) 0.011(3) -0.004(2) -0.011(2) C4 0.026(3) 0.034(3) 0.023(3) 0.000(2) -0.001(2) -0.009(2) C5 0.026(3) 0.027(3) 0.031(3) 0.008(2) 0.004(2) -0.003(2) C6 0.028(3) 0.026(3) 0.029(3) -0.001(2) 0.008(2) -0.003(2) C7 0.027(3) 0.035(3) 0.031(3) -0.003(2) 0.009(2) -0.004(2) C8 0.035(3) 0.040(3) 0.023(3) 0.006(2) 0.000(2) -0.013(3) C9 0.022(3) 0.034(3) 0.031(3) 0.003(2) 0.003(2) -0.007(2) C10 0.031(3) 0.025(3) 0.024(3) 0.004(2) -0.002(2) -0.005(2) C11 0.028(3) 0.029(3) 0.027(3) 0.001(2) -0.002(2) -0.007(2) C12 0.030(3) 0.022(3) 0.035(3) 0.008(2) 0.000(2) -0.003(2) C13 0.026(3) 0.028(3) 0.038(3) 0.002(2) 0.008(2) 0.001(2) C14 0.032(3) 0.030(3) 0.026(3) -0.003(2) 0.001(2) -0.012(2) C15 0.032(3) 0.028(3) 0.026(3) 0.002(2) 0.002(2) -0.005(2) C16 0.031(3) 0.034(3) 0.022(3) -0.005(2) 0.001(2) -0.009(2) C17 0.024(3) 0.038(3) 0.029(3) 0.000(2) 0.005(2) -0.005(2) C18 0.030(3) 0.040(3) 0.029(3) 0.009(3) -0.001(2) -0.005(2) C19 0.029(3) 0.037(3) 0.030(3) 0.000(2) 0.001(2) -0.007(2) C20 0.025(3) 0.030(3) 0.027(3) 0.003(2) 0.004(2) 0.000(2) C21 0.032(3) 0.025(3) 0.037(3) 0.006(3) 0.001(2) -0.004(3) C22 0.023(3) 0.036(3) 0.042(3) 0.006(3) 0.004(2) -0.005(3) C23 0.025(3) 0.033(3) 0.028(3) 0.007(2) 0.008(2) 0.009(2) C24 0.031(3) 0.030(3) 0.039(3) 0.010(2) 0.003(2) -0.008(2) C25 0.026(3) 0.036(3) 0.039(3) 0.007(3) 0.004(2) -0.007(2) C26 0.035(4) 0.048(4) 0.073(5) 0.012(4) 0.006(3) 0.003(3) C27 0.033(3) 0.028(3) 0.022(3) 0.005(2) 0.006(2) 0.004(2) C28 0.033(3) 0.036(3) 0.025(3) 0.007(2) 0.000(2) 0.000(2) C29 0.035(3) 0.038(3) 0.033(3) 0.008(3) 0.004(3) -0.009(3) C30 0.036(3) 0.031(3) 0.024(3) 0.013(2) 0.005(2) 0.004(2) C31 0.027(3) 0.042(3) 0.026(3) 0.007(3) -0.006(2) -0.002(2) C32 0.022(3) 0.034(3) 0.029(3) -0.003(2) 0.002(2) -0.004(2) C33 0.048(4) 0.039(4) 0.033(3) 0.010(3) -0.001(3) 0.002(3) C34 0.029(3) 0.034(3) 0.028(3) -0.001(2) 0.000(2) -0.006(2) C35 0.034(3) 0.041(3) 0.029(3) 0.000(3) -0.001(2) -0.007(3) C36 0.030(3) 0.036(3) 0.031(3) 0.006(3) -0.002(3) -0.007(3) C37 0.035(3) 0.029(3) 0.029(3) 0.008(2) 0.004(2) -0.002(2) C38 0.032(3) 0.042(3) 0.031(3) 0.003(3) 0.005(3) 0.004(3) C39 0.032(3) 0.034(3) 0.028(3) -0.002(2) -0.003(2) -0.004(2) C40 0.042(4) 0.067(5) 0.043(4) 0.021(3) -0.010(3) -0.002(3) C41 0.044(3) 0.051(4) 0.043(4) 0.021(3) -0.004(3) -0.005(3) C42 0.059(4) 0.037(4) 0.042(4) 0.006(3) 0.003(3) -0.009(3) C43 0.046(4) 0.054(4) 0.042(4) 0.018(3) -0.006(3) -0.004(3) C44 0.059(4) 0.039(4) 0.044(4) 0.007(3) -0.013(3) -0.014(3) C45 0.041(3) 0.045(4) 0.036(3) 0.004(3) -0.006(3) -0.007(3) C46 0.042(4) 0.043(4) 0.039(3) 0.010(3) -0.001(3) 0.000(3) Fe 0.0247(4) 0.0285(4) 0.0239(4) 0.0032(3) 0.0007(3) -0.0035(3) N1 0.030(2) 0.022(2) 0.025(2) 0.0066(19) 0.0055(19) 0.0047(19) N2 0.026(2) 0.025(2) 0.023(2) -0.0002(18) 0.0036(17) 0.0011(18) N3 0.029(2) 0.028(2) 0.019(2) -0.0008(18) 0.0031(17) 0.0012(18) N4 0.025(2) 0.029(2) 0.018(2) 0.0032(18) 0.0042(17) -0.0074(18) N5 0.022(2) 0.029(2) 0.032(2) 0.0004(19) -0.0021(18) -0.0057(18) O1 0.059(3) 0.048(3) 0.046(2) 0.000(2) 0.000(2) 0.002(2) O2 0.0287(19) 0.031(2) 0.052(2) 0.0020(17) 0.0048(17) 0.0056(16) O3 0.038(2) 0.037(2) 0.0325(19) 0.0128(17) -0.0033(16) -0.0035(16) O4 0.033(2) 0.058(2) 0.038(2) 0.0107(18) 0.0024(17) 0.0052(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.378(5) . ? C1 C19 1.423(6) . ? C1 C2 1.432(6) . ? C2 C3 1.348(6) . ? C2 H2 0.98(4) . ? C3 C4 1.431(6) . ? C3 H3 1.10(4) . ? C4 C5 1.383(6) . ? C4 N2 1.384(5) . ? C5 C6 1.435(6) . ? C5 C20 1.486(6) . ? C6 N3 1.399(5) . ? C6 C7 1.412(6) . ? C7 C8 1.363(6) . ? C7 H7 0.97(5) . ? C8 C9 1.422(6) . ? C8 H8 1.05(3) . ? C9 N3 1.388(5) . ? C9 C10 1.419(6) . ? C10 C11 1.389(6) . ? C10 C27 1.486(6) . ? C11 N4 1.393(5) . ? C11 C12 1.437(6) . ? C12 C13 1.341(6) . ? C12 H12 0.86(4) . ? C13 C14 1.423(6) . ? C13 H13 0.92(3) . ? C14 N4 1.394(5) . ? C14 C15 1.419(6) . ? C15 C16 1.379(6) . ? C15 C34 1.499(6) . ? C16 N5 1.394(5) . ? C16 C17 1.418(6) . ? C17 C18 1.388(6) . ? C17 H17 0.95(4) . ? C18 C19 1.418(6) . ? C18 H18 1.13(4) . ? C19 N5 1.382(5) . ? C20 C21 1.385(6) . ? C20 C25 1.396(6) . ? C21 C22 1.385(6) . ? C21 H21 0.85(4) . ? C22 C23 1.379(6) . ? C22 H22 0.84(4) . ? C23 O2 1.370(5) . ? C23 C24 1.388(6) . ? C24 C25 1.383(6) . ? C24 H24 1.05(4) . ? C25 H25 1.04(4) . ? C26 O2 1.434(6) . ? C26 H26A 1.04(5) . ? C26 H26B 1.02(5) . ? C26 H26C 0.97(5) . ? C27 C28 1.396(6) . ? C27 C32 1.399(6) . ? C28 C29 1.371(6) . ? C28 H28 0.86(4) . ? C29 C30 1.385(6) . ? C29 H29 0.92(4) . ? C30 O3 1.375(5) . ? C30 C31 1.385(6) . ? C31 C32 1.380(6) . ? C31 H31 0.92(3) . ? C32 H32 0.91(5) . ? C33 O3 1.427(6) . ? C33 H33A 1.01(4) . ? C33 H33B 1.15(5) . ? C33 H33C 0.97(4) . ? C34 C35 1.383(6) . ? C34 C39 1.401(6) . ? C35 C36 1.392(6) . ? C35 H35 1.02(4) . ? C36 C37 1.383(6) . ? C36 H36 0.90(4) . ? C37 O4 1.384(5) . ? C37 C38 1.393(6) . ? C38 C39 1.385(6) . ? C38 H38 1.03(5) . ? C39 H39 1.02(4) . ? C40 O4 1.456(6) . ? C40 H40A 1.03(4) . ? C40 H40B 1.09(6) . ? C40 H40C 1.16(5) . ? C41 C42 1.377(7) . ? C41 C43 1.382(7) 2_577 ? C41 H41 1.00(6) . ? C42 C43 1.373(7) . ? C42 H42 0.92(5) . ? C43 C41 1.382(7) 2_577 ? C43 H43 0.96(6) . ? C44 C45 1.371(7) . ? C44 C46 1.381(7) 2_767 ? C44 H44 0.88(4) . ? C45 C46 1.370(7) . ? C45 H45 1.03(4) . ? C46 C44 1.381(7) 2_767 ? C46 H46 0.82(5) . ? Fe N1 1.702(4) . ? Fe N5 1.878(4) . ? Fe N2 1.890(4) . ? Fe N4 1.900(4) . ? Fe N3 1.922(4) . ? N1 O1 1.076(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 N2 C1 C19 110.6(4) . . ? N2 C1 C2 109.1(4) . . ? C19 C1 C2 140.2(4) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 H2 128(2) . . ? C1 C2 H2 125(2) . . ? C2 C3 C4 109.1(5) . . ? C2 C3 H3 127(2) . . ? C4 C3 H3 124(2) . . ? C5 C4 N2 120.2(4) . . ? C5 C4 C3 132.0(5) . . ? N2 C4 C3 107.6(4) . . ? C4 C5 C6 122.2(4) . . ? C4 C5 C20 118.3(4) . . ? C6 C5 C20 119.4(4) . . ? N3 C6 C7 109.3(4) . . ? N3 C6 C5 124.5(4) . . ? C7 C6 C5 126.2(4) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 H7 121(3) . . ? C6 C7 H7 131(3) . . ? C7 C8 C9 107.7(4) . . ? C7 C8 H8 128.3(19) . . ? C9 C8 H8 123.8(19) . . ? N3 C9 C10 123.9(4) . . ? N3 C9 C8 109.1(4) . . ? C10 C9 C8 126.9(4) . . ? C11 C10 C9 123.8(4) . . ? C11 C10 C27 117.4(4) . . ? C9 C10 C27 118.8(4) . . ? C10 C11 N4 124.1(4) . . ? C10 C11 C12 127.6(4) . . ? N4 C11 C12 108.2(4) . . ? C13 C12 C11 108.4(5) . . ? C13 C12 H12 128(3) . . ? C11 C12 H12 124(3) . . ? C12 C13 C14 107.8(5) . . ? C12 C13 H13 133(2) . . ? C14 C13 H13 119(2) . . ? N4 C14 C15 125.0(4) . . ? N4 C14 C13 109.2(4) . . ? C15 C14 C13 125.6(4) . . ? C16 C15 C14 122.6(4) . . ? C16 C15 C34 118.2(4) . . ? C14 C15 C34 119.2(4) . . ? C15 C16 N5 119.1(4) . . ? C15 C16 C17 132.4(4) . . ? N5 C16 C17 108.3(4) . . ? C18 C17 C16 108.5(4) . . ? C18 C17 H17 124(2) . . ? C16 C17 H17 128(2) . . ? C17 C18 C19 106.1(4) . . ? C17 C18 H18 134(2) . . ? C19 C18 H18 120(2) . . ? N5 C19 C18 110.1(4) . . ? N5 C19 C1 111.2(4) . . ? C18 C19 C1 138.7(5) . . ? C21 C20 C25 117.8(4) . . ? C21 C20 C5 121.9(4) . . ? C25 C20 C5 120.0(4) . . ? C22 C21 C20 121.8(5) . . ? C22 C21 H21 118(3) . . ? C20 C21 H21 121(3) . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 121(3) . . ? O2 C23 C22 124.9(4) . . ? O2 C23 C24 114.4(4) . . ? C22 C23 C24 120.7(5) . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24 120(2) . . ? C23 C24 H24 121(2) . . ? C24 C25 C20 121.4(4) . . ? C24 C25 H25 119(2) . . ? C20 C25 H25 120(2) . . ? O2 C26 H26A 95(3) . . ? O2 C26 H26B 108(3) . . ? H26A C26 H26B 116(4) . . ? O2 C26 H26C 104(3) . . ? H26A C26 H26C 111(4) . . ? H26B C26 H26C 119(4) . . ? C28 C27 C32 117.4(4) . . ? C28 C27 C10 123.1(4) . . ? C32 C27 C10 119.5(4) . . ? C29 C28 C27 121.2(5) . . ? C29 C28 H28 125(3) . . ? C27 C28 H28 114(3) . . ? C28 C29 C30 120.5(5) . . ? C28 C29 H29 119(2) . . ? C30 C29 H29 120(2) . . ? O3 C30 C31 124.6(4) . . ? O3 C30 C29 115.8(4) . . ? C31 C30 C29 119.6(4) . . ? C32 C31 C30 119.6(5) . . ? C32 C31 H31 115(2) . . ? C30 C31 H31 125(2) . . ? C31 C32 C27 121.6(5) . . ? C31 C32 H32 120(3) . . ? C27 C32 H32 119(3) . . ? O3 C33 H33A 108(2) . . ? O3 C33 H33B 109(2) . . ? H33A C33 H33B 106(3) . . ? O3 C33 H33C 107(3) . . ? H33A C33 H33C 120(4) . . ? H33B C33 H33C 107(4) . . ? C35 C34 C39 117.9(4) . . ? C35 C34 C15 121.0(4) . . ? C39 C34 C15 121.2(4) . . ? C34 C35 C36 122.3(5) . . ? C34 C35 H35 123(2) . . ? C36 C35 H35 114(2) . . ? C37 C36 C35 118.4(5) . . ? C37 C36 H36 121(3) . . ? C35 C36 H36 121(3) . . ? C36 C37 O4 123.9(4) . . ? C36 C37 C38 121.1(5) . . ? O4 C37 C38 115.0(4) . . ? C39 C38 C37 119.2(5) . . ? C39 C38 H38 125(3) . . ? C37 C38 H38 116(3) . . ? C38 C39 C34 121.1(5) . . ? C38 C39 H39 120(2) . . ? C34 C39 H39 118(2) . . ? O4 C40 H40A 109(2) . . ? O4 C40 H40B 102(3) . . ? H40A C40 H40B 110(4) . . ? O4 C40 H40C 103(2) . . ? H40A C40 H40C 117(3) . . ? H40B C40 H40C 114(4) . . ? C42 C41 C43 119.2(6) . 2_577 ? C42 C41 H41 119(4) . . ? C43 C41 H41 121(4) 2_577 . ? C43 C42 C41 120.8(6) . . ? C43 C42 H42 124(3) . . ? C41 C42 H42 115(3) . . ? C42 C43 C41 120.0(6) . 2_577 ? C42 C43 H43 125(4) . . ? C41 C43 H43 115(4) 2_577 . ? C45 C44 C46 120.8(6) . 2_767 ? C45 C44 H44 120(3) . . ? C46 C44 H44 120(3) 2_767 . ? C46 C45 C44 120.1(5) . . ? C46 C45 H45 125(2) . . ? C44 C45 H45 114(2) . . ? C45 C46 C44 119.1(6) . 2_767 ? C45 C46 H46 125(4) . . ? C44 C46 H46 116(4) 2_767 . ? N1 Fe N5 104.46(16) . . ? N1 Fe N2 105.85(16) . . ? N5 Fe N2 79.42(16) . . ? N1 Fe N4 99.40(16) . . ? N5 Fe N4 87.71(16) . . ? N2 Fe N4 153.79(14) . . ? N1 Fe N3 105.29(16) . . ? N5 Fe N3 149.77(14) . . ? N2 Fe N3 87.45(15) . . ? N4 Fe N3 92.64(15) . . ? O1 N1 Fe 172.0(4) . . ? C1 N2 C4 107.5(4) . . ? C1 N2 Fe 118.4(3) . . ? C4 N2 Fe 133.7(3) . . ? C9 N3 C6 106.1(4) . . ? C9 N3 Fe 124.2(3) . . ? C6 N3 Fe 126.9(3) . . ? C11 N4 C14 106.3(4) . . ? C11 N4 Fe 125.7(3) . . ? C14 N4 Fe 126.8(3) . . ? C19 N5 C16 107.0(4) . . ? C19 N5 Fe 118.2(3) . . ? C16 N5 Fe 133.3(3) . . ? C23 O2 C26 117.8(4) . . ? C30 O3 C33 115.9(4) . . ? C37 O4 C40 117.1(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 N2 C1 C2 C3 -1.0(5) . . . . ? C19 C1 C2 C3 176.6(6) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C3 C4 C5 -172.9(5) . . . . ? C2 C3 C4 N2 1.6(5) . . . . ? N2 C4 C5 C6 -1.1(7) . . . . ? C3 C4 C5 C6 172.8(4) . . . . ? N2 C4 C5 C20 -177.6(4) . . . . ? C3 C4 C5 C20 -3.6(7) . . . . ? C4 C5 C6 N3 -0.8(7) . . . . ? C20 C5 C6 N3 175.6(4) . . . . ? C4 C5 C6 C7 177.5(4) . . . . ? C20 C5 C6 C7 -6.1(7) . . . . ? N3 C6 C7 C8 -0.2(5) . . . . ? C5 C6 C7 C8 -178.7(4) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C7 C8 C9 N3 0.0(5) . . . . ? C7 C8 C9 C10 -179.1(4) . . . . ? N3 C9 C10 C11 0.9(7) . . . . ? C8 C9 C10 C11 179.9(4) . . . . ? N3 C9 C10 C27 -178.2(4) . . . . ? C8 C9 C10 C27 0.7(7) . . . . ? C9 C10 C11 N4 2.8(7) . . . . ? C27 C10 C11 N4 -178.1(4) . . . . ? C9 C10 C11 C12 -173.0(4) . . . . ? C27 C10 C11 C12 6.2(7) . . . . ? C10 C11 C12 C13 178.3(4) . . . . ? N4 C11 C12 C13 2.0(5) . . . . ? C11 C12 C13 C14 -0.3(5) . . . . ? C12 C13 C14 N4 -1.6(5) . . . . ? C12 C13 C14 C15 -176.6(4) . . . . ? N4 C14 C15 C16 -2.9(7) . . . . ? C13 C14 C15 C16 171.4(4) . . . . ? N4 C14 C15 C34 175.3(4) . . . . ? C13 C14 C15 C34 -10.4(7) . . . . ? C14 C15 C16 N5 2.1(6) . . . . ? C34 C15 C16 N5 -176.1(4) . . . . ? C14 C15 C16 C17 -173.2(4) . . . . ? C34 C15 C16 C17 8.6(7) . . . . ? C15 C16 C17 C18 176.2(5) . . . . ? N5 C16 C17 C18 0.5(5) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 N5 -0.4(5) . . . . ? C17 C18 C19 C1 179.4(5) . . . . ? N2 C1 C19 N5 0.3(5) . . . . ? C2 C1 C19 N5 -177.3(5) . . . . ? N2 C1 C19 C18 -179.5(5) . . . . ? C2 C1 C19 C18 2.9(11) . . . . ? C4 C5 C20 C21 119.4(5) . . . . ? C6 C5 C20 C21 -57.1(6) . . . . ? C4 C5 C20 C25 -54.0(6) . . . . ? C6 C5 C20 C25 129.5(5) . . . . ? C25 C20 C21 C22 -0.2(7) . . . . ? C5 C20 C21 C22 -173.7(4) . . . . ? C20 C21 C22 C23 0.0(8) . . . . ? C21 C22 C23 O2 178.8(4) . . . . ? C21 C22 C23 C24 -0.5(7) . . . . ? O2 C23 C24 C25 -178.2(4) . . . . ? C22 C23 C24 C25 1.2(7) . . . . ? C23 C24 C25 C20 -1.4(7) . . . . ? C21 C20 C25 C24 0.9(7) . . . . ? C5 C20 C25 C24 174.5(4) . . . . ? C11 C10 C27 C28 -120.7(5) . . . . ? C9 C10 C27 C28 58.5(6) . . . . ? C11 C10 C27 C32 56.8(6) . . . . ? C9 C10 C27 C32 -124.1(5) . . . . ? C32 C27 C28 C29 -2.7(7) . . . . ? C10 C27 C28 C29 174.8(4) . . . . ? C27 C28 C29 C30 0.9(7) . . . . ? C28 C29 C30 O3 -178.5(4) . . . . ? C28 C29 C30 C31 1.3(7) . . . . ? O3 C30 C31 C32 178.3(4) . . . . ? C29 C30 C31 C32 -1.5(7) . . . . ? C30 C31 C32 C27 -0.4(7) . . . . ? C28 C27 C32 C31 2.5(7) . . . . ? C10 C27 C32 C31 -175.1(4) . . . . ? C16 C15 C34 C35 112.7(5) . . . . ? C14 C15 C34 C35 -65.5(6) . . . . ? C16 C15 C34 C39 -65.7(6) . . . . ? C14 C15 C34 C39 116.1(5) . . . . ? C39 C34 C35 C36 1.0(7) . . . . ? C15 C34 C35 C36 -177.4(4) . . . . ? C34 C35 C36 C37 -0.9(7) . . . . ? C35 C36 C37 O4 -177.6(4) . . . . ? C35 C36 C37 C38 -0.4(7) . . . . ? C36 C37 C38 C39 1.4(7) . . . . ? O4 C37 C38 C39 178.9(4) . . . . ? C37 C38 C39 C34 -1.3(7) . . . . ? C35 C34 C39 C38 0.1(7) . . . . ? C15 C34 C39 C38 178.5(4) . . . . ? C43 C41 C42 C43 -0.5(9) 2_577 . . . ? C41 C42 C43 C41 0.5(9) . . . 2_577 ? C46 C44 C45 C46 -0.6(9) 2_767 . . . ? C44 C45 C46 C44 0.6(9) . . . 2_767 ? N5 Fe N1 O1 -38(3) . . . . ? N2 Fe N1 O1 -121(3) . . . . ? N4 Fe N1 O1 52(3) . . . . ? N3 Fe N1 O1 147(3) . . . . ? C19 C1 N2 C4 -176.4(4) . . . . ? C2 C1 N2 C4 2.0(5) . . . . ? C19 C1 N2 Fe 10.6(5) . . . . ? C2 C1 N2 Fe -171.1(3) . . . . ? C5 C4 N2 C1 173.1(4) . . . . ? C3 C4 N2 C1 -2.2(5) . . . . ? C5 C4 N2 Fe -15.4(6) . . . . ? C3 C4 N2 Fe 169.3(3) . . . . ? N1 Fe N2 C1 89.0(3) . . . . ? N5 Fe N2 C1 -13.2(3) . . . . ? N4 Fe N2 C1 -75.0(5) . . . . ? N3 Fe N2 C1 -165.8(3) . . . . ? N1 Fe N2 C4 -81.8(4) . . . . ? N5 Fe N2 C4 176.0(4) . . . . ? N4 Fe N2 C4 114.2(4) . . . . ? N3 Fe N2 C4 23.4(4) . . . . ? C10 C9 N3 C6 179.0(4) . . . . ? C8 C9 N3 C6 -0.1(5) . . . . ? C10 C9 N3 Fe -19.1(6) . . . . ? C8 C9 N3 Fe 161.7(3) . . . . ? C7 C6 N3 C9 0.2(5) . . . . ? C5 C6 N3 C9 178.7(4) . . . . ? C7 C6 N3 Fe -161.0(3) . . . . ? C5 C6 N3 Fe 17.5(6) . . . . ? N1 Fe N3 C9 -75.2(3) . . . . ? N5 Fe N3 C9 115.3(4) . . . . ? N2 Fe N3 C9 179.1(3) . . . . ? N4 Fe N3 C9 25.3(3) . . . . ? N1 Fe N3 C6 82.9(4) . . . . ? N5 Fe N3 C6 -86.7(5) . . . . ? N2 Fe N3 C6 -22.9(3) . . . . ? N4 Fe N3 C6 -176.6(3) . . . . ? C10 C11 N4 C14 -179.4(4) . . . . ? C12 C11 N4 C14 -2.9(5) . . . . ? C10 C11 N4 Fe 12.5(6) . . . . ? C12 C11 N4 Fe -171.0(3) . . . . ? C15 C14 N4 C11 177.9(4) . . . . ? C13 C14 N4 C11 2.8(5) . . . . ? C15 C14 N4 Fe -14.2(6) . . . . ? C13 C14 N4 Fe 170.7(3) . . . . ? N1 Fe N4 C11 83.6(3) . . . . ? N5 Fe N4 C11 -172.1(3) . . . . ? N2 Fe N4 C11 -111.9(4) . . . . ? N3 Fe N4 C11 -22.4(3) . . . . ? N1 Fe N4 C14 -82.0(4) . . . . ? N5 Fe N4 C14 22.3(3) . . . . ? N2 Fe N4 C14 82.4(5) . . . . ? N3 Fe N4 C14 172.0(3) . . . . ? C18 C19 N5 C16 0.7(5) . . . . ? C1 C19 N5 C16 -179.1(4) . . . . ? C18 C19 N5 Fe 168.7(3) . . . . ? C1 C19 N5 Fe -11.1(5) . . . . ? C15 C16 N5 C19 -177.1(4) . . . . ? C17 C16 N5 C19 -0.7(5) . . . . ? C15 C16 N5 Fe 17.5(6) . . . . ? C17 C16 N5 Fe -166.2(3) . . . . ? N1 Fe N5 C19 -90.5(3) . . . . ? N2 Fe N5 C19 13.3(3) . . . . ? N4 Fe N5 C19 170.3(3) . . . . ? N3 Fe N5 C19 79.0(4) . . . . ? N1 Fe N5 C16 73.6(4) . . . . ? N2 Fe N5 C16 177.4(4) . . . . ? N4 Fe N5 C16 -25.5(4) . . . . ? N3 Fe N5 C16 -116.8(4) . . . . ? C22 C23 O2 C26 -5.6(7) . . . . ? C24 C23 O2 C26 173.7(5) . . . . ? C31 C30 O3 C33 0.6(6) . . . . ? C29 C30 O3 C33 -179.6(4) . . . . ? C36 C37 O4 C40 0.5(6) . . . . ? C38 C37 O4 C40 -176.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.781 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.090 #===END