data_febco3-155k-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraphenylphosphonium salt of fac{tris[benzoylcyanoximato{Iron(II)]} ; _chemical_name_common 'tris[benzoylcyanoximato]iron(II)}, PPh4 salt' _chemical_melting_point 'oxidizes upon heating on air up to 100 C' _chemical_formula_moiety 'C27 H15 Fe N6 O6, C24 H20 P' _chemical_formula_sum 'C51 H35 Fe N6 O6 P' _chemical_compound_source 'synthesized new Fe(II) complex' _chemical_formula_weight 914.67 _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. ; _publ_contact_author_name 'Prof. Nikolay Gerasimchuk' _publ_contact_author_address ; Department of Chemistry, Temple Hall 456, Missouri State University, Springfield, MO 65897, USA. ; _publ_contact_author_phone '1 417 836 5165' _publ_contact_author_fax '1 417 836 5507' _publ_contact_author_email 'NNGerasimchuk@missouristate.edu' 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2043(12) _cell_length_b 25.991(3) _cell_length_c 13.8507(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.4370(10) _cell_angle_gamma 90.00 _cell_volume 4389.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 155(2) _cell_measurement_reflns_used 317 _cell_measurement_theta_min 2.182 _cell_measurement_theta_max 27.021 _exptl_crystal_description plate _exptl_crystal_colour blue-purple _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.9370 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2005)' _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G.M. (2003). SADABS. Version 2.10. University of Gottingen, Germany) ; _diffrn_ambient_temperature 155(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 45003 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9000 _reflns_number_gt 7255 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0308P)^2^+2.2454P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9000 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.40919(13) 0.06357(7) 0.22807(12) 0.0233(4) Uani 1 1 d . . . C2 C 0.32947(14) 0.09082(7) 0.17051(13) 0.0269(4) Uani 1 1 d . . . C3 C 0.39532(13) 0.01546(6) 0.27479(12) 0.0231(4) Uani 1 1 d . . . C4 C 0.30010(13) -0.01890(6) 0.25904(12) 0.0233(4) Uani 1 1 d . . . C5 C 0.28020(15) -0.05520(7) 0.32991(13) 0.0292(4) Uani 1 1 d . . . H5 H 0.3253 -0.0563 0.3875 0.035 Uiso 1 1 calc R . . C6 C 0.19448(16) -0.08986(7) 0.31660(15) 0.0343(4) Uani 1 1 d . . . H6 H 0.1815 -0.1149 0.3648 0.041 Uiso 1 1 calc R . . C7 C 0.12797(15) -0.08813(7) 0.23339(15) 0.0351(4) Uani 1 1 d . . . H7 H 0.0694 -0.1120 0.2245 0.042 Uiso 1 1 calc R . . C8 C 0.14642(16) -0.05185(8) 0.16316(15) 0.0356(5) Uani 1 1 d . . . H8 H 0.0999 -0.0505 0.1065 0.043 Uiso 1 1 calc R . . C9 C 0.23264(15) -0.01729(7) 0.17500(14) 0.0298(4) Uani 1 1 d . . . H9 H 0.2457 0.0074 0.1262 0.036 Uiso 1 1 calc R . . C10 C 0.67754(14) 0.13594(6) 0.43621(12) 0.0232(4) Uani 1 1 d . . . C11 C 0.75892(15) 0.17342(7) 0.46198(12) 0.0264(4) Uani 1 1 d . . . C12 C 0.57650(14) 0.12642(7) 0.47963(12) 0.0237(4) Uani 1 1 d . . . C13 C 0.53225(14) 0.15696(7) 0.55883(13) 0.0271(4) Uani 1 1 d . . . C14 C 0.45876(16) 0.13271(8) 0.61874(14) 0.0357(4) Uani 1 1 d . . . H14 H 0.4399 0.0976 0.6083 0.043 Uiso 1 1 calc R . . C15 C 0.41362(18) 0.15979(9) 0.69308(15) 0.0454(5) Uani 1 1 d . . . H15 H 0.3629 0.1434 0.7332 0.054 Uiso 1 1 calc R . . C16 C 0.44204(18) 0.21065(9) 0.70931(15) 0.0449(5) Uani 1 1 d . . . H16 H 0.4122 0.2288 0.7616 0.054 Uiso 1 1 calc R . . C17 C 0.51340(18) 0.23518(8) 0.65010(15) 0.0411(5) Uani 1 1 d . . . H17 H 0.5317 0.2703 0.6610 0.049 Uiso 1 1 calc R . . C18 C 0.55864(16) 0.20853(7) 0.57434(14) 0.0335(4) Uani 1 1 d . . . H18 H 0.6075 0.2255 0.5332 0.040 Uiso 1 1 calc R . . C19 C 0.75008(13) -0.01947(6) 0.30162(12) 0.0233(4) Uani 1 1 d . . . C20 C 0.81630(14) -0.05050(7) 0.24282(13) 0.0254(4) Uani 1 1 d . . . C21 C 0.74557(13) -0.02023(6) 0.40369(13) 0.0236(4) Uani 1 1 d . . . C22 C 0.81988(14) -0.05057(6) 0.46868(12) 0.0244(4) Uani 1 1 d . . . C23 C 0.77698(15) -0.07289(7) 0.55046(14) 0.0318(4) Uani 1 1 d . . . H23 H 0.7009 -0.0701 0.5615 0.038 Uiso 1 1 calc R . . C24 C 0.84595(16) -0.09916(8) 0.61574(14) 0.0371(5) Uani 1 1 d . . . H24 H 0.8166 -0.1151 0.6707 0.045 Uiso 1 1 calc R . . C25 C 0.95730(16) -0.10214(8) 0.60109(14) 0.0348(4) Uani 1 1 d . . . H25 H 1.0044 -0.1198 0.6463 0.042 Uiso 1 1 calc R . . C26 C 0.99981(15) -0.07938(7) 0.52054(14) 0.0321(4) Uani 1 1 d . . . H26 H 1.0764 -0.0811 0.5111 0.039 Uiso 1 1 calc R . . C27 C 0.93147(14) -0.05403(7) 0.45330(13) 0.0275(4) Uani 1 1 d . . . H27 H 0.9608 -0.0392 0.3973 0.033 Uiso 1 1 calc R . . C28 C 0.67655(14) 0.23783(7) 0.09984(13) 0.0255(4) Uani 1 1 d . . . C29 C 0.62442(16) 0.28489(7) 0.07984(14) 0.0330(4) Uani 1 1 d . . . H29 H 0.6101 0.2953 0.0148 0.040 Uiso 1 1 calc R . . C30 C 0.59390(17) 0.31610(7) 0.15447(15) 0.0380(5) Uani 1 1 d . . . H30 H 0.5585 0.3480 0.1407 0.046 Uiso 1 1 calc R . . C31 C 0.61454(17) 0.30118(8) 0.24931(15) 0.0369(5) Uani 1 1 d . . . H31 H 0.5939 0.3229 0.3006 0.044 Uiso 1 1 calc R . . C32 C 0.66515(17) 0.25466(8) 0.26924(14) 0.0361(5) Uani 1 1 d . . . H32 H 0.6785 0.2444 0.3345 0.043 Uiso 1 1 calc R . . C33 C 0.69655(15) 0.22295(7) 0.19543(13) 0.0293(4) Uani 1 1 d . . . H33 H 0.7317 0.1911 0.2099 0.035 Uiso 1 1 calc R . . C34 C 0.75278(14) 0.23236(7) -0.09774(13) 0.0254(4) Uani 1 1 d . . . C35 C 0.74083(15) 0.21163(7) -0.18997(13) 0.0316(4) Uani 1 1 d . . . H35 H 0.6972 0.1818 -0.2012 0.038 Uiso 1 1 calc R . . C36 C 0.79318(17) 0.23488(8) -0.26557(14) 0.0374(5) Uani 1 1 d . . . H36 H 0.7857 0.2206 -0.3287 0.045 Uiso 1 1 calc R . . C37 C 0.85579(16) 0.27836(8) -0.24992(14) 0.0356(4) Uani 1 1 d . . . H37 H 0.8921 0.2937 -0.3020 0.043 Uiso 1 1 calc R . . C38 C 0.86587(17) 0.29970(8) -0.15855(14) 0.0360(4) Uani 1 1 d . . . H38 H 0.9078 0.3302 -0.1483 0.043 Uiso 1 1 calc R . . C39 C 0.81523(15) 0.27690(7) -0.08205(14) 0.0319(4) Uani 1 1 d . . . H39 H 0.8228 0.2914 -0.0192 0.038 Uiso 1 1 calc R . . C40 C 0.81973(14) 0.15308(7) 0.03644(12) 0.0243(4) Uani 1 1 d . . . C41 C 0.80390(15) 0.11223(7) 0.09925(14) 0.0315(4) Uani 1 1 d . . . H41 H 0.7335 0.1061 0.1235 0.038 Uiso 1 1 calc R . . C42 C 0.89149(17) 0.08055(8) 0.12624(15) 0.0371(5) Uani 1 1 d . . . H42 H 0.8808 0.0525 0.1689 0.045 Uiso 1 1 calc R . . C43 C 0.99388(16) 0.08950(8) 0.09155(15) 0.0356(4) Uani 1 1 d . . . H43 H 1.0536 0.0679 0.1112 0.043 Uiso 1 1 calc R . . C44 C 1.01025(15) 0.12964(8) 0.02835(14) 0.0351(4) Uani 1 1 d . . . H44 H 1.0809 0.1354 0.0041 0.042 Uiso 1 1 calc R . . C45 C 0.92380(14) 0.16150(7) 0.00034(13) 0.0296(4) Uani 1 1 d . . . H45 H 0.9350 0.1890 -0.0433 0.035 Uiso 1 1 calc R . . C46 C 0.58823(14) 0.15863(7) -0.02968(13) 0.0270(4) Uani 1 1 d . . . C47 C 0.48553(15) 0.18197(8) -0.02662(13) 0.0302(4) Uani 1 1 d . . . H47 H 0.4797 0.2172 -0.0094 0.036 Uiso 1 1 calc R . . C48 C 0.39241(16) 0.15345(9) -0.04883(14) 0.0379(5) Uani 1 1 d . . . H48 H 0.3223 0.1692 -0.0469 0.045 Uiso 1 1 calc R . . C49 C 0.40057(17) 0.10221(9) -0.07376(15) 0.0417(5) Uani 1 1 d . . . H49 H 0.3359 0.0827 -0.0876 0.050 Uiso 1 1 calc R . . C50 C 0.50141(18) 0.07921(9) -0.07866(17) 0.0474(6) Uani 1 1 d . . . H50 H 0.5065 0.0441 -0.0968 0.057 Uiso 1 1 calc R . . C51 C 0.59611(17) 0.10737(8) -0.05715(16) 0.0413(5) Uani 1 1 d . . . H51 H 0.6660 0.0916 -0.0612 0.050 Uiso 1 1 calc R . . Fe1 Fe 0.592684(19) 0.050230(9) 0.345409(17) 0.02148(7) Uani 1 1 d . . . N1 N 0.50914(11) 0.08596(5) 0.25087(10) 0.0224(3) Uani 1 1 d . . . N2 N 0.26322(13) 0.11356(7) 0.12750(13) 0.0383(4) Uani 1 1 d . . . N3 N 0.69881(11) 0.10126(5) 0.36355(10) 0.0226(3) Uani 1 1 d . . . N4 N 0.82546(14) 0.20288(7) 0.48176(12) 0.0390(4) Uani 1 1 d . . . N5 N 0.67353(11) 0.01312(5) 0.25817(10) 0.0225(3) Uani 1 1 d . . . N6 N 0.86636(13) -0.07521(7) 0.19237(12) 0.0363(4) Uani 1 1 d . . . O1 O 0.53281(10) 0.12788(5) 0.21230(9) 0.0291(3) Uani 1 1 d . . . O2 O 0.47168(9) 0.00144(4) 0.33422(8) 0.0244(3) Uani 1 1 d . . . O3 O 0.78679(9) 0.10562(5) 0.32105(9) 0.0298(3) Uani 1 1 d . . . O4 O 0.52189(9) 0.08788(4) 0.44836(8) 0.0245(3) Uani 1 1 d . . . O5 O 0.66447(10) 0.01475(5) 0.16783(8) 0.0279(3) Uani 1 1 d . . . O6 O 0.67184(9) 0.00694(5) 0.44091(8) 0.0248(3) Uani 1 1 d . . . P1 P 0.70845(4) 0.195522(17) 0.00254(3) 0.02360(10) 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 0.0197(8) 0.0249(9) 0.0250(9) 0.0005(7) -0.0017(7) 0.0003(7) C2 0.0245(9) 0.0266(9) 0.0294(9) 0.0027(8) 0.0003(7) -0.0047(7) C3 0.0216(8) 0.0235(9) 0.0241(9) -0.0015(7) -0.0011(7) 0.0022(7) C4 0.0203(8) 0.0225(9) 0.0271(9) -0.0027(7) -0.0001(7) 0.0004(7) C5 0.0291(9) 0.0292(10) 0.0289(10) 0.0007(8) -0.0025(7) -0.0021(8) C6 0.0347(11) 0.0302(10) 0.0382(11) 0.0025(9) 0.0037(8) -0.0067(8) C7 0.0249(10) 0.0307(10) 0.0495(12) -0.0058(9) 0.0006(8) -0.0056(8) C8 0.0294(10) 0.0351(11) 0.0411(11) -0.0037(9) -0.0111(8) -0.0019(8) C9 0.0300(10) 0.0278(10) 0.0311(10) 0.0014(8) -0.0054(8) -0.0021(8) C10 0.0244(9) 0.0219(9) 0.0227(9) -0.0008(7) -0.0045(7) 0.0002(7) C11 0.0292(9) 0.0267(9) 0.0229(9) 0.0006(7) -0.0014(7) 0.0002(8) C12 0.0251(9) 0.0225(9) 0.0231(9) 0.0033(7) -0.0043(7) 0.0042(7) C13 0.0254(9) 0.0306(10) 0.0249(9) 0.0006(8) -0.0039(7) 0.0071(7) C14 0.0373(11) 0.0394(11) 0.0306(10) 0.0019(9) 0.0036(8) 0.0047(9) C15 0.0443(13) 0.0585(15) 0.0340(11) 0.0049(11) 0.0108(9) 0.0119(11) C16 0.0477(13) 0.0593(15) 0.0276(11) -0.0079(10) -0.0013(9) 0.0216(11) C17 0.0485(13) 0.0370(11) 0.0368(11) -0.0091(9) -0.0095(9) 0.0152(10) C18 0.0360(10) 0.0334(10) 0.0309(10) -0.0029(8) -0.0021(8) 0.0061(8) C19 0.0209(8) 0.0224(9) 0.0263(9) -0.0010(7) -0.0018(7) 0.0013(7) C20 0.0230(9) 0.0259(9) 0.0267(9) 0.0021(8) -0.0049(7) -0.0002(7) C21 0.0216(8) 0.0202(8) 0.0287(9) -0.0004(7) -0.0024(7) -0.0019(7) C22 0.0254(9) 0.0223(9) 0.0251(9) -0.0016(7) -0.0029(7) 0.0014(7) C23 0.0269(10) 0.0374(11) 0.0311(10) 0.0015(8) 0.0000(8) 0.0042(8) C24 0.0386(11) 0.0430(12) 0.0294(10) 0.0079(9) -0.0010(8) 0.0040(9) C25 0.0348(11) 0.0359(11) 0.0326(10) 0.0031(9) -0.0100(8) 0.0082(9) C26 0.0234(9) 0.0360(11) 0.0362(11) -0.0037(9) -0.0055(8) 0.0043(8) C27 0.0256(9) 0.0281(9) 0.0284(9) -0.0015(8) -0.0023(7) -0.0010(7) C28 0.0240(9) 0.0232(9) 0.0292(9) -0.0009(7) -0.0007(7) -0.0019(7) C29 0.0395(11) 0.0296(10) 0.0297(10) 0.0039(8) -0.0021(8) 0.0048(8) C30 0.0483(12) 0.0250(10) 0.0406(12) 0.0011(9) 0.0031(9) 0.0100(9) C31 0.0473(12) 0.0291(10) 0.0346(11) -0.0038(9) 0.0072(9) 0.0031(9) C32 0.0468(12) 0.0324(10) 0.0291(10) 0.0020(8) 0.0031(9) 0.0025(9) C33 0.0328(10) 0.0226(9) 0.0325(10) 0.0025(8) -0.0001(8) 0.0005(7) C34 0.0240(9) 0.0249(9) 0.0270(9) 0.0014(7) -0.0025(7) 0.0025(7) C35 0.0332(10) 0.0293(10) 0.0319(10) -0.0010(8) -0.0043(8) -0.0024(8) C36 0.0452(12) 0.0401(11) 0.0266(10) -0.0030(9) -0.0035(9) -0.0013(9) C37 0.0384(11) 0.0386(11) 0.0299(10) 0.0065(9) 0.0021(8) 0.0005(9) C38 0.0404(11) 0.0310(10) 0.0363(11) 0.0023(9) -0.0008(9) -0.0084(9) C39 0.0361(10) 0.0293(10) 0.0299(10) -0.0002(8) -0.0030(8) -0.0054(8) C40 0.0240(9) 0.0220(9) 0.0267(9) -0.0020(7) -0.0023(7) 0.0008(7) C41 0.0303(10) 0.0287(10) 0.0359(11) 0.0035(8) 0.0054(8) 0.0017(8) C42 0.0402(11) 0.0323(11) 0.0390(11) 0.0084(9) 0.0038(9) 0.0065(9) C43 0.0292(10) 0.0373(11) 0.0397(11) 0.0015(9) -0.0039(8) 0.0088(8) C44 0.0250(10) 0.0409(11) 0.0395(11) 0.0001(9) 0.0012(8) -0.0001(8) C45 0.0273(9) 0.0308(10) 0.0304(10) 0.0019(8) -0.0002(7) -0.0017(8) C46 0.0248(9) 0.0285(9) 0.0276(9) -0.0030(8) -0.0002(7) -0.0048(7) C47 0.0271(9) 0.0338(10) 0.0293(10) 0.0031(8) -0.0010(7) 0.0011(8) C48 0.0258(10) 0.0536(13) 0.0339(11) 0.0032(10) -0.0018(8) -0.0021(9) C49 0.0328(11) 0.0571(14) 0.0347(11) -0.0037(10) -0.0037(9) -0.0179(10) C50 0.0414(12) 0.0414(13) 0.0592(15) -0.0166(11) -0.0013(11) -0.0122(10) C51 0.0293(10) 0.0356(11) 0.0588(14) -0.0148(10) -0.0009(9) -0.0024(9) Fe1 0.01902(12) 0.02108(13) 0.02401(13) -0.00038(10) -0.00288(9) 0.00065(10) N1 0.0210(7) 0.0212(7) 0.0248(7) -0.0002(6) 0.0007(6) 0.0006(6) N2 0.0285(9) 0.0406(10) 0.0448(10) 0.0146(8) -0.0077(7) -0.0010(7) N3 0.0210(7) 0.0247(7) 0.0219(7) 0.0015(6) -0.0029(6) 0.0024(6) N4 0.0403(10) 0.0360(9) 0.0401(10) -0.0043(8) -0.0038(8) -0.0105(8) N5 0.0221(7) 0.0205(7) 0.0246(8) 0.0000(6) -0.0035(6) -0.0034(6) N6 0.0347(9) 0.0396(10) 0.0345(9) -0.0046(8) -0.0015(7) 0.0081(8) O1 0.0273(7) 0.0226(6) 0.0373(7) 0.0079(6) -0.0017(5) -0.0026(5) O2 0.0225(6) 0.0224(6) 0.0278(6) 0.0029(5) -0.0039(5) 0.0000(5) O3 0.0209(6) 0.0378(7) 0.0311(7) -0.0036(6) 0.0041(5) -0.0046(5) O4 0.0222(6) 0.0245(6) 0.0266(6) 0.0006(5) -0.0009(5) 0.0009(5) O5 0.0327(7) 0.0298(7) 0.0206(6) -0.0011(5) -0.0047(5) 0.0006(5) O6 0.0222(6) 0.0267(6) 0.0253(6) -0.0004(5) -0.0019(5) 0.0033(5) P1 0.0222(2) 0.0217(2) 0.0266(2) -0.00081(18) -0.00194(17) -0.00044(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 N1 1.376(2) . yes C1 C2 1.420(2) . yes C1 C3 1.421(2) . yes C2 N2 1.148(2) . yes C3 O2 1.2703(19) . yes C3 C4 1.475(2) . yes C4 C5 1.390(2) . yes C4 C9 1.398(2) . yes C5 C6 1.387(3) . yes C5 H5 0.9500 . no C6 C7 1.382(3) . yes C6 H6 0.9500 . no C7 C8 1.380(3) . yes C7 H7 0.9500 . no C8 C9 1.388(3) . yes C8 H8 0.9500 . no C9 H9 0.9500 . no C10 N3 1.384(2) . yes C10 C12 1.417(2) . yes C10 C11 1.426(2) . yes C11 N4 1.141(2) . yes C12 O4 1.269(2) . yes C12 C13 1.475(2) . yes C13 C18 1.393(3) . yes C13 C14 1.398(3) . yes C14 C15 1.381(3) . yes C14 H14 0.9500 . no C15 C16 1.382(3) . yes C15 H15 0.9500 . no C16 C17 1.378(3) . yes C16 H16 0.9500 . no C17 C18 1.391(3) . yes C17 H17 0.9500 . no C18 H18 0.9500 . no C19 N5 1.380(2) . yes C19 C21 1.417(2) . yes C19 C20 1.422(2) . yes C20 N6 1.145(2) . yes C21 O6 1.270(2) . yes C21 C22 1.478(2) . yes C22 C27 1.390(2) . yes C22 C23 1.394(3) . yes C23 C24 1.388(3) . yes C23 H23 0.9500 . no C24 C25 1.385(3) . yes C24 H24 0.9500 . no C25 C26 1.383(3) . yes C25 H25 0.9500 . no C26 C27 1.390(2) . yes C26 H26 0.9500 . no C27 H27 0.9500 . no C28 C33 1.391(3) . yes C28 C29 1.401(2) . yes C28 P1 1.7949(18) . yes C29 C30 1.378(3) . yes C29 H29 0.9500 . no C30 C31 1.382(3) . yes C30 H30 0.9500 . no C31 C32 1.380(3) . yes C31 H31 0.9500 . no C32 C33 1.380(3) . yes C32 H32 0.9500 . no C33 H33 0.9500 . no C34 C35 1.388(3) . yes C34 C39 1.398(2) . yes C34 P1 1.7896(18) . yes C35 C36 1.388(3) . yes C35 H35 0.9500 . no C36 C37 1.376(3) . yes C36 H36 0.9500 . no C37 C38 1.383(3) . yes C37 H37 0.9500 . no C38 C39 1.383(3) . yes C38 H38 0.9500 . no C39 H39 0.9500 . no C40 C41 1.391(3) . yes C40 C45 1.402(2) . yes C40 P1 1.7966(17) . yes C41 C42 1.388(3) . yes C41 H41 0.9500 . no C42 C43 1.378(3) . yes C42 H42 0.9500 . no C43 C44 1.382(3) . yes C43 H43 0.9500 . no C44 C45 1.384(3) . yes C44 H44 0.9500 . no C45 H45 0.9500 . no C46 C51 1.390(3) . yes C46 C47 1.395(2) . yes C46 P1 1.7931(18) . yes C47 C48 1.381(3) . yes C47 H47 0.9500 . no C48 C49 1.380(3) . yes C48 H48 0.9500 . no C49 C50 1.372(3) . yes C49 H49 0.9500 . no C50 C51 1.390(3) . yes C50 H50 0.9500 . no C51 H51 0.9500 . no Fe1 N5 1.8615(14) . yes Fe1 N3 1.8634(14) . yes Fe1 N1 1.8716(14) . yes Fe1 O2 1.9477(12) . yes Fe1 O6 1.9596(12) . yes Fe1 O4 1.9602(12) . yes N1 O1 1.2528(18) . yes N3 O3 1.2514(18) . yes N5 O5 1.2522(18) . yes 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 C2 119.83(15) . . yes N1 C1 C3 112.90(14) . . yes C2 C1 C3 127.02(15) . . yes N2 C2 C1 177.1(2) . . yes O2 C3 C1 116.69(15) . . yes O2 C3 C4 118.29(15) . . yes C1 C3 C4 125.02(15) . . yes C5 C4 C9 119.60(16) . . yes C5 C4 C3 117.83(15) . . yes C9 C4 C3 122.53(16) . . yes C6 C5 C4 120.02(17) . . yes C6 C5 H5 120.0 . . no C4 C5 H5 120.0 . . no C7 C6 C5 120.18(18) . . yes C7 C6 H6 119.9 . . no C5 C6 H6 119.9 . . no C8 C7 C6 120.16(18) . . yes C8 C7 H7 119.9 . . no C6 C7 H7 119.9 . . no C7 C8 C9 120.30(18) . . yes C7 C8 H8 119.9 . . no C9 C8 H8 119.9 . . no C8 C9 C4 119.73(17) . . yes C8 C9 H9 120.1 . . no C4 C9 H9 120.1 . . no N3 C10 C12 112.87(15) . . yes N3 C10 C11 118.48(15) . . yes C12 C10 C11 128.52(16) . . yes N4 C11 C10 178.7(2) . . yes O4 C12 C10 116.55(15) . . yes O4 C12 C13 118.36(15) . . yes C10 C12 C13 125.08(16) . . yes C18 C13 C14 119.50(18) . . yes C18 C13 C12 122.88(17) . . yes C14 C13 C12 117.60(17) . . yes C15 C14 C13 119.9(2) . . yes C15 C14 H14 120.0 . . no C13 C14 H14 120.0 . . no C14 C15 C16 120.2(2) . . yes C14 C15 H15 119.9 . . no C16 C15 H15 119.9 . . no C17 C16 C15 120.4(2) . . yes C17 C16 H16 119.8 . . no C15 C16 H16 119.8 . . no C16 C17 C18 120.0(2) . . yes C16 C17 H17 120.0 . . no C18 C17 H17 120.0 . . no C17 C18 C13 119.91(19) . . yes C17 C18 H18 120.0 . . no C13 C18 H18 120.0 . . no N5 C19 C21 112.90(15) . . yes N5 C19 C20 119.27(15) . . yes C21 C19 C20 127.62(16) . . yes N6 C20 C19 177.10(19) . . yes O6 C21 C19 117.09(15) . . yes O6 C21 C22 118.44(15) . . yes C19 C21 C22 124.47(15) . . yes C27 C22 C23 120.11(16) . . yes C27 C22 C21 121.39(16) . . yes C23 C22 C21 118.34(16) . . yes C24 C23 C22 119.70(17) . . yes C24 C23 H23 120.2 . . no C22 C23 H23 120.2 . . no C25 C24 C23 120.25(19) . . yes C25 C24 H24 119.9 . . no C23 C24 H24 119.9 . . no C26 C25 C24 119.90(17) . . yes C26 C25 H25 120.1 . . no C24 C25 H25 120.1 . . no C25 C26 C27 120.55(17) . . yes C25 C26 H26 119.7 . . no C27 C26 H26 119.7 . . no C26 C27 C22 119.47(17) . . yes C26 C27 H27 120.3 . . no C22 C27 H27 120.3 . . no C33 C28 C29 119.40(17) . . yes C33 C28 P1 120.63(13) . . yes C29 C28 P1 119.84(14) . . yes C30 C29 C28 120.05(18) . . yes C30 C29 H29 120.0 . . no C28 C29 H29 120.0 . . no C29 C30 C31 120.24(18) . . yes C29 C30 H30 119.9 . . no C31 C30 H30 119.9 . . no C32 C31 C30 119.84(19) . . yes C32 C31 H31 120.1 . . no C30 C31 H31 120.1 . . no C33 C32 C31 120.74(18) . . yes C33 C32 H32 119.6 . . no C31 C32 H32 119.6 . . no C32 C33 C28 119.74(17) . . yes C32 C33 H33 120.1 . . no C28 C33 H33 120.1 . . no C35 C34 C39 119.97(17) . . yes C35 C34 P1 118.89(14) . . yes C39 C34 P1 120.21(14) . . yes C36 C35 C34 119.45(18) . . yes C36 C35 H35 120.3 . . no C34 C35 H35 120.3 . . no C37 C36 C35 120.59(18) . . yes C37 C36 H36 119.7 . . no C35 C36 H36 119.7 . . no C36 C37 C38 120.07(19) . . yes C36 C37 H37 120.0 . . no C38 C37 H37 120.0 . . no C37 C38 C39 120.28(18) . . yes C37 C38 H38 119.9 . . no C39 C38 H38 119.9 . . no C38 C39 C34 119.62(18) . . yes C38 C39 H39 120.2 . . no C34 C39 H39 120.2 . . no C41 C40 C45 119.61(16) . . yes C41 C40 P1 120.56(14) . . yes C45 C40 P1 119.82(13) . . yes C42 C41 C40 119.69(17) . . yes C42 C41 H41 120.2 . . no C40 C41 H41 120.2 . . no C43 C42 C41 120.36(18) . . yes C43 C42 H42 119.8 . . no C41 C42 H42 119.8 . . no C42 C43 C44 120.41(18) . . yes C42 C43 H43 119.8 . . no C44 C43 H43 119.8 . . no C43 C44 C45 120.02(18) . . yes C43 C44 H44 120.0 . . no C45 C44 H44 120.0 . . no C44 C45 C40 119.89(17) . . yes C44 C45 H45 120.1 . . no C40 C45 H45 120.1 . . no C51 C46 C47 119.86(17) . . yes C51 C46 P1 121.01(14) . . yes C47 C46 P1 119.12(14) . . yes C48 C47 C46 119.47(18) . . yes C48 C47 H47 120.3 . . no C46 C47 H47 120.3 . . no C49 C48 C47 120.42(19) . . yes C49 C48 H48 119.8 . . no C47 C48 H48 119.8 . . no C50 C49 C48 120.45(19) . . yes C50 C49 H49 119.8 . . no C48 C49 H49 119.8 . . no C49 C50 C51 120.0(2) . . yes C49 C50 H50 120.0 . . no C51 C50 H50 120.0 . . no C50 C51 C46 119.79(19) . . yes C50 C51 H51 120.1 . . no C46 C51 H51 120.1 . . no N5 Fe1 N3 94.11(6) . . yes N5 Fe1 N1 95.22(6) . . yes N3 Fe1 N1 95.51(6) . . yes N5 Fe1 O2 91.84(5) . . yes N3 Fe1 O2 173.98(6) . . yes N1 Fe1 O2 83.03(5) . . yes N5 Fe1 O6 83.16(6) . . yes N3 Fe1 O6 89.87(5) . . yes N1 Fe1 O6 174.48(6) . . yes O2 Fe1 O6 91.73(5) . . yes N5 Fe1 O4 173.25(5) . . yes N3 Fe1 O4 82.64(6) . . yes N1 Fe1 O4 91.00(6) . . yes O2 Fe1 O4 91.53(5) . . yes O6 Fe1 O4 90.88(5) . . yes O1 N1 C1 119.22(14) . . yes O1 N1 Fe1 126.96(11) . . yes C1 N1 Fe1 113.71(11) . . yes O3 N3 C10 118.32(14) . . yes O3 N3 Fe1 127.33(11) . . yes C10 N3 Fe1 114.26(11) . . yes O5 N5 C19 119.07(14) . . yes O5 N5 Fe1 127.19(11) . . yes C19 N5 Fe1 113.75(11) . . yes C3 O2 Fe1 113.43(11) . . yes C12 O4 Fe1 113.63(11) . . yes C21 O6 Fe1 112.50(11) . . yes C34 P1 C46 111.35(8) . . yes C34 P1 C28 109.72(8) . . yes C46 P1 C28 108.25(8) . . yes C34 P1 C40 106.33(8) . . yes C46 P1 C40 109.77(8) . . yes C28 P1 C40 111.44(8) . . yes 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 N1 C1 C3 O2 4.2(2) . . . . yes C2 C1 C3 O2 -169.95(17) . . . . yes N1 C1 C3 C4 -175.58(15) . . . . yes C2 C1 C3 C4 10.3(3) . . . . yes O2 C3 C4 C5 20.8(2) . . . . yes C1 C3 C4 C5 -159.49(17) . . . . yes O2 C3 C4 C9 -157.01(17) . . . . yes C1 C3 C4 C9 22.7(3) . . . . yes C9 C4 C5 C6 0.6(3) . . . . yes C3 C4 C5 C6 -177.24(16) . . . . yes C4 C5 C6 C7 -0.6(3) . . . . yes C5 C6 C7 C8 -0.1(3) . . . . yes C6 C7 C8 C9 0.8(3) . . . . yes C7 C8 C9 C4 -0.8(3) . . . . yes C5 C4 C9 C8 0.1(3) . . . . yes C3 C4 C9 C8 177.85(17) . . . . yes N3 C10 C12 O4 1.4(2) . . . . yes C11 C10 C12 O4 -174.37(16) . . . . yes N3 C10 C12 C13 179.97(15) . . . . yes C11 C10 C12 C13 4.2(3) . . . . yes O4 C12 C13 C18 -154.83(17) . . . . yes C10 C12 C13 C18 26.6(3) . . . . yes O4 C12 C13 C14 23.6(2) . . . . yes C10 C12 C13 C14 -154.89(17) . . . . yes C18 C13 C14 C15 -0.5(3) . . . . yes C12 C13 C14 C15 -179.02(17) . . . . yes C13 C14 C15 C16 -0.9(3) . . . . yes C14 C15 C16 C17 1.6(3) . . . . yes C15 C16 C17 C18 -1.0(3) . . . . yes C16 C17 C18 C13 -0.4(3) . . . . yes C14 C13 C18 C17 1.2(3) . . . . yes C12 C13 C18 C17 179.59(17) . . . . yes N5 C19 C21 O6 2.2(2) . . . . yes C20 C19 C21 O6 -172.56(16) . . . . yes N5 C19 C21 C22 -178.27(15) . . . . yes C20 C19 C21 C22 7.0(3) . . . . yes O6 C21 C22 C27 -138.88(17) . . . . yes C19 C21 C22 C27 41.6(3) . . . . yes O6 C21 C22 C23 36.6(2) . . . . yes C19 C21 C22 C23 -142.97(18) . . . . yes C27 C22 C23 C24 -0.9(3) . . . . yes C21 C22 C23 C24 -176.37(17) . . . . yes C22 C23 C24 C25 1.6(3) . . . . yes C23 C24 C25 C26 -0.7(3) . . . . yes C24 C25 C26 C27 -0.8(3) . . . . yes C25 C26 C27 C22 1.5(3) . . . . yes C23 C22 C27 C26 -0.7(3) . . . . yes C21 C22 C27 C26 174.68(16) . . . . yes C33 C28 C29 C30 0.3(3) . . . . yes P1 C28 C29 C30 176.13(15) . . . . yes C28 C29 C30 C31 0.0(3) . . . . yes C29 C30 C31 C32 -0.5(3) . . . . yes C30 C31 C32 C33 0.7(3) . . . . yes C31 C32 C33 C28 -0.3(3) . . . . yes C29 C28 C33 C32 -0.2(3) . . . . yes P1 C28 C33 C32 -175.94(15) . . . . yes C39 C34 C35 C36 1.3(3) . . . . yes P1 C34 C35 C36 -167.70(15) . . . . yes C34 C35 C36 C37 -0.5(3) . . . . yes C35 C36 C37 C38 -0.9(3) . . . . yes C36 C37 C38 C39 1.4(3) . . . . yes C37 C38 C39 C34 -0.6(3) . . . . yes C35 C34 C39 C38 -0.8(3) . . . . yes P1 C34 C39 C38 168.13(15) . . . . yes C45 C40 C41 C42 0.6(3) . . . . yes P1 C40 C41 C42 -178.59(15) . . . . yes C40 C41 C42 C43 0.3(3) . . . . yes C41 C42 C43 C44 -1.0(3) . . . . yes C42 C43 C44 C45 0.7(3) . . . . yes C43 C44 C45 C40 0.2(3) . . . . yes C41 C40 C45 C44 -0.9(3) . . . . yes P1 C40 C45 C44 178.33(14) . . . . yes C51 C46 C47 C48 1.5(3) . . . . yes P1 C46 C47 C48 -178.28(14) . . . . yes C46 C47 C48 C49 0.1(3) . . . . yes C47 C48 C49 C50 -1.3(3) . . . . yes C48 C49 C50 C51 0.9(3) . . . . yes C49 C50 C51 C46 0.7(3) . . . . yes C47 C46 C51 C50 -1.9(3) . . . . yes P1 C46 C51 C50 177.87(17) . . . . yes C2 C1 N1 O1 -7.4(2) . . . . yes C3 C1 N1 O1 178.06(14) . . . . yes C2 C1 N1 Fe1 169.02(13) . . . . yes C3 C1 N1 Fe1 -5.55(18) . . . . yes N5 Fe1 N1 O1 -88.63(14) . . . . yes N3 Fe1 N1 O1 6.03(14) . . . . yes O2 Fe1 N1 O1 -179.85(14) . . . . yes O4 Fe1 N1 O1 88.73(14) . . . . yes N5 Fe1 N1 C1 95.32(12) . . . . yes N3 Fe1 N1 C1 -170.02(12) . . . . yes O2 Fe1 N1 C1 4.10(11) . . . . yes O4 Fe1 N1 C1 -87.32(12) . . . . yes C12 C10 N3 O3 -179.01(14) . . . . yes C11 C10 N3 O3 -2.8(2) . . . . yes C12 C10 N3 Fe1 -2.23(18) . . . . yes C11 C10 N3 Fe1 174.02(12) . . . . yes N5 Fe1 N3 O3 4.17(14) . . . . yes N1 Fe1 N3 O3 -91.49(14) . . . . yes O6 Fe1 N3 O3 87.30(14) . . . . yes O4 Fe1 N3 O3 178.21(14) . . . . yes N5 Fe1 N3 C10 -172.27(11) . . . . yes N1 Fe1 N3 C10 92.07(12) . . . . yes O6 Fe1 N3 C10 -89.13(11) . . . . yes O4 Fe1 N3 C10 1.78(11) . . . . yes C21 C19 N5 O5 -175.49(14) . . . . yes C20 C19 N5 O5 -0.3(2) . . . . yes C21 C19 N5 Fe1 4.00(18) . . . . yes C20 C19 N5 Fe1 179.22(12) . . . . yes N3 Fe1 N5 O5 -97.13(14) . . . . yes N1 Fe1 N5 O5 -1.21(14) . . . . yes O2 Fe1 N5 O5 81.96(13) . . . . yes O6 Fe1 N5 O5 173.49(14) . . . . yes N3 Fe1 N5 C19 83.43(12) . . . . yes N1 Fe1 N5 C19 179.35(11) . . . . yes O2 Fe1 N5 C19 -97.48(11) . . . . yes O6 Fe1 N5 C19 -5.95(11) . . . . yes C1 C3 O2 Fe1 -0.79(19) . . . . yes C4 C3 O2 Fe1 178.96(11) . . . . yes N5 Fe1 O2 C3 -96.88(12) . . . . yes N1 Fe1 O2 C3 -1.84(12) . . . . yes O6 Fe1 O2 C3 179.91(12) . . . . yes O4 Fe1 O2 C3 88.97(12) . . . . yes C10 C12 O4 Fe1 0.03(18) . . . . yes C13 C12 O4 Fe1 -178.63(11) . . . . yes N3 Fe1 O4 C12 -1.01(11) . . . . yes N1 Fe1 O4 C12 -96.44(11) . . . . yes O2 Fe1 O4 C12 -179.49(11) . . . . yes O6 Fe1 O4 C12 88.75(11) . . . . yes C19 C21 O6 Fe1 -6.92(19) . . . . yes C22 C21 O6 Fe1 173.49(11) . . . . yes N5 Fe1 O6 C21 7.20(11) . . . . yes N3 Fe1 O6 C21 -86.96(12) . . . . yes O2 Fe1 O6 C21 98.84(11) . . . . ? O4 Fe1 O6 C21 -169.60(11) . . . . ? C35 C34 P1 C46 -35.34(17) . . . . ? C39 C34 P1 C46 155.64(14) . . . . ? C35 C34 P1 C28 -155.16(14) . . . . ? C39 C34 P1 C28 35.82(17) . . . . ? C35 C34 P1 C40 84.19(16) . . . . ? C39 C34 P1 C40 -84.83(16) . . . . ? C51 C46 P1 C34 96.19(18) . . . . ? C47 C46 P1 C34 -84.04(16) . . . . ? C51 C46 P1 C28 -143.12(17) . . . . ? C47 C46 P1 C28 36.65(17) . . . . ? C51 C46 P1 C40 -21.28(19) . . . . ? C47 C46 P1 C40 158.49(14) . . . . ? C33 C28 P1 C34 -145.69(14) . . . . ? C29 C28 P1 C34 38.54(17) . . . . ? C33 C28 P1 C46 92.61(16) . . . . ? C29 C28 P1 C46 -83.16(16) . . . . ? C33 C28 P1 C40 -28.20(17) . . . . ? C29 C28 P1 C40 156.03(14) . . . . ? C41 C40 P1 C34 -167.02(15) . . . . ? C45 C40 P1 C34 13.78(17) . . . . ? C41 C40 P1 C46 -46.46(17) . . . . ? C45 C40 P1 C46 134.34(15) . . . . ? C41 C40 P1 C28 73.46(16) . . . . ? C45 C40 P1 C28 -105.74(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.371 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.046