data_febco-293k _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 12.247(2) _cell_length_b 26.068(5) _cell_length_c 14.007(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.835(2) _cell_angle_gamma 90.00 _cell_volume 4466.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 258 _cell_measurement_theta_min 2.164 _cell_measurement_theta_max 22.91 _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 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6641 _exptl_absorpt_correction_T_max 0.7455 _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 293 _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 43945 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0420 _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 1.56 _diffrn_reflns_theta_max 26.02 _reflns_number_total 8796 _reflns_number_gt 6312 _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^)+(0.0338P)^2^+1.5996P] 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 8796 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.59010(16) 0.06444(8) 0.27021(15) 0.0407(5) Uani 1 1 d . . . C2 C 0.66909(18) 0.09186(9) 0.32789(17) 0.0482(6) Uani 1 1 d . . . C3 C 0.60392(16) 0.01676(8) 0.22443(15) 0.0408(5) Uani 1 1 d . . . C4 C 0.69907(16) -0.01726(8) 0.24011(16) 0.0422(5) Uani 1 1 d . . . C5 C 0.71940(19) -0.05304(9) 0.17071(18) 0.0541(6) Uani 1 1 d . . . H5 H 0.6747 -0.0544 0.1151 0.065 Uiso 1 1 calc R . . C6 C 0.8058(2) -0.08685(10) 0.1833(2) 0.0673(7) Uani 1 1 d . . . H6 H 0.8191 -0.1108 0.1361 0.081 Uiso 1 1 calc R . . C7 C 0.8718(2) -0.08517(11) 0.2651(2) 0.0694(8) Uani 1 1 d . . . H7 H 0.9297 -0.1081 0.2735 0.083 Uiso 1 1 calc R . . C8 C 0.8527(2) -0.04987(11) 0.3343(2) 0.0694(8) Uani 1 1 d . . . H8 H 0.8983 -0.0486 0.3893 0.083 Uiso 1 1 calc R . . C9 C 0.76603(19) -0.01594(9) 0.32315(18) 0.0576(6) Uani 1 1 d . . . H9 H 0.7527 0.0076 0.3710 0.069 Uiso 1 1 calc R . . C10 C 0.32251(17) 0.13626(8) 0.06307(15) 0.0413(5) Uani 1 1 d . . . C11 C 0.2417(2) 0.17343(9) 0.03733(16) 0.0501(6) Uani 1 1 d . . . C12 C 0.42250(17) 0.12675(8) 0.02053(15) 0.0415(5) Uani 1 1 d . . . C13 C 0.46601(18) 0.15678(9) -0.05824(16) 0.0483(6) Uani 1 1 d . . . C14 C 0.5364(2) 0.13245(11) -0.11773(19) 0.0668(7) Uani 1 1 d . . . H14 H 0.5541 0.0981 -0.1078 0.080 Uiso 1 1 calc R . . C15 C 0.5804(3) 0.15899(16) -0.1915(2) 0.0885(10) Uani 1 1 d . . . H15 H 0.6285 0.1427 -0.2309 0.106 Uiso 1 1 calc R . . C16 C 0.5535(3) 0.20928(16) -0.2072(2) 0.0882(10) Uani 1 1 d . . . H16 H 0.5820 0.2267 -0.2583 0.106 Uiso 1 1 calc R . . C17 C 0.4854(3) 0.23423(12) -0.1487(2) 0.0784(9) Uani 1 1 d . . . H17 H 0.4686 0.2686 -0.1593 0.094 Uiso 1 1 calc R . . C18 C 0.4408(2) 0.20802(10) -0.07274(18) 0.0627(7) Uani 1 1 d . . . H18 H 0.3947 0.2249 -0.0323 0.075 Uiso 1 1 calc R . . C19 C 0.25195(17) -0.01875(8) 0.19665(15) 0.0408(5) Uani 1 1 d . . . C20 C 0.18758(18) -0.04986(9) 0.25434(17) 0.0469(5) Uani 1 1 d . . . C21 C 0.25586(16) -0.01942(8) 0.09622(16) 0.0413(5) Uani 1 1 d . . . C22 C 0.18231(17) -0.04998(8) 0.03200(15) 0.0429(5) Uani 1 1 d . . . C23 C 0.2239(2) -0.07214(10) -0.04865(18) 0.0578(6) Uani 1 1 d . . . H23 H 0.2980 -0.0694 -0.0595 0.069 Uiso 1 1 calc R . . C24 C 0.1553(2) -0.09828(11) -0.11263(19) 0.0689(7) Uani 1 1 d . . . H24 H 0.1834 -0.1138 -0.1659 0.083 Uiso 1 1 calc R . . C25 C 0.0456(2) -0.10155(11) -0.09803(19) 0.0655(7) Uani 1 1 d . . . H25 H -0.0005 -0.1190 -0.1416 0.079 Uiso 1 1 calc R . . C26 C 0.0042(2) -0.07919(10) -0.01948(19) 0.0613(7) Uani 1 1 d . . . H26 H -0.0704 -0.0811 -0.0104 0.074 Uiso 1 1 calc R . . C27 C 0.07169(18) -0.05378(9) 0.04667(17) 0.0499(6) Uani 1 1 d . . . H27 H 0.0430 -0.0393 0.1007 0.060 Uiso 1 1 calc R . . C28 C 0.17939(17) 0.15198(8) 0.46243(16) 0.0448(5) Uani 1 1 d . . . C29 C 0.1947(2) 0.11215(9) 0.39930(19) 0.0579(6) Uani 1 1 d . . . H29 H 0.2632 0.1066 0.3753 0.069 Uiso 1 1 calc R . . C30 C 0.1078(2) 0.08063(11) 0.3719(2) 0.0697(8) Uani 1 1 d . . . H30 H 0.1181 0.0537 0.3297 0.084 Uiso 1 1 calc R . . C31 C 0.0073(2) 0.08878(11) 0.4064(2) 0.0698(8) Uani 1 1 d . . . H31 H -0.0509 0.0677 0.3868 0.084 Uiso 1 1 calc R . . C32 C -0.0088(2) 0.12782(11) 0.4698(2) 0.0685(7) Uani 1 1 d . . . H32 H -0.0775 0.1329 0.4937 0.082 Uiso 1 1 calc R . . C33 C 0.07663(18) 0.15946(10) 0.49804(18) 0.0559(6) Uani 1 1 d . . . H33 H 0.0656 0.1859 0.5411 0.067 Uiso 1 1 calc R . . C34 C 0.24661(18) 0.23019(8) 0.59630(16) 0.0463(5) Uani 1 1 d . . . C35 C 0.2585(2) 0.20950(10) 0.68685(18) 0.0591(6) Uani 1 1 d . . . H35 H 0.3002 0.1801 0.6976 0.071 Uiso 1 1 calc R . . C36 C 0.2080(2) 0.23277(12) 0.76138(19) 0.0707(8) Uani 1 1 d . . . H36 H 0.2162 0.2188 0.8224 0.085 Uiso 1 1 calc R . . C37 C 0.1463(2) 0.27589(11) 0.7469(2) 0.0671(7) Uani 1 1 d . . . H37 H 0.1116 0.2909 0.7975 0.080 Uiso 1 1 calc R . . C38 C 0.1357(2) 0.29694(11) 0.6576(2) 0.0693(8) Uani 1 1 d . . . H38 H 0.0948 0.3267 0.6479 0.083 Uiso 1 1 calc R . . C39 C 0.1849(2) 0.27461(9) 0.58201(18) 0.0597(7) Uani 1 1 d . . . H39 H 0.1769 0.2891 0.5214 0.072 Uiso 1 1 calc R . . C40 C 0.41002(18) 0.15742(9) 0.52834(16) 0.0490(6) Uani 1 1 d . . . C41 C 0.4023(2) 0.10686(11) 0.5562(2) 0.0777(9) Uani 1 1 d . . . H41 H 0.3340 0.0916 0.5602 0.093 Uiso 1 1 calc R . . C42 C 0.4960(3) 0.07889(13) 0.5781(2) 0.0898(10) Uani 1 1 d . . . H42 H 0.4908 0.0446 0.5959 0.108 Uiso 1 1 calc R . . C43 C 0.5958(2) 0.10131(14) 0.5737(2) 0.0789(9) Uani 1 1 d . . . H43 H 0.6588 0.0823 0.5881 0.095 Uiso 1 1 calc R . . C44 C 0.6040(2) 0.15162(13) 0.5482(2) 0.0710(8) Uani 1 1 d . . . H44 H 0.6725 0.1669 0.5463 0.085 Uiso 1 1 calc R . . C45 C 0.51149(19) 0.17998(10) 0.52544(17) 0.0570(6) Uani 1 1 d . . . H45 H 0.5175 0.2143 0.5081 0.068 Uiso 1 1 calc R . . C46 C 0.32121(18) 0.23664(8) 0.40138(16) 0.0458(5) Uani 1 1 d . . . C47 C 0.3003(2) 0.22275(9) 0.30740(17) 0.0540(6) Uani 1 1 d . . . H47 H 0.2655 0.1918 0.2928 0.065 Uiso 1 1 calc R . . C48 C 0.3308(2) 0.25461(10) 0.23522(19) 0.0678(7) Uani 1 1 d . . . H48 H 0.3167 0.2449 0.1719 0.081 Uiso 1 1 calc R . . C49 C 0.3816(2) 0.30031(10) 0.2552(2) 0.0717(8) Uani 1 1 d . . . H49 H 0.4015 0.3217 0.2059 0.086 Uiso 1 1 calc R . . C50 C 0.4029(2) 0.31436(10) 0.3482(2) 0.0730(8) Uani 1 1 d . . . H50 H 0.4377 0.3454 0.3620 0.088 Uiso 1 1 calc R . . C51 C 0.3735(2) 0.28319(9) 0.42140(19) 0.0630(7) Uani 1 1 d . . . H51 H 0.3884 0.2931 0.4845 0.076 Uiso 1 1 calc R . . Fe1 Fe 0.40740(2) 0.051210(11) 0.15354(2) 0.03920(9) Uani 1 1 d . . . N1 N 0.49106(13) 0.08690(7) 0.24662(13) 0.0410(4) Uani 1 1 d . . . N2 N 0.73421(17) 0.11418(9) 0.37055(17) 0.0727(7) Uani 1 1 d . . . N3 N 0.30146(13) 0.10193(7) 0.13496(12) 0.0402(4) Uani 1 1 d . . . N4 N 0.1761(2) 0.20275(9) 0.01712(17) 0.0750(7) Uani 1 1 d . . . N5 N 0.32788(13) 0.01415(6) 0.23935(13) 0.0409(4) Uani 1 1 d . . . N6 N 0.13847(18) -0.07476(9) 0.30358(16) 0.0668(6) Uani 1 1 d . . . O1 O 0.46798(12) 0.12886(6) 0.28379(12) 0.0538(4) Uani 1 1 d . . . O2 O 0.52800(11) 0.00282(5) 0.16541(10) 0.0438(4) Uani 1 1 d . . . O3 O 0.21457(12) 0.10637(6) 0.17644(11) 0.0546(4) Uani 1 1 d . . . O4 O 0.47713(11) 0.08855(6) 0.05186(10) 0.0444(4) Uani 1 1 d . . . O5 O 0.33712(12) 0.01560(6) 0.32860(11) 0.0510(4) Uani 1 1 d . . . O6 O 0.32824(11) 0.00783(6) 0.05933(10) 0.0443(4) Uani 1 1 d . . . P1 P 0.29012(5) 0.19412(2) 0.49666(4) 0.04392(15) 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 0.0337(11) 0.0431(12) 0.0446(12) -0.0022(10) -0.0046(9) 0.0003(9) C2 0.0413(13) 0.0502(14) 0.0526(14) -0.0073(11) -0.0040(11) 0.0048(11) C3 0.0358(11) 0.0426(12) 0.0436(12) 0.0000(10) -0.0010(9) -0.0013(9) C4 0.0353(11) 0.0411(12) 0.0496(13) 0.0038(10) -0.0028(10) -0.0001(9) C5 0.0528(14) 0.0541(15) 0.0548(15) -0.0028(12) -0.0010(11) 0.0073(12) C6 0.0626(17) 0.0625(17) 0.0773(19) -0.0054(14) 0.0089(15) 0.0184(14) C7 0.0474(15) 0.0578(17) 0.102(2) 0.0074(16) -0.0018(15) 0.0123(13) C8 0.0534(15) 0.0649(18) 0.087(2) 0.0087(16) -0.0260(14) 0.0053(14) C9 0.0547(15) 0.0522(15) 0.0643(16) -0.0022(12) -0.0134(12) 0.0060(12) C10 0.0404(12) 0.0406(12) 0.0423(12) 0.0000(10) -0.0058(9) -0.0007(9) C11 0.0557(14) 0.0501(14) 0.0439(13) 0.0013(11) -0.0038(11) 0.0032(12) C12 0.0411(12) 0.0417(12) 0.0409(12) -0.0051(10) -0.0053(9) -0.0094(10) C13 0.0473(13) 0.0540(14) 0.0430(13) 0.0004(11) -0.0045(10) -0.0137(11) C14 0.0679(17) 0.0751(18) 0.0587(17) -0.0031(14) 0.0147(14) -0.0111(15) C15 0.088(2) 0.116(3) 0.063(2) -0.004(2) 0.0231(17) -0.022(2) C16 0.093(2) 0.118(3) 0.0539(19) 0.015(2) -0.0011(17) -0.042(2) C17 0.092(2) 0.0715(19) 0.070(2) 0.0224(16) -0.0161(17) -0.0315(17) C18 0.0697(17) 0.0609(17) 0.0568(16) 0.0068(13) -0.0027(13) -0.0147(13) C19 0.0390(11) 0.0384(12) 0.0446(13) 0.0014(10) -0.0026(9) -0.0024(9) C20 0.0434(13) 0.0464(13) 0.0501(14) -0.0002(11) -0.0058(11) -0.0026(11) C21 0.0353(11) 0.0380(12) 0.0498(13) -0.0003(10) -0.0052(10) 0.0003(9) C22 0.0400(12) 0.0423(12) 0.0455(13) 0.0050(10) -0.0059(10) -0.0033(10) C23 0.0491(14) 0.0687(17) 0.0555(15) -0.0095(13) 0.0010(12) -0.0096(12) C24 0.0683(18) 0.0810(19) 0.0570(16) -0.0200(14) -0.0016(13) -0.0108(15) C25 0.0627(17) 0.0715(18) 0.0601(17) -0.0070(14) -0.0187(13) -0.0167(14) C26 0.0436(14) 0.0731(18) 0.0660(18) 0.0045(14) -0.0104(12) -0.0104(12) C27 0.0445(13) 0.0548(14) 0.0497(14) 0.0004(11) -0.0046(10) -0.0010(11) C28 0.0431(12) 0.0402(12) 0.0504(13) -0.0003(10) -0.0039(10) 0.0009(10) C29 0.0508(14) 0.0507(14) 0.0729(17) -0.0086(13) 0.0097(13) -0.0076(12) C30 0.0687(18) 0.0612(17) 0.080(2) -0.0197(15) 0.0086(15) -0.0155(14) C31 0.0550(17) 0.0732(19) 0.080(2) -0.0068(16) -0.0061(14) -0.0190(14) C32 0.0430(14) 0.0797(19) 0.083(2) -0.0085(16) 0.0014(13) -0.0028(13) C33 0.0442(14) 0.0603(15) 0.0628(16) -0.0071(13) -0.0001(12) 0.0042(12) C34 0.0456(13) 0.0440(13) 0.0484(14) -0.0021(10) -0.0071(10) 0.0000(10) C35 0.0622(16) 0.0590(16) 0.0552(16) 0.0035(13) -0.0064(12) 0.0066(13) C36 0.083(2) 0.081(2) 0.0469(16) 0.0006(14) -0.0024(14) 0.0027(16) C37 0.0736(18) 0.0696(18) 0.0580(17) -0.0144(14) 0.0036(14) 0.0034(15) C38 0.0777(19) 0.0619(17) 0.0679(19) -0.0092(15) -0.0003(15) 0.0193(14) C39 0.0700(16) 0.0551(15) 0.0531(15) 0.0003(12) -0.0059(13) 0.0153(13) C40 0.0431(13) 0.0520(14) 0.0516(14) 0.0057(11) -0.0004(10) 0.0064(11) C41 0.0558(16) 0.0645(18) 0.112(2) 0.0290(17) -0.0019(16) 0.0081(14) C42 0.074(2) 0.076(2) 0.119(3) 0.0341(19) -0.0021(19) 0.0238(17) C43 0.0604(19) 0.106(3) 0.0696(19) 0.0089(18) -0.0047(15) 0.0334(18) C44 0.0428(14) 0.104(2) 0.0661(18) -0.0029(17) -0.0038(12) 0.0061(15) C45 0.0459(14) 0.0665(16) 0.0581(16) -0.0018(13) -0.0036(11) 0.0013(12) C46 0.0446(12) 0.0392(12) 0.0532(14) -0.0028(11) -0.0028(10) 0.0017(10) C47 0.0649(15) 0.0403(13) 0.0564(15) -0.0035(11) 0.0005(12) -0.0017(11) C48 0.094(2) 0.0588(17) 0.0512(16) -0.0025(13) 0.0043(14) -0.0051(15) C49 0.098(2) 0.0518(16) 0.0664(19) 0.0061(14) 0.0145(16) -0.0070(15) C50 0.098(2) 0.0450(15) 0.076(2) -0.0007(14) 0.0049(17) -0.0199(15) C51 0.0810(18) 0.0503(15) 0.0568(16) -0.0056(13) -0.0051(13) -0.0131(13) Fe1 0.03299(16) 0.03906(17) 0.04485(19) 0.00022(14) -0.00499(12) -0.00150(13) N1 0.0360(9) 0.0378(10) 0.0490(11) -0.0008(8) 0.0005(8) -0.0012(8) N2 0.0506(13) 0.0815(16) 0.0837(16) -0.0284(13) -0.0186(12) -0.0014(12) N3 0.0328(9) 0.0466(11) 0.0405(10) -0.0015(8) -0.0048(8) -0.0024(8) N4 0.0760(16) 0.0702(15) 0.0778(16) 0.0116(13) -0.0073(13) 0.0242(13) N5 0.0382(10) 0.0400(10) 0.0437(11) 0.0005(8) -0.0066(8) 0.0038(8) N6 0.0625(14) 0.0727(15) 0.0652(14) 0.0100(12) 0.0021(11) -0.0188(12) O1 0.0479(9) 0.0426(9) 0.0701(11) -0.0146(8) -0.0044(8) 0.0054(7) O2 0.0391(8) 0.0407(8) 0.0506(9) -0.0061(7) -0.0086(7) -0.0007(6) O3 0.0375(9) 0.0705(11) 0.0560(10) 0.0098(8) 0.0057(7) 0.0087(8) O4 0.0375(8) 0.0448(9) 0.0508(9) -0.0005(7) 0.0000(7) -0.0010(7) O5 0.0585(10) 0.0529(10) 0.0406(9) 0.0023(7) -0.0072(7) -0.0036(8) O6 0.0392(8) 0.0486(9) 0.0447(9) -0.0008(7) -0.0023(7) -0.0079(7) P1 0.0406(3) 0.0399(3) 0.0506(4) 0.0007(3) -0.0046(3) 0.0015(2) _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 1.372(2) . ? C1 C3 1.413(3) . ? C1 C2 1.422(3) . ? C2 N2 1.133(3) . ? C3 O2 1.266(2) . ? C3 C4 1.472(3) . ? C4 C5 1.379(3) . ? C4 C9 1.390(3) . ? C5 C6 1.382(3) . ? C5 H5 0.9300 . ? C6 C7 1.370(4) . ? C6 H6 0.9300 . ? C7 C8 1.365(4) . ? C7 H7 0.9300 . ? C8 C9 1.385(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N3 1.381(3) . ? C10 C12 1.410(3) . ? C10 C11 1.418(3) . ? C11 N4 1.135(3) . ? C12 O4 1.266(2) . ? C12 C13 1.474(3) . ? C13 C14 1.382(3) . ? C13 C18 1.383(3) . ? C14 C15 1.376(4) . ? C14 H14 0.9300 . ? C15 C16 1.367(5) . ? C15 H15 0.9300 . ? C16 C17 1.363(4) . ? C16 H16 0.9300 . ? C17 C18 1.398(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N5 1.379(3) . ? C19 C21 1.410(3) . ? C19 C20 1.412(3) . ? C20 N6 1.140(3) . ? C21 O6 1.266(2) . ? C21 C22 1.475(3) . ? C22 C27 1.384(3) . ? C22 C23 1.388(3) . ? C23 C24 1.378(3) . ? C23 H23 0.9300 . ? C24 C25 1.371(4) . ? C24 H24 0.9300 . ? C25 C26 1.365(4) . ? C25 H25 0.9300 . ? C26 C27 1.380(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.383(3) . ? C28 C33 1.390(3) . ? C28 P1 1.792(2) . ? C29 C30 1.384(3) . ? C29 H29 0.9300 . ? C30 C31 1.360(4) . ? C30 H30 0.9300 . ? C31 C32 1.371(4) . ? C31 H31 0.9300 . ? C32 C33 1.375(3) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.379(3) . ? C34 C39 1.392(3) . ? C34 P1 1.786(2) . ? C35 C36 1.379(4) . ? C35 H35 0.9300 . ? C36 C37 1.364(4) . ? C36 H36 0.9300 . ? C37 C38 1.366(4) . ? C37 H37 0.9300 . ? C38 C39 1.373(3) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.377(3) . ? C40 C41 1.379(3) . ? C40 P1 1.790(2) . ? C41 C42 1.382(4) . ? C41 H41 0.9300 . ? C42 C43 1.359(4) . ? C42 H42 0.9300 . ? C43 C44 1.364(4) . ? C43 H43 0.9300 . ? C44 C45 1.377(3) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.377(3) . ? C46 C51 1.394(3) . ? C46 P1 1.790(2) . ? C47 C48 1.374(3) . ? C47 H47 0.9300 . ? C48 C49 1.367(4) . ? C48 H48 0.9300 . ? C49 C50 1.365(4) . ? C49 H49 0.9300 . ? C50 C51 1.370(4) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? Fe1 N5 1.8552(18) . ? Fe1 N3 1.8617(17) . ? Fe1 N1 1.8663(17) . ? Fe1 O2 1.9431(14) . ? Fe1 O4 1.9558(15) . ? Fe1 O6 1.9580(14) . ? N1 O1 1.250(2) . ? N3 O3 1.243(2) . ? N5 O5 1.250(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 C3 112.98(17) . . ? N1 C1 C2 119.38(19) . . ? C3 C1 C2 127.36(19) . . ? N2 C2 C1 177.2(3) . . ? O2 C3 C1 116.63(18) . . ? O2 C3 C4 118.34(18) . . ? C1 C3 C4 125.04(18) . . ? C5 C4 C9 119.2(2) . . ? C5 C4 C3 118.13(19) . . ? C9 C4 C3 122.7(2) . . ? C4 C5 C6 120.3(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 119.7(2) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? N3 C10 C12 113.05(18) . . ? N3 C10 C11 118.36(19) . . ? C12 C10 C11 128.5(2) . . ? N4 C11 C10 179.1(3) . . ? O4 C12 C10 116.54(19) . . ? O4 C12 C13 118.2(2) . . ? C10 C12 C13 125.2(2) . . ? C14 C13 C18 119.7(2) . . ? C14 C13 C12 117.8(2) . . ? C18 C13 C12 122.4(2) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 119.4(3) . . ? C13 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N5 C19 C21 112.63(18) . . ? N5 C19 C20 119.49(19) . . ? C21 C19 C20 127.66(19) . . ? N6 C20 C19 177.5(2) . . ? O6 C21 C19 117.34(19) . . ? O6 C21 C22 118.23(19) . . ? C19 C21 C22 124.43(19) . . ? C27 C22 C23 119.5(2) . . ? C27 C22 C21 121.4(2) . . ? C23 C22 C21 118.9(2) . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.8(2) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 119.5(2) . . ? C26 C27 H27 120.2 . . ? C22 C27 H27 120.2 . . ? C29 C28 C33 119.2(2) . . ? C29 C28 P1 120.45(18) . . ? C33 C28 P1 120.30(18) . . ? C28 C29 C30 119.8(2) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 120.0(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.1(2) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C35 C34 C39 119.3(2) . . ? C35 C34 P1 119.40(18) . . ? C39 C34 P1 120.43(18) . . ? C34 C35 C36 119.6(2) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C37 C36 C35 121.0(3) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 119.6(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C39 120.7(3) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 119.8(2) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? C45 C40 C41 119.4(2) . . ? C45 C40 P1 119.66(19) . . ? C41 C40 P1 120.91(19) . . ? C40 C41 C42 119.9(3) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.2(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 120.5(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C40 119.8(3) . . ? C44 C45 H45 120.1 . . ? C40 C45 H45 120.1 . . ? C47 C46 C51 118.9(2) . . ? C47 C46 P1 120.89(17) . . ? C51 C46 P1 120.10(18) . . ? C48 C47 C46 120.0(2) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 120.9(3) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C50 C49 C48 119.5(3) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 120.6(3) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C50 C51 C46 120.1(2) . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? N5 Fe1 N3 94.35(7) . . ? N5 Fe1 N1 95.43(8) . . ? N3 Fe1 N1 95.65(7) . . ? N5 Fe1 O2 91.59(7) . . ? N3 Fe1 O2 173.99(7) . . ? N1 Fe1 O2 82.83(7) . . ? N5 Fe1 O4 173.20(7) . . ? N3 Fe1 O4 82.60(7) . . ? N1 Fe1 O4 90.93(7) . . ? O2 Fe1 O4 91.60(6) . . ? N5 Fe1 O6 82.97(7) . . ? N3 Fe1 O6 89.86(7) . . ? N1 Fe1 O6 174.38(7) . . ? O2 Fe1 O6 91.82(6) . . ? O4 Fe1 O6 90.93(6) . . ? O1 N1 C1 119.24(17) . . ? O1 N1 Fe1 126.85(14) . . ? C1 N1 Fe1 113.80(14) . . ? O3 N3 C10 118.40(17) . . ? O3 N3 Fe1 127.43(14) . . ? C10 N3 Fe1 114.09(14) . . ? O5 N5 C19 118.56(18) . . ? O5 N5 Fe1 127.42(14) . . ? C19 N5 Fe1 114.02(14) . . ? C3 O2 Fe1 113.58(13) . . ? C12 O4 Fe1 113.67(13) . . ? C21 O6 Fe1 112.48(13) . . ? C34 P1 C40 111.13(11) . . ? C34 P1 C46 109.83(11) . . ? C40 P1 C46 108.28(11) . . ? C34 P1 C28 106.30(10) . . ? C40 P1 C28 109.84(11) . . ? C46 P1 C28 111.48(10) . . ? 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 3.7(3) . . . . ? C2 C1 C3 O2 -170.1(2) . . . . ? N1 C1 C3 C4 -176.46(19) . . . . ? C2 C1 C3 C4 9.7(4) . . . . ? O2 C3 C4 C5 20.8(3) . . . . ? C1 C3 C4 C5 -159.1(2) . . . . ? O2 C3 C4 C9 -156.8(2) . . . . ? C1 C3 C4 C9 23.4(3) . . . . ? C9 C4 C5 C6 -0.5(4) . . . . ? C3 C4 C5 C6 -178.1(2) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C7 C8 C9 C4 -1.1(4) . . . . ? C5 C4 C9 C8 1.0(4) . . . . ? C3 C4 C9 C8 178.5(2) . . . . ? N3 C10 C12 O4 1.2(3) . . . . ? C11 C10 C12 O4 -174.6(2) . . . . ? N3 C10 C12 C13 179.54(18) . . . . ? C11 C10 C12 C13 3.8(4) . . . . ? O4 C12 C13 C14 24.8(3) . . . . ? C10 C12 C13 C14 -153.5(2) . . . . ? O4 C12 C13 C18 -153.7(2) . . . . ? C10 C12 C13 C18 28.0(3) . . . . ? C18 C13 C14 C15 -0.6(4) . . . . ? C12 C13 C14 C15 -179.2(2) . . . . ? C13 C14 C15 C16 -0.9(5) . . . . ? C14 C15 C16 C17 1.8(5) . . . . ? C15 C16 C17 C18 -1.1(5) . . . . ? C14 C13 C18 C17 1.3(4) . . . . ? C12 C13 C18 C17 179.7(2) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? N5 C19 C21 O6 2.3(3) . . . . ? C20 C19 C21 O6 -172.4(2) . . . . ? N5 C19 C21 C22 -178.32(18) . . . . ? C20 C19 C21 C22 7.0(4) . . . . ? O6 C21 C22 C27 -138.7(2) . . . . ? C19 C21 C22 C27 42.0(3) . . . . ? O6 C21 C22 C23 36.5(3) . . . . ? C19 C21 C22 C23 -142.9(2) . . . . ? C27 C22 C23 C24 -0.9(4) . . . . ? C21 C22 C23 C24 -176.1(2) . . . . ? C22 C23 C24 C25 1.4(4) . . . . ? C23 C24 C25 C26 -0.5(4) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C25 C26 C27 C22 1.4(4) . . . . ? C23 C22 C27 C26 -0.5(3) . . . . ? C21 C22 C27 C26 174.6(2) . . . . ? C33 C28 C29 C30 0.5(4) . . . . ? P1 C28 C29 C30 -178.6(2) . . . . ? C28 C29 C30 C31 0.3(4) . . . . ? C29 C30 C31 C32 -1.0(5) . . . . ? C30 C31 C32 C33 0.8(4) . . . . ? C31 C32 C33 C28 0.0(4) . . . . ? C29 C28 C33 C32 -0.7(4) . . . . ? P1 C28 C33 C32 178.4(2) . . . . ? C39 C34 C35 C36 0.7(4) . . . . ? P1 C34 C35 C36 -168.6(2) . . . . ? C34 C35 C36 C37 0.2(4) . . . . ? C35 C36 C37 C38 -1.2(4) . . . . ? C36 C37 C38 C39 1.3(4) . . . . ? C37 C38 C39 C34 -0.3(4) . . . . ? C35 C34 C39 C38 -0.7(4) . . . . ? P1 C34 C39 C38 168.5(2) . . . . ? C45 C40 C41 C42 -1.9(4) . . . . ? P1 C40 C41 C42 178.4(3) . . . . ? C40 C41 C42 C43 1.0(5) . . . . ? C41 C42 C43 C44 0.4(5) . . . . ? C42 C43 C44 C45 -0.9(5) . . . . ? C43 C44 C45 C40 0.0(4) . . . . ? C41 C40 C45 C44 1.4(4) . . . . ? P1 C40 C45 C44 -178.9(2) . . . . ? C51 C46 C47 C48 0.0(4) . . . . ? P1 C46 C47 C48 -176.0(2) . . . . ? C46 C47 C48 C49 -0.3(4) . . . . ? C47 C48 C49 C50 0.4(5) . . . . ? C48 C49 C50 C51 -0.3(5) . . . . ? C49 C50 C51 C46 0.0(4) . . . . ? C47 C46 C51 C50 0.2(4) . . . . ? P1 C46 C51 C50 176.2(2) . . . . ? C3 C1 N1 O1 178.72(18) . . . . ? C2 C1 N1 O1 -6.9(3) . . . . ? C3 C1 N1 Fe1 -4.8(2) . . . . ? C2 C1 N1 Fe1 169.54(16) . . . . ? N5 Fe1 N1 O1 -89.45(18) . . . . ? N3 Fe1 N1 O1 5.48(18) . . . . ? O2 Fe1 N1 O1 179.63(18) . . . . ? O4 Fe1 N1 O1 88.13(18) . . . . ? N5 Fe1 N1 C1 94.40(15) . . . . ? N3 Fe1 N1 C1 -170.68(15) . . . . ? O2 Fe1 N1 C1 3.47(14) . . . . ? O4 Fe1 N1 C1 -88.02(15) . . . . ? C12 C10 N3 O3 -179.01(17) . . . . ? C11 C10 N3 O3 -2.8(3) . . . . ? C12 C10 N3 Fe1 -2.1(2) . . . . ? C11 C10 N3 Fe1 174.19(15) . . . . ? N5 Fe1 N3 O3 4.43(18) . . . . ? N1 Fe1 N3 O3 -91.47(17) . . . . ? O4 Fe1 N3 O3 178.32(18) . . . . ? O6 Fe1 N3 O3 87.37(17) . . . . ? N5 Fe1 N3 C10 -172.18(14) . . . . ? N1 Fe1 N3 C10 91.92(15) . . . . ? O4 Fe1 N3 C10 1.71(14) . . . . ? O6 Fe1 N3 C10 -89.24(14) . . . . ? C21 C19 N5 O5 -175.45(18) . . . . ? C20 C19 N5 O5 -0.3(3) . . . . ? C21 C19 N5 Fe1 3.7(2) . . . . ? C20 C19 N5 Fe1 178.81(16) . . . . ? N3 Fe1 N5 O5 -97.27(17) . . . . ? N1 Fe1 N5 O5 -1.17(18) . . . . ? O2 Fe1 N5 O5 81.77(17) . . . . ? O6 Fe1 N5 O5 173.41(17) . . . . ? N3 Fe1 N5 C19 83.69(14) . . . . ? N1 Fe1 N5 C19 179.80(14) . . . . ? O2 Fe1 N5 C19 -97.26(14) . . . . ? O6 Fe1 N5 C19 -5.63(14) . . . . ? C1 C3 O2 Fe1 -0.9(2) . . . . ? C4 C3 O2 Fe1 179.30(14) . . . . ? N5 Fe1 O2 C3 -96.73(15) . . . . ? N1 Fe1 O2 C3 -1.46(14) . . . . ? O4 Fe1 O2 C3 89.28(15) . . . . ? O6 Fe1 O2 C3 -179.75(14) . . . . ? C10 C12 O4 Fe1 0.2(2) . . . . ? C13 C12 O4 Fe1 -178.26(14) . . . . ? N3 Fe1 O4 C12 -1.07(14) . . . . ? N1 Fe1 O4 C12 -96.64(14) . . . . ? O2 Fe1 O4 C12 -179.49(13) . . . . ? O6 Fe1 O4 C12 88.66(14) . . . . ? C19 C21 O6 Fe1 -6.8(2) . . . . ? C22 C21 O6 Fe1 173.80(14) . . . . ? N5 Fe1 O6 C21 6.92(14) . . . . ? N3 Fe1 O6 C21 -87.48(14) . . . . ? O2 Fe1 O6 C21 98.30(14) . . . . ? O4 Fe1 O6 C21 -170.07(14) . . . . ? C35 C34 P1 C40 -35.5(2) . . . . ? C39 C34 P1 C40 155.33(19) . . . . ? C35 C34 P1 C46 -155.28(19) . . . . ? C39 C34 P1 C46 35.5(2) . . . . ? C35 C34 P1 C28 84.0(2) . . . . ? C39 C34 P1 C28 -85.2(2) . . . . ? C45 C40 P1 C34 -84.7(2) . . . . ? C41 C40 P1 C34 95.0(2) . . . . ? C45 C40 P1 C46 36.1(2) . . . . ? C41 C40 P1 C46 -144.3(2) . . . . ? C45 C40 P1 C28 158.00(19) . . . . ? C41 C40 P1 C28 -22.4(3) . . . . ? C47 C46 P1 C34 -145.19(19) . . . . ? C51 C46 P1 C34 38.8(2) . . . . ? C47 C46 P1 C40 93.3(2) . . . . ? C51 C46 P1 C40 -82.7(2) . . . . ? C47 C46 P1 C28 -27.6(2) . . . . ? C51 C46 P1 C28 156.39(19) . . . . ? C29 C28 P1 C34 -167.58(19) . . . . ? C33 C28 P1 C34 13.4(2) . . . . ? C29 C28 P1 C40 -47.3(2) . . . . ? C33 C28 P1 C40 133.7(2) . . . . ? C29 C28 P1 C46 72.8(2) . . . . ? C33 C28 P1 C46 -106.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.361 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.041