#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/67/4316766.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4316766 loop_ _publ_author_name 'Jinzhu Chen' 'David J. Szalda' 'Etsuko Fujita' 'Carol Creutz' _publ_section_title ; Iron(II) and Ruthenium(II) Complexes Containing P, N, and H Ligands: Structure, Spectroscopy, Electrochemistry, and Reactivity ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9380 _journal_page_last 9391 _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C23 H43 F6 Fe N9 O P4' _chemical_formula_weight 755.39 _chemical_name_systematic ; ? ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.6307(2) _cell_length_b 15.3630(3) _cell_length_c 18.6298(3) _cell_measurement_reflns_used 9944 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 34.69 _cell_measurement_theta_min 3.20 _cell_volume 3042.61(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 56943 _diffrn_reflns_theta_full 36.76 _diffrn_reflns_theta_max 36.76 _diffrn_reflns_theta_min 3.80 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_correction_T_min 0.6697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS Version 2007/2 (Sheldrick, Bruker AXS Inc.) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1568 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _refine_diff_density_max 0.816 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.083 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 15121 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0435 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+0.5568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1219 _refine_ls_wR_factor_ref 0.1312 _reflns_number_gt 12594 _reflns_number_total 15121 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic101077t_si_004_1.cif _[local]_cod_data_source_block (8) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 4316766 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.88753(2) 0.498024(16) 0.917258(13) 0.02417(5) Uani 1 1 d . . . C51 C 0.9558(5) 0.6252(2) 0.9151(4) 0.105(2) Uani 1 1 d . . . H51 H 0.9057 0.6744 0.9206 0.0556(15) Uiso 1 1 calc R . . C52 C 0.9836(4) 0.5872(3) 0.8525(2) 0.0744(12) Uani 1 1 d . . . H52 H 0.9553 0.6062 0.8079 0.0556(15) Uiso 1 1 calc R . . C53 C 1.0562(3) 0.5198(3) 0.8627(3) 0.0826(15) Uani 1 1 d . . . H53 H 1.0881 0.4833 0.8272 0.0556(15) Uiso 1 1 calc R . . C54 C 1.0774(4) 0.5124(5) 0.9363(5) 0.167(4) Uani 1 1 d . . . H54 H 1.1254 0.4707 0.9599 0.0556(15) Uiso 1 1 calc R . . C55 C 1.0095(7) 0.5827(5) 0.9671(2) 0.140(3) Uani 1 1 d . . . H55 H 1.0044 0.5959 1.0158 0.0556(15) Uiso 1 1 calc R . . P2 P 0.83818(4) 0.40453(3) 0.83311(2) 0.02162(7) Uani 1 1 d . . . C211 C 0.8513(2) 0.44070(13) 0.73814(10) 0.0305(3) Uani 1 1 d . . . H21A H 0.7932 0.4884 0.7301 0.0556(15) Uiso 1 1 calc R . . H21B H 0.9357 0.4623 0.7297 0.0556(15) Uiso 1 1 calc R . . N211 N 0.82405(18) 0.37070(12) 0.68644(9) 0.0325(3) Uani 1 1 d . . . C221 C 0.93489(19) 0.30452(13) 0.82493(12) 0.0330(4) Uani 1 1 d . . . H22A H 1.0226 0.3208 0.8200 0.0556(15) Uiso 1 1 calc R . . H22B H 0.9265 0.2705 0.8685 0.0556(15) Uiso 1 1 calc R . . N221 N 0.8983(2) 0.25039(12) 0.76316(11) 0.0387(4) Uani 1 1 d . . . C231 C 0.68134(16) 0.35258(13) 0.82422(10) 0.0282(3) Uani 1 1 d . . . H23A H 0.6621 0.3212 0.8681 0.0556(15) Uiso 1 1 calc R . . H23B H 0.6181 0.3975 0.8181 0.0556(15) Uiso 1 1 calc R . . N231 N 0.67528(17) 0.29226(12) 0.76341(9) 0.0333(3) Uani 1 1 d . . . C212 C 0.9121(2) 0.29827(17) 0.69562(12) 0.0405(5) Uani 1 1 d . . . H12A H 0.9972 0.3208 0.6928 0.0556(15) Uiso 1 1 calc R . . H12B H 0.9009 0.2579 0.6561 0.0556(15) Uiso 1 1 calc R . . C213 C 0.6960(2) 0.33759(16) 0.69640(11) 0.0363(4) Uani 1 1 d . . . H13A H 0.6378 0.3861 0.6936 0.0556(15) Uiso 1 1 calc R . . H13B H 0.6765 0.2983 0.6572 0.0556(15) Uiso 1 1 calc R . . C223 C 0.7657(3) 0.22207(15) 0.77008(14) 0.0424(5) Uani 1 1 d . . . H23C H 0.7483 0.1789 0.7334 0.0556(15) Uiso 1 1 calc R . . H23D H 0.7547 0.1944 0.8165 0.0556(15) Uiso 1 1 calc R . . P3 P 0.86883(4) 0.40499(3) 1.00649(2) 0.02365(8) Uani 1 1 d . . . C311 C 0.8375(2) 0.45119(13) 1.09692(10) 0.0312(3) Uani 1 1 d . . . H31A H 0.9017 0.4940 1.1078 0.0556(15) Uiso 1 1 calc R . . H31B H 0.7570 0.4810 1.0960 0.0556(15) Uiso 1 1 calc R . . N311 N 0.83543(19) 0.38580(13) 1.15414(9) 0.0355(4) Uani 1 1 d . . . C321 C 0.7531(2) 0.31364(13) 1.01065(11) 0.0322(4) Uani 1 1 d . . . H32A H 0.6688 0.3369 1.0052 0.0556(15) Uiso 1 1 calc R . . H32B H 0.7685 0.2742 0.9709 0.0556(15) Uiso 1 1 calc R . . N321 N 0.7602(2) 0.26455(12) 1.07862(11) 0.0380(4) Uani 1 1 d . . . C331 C 1.0081(2) 0.33914(18) 1.03213(12) 0.0406(5) Uani 1 1 d . . . H33A H 1.0302 0.3011 0.9925 0.0556(15) Uiso 1 1 calc R . . H33B H 1.0787 0.3778 1.0406 0.0556(15) Uiso 1 1 calc R . . N331 N 0.9870(2) 0.28614(15) 1.09659(11) 0.0425(4) Uani 1 1 d . . . C312 C 0.7380(2) 0.32081(16) 1.14072(12) 0.0394(5) Uani 1 1 d . . . H12C H 0.6585 0.3507 1.1340 0.0556(15) Uiso 1 1 calc R . . H12D H 0.7300 0.2845 1.1831 0.0556(15) Uiso 1 1 calc R . . C313 C 0.9578(3) 0.34075(19) 1.15931(13) 0.0444(5) Uani 1 1 d . . . H13C H 1.0236 0.3839 1.1649 0.0556(15) Uiso 1 1 calc R . . H13D H 0.9578 0.3045 1.2019 0.0556(15) Uiso 1 1 calc R . . C323 C 0.8847(3) 0.22493(15) 1.08665(14) 0.0471(6) Uani 1 1 d . . . H32C H 0.8828 0.1858 1.1275 0.0556(15) Uiso 1 1 calc R . . H32D H 0.9021 0.1902 1.0443 0.0556(15) Uiso 1 1 calc R . . P4 P 0.69861(5) 0.55314(3) 0.92996(2) 0.02589(8) Uani 1 1 d . . . C411 C 0.56423(19) 0.48876(13) 0.96403(11) 0.0320(3) Uani 1 1 d . . . H41A H 0.5503 0.4399 0.9321 0.0556(15) Uiso 1 1 calc R . . H41B H 0.5859 0.4655 1.0108 0.0556(15) Uiso 1 1 calc R . . N411 N 0.44575(19) 0.53884(14) 0.97042(11) 0.0399(4) Uani 1 1 d . . . C431 C 0.6798(2) 0.64565(14) 0.99348(13) 0.0398(5) Uani 1 1 d . . . H43A H 0.7061 0.6272 1.0410 0.0556(15) Uiso 1 1 calc R . . H43B H 0.7346 0.6929 0.9787 0.0556(15) Uiso 1 1 calc R . . N421 N 0.4933(2) 0.64078(15) 0.87283(11) 0.0465(5) Uani 1 1 d . . . C421 C 0.6153(2) 0.60398(15) 0.85248(11) 0.0387(4) Uani 1 1 d . . . H42A H 0.6677 0.6497 0.8325 0.0556(15) Uiso 1 1 calc R . . H42B H 0.6027 0.5605 0.8155 0.0556(15) Uiso 1 1 calc R . . N431 N 0.5492(2) 0.67806(13) 0.99727(11) 0.0450(5) Uani 1 1 d . . . C413 C 0.4632(3) 0.61175(18) 1.02174(13) 0.0473(6) Uani 1 1 d . . . H13E H 0.3821 0.6384 1.0309 0.0556(15) Uiso 1 1 calc R . . H13F H 0.4940 0.5884 1.0668 0.0556(15) Uiso 1 1 calc R . . C412 C 0.4089(2) 0.5746(2) 0.90035(14) 0.0477(6) Uani 1 1 d . . . H12E H 0.4047 0.5273 0.8659 0.0556(15) Uiso 1 1 calc R . . H12F H 0.3253 0.5993 0.9045 0.0556(15) Uiso 1 1 calc R . . C423 C 0.5077(3) 0.70950(17) 0.92699(15) 0.0524(7) Uani 1 1 d . . . H23E H 0.5682 0.7518 0.9096 0.0556(15) Uiso 1 1 calc R . . H23F H 0.4278 0.7391 0.9327 0.0556(15) Uiso 1 1 calc R . . P1 P 0.20202(7) 0.58831(6) 1.20003(4) 0.04983(16) Uani 1 1 d . . . F1 F 0.2710(3) 0.6124(2) 1.27214(16) 0.1162(12) Uani 1 1 d . . . F2 F 0.1333(4) 0.5662(3) 1.12959(17) 0.1566(18) Uani 1 1 d . . . F3 F 0.3231(4) 0.5355(3) 1.1818(2) 0.170(2) Uani 1 1 d . . . F4 F 0.0977(4) 0.6573(4) 1.2146(2) 0.167(2) Uani 1 1 d . . . F5 F 0.2699(4) 0.6631(4) 1.1587(3) 0.178(2) Uani 1 1 d . . . F6 F 0.1381(8) 0.5188(5) 1.2381(3) 0.275(4) Uani 1 1 d . . . O1 O 0.3427(5) 0.4044(2) 1.0656(2) 0.1210(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02652(10) 0.02445(10) 0.02156(9) -0.00129(9) 0.00012(7) -0.00793(8) C51 0.096(3) 0.0474(17) 0.171(5) -0.041(3) 0.072(4) -0.0439(19) C52 0.078(2) 0.079(2) 0.067(2) 0.0266(18) -0.0006(17) -0.050(2) C53 0.0462(15) 0.065(2) 0.137(4) -0.028(2) 0.046(2) -0.0285(15) C54 0.0481(19) 0.146(5) 0.306(10) 0.157(6) -0.086(4) -0.064(3) C55 0.171(6) 0.211(7) 0.0368(15) -0.010(3) -0.002(2) -0.165(6) P2 0.02278(15) 0.02251(17) 0.01958(15) -0.00094(14) 0.00084(12) -0.00205(13) C211 0.0399(9) 0.0298(8) 0.0217(7) 0.0003(6) 0.0037(6) -0.0025(7) N211 0.0404(8) 0.0365(8) 0.0207(6) -0.0037(6) 0.0030(6) 0.0014(7) C221 0.0333(8) 0.0297(8) 0.0360(9) -0.0019(7) -0.0050(7) 0.0075(7) N221 0.0483(10) 0.0290(8) 0.0388(9) -0.0082(7) -0.0040(8) 0.0100(7) C231 0.0250(7) 0.0350(9) 0.0248(7) -0.0024(6) 0.0009(5) -0.0060(6) N231 0.0360(8) 0.0347(8) 0.0291(7) -0.0045(6) -0.0032(6) -0.0089(6) C212 0.0428(11) 0.0435(11) 0.0352(10) -0.0105(9) 0.0100(8) 0.0086(9) C213 0.0389(9) 0.0440(11) 0.0259(8) -0.0035(7) -0.0078(7) -0.0026(8) C223 0.0611(14) 0.0273(9) 0.0388(11) -0.0064(8) -0.0053(10) -0.0068(9) P3 0.02493(17) 0.02561(18) 0.02040(16) 0.00013(14) -0.00171(13) 0.00239(14) C311 0.0414(9) 0.0295(8) 0.0228(7) -0.0033(6) -0.0021(6) 0.0052(7) N311 0.0445(9) 0.0400(9) 0.0219(6) 0.0019(6) -0.0007(6) 0.0082(7) C321 0.0421(9) 0.0253(8) 0.0293(8) 0.0037(6) -0.0071(7) -0.0035(7) N321 0.0530(10) 0.0277(7) 0.0332(8) 0.0097(7) -0.0022(8) 0.0008(7) C331 0.0335(9) 0.0520(12) 0.0363(10) 0.0062(9) 0.0020(7) 0.0178(9) N331 0.0462(10) 0.0480(11) 0.0332(9) 0.0059(7) -0.0038(7) 0.0222(9) C312 0.0456(11) 0.0429(11) 0.0296(9) 0.0099(8) 0.0066(8) 0.0068(9) C313 0.0497(12) 0.0538(14) 0.0297(10) 0.0032(9) -0.0134(8) 0.0127(10) C323 0.0699(16) 0.0328(10) 0.0386(11) 0.0067(8) -0.0030(11) 0.0203(10) P4 0.0349(2) 0.02087(17) 0.02192(18) 0.00035(14) -0.00169(15) 0.00135(15) C411 0.0330(8) 0.0300(9) 0.0329(8) 0.0036(7) 0.0049(6) 0.0038(7) N411 0.0374(9) 0.0440(10) 0.0384(9) 0.0006(8) 0.0051(7) 0.0095(8) C431 0.0534(12) 0.0298(9) 0.0362(10) -0.0084(8) -0.0091(9) 0.0068(8) N421 0.0545(12) 0.0500(12) 0.0349(9) 0.0064(8) -0.0082(8) 0.0200(10) C421 0.0539(11) 0.0379(10) 0.0242(7) 0.0062(7) -0.0007(8) 0.0076(9) N431 0.0648(13) 0.0360(9) 0.0342(9) -0.0046(7) -0.0026(8) 0.0200(9) C413 0.0592(14) 0.0491(13) 0.0335(10) -0.0007(9) 0.0098(10) 0.0226(11) C412 0.0417(11) 0.0582(15) 0.0432(12) -0.0011(10) -0.0088(9) 0.0123(10) C423 0.0743(18) 0.0356(11) 0.0473(13) 0.0057(10) -0.0049(13) 0.0240(11) P1 0.0395(3) 0.0681(5) 0.0419(3) -0.0083(3) -0.0061(2) 0.0016(3) F1 0.127(3) 0.138(3) 0.0831(18) -0.0431(18) -0.0533(18) 0.035(2) F2 0.194(4) 0.199(4) 0.0769(19) -0.017(2) -0.075(2) -0.042(4) F3 0.154(3) 0.208(4) 0.149(4) -0.089(3) -0.035(3) 0.114(3) F4 0.100(2) 0.265(6) 0.137(3) -0.051(4) -0.016(2) 0.099(3) F5 0.124(3) 0.196(5) 0.215(5) 0.081(4) 0.009(4) -0.053(3) F6 0.350(9) 0.303(7) 0.172(4) 0.144(5) -0.074(5) -0.228(7) O1 0.203(5) 0.0626(17) 0.098(2) -0.0165(16) 0.065(3) -0.033(2) 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' F F 0.0171 0.0103 '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' 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 C55 Fe1 C54 40.3(3) . . ? C55 Fe1 C51 36.6(2) . . ? C54 Fe1 C51 64.0(2) . . ? C55 Fe1 C53 65.0(2) . . ? C54 Fe1 C53 39.2(3) . . ? C51 Fe1 C53 62.72(16) . . ? C55 Fe1 C52 62.54(16) . . ? C54 Fe1 C52 63.29(18) . . ? C51 Fe1 C52 37.36(18) . . ? C53 Fe1 C52 36.39(17) . . ? C55 Fe1 P2 152.68(19) . . ? C54 Fe1 P2 115.3(3) . . ? C51 Fe1 P2 133.19(19) . . ? C53 Fe1 P2 87.83(12) . . ? C52 Fe1 P2 97.68(12) . . ? C55 Fe1 P4 106.5(3) . . ? C54 Fe1 P4 146.8(3) . . ? C51 Fe1 P4 87.64(14) . . ? C53 Fe1 P4 141.00(15) . . ? C52 Fe1 P4 104.87(14) . . ? P2 Fe1 P4 96.380(18) . . ? C55 Fe1 P3 97.26(17) . . ? C54 Fe1 P3 91.63(16) . . ? C51 Fe1 P3 130.9(2) . . ? C53 Fe1 P3 123.32(16) . . ? C52 Fe1 P3 154.81(12) . . ? P2 Fe1 P3 95.343(18) . . ? P4 Fe1 P3 94.966(19) . . ? C55 C51 C52 109.5(5) . . ? C55 C51 Fe1 70.6(2) . . ? C52 C51 Fe1 71.66(18) . . ? C55 C51 H51 125.3 . . ? C52 C51 H51 125.3 . . ? Fe1 C51 H51 124.1 . . ? C53 C52 C51 110.5(5) . . ? C53 C52 Fe1 71.65(19) . . ? C51 C52 Fe1 70.98(19) . . ? C53 C52 H52 124.8 . . ? C51 C52 H52 124.8 . . ? Fe1 C52 H52 124.2 . . ? C52 C53 C54 107.6(5) . . ? C52 C53 Fe1 71.96(18) . . ? C54 C53 Fe1 69.3(2) . . ? C52 C53 H53 126.2 . . ? C54 C53 H53 126.2 . . ? Fe1 C53 H53 124.2 . . ? C53 C54 C55 104.7(4) . . ? C53 C54 Fe1 71.4(2) . . ? C55 C54 Fe1 69.7(2) . . ? C53 C54 H54 127.6 . . ? C55 C54 H54 127.6 . . ? Fe1 C54 H54 123.0 . . ? C51 C55 C54 107.6(4) . . ? C51 C55 Fe1 72.8(2) . . ? C54 C55 Fe1 69.9(2) . . ? C51 C55 H55 126.2 . . ? C54 C55 H55 126.2 . . ? Fe1 C55 H55 122.8 . . ? C221 P2 C231 97.72(9) . . ? C221 P2 C211 97.35(10) . . ? C231 P2 C211 96.36(9) . . ? C221 P2 Fe1 117.99(7) . . ? C231 P2 Fe1 124.14(6) . . ? C211 P2 Fe1 117.86(7) . . ? N211 C211 P2 112.92(13) . . ? N211 C211 H21A 109.0 . . ? P2 C211 H21A 109.0 . . ? N211 C211 H21B 109.0 . . ? P2 C211 H21B 109.0 . . ? H21A C211 H21B 107.8 . . ? C212 N211 C213 108.39(18) . . ? C212 N211 C211 110.67(17) . . ? C213 N211 C211 110.69(16) . . ? N221 C221 P2 112.69(14) . . ? N221 C221 H22A 109.1 . . ? P2 C221 H22A 109.1 . . ? N221 C221 H22B 109.1 . . ? P2 C221 H22B 109.1 . . ? H22A C221 H22B 107.8 . . ? C212 N221 C221 111.18(18) . . ? C212 N221 C223 108.5(2) . . ? C221 N221 C223 110.44(18) . . ? N231 C231 P2 112.37(13) . . ? N231 C231 H23A 109.1 . . ? P2 C231 H23A 109.1 . . ? N231 C231 H23B 109.1 . . ? P2 C231 H23B 109.1 . . ? H23A C231 H23B 107.9 . . ? C213 N231 C223 109.34(19) . . ? C213 N231 C231 110.87(17) . . ? C223 N231 C231 112.02(17) . . ? N211 C212 N221 114.69(17) . . ? N211 C212 H12A 108.6 . . ? N221 C212 H12A 108.6 . . ? N211 C212 H12B 108.6 . . ? N221 C212 H12B 108.6 . . ? H12A C212 H12B 107.6 . . ? N231 C213 N211 114.71(17) . . ? N231 C213 H13A 108.6 . . ? N211 C213 H13A 108.6 . . ? N231 C213 H13B 108.6 . . ? N211 C213 H13B 108.6 . . ? H13A C213 H13B 107.6 . . ? N231 C223 N221 113.90(18) . . ? N231 C223 H23C 108.8 . . ? N221 C223 H23C 108.8 . . ? N231 C223 H23D 108.8 . . ? N221 C223 H23D 108.8 . . ? H23C C223 H23D 107.7 . . ? C331 P3 C311 96.78(10) . . ? C331 P3 C321 96.05(11) . . ? C311 P3 C321 97.54(10) . . ? C331 P3 Fe1 118.44(8) . . ? C311 P3 Fe1 116.93(7) . . ? C321 P3 Fe1 125.35(6) . . ? N311 C311 P3 113.61(14) . . ? N311 C311 H31A 108.8 . . ? P3 C311 H31A 108.8 . . ? N311 C311 H31B 108.8 . . ? P3 C311 H31B 108.8 . . ? H31A C311 H31B 107.7 . . ? C312 N311 C311 110.79(16) . . ? C312 N311 C313 108.38(19) . . ? C311 N311 C313 110.85(19) . . ? N321 C321 P3 112.67(14) . . ? N321 C321 H32A 109.1 . . ? P3 C321 H32A 109.1 . . ? N321 C321 H32B 109.1 . . ? P3 C321 H32B 109.1 . . ? H32A C321 H32B 107.8 . . ? C312 N321 C323 108.1(2) . . ? C312 N321 C321 111.61(16) . . ? C323 N321 C321 110.3(2) . . ? N331 C331 P3 112.99(15) . . ? N331 C331 H33A 109.0 . . ? P3 C331 H33A 109.0 . . ? N331 C331 H33B 109.0 . . ? P3 C331 H33B 109.0 . . ? H33A C331 H33B 107.8 . . ? C323 N331 C331 111.7(2) . . ? C323 N331 C313 108.2(2) . . ? C331 N331 C313 111.4(2) . . ? N311 C312 N321 115.16(19) . . ? N311 C312 H12C 108.5 . . ? N321 C312 H12C 108.5 . . ? N311 C312 H12D 108.5 . . ? N321 C312 H12D 108.5 . . ? H12C C312 H12D 107.5 . . ? N331 C313 N311 113.66(18) . . ? N331 C313 H13C 108.8 . . ? N311 C313 H13C 108.8 . . ? N331 C313 H13D 108.8 . . ? N311 C313 H13D 108.8 . . ? H13C C313 H13D 107.7 . . ? N331 C323 N321 114.91(18) . . ? N331 C323 H32C 108.5 . . ? N321 C323 H32C 108.5 . . ? N331 C323 H32D 108.5 . . ? N321 C323 H32D 108.5 . . ? H32C C323 H32D 107.5 . . ? C411 P4 C431 96.16(11) . . ? C411 P4 C421 97.06(11) . . ? C431 P4 C421 96.98(10) . . ? C411 P4 Fe1 122.54(6) . . ? C431 P4 Fe1 117.52(8) . . ? C421 P4 Fe1 120.88(8) . . ? N411 C411 P4 114.00(14) . . ? N411 C411 H41A 108.8 . . ? P4 C411 H41A 108.8 . . ? N411 C411 H41B 108.8 . . ? P4 C411 H41B 108.8 . . ? H41A C411 H41B 107.6 . . ? C412 N411 C411 110.44(18) . . ? C412 N411 C413 108.9(2) . . ? C411 N411 C413 109.73(19) . . ? N431 C431 P4 112.89(16) . . ? N431 C431 H43A 109.0 . . ? P4 C431 H43A 109.0 . . ? N431 C431 H43B 109.0 . . ? P4 C431 H43B 109.0 . . ? H43A C431 H43B 107.8 . . ? C412 N421 C421 111.6(2) . . ? C412 N421 C423 109.0(2) . . ? C421 N421 C423 111.3(2) . . ? N421 C421 P4 112.44(15) . . ? N421 C421 H42A 109.1 . . ? P4 C421 H42A 109.1 . . ? N421 C421 H42B 109.1 . . ? P4 C421 H42B 109.1 . . ? H42A C421 H42B 107.8 . . ? C413 N431 C423 109.0(2) . . ? C413 N431 C431 111.89(19) . . ? C423 N431 C431 110.6(2) . . ? N431 C413 N411 114.11(19) . . ? N431 C413 H13E 108.7 . . ? N411 C413 H13E 108.7 . . ? N431 C413 H13F 108.7 . . ? N411 C413 H13F 108.7 . . ? H13E C413 H13F 107.6 . . ? N421 C412 N411 114.3(2) . . ? N421 C412 H12E 108.7 . . ? N411 C412 H12E 108.7 . . ? N421 C412 H12F 108.7 . . ? N411 C412 H12F 108.7 . . ? H12E C412 H12F 107.6 . . ? N431 C423 N421 114.14(19) . . ? N431 C423 H23E 108.7 . . ? N421 C423 H23E 108.7 . . ? N431 C423 H23F 108.7 . . ? N421 C423 H23F 108.7 . . ? H23E C423 H23F 107.6 . . ? F6 P1 F2 91.8(3) . . ? F6 P1 F4 94.7(4) . . ? F2 P1 F4 87.7(2) . . ? F6 P1 F3 96.4(4) . . ? F2 P1 F3 95.2(2) . . ? F4 P1 F3 168.4(3) . . ? F6 P1 F5 179.6(3) . . ? F2 P1 F5 87.8(3) . . ? F4 P1 F5 85.1(3) . . ? F3 P1 F5 83.9(3) . . ? F6 P1 F1 88.5(3) . . ? F2 P1 F1 179.1(2) . . ? F4 P1 F1 91.4(2) . . ? F3 P1 F1 85.60(19) . . ? F5 P1 F1 91.9(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C55 2.058(3) . ? Fe1 C54 2.061(3) . ? Fe1 C51 2.084(3) . ? Fe1 C53 2.089(3) . ? Fe1 C52 2.093(3) . ? Fe1 P2 2.1900(5) . ? Fe1 P4 2.1924(6) . ? Fe1 P3 2.2013(5) . ? C51 C55 1.301(9) . ? C51 C52 1.338(6) . ? C51 H51 0.9300 . ? C52 C53 1.306(6) . ? C52 H52 0.9300 . ? C53 C54 1.394(9) . ? C53 H53 0.9300 . ? C54 C55 1.420(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? P2 C221 1.855(2) . ? P2 C231 1.8559(17) . ? P2 C211 1.8596(19) . ? C211 N211 1.472(3) . ? C211 H21A 0.9700 . ? C211 H21B 0.9700 . ? N211 C212 1.464(3) . ? N211 C213 1.465(3) . ? C221 N221 1.472(3) . ? C221 H22A 0.9700 . ? C221 H22B 0.9700 . ? N221 C212 1.465(3) . ? N221 C223 1.481(4) . ? C231 N231 1.465(3) . ? C231 H23A 0.9700 . ? C231 H23B 0.9700 . ? N231 C213 1.446(3) . ? N231 C223 1.450(3) . ? C212 H12A 0.9700 . ? C212 H12B 0.9700 . ? C213 H13A 0.9700 . ? C213 H13B 0.9700 . ? C223 H23C 0.9700 . ? C223 H23D 0.9700 . ? P3 C331 1.856(2) . ? P3 C311 1.8582(18) . ? P3 C321 1.868(2) . ? C311 N311 1.465(3) . ? C311 H31A 0.9700 . ? C311 H31B 0.9700 . ? N311 C312 1.460(3) . ? N311 C313 1.476(3) . ? C321 N321 1.476(3) . ? C321 H32A 0.9700 . ? C321 H32B 0.9700 . ? N321 C312 1.463(3) . ? N321 C323 1.464(3) . ? C331 N331 1.468(3) . ? C331 H33A 0.9700 . ? C331 H33B 0.9700 . ? N331 C323 1.449(4) . ? N331 C313 1.472(3) . ? C312 H12C 0.9700 . ? C312 H12D 0.9700 . ? C313 H13C 0.9700 . ? C313 H13D 0.9700 . ? C323 H32C 0.9700 . ? C323 H32D 0.9700 . ? P4 C411 1.850(2) . ? P4 C431 1.860(2) . ? P4 C421 1.865(2) . ? C411 N411 1.481(3) . ? C411 H41A 0.9700 . ? C411 H41B 0.9700 . ? N411 C412 1.469(3) . ? N411 C413 1.484(3) . ? C431 N431 1.477(3) . ? C431 H43A 0.9700 . ? C431 H43B 0.9700 . ? N421 C412 1.450(4) . ? N421 C421 1.465(3) . ? N421 C423 1.468(4) . ? C421 H42A 0.9700 . ? C421 H42B 0.9700 . ? N431 C413 1.443(4) . ? N431 C423 1.463(3) . ? C413 H13E 0.9700 . ? C413 H13F 0.9700 . ? C412 H12E 0.9700 . ? C412 H12F 0.9700 . ? C423 H23E 0.9700 . ? C423 H23F 0.9700 . ? P1 F6 1.451(4) . ? P1 F2 1.540(3) . ? P1 F4 1.558(4) . ? P1 F3 1.559(3) . ? P1 F5 1.560(4) . ? P1 F1 1.575(2) . ?