# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'George Richter-Addo' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Oklahoma 620 Parrington Oval Norman OK 73019 UNITED STATES OF AMERICA ; _publ_contact_author_email GRICHTERADDO@OU.EDU _publ_section_title ; The first structurally characterized nitrosyl heme thiolate model complex ; _publ_section_references ; Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2002) SADABS. Version 2.03. University of Gottingen, Germany Sheldrick, G. M. (2000) SHELXTL. Version 6.10. Bruker AXS, Inc., Madison, Wisconsin, USA. van der Sluis, P. and Spek, A. L. (1990) Acta Cryst., A46, 194-201. ; _publ_section_acknowledgements ; The authors wish to thank the National Science Foundation (CHE-0130835) and the University of Oklahoma for funds to acquire the diffractometer and computers used in this work. ; loop_ _publ_author_name 'G. Richter-Addo' 'Lin Cheng.' 'Douglas R. Powell' 'Nan Xu.' data_gr5129 _database_code_depnum_ccdc_archive 'CCDC 298938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H49 F6 Fe N7 O3 S, 0.5(C6 H14)' _chemical_formula_sum 'C49 H56 F6 Fe N7 O3 S' _chemical_formula_weight 992.92 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' S S 0.1246 0.1234 '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 9.181(5) _cell_length_b 12.455(7) _cell_length_c 21.261(12) _cell_angle_alpha 98.573(9) _cell_angle_beta 94.080(9) _cell_angle_gamma 99.425(9) _cell_volume 2360(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4131 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.26 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8985 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The weak data were truncated at 1.0 Angstrom resolution because data beyond this region were unobserved as evidenced by the Rint values of 0.39 or greater. ; _diffrn_ambient_temperature 100(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 APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9889 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.1525 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 20.82 _reflns_number_total 4873 _reflns_number_gt 2692 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _refine_special_details ; The severely disordered solvent site (near a center of symmetry) was best modeled using the Squeeze program. ; _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4873 _refine_ls_number_parameters 586 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.32552(15) 0.38737(12) 0.29597(7) 0.0231(5) Uani 1 1 d . . . S1 S 0.4008(3) 0.2452(2) 0.22674(13) 0.0265(7) Uani 1 1 d . . . F1 F 0.4880(7) 0.3966(5) 0.0659(3) 0.0485(18) Uani 1 1 d . . . F2 F 0.3296(7) 0.4354(5) -0.0041(3) 0.0487(18) Uani 1 1 d . . . F3 F 0.4570(6) 0.3075(5) -0.0295(3) 0.0453(17) Uani 1 1 d . . . F4 F 0.4432(7) 0.0393(5) 0.3657(3) 0.0500(18) Uani 1 1 d . . . F5 F 0.2783(7) -0.0688(6) 0.4044(3) 0.064(2) Uani 1 1 d . . . F6 F 0.4125(7) -0.1361(5) 0.3346(3) 0.066(2) Uani 1 1 d . . . O1 O 0.2811(8) 0.6025(7) 0.3411(4) 0.044(2) Uani 1 1 d . . . O2 O 0.1674(9) 0.2184(7) -0.0096(4) 0.056(2) Uani 1 1 d . . . O3 O 0.1269(9) -0.1272(7) 0.2808(4) 0.057(3) Uani 1 1 d . . . N1 N 0.2107(8) 0.4229(6) 0.2198(4) 0.020(2) Uani 1 1 d . . . N2 N 0.5142(8) 0.4741(6) 0.2733(4) 0.018(2) Uani 1 1 d . . . N3 N 0.4409(8) 0.3470(7) 0.3707(4) 0.021(2) Uani 1 1 d . . . N4 N 0.1444(8) 0.2904(6) 0.3162(4) 0.023(2) Uani 1 1 d . . . N5 N 0.2928(8) 0.5081(8) 0.3326(4) 0.025(2) Uani 1 1 d . . . N6 N 0.2711(9) 0.2485(7) 0.0947(4) 0.031(2) Uani 1 1 d . . . H6 H 0.3395 0.2950 0.1208 0.037 Uiso 1 1 calc R . . N7 N 0.2449(9) 0.0425(7) 0.2688(4) 0.033(2) Uani 1 1 d . . . H7 H 0.3119 0.0973 0.2895 0.039 Uiso 1 1 calc R . . C1 C 0.0620(11) 0.3838(9) 0.1986(5) 0.028(3) Uani 1 1 d . . . C2 C 0.0231(11) 0.4413(8) 0.1457(5) 0.025(3) Uani 1 1 d . . . C3 C 0.1454(11) 0.5106(9) 0.1341(5) 0.030(3) Uani 1 1 d . . . C4 C 0.2632(11) 0.4985(8) 0.1812(5) 0.022(3) Uani 1 1 d . . . C5 C 0.4110(11) 0.5498(8) 0.1843(5) 0.026(3) Uani 1 1 d . . . H5 H 0.4335 0.5987 0.1546 0.031 Uiso 1 1 calc R . . C6 C 0.5295(11) 0.5376(8) 0.2257(4) 0.025(3) Uani 1 1 d . . . C7 C 0.6798(10) 0.5932(8) 0.2258(5) 0.021(3) Uani 1 1 d U . . C8 C 0.7627(10) 0.5600(8) 0.2742(5) 0.027(3) Uani 1 1 d . . . C9 C 0.6586(11) 0.4882(8) 0.3040(5) 0.025(3) Uani 1 1 d . . . C10 C 0.6904(11) 0.4426(8) 0.3575(5) 0.026(3) Uani 1 1 d . . . H10 H 0.7918 0.4553 0.3739 0.031 Uiso 1 1 calc R . . C11 C 0.5926(11) 0.3812(8) 0.3896(5) 0.023(3) Uani 1 1 d . . . C12 C 0.6272(11) 0.3381(8) 0.4483(5) 0.022(3) Uani 1 1 d . . . C13 C 0.5040(11) 0.2804(8) 0.4647(5) 0.025(3) Uani 1 1 d . . . C14 C 0.3877(10) 0.2861(7) 0.4147(5) 0.019(2) Uani 1 1 d . . . C15 C 0.2390(11) 0.2337(8) 0.4132(5) 0.029(3) Uani 1 1 d . . . H15 H 0.2153 0.1913 0.4459 0.035 Uiso 1 1 calc R . . C16 C 0.1262(10) 0.2384(8) 0.3690(5) 0.017(2) Uani 1 1 d . . . C17 C -0.0280(11) 0.1881(8) 0.3677(5) 0.028(3) Uani 1 1 d . . . C18 C -0.1047(10) 0.2094(8) 0.3151(5) 0.023(3) Uani 1 1 d . . . C19 C 0.0012(10) 0.2712(8) 0.2821(5) 0.023(3) Uani 1 1 d . . . C20 C -0.0333(11) 0.3169(8) 0.2283(5) 0.027(3) Uani 1 1 d . . . H20 H -0.1337 0.2997 0.2104 0.032 Uiso 1 1 calc R . . C21 C -0.1325(11) 0.4181(8) 0.1091(5) 0.033(3) Uani 1 1 d . . . H21A H -0.1415 0.4771 0.0833 0.040 Uiso 1 1 calc R . . H21B H -0.2080 0.4194 0.1401 0.040 Uiso 1 1 calc R . . C22 C -0.1632(11) 0.3048(9) 0.0643(5) 0.039(3) Uani 1 1 d . . . H22A H -0.0883 0.3030 0.0337 0.058 Uiso 1 1 calc R . . H22B H -0.2620 0.2939 0.0411 0.058 Uiso 1 1 calc R . . H22C H -0.1588 0.2459 0.0899 0.058 Uiso 1 1 calc R . . C23 C 0.1601(12) 0.5925(8) 0.0894(5) 0.030(3) Uani 1 1 d . . . H23A H 0.0803 0.5685 0.0538 0.036 Uiso 1 1 calc R . . H23B H 0.2562 0.5929 0.0710 0.036 Uiso 1 1 calc R . . C24 C 0.1520(14) 0.7112(9) 0.1206(6) 0.056(4) Uani 1 1 d . . . H24A H 0.0557 0.7124 0.1376 0.083 Uiso 1 1 calc R . . H24B H 0.1635 0.7601 0.0885 0.083 Uiso 1 1 calc R . . H24C H 0.2316 0.7365 0.1554 0.083 Uiso 1 1 calc R . . C25 C 0.7324(11) 0.6673(8) 0.1796(5) 0.036(3) Uani 1 1 d . . . H25A H 0.6807 0.6372 0.1366 0.044 Uiso 1 1 calc R . . H25B H 0.8401 0.6697 0.1769 0.044 Uiso 1 1 calc R . . C26 C 0.7031(12) 0.7848(9) 0.2002(6) 0.051(4) Uani 1 1 d . . . H26A H 0.5981 0.7819 0.2067 0.076 Uiso 1 1 calc R . . H26B H 0.7284 0.8292 0.1668 0.076 Uiso 1 1 calc R . . H26C H 0.7642 0.8183 0.2402 0.076 Uiso 1 1 calc R . . C27 C 0.9234(10) 0.5962(8) 0.2978(5) 0.030(3) Uani 1 1 d . . . H27A H 0.9772 0.6244 0.2632 0.036 Uiso 1 1 calc R . . H27B H 0.9645 0.5313 0.3078 0.036 Uiso 1 1 calc R . . C28 C 0.9515(11) 0.6852(8) 0.3570(5) 0.036(3) Uani 1 1 d . . . H28A H 0.9033 0.7471 0.3489 0.054 Uiso 1 1 calc R . . H28B H 1.0585 0.7111 0.3669 0.054 Uiso 1 1 calc R . . H28C H 0.9108 0.6546 0.3932 0.054 Uiso 1 1 calc R . . C29 C 0.7802(10) 0.3715(8) 0.4862(5) 0.028(3) Uani 1 1 d . . . H29A H 0.7888 0.3206 0.5174 0.034 Uiso 1 1 calc R . . H29B H 0.8570 0.3625 0.4564 0.034 Uiso 1 1 calc R . . C30 C 0.8113(11) 0.4892(8) 0.5221(5) 0.033(3) Uani 1 1 d . . . H30A H 0.8202 0.5407 0.4913 0.049 Uiso 1 1 calc R . . H30B H 0.9042 0.5011 0.5499 0.049 Uiso 1 1 calc R . . H30C H 0.7297 0.5017 0.5480 0.049 Uiso 1 1 calc R . . C31 C 0.4791(10) 0.2252(8) 0.5225(5) 0.025(3) Uani 1 1 d . . . H31A H 0.4212 0.1500 0.5082 0.030 Uiso 1 1 calc R . . H31B H 0.5764 0.2177 0.5429 0.030 Uiso 1 1 calc R . . C32 C 0.3994(11) 0.2858(9) 0.5710(5) 0.042(3) Uani 1 1 d . . . H32A H 0.4511 0.3624 0.5826 0.064 Uiso 1 1 calc R . . H32B H 0.3972 0.2502 0.6091 0.064 Uiso 1 1 calc R . . H32C H 0.2977 0.2845 0.5531 0.064 Uiso 1 1 calc R . . C33 C -0.0889(11) 0.1245(7) 0.4192(5) 0.028(3) Uani 1 1 d . . . H33A H -0.0341 0.1597 0.4610 0.034 Uiso 1 1 calc R . . H33B H -0.1942 0.1318 0.4217 0.034 Uiso 1 1 calc R . . C34 C -0.0792(13) 0.0018(9) 0.4091(6) 0.054(4) Uani 1 1 d . . . H34A H -0.1186 -0.0318 0.3653 0.082 Uiso 1 1 calc R . . H34B H -0.1375 -0.0346 0.4393 0.082 Uiso 1 1 calc R . . H34C H 0.0246 -0.0067 0.4162 0.082 Uiso 1 1 calc R . . C35 C -0.2685(10) 0.1738(8) 0.2940(5) 0.032(3) Uani 1 1 d . . . H35A H -0.3235 0.1719 0.3323 0.038 Uiso 1 1 calc R . . H35B H -0.3026 0.2293 0.2703 0.038 Uiso 1 1 calc R . . C36 C -0.3052(11) 0.0624(9) 0.2522(6) 0.058(4) Uani 1 1 d . . . H36A H -0.2572 0.0652 0.2126 0.086 Uiso 1 1 calc R . . H36B H -0.4129 0.0422 0.2419 0.086 Uiso 1 1 calc R . . H36C H -0.2694 0.0073 0.2748 0.086 Uiso 1 1 calc R . . C37 C 0.2432(10) 0.1532(8) 0.1840(5) 0.027(3) Uani 1 1 d . . . C38 C 0.1888(10) 0.1659(8) 0.1221(5) 0.025(3) Uani 1 1 d . . . C39 C 0.0644(11) 0.0922(9) 0.0902(5) 0.032(3) Uani 1 1 d . . . H39 H 0.0249 0.1011 0.0492 0.039 Uiso 1 1 calc R . . C40 C -0.0003(11) 0.0063(9) 0.1193(6) 0.040(3) Uani 1 1 d . . . H40 H -0.0841 -0.0435 0.0973 0.048 Uiso 1 1 calc R . . C41 C 0.0523(11) -0.0096(8) 0.1790(6) 0.032(3) Uani 1 1 d . . . H41 H 0.0046 -0.0687 0.1979 0.038 Uiso 1 1 calc R . . C42 C 0.1759(10) 0.0618(8) 0.2109(5) 0.023(3) Uani 1 1 d . . . C43 C 0.2604(12) 0.2665(9) 0.0343(6) 0.031(3) Uani 1 1 d . . . C44 C 0.3843(13) 0.3511(10) 0.0170(5) 0.036(3) Uani 1 1 d . . . C45 C 0.2222(12) -0.0470(9) 0.2959(5) 0.031(3) Uani 1 1 d . . . C46 C 0.3409(14) -0.0527(11) 0.3514(6) 0.044(3) 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 0.0194(9) 0.0231(9) 0.0256(10) 0.0038(7) -0.0024(7) 0.0022(7) S1 0.0214(15) 0.0232(16) 0.0344(18) 0.0049(14) -0.0028(13) 0.0047(13) F1 0.050(4) 0.054(4) 0.033(4) 0.005(3) -0.003(4) -0.013(3) F2 0.063(4) 0.032(4) 0.057(5) 0.017(4) 0.005(4) 0.018(3) F3 0.048(4) 0.049(4) 0.040(4) 0.005(4) 0.004(4) 0.016(3) F4 0.046(4) 0.041(4) 0.064(5) 0.020(4) -0.006(4) 0.008(4) F5 0.052(4) 0.085(6) 0.061(5) 0.037(4) 0.007(4) 0.008(4) F6 0.074(5) 0.049(5) 0.091(6) 0.029(4) 0.004(4) 0.037(4) O1 0.041(5) 0.035(5) 0.055(6) 0.005(4) -0.008(4) 0.011(4) O2 0.053(5) 0.076(6) 0.027(5) 0.004(5) -0.023(5) -0.010(5) O3 0.066(6) 0.036(5) 0.066(6) 0.029(5) -0.014(5) -0.017(5) N1 0.019(5) 0.009(5) 0.033(6) 0.003(4) -0.003(4) 0.005(4) N2 0.017(5) 0.013(5) 0.018(5) -0.010(4) -0.006(4) 0.000(4) N3 0.004(5) 0.042(6) 0.014(5) 0.008(5) -0.003(4) -0.007(4) N4 0.012(5) 0.024(5) 0.029(6) -0.007(5) -0.005(4) 0.002(4) N5 0.011(5) 0.032(6) 0.032(6) 0.011(5) -0.005(4) 0.006(4) N6 0.040(6) 0.034(6) 0.014(6) -0.006(5) -0.005(5) 0.002(5) N7 0.029(5) 0.032(6) 0.037(6) 0.012(5) 0.004(5) -0.003(4) C1 0.021(7) 0.031(7) 0.032(7) -0.004(6) -0.003(6) 0.011(6) C2 0.032(7) 0.030(7) 0.017(6) 0.000(6) 0.003(5) 0.017(6) C3 0.028(7) 0.036(7) 0.027(7) 0.006(6) 0.007(6) 0.006(6) C4 0.027(7) 0.011(6) 0.025(7) -0.003(5) 0.003(5) -0.002(5) C5 0.041(8) 0.012(6) 0.023(7) 0.000(5) 0.005(6) 0.000(6) C6 0.035(7) 0.031(7) 0.006(6) 0.002(6) 0.005(5) -0.002(6) C7 0.024(5) 0.015(5) 0.026(5) 0.008(4) 0.011(4) -0.001(4) C8 0.018(6) 0.026(7) 0.035(7) 0.009(6) 0.005(6) -0.010(5) C9 0.031(7) 0.016(6) 0.022(7) -0.011(5) -0.002(6) 0.002(5) C10 0.023(6) 0.029(7) 0.024(7) -0.007(6) 0.004(6) 0.005(5) C11 0.024(7) 0.027(7) 0.020(7) 0.002(6) -0.002(5) 0.012(5) C12 0.018(6) 0.011(6) 0.035(7) 0.002(5) 0.004(5) 0.000(5) C13 0.025(7) 0.031(7) 0.023(7) 0.008(6) -0.002(6) 0.015(6) C14 0.014(6) 0.011(6) 0.027(7) -0.004(5) -0.002(5) -0.004(5) C15 0.044(8) 0.020(7) 0.030(7) 0.012(6) 0.008(6) 0.011(6) C16 0.008(6) 0.021(6) 0.024(7) 0.016(5) -0.001(5) -0.005(5) C17 0.034(7) 0.026(7) 0.021(7) 0.006(6) 0.000(6) 0.001(6) C18 0.021(6) 0.024(7) 0.022(7) -0.002(5) 0.011(6) 0.005(5) C19 0.012(6) 0.022(6) 0.033(7) -0.007(6) 0.003(6) 0.008(5) C20 0.018(6) 0.021(7) 0.032(7) -0.013(6) -0.002(6) -0.005(5) C21 0.037(7) 0.021(7) 0.043(8) 0.003(6) -0.006(6) 0.015(5) C22 0.030(7) 0.052(8) 0.030(7) 0.002(6) -0.007(6) 0.002(6) C23 0.041(7) 0.019(7) 0.031(7) 0.003(6) -0.006(6) 0.013(5) C24 0.083(10) 0.039(8) 0.060(9) 0.032(7) 0.025(8) 0.027(7) C25 0.025(7) 0.030(7) 0.047(8) 0.005(6) -0.005(6) -0.012(5) C26 0.051(8) 0.046(9) 0.054(9) 0.027(7) -0.004(7) -0.008(7) C27 0.027(7) 0.029(7) 0.034(7) 0.000(6) 0.007(5) 0.008(5) C28 0.032(7) 0.027(7) 0.043(8) -0.004(6) 0.004(6) -0.004(5) C29 0.017(6) 0.039(7) 0.027(7) 0.006(6) 0.000(5) -0.001(5) C30 0.030(6) 0.021(7) 0.040(7) 0.006(6) -0.006(6) -0.010(5) C31 0.021(6) 0.017(6) 0.034(7) 0.003(6) -0.003(5) -0.006(5) C32 0.043(7) 0.054(8) 0.040(8) 0.023(7) 0.006(6) 0.021(7) C33 0.030(6) 0.016(6) 0.038(7) 0.002(5) -0.001(6) 0.011(5) C34 0.061(8) 0.037(8) 0.070(10) 0.014(7) 0.018(7) 0.010(7) C35 0.011(6) 0.028(7) 0.057(8) 0.013(6) 0.008(6) -0.002(5) C36 0.015(6) 0.052(9) 0.094(11) -0.022(8) -0.004(7) 0.008(6) C37 0.025(6) 0.015(6) 0.043(8) 0.013(6) 0.014(6) -0.001(5) C38 0.015(6) 0.025(7) 0.034(7) 0.007(6) -0.006(5) 0.001(5) C39 0.024(7) 0.028(7) 0.042(8) -0.002(6) -0.007(6) 0.009(6) C40 0.026(7) 0.033(8) 0.053(9) -0.002(7) -0.006(6) -0.006(6) C41 0.015(6) 0.023(7) 0.060(9) 0.015(6) 0.000(6) 0.009(5) C42 0.009(6) 0.034(7) 0.022(7) -0.008(6) 0.005(5) 0.002(5) C43 0.036(7) 0.026(7) 0.033(9) 0.001(6) 0.007(7) 0.013(6) C44 0.051(8) 0.044(8) 0.016(7) -0.002(6) 0.008(7) 0.025(7) C45 0.038(7) 0.013(7) 0.042(8) 0.015(6) 0.006(6) -0.005(6) C46 0.052(9) 0.043(9) 0.045(9) 0.021(7) 0.018(7) 0.017(8) _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 Fe1 N5 1.671(9) . ? Fe1 N4 2.003(8) . ? Fe1 N1 2.013(7) . ? Fe1 N2 2.015(8) . ? Fe1 N3 2.017(7) . ? Fe1 S1 2.356(3) . ? S1 C37 1.786(10) . ? F1 C44 1.349(11) . ? F2 C44 1.355(11) . ? F3 C44 1.331(11) . ? F4 C46 1.338(13) . ? F5 C46 1.328(12) . ? F6 C46 1.337(12) . ? O1 N5 1.187(9) . ? O2 C43 1.229(12) . ? O3 C45 1.202(11) . ? N1 C4 1.389(11) . ? N1 C1 1.391(12) . ? N2 C6 1.374(11) . ? N2 C9 1.408(11) . ? N3 C14 1.359(11) . ? N3 C11 1.399(11) . ? N4 C16 1.382(11) . ? N4 C19 1.422(11) . ? N6 C43 1.335(13) . ? N6 C38 1.399(12) . ? N6 H6 0.8800 . ? N7 C45 1.323(12) . ? N7 C42 1.413(12) . ? N7 H7 0.8800 . ? C1 C20 1.362(13) . ? C1 C2 1.474(13) . ? C2 C3 1.362(13) . ? C2 C21 1.539(13) . ? C3 C4 1.464(13) . ? C3 C23 1.490(13) . ? C4 C5 1.394(13) . ? C5 C6 1.394(13) . ? C5 H5 0.9500 . ? C6 C7 1.439(13) . ? C7 C8 1.388(13) . ? C7 C25 1.498(13) . ? C8 C9 1.445(13) . ? C8 C27 1.497(13) . ? C9 C10 1.379(13) . ? C10 C11 1.371(13) . ? C10 H10 0.9500 . ? C11 C12 1.464(13) . ? C12 C13 1.335(13) . ? C12 C29 1.531(13) . ? C13 C14 1.469(12) . ? C13 C31 1.508(13) . ? C14 C15 1.409(13) . ? C15 C16 1.364(12) . ? C15 H15 0.9500 . ? C16 C17 1.448(13) . ? C17 C18 1.363(12) . ? C17 C33 1.530(13) . ? C18 C19 1.429(13) . ? C18 C35 1.512(13) . ? C19 C20 1.390(13) . ? C20 H20 0.9500 . ? C21 C22 1.552(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.543(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.537(14) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.524(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.520(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.491(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.529(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.506(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.414(13) . ? C37 C42 1.422(13) . ? C38 C39 1.403(13) . ? C39 C40 1.387(14) . ? C39 H39 0.9500 . ? C40 C41 1.378(14) . ? C40 H40 0.9500 . ? C41 C42 1.386(13) . ? C41 H41 0.9500 . ? C43 C44 1.524(15) . ? C45 C46 1.567(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Fe1 N4 98.4(3) . . ? N5 Fe1 N1 84.2(3) . . ? N4 Fe1 N1 90.7(3) . . ? N5 Fe1 N2 86.1(3) . . ? N4 Fe1 N2 175.5(3) . . ? N1 Fe1 N2 90.7(3) . . ? N5 Fe1 N3 97.6(3) . . ? N4 Fe1 N3 88.9(3) . . ? N1 Fe1 N3 178.2(3) . . ? N2 Fe1 N3 89.6(3) . . ? N5 Fe1 S1 165.5(3) . . ? N4 Fe1 S1 94.1(2) . . ? N1 Fe1 S1 88.1(2) . . ? N2 Fe1 S1 81.6(2) . . ? N3 Fe1 S1 90.1(2) . . ? C37 S1 Fe1 110.6(3) . . ? C4 N1 C1 106.8(8) . . ? C4 N1 Fe1 125.9(6) . . ? C1 N1 Fe1 127.1(7) . . ? C6 N2 C9 104.1(8) . . ? C6 N2 Fe1 127.5(6) . . ? C9 N2 Fe1 128.3(7) . . ? C14 N3 C11 105.6(7) . . ? C14 N3 Fe1 127.7(6) . . ? C11 N3 Fe1 126.6(7) . . ? C16 N4 C19 105.3(8) . . ? C16 N4 Fe1 128.3(6) . . ? C19 N4 Fe1 126.0(7) . . ? O1 N5 Fe1 159.6(8) . . ? C43 N6 C38 129.0(9) . . ? C43 N6 H6 115.5 . . ? C38 N6 H6 115.5 . . ? C45 N7 C42 128.7(9) . . ? C45 N7 H7 115.6 . . ? C42 N7 H7 115.6 . . ? C20 C1 N1 124.9(9) . . ? C20 C1 C2 126.8(9) . . ? N1 C1 C2 107.7(9) . . ? C3 C2 C1 109.5(9) . . ? C3 C2 C21 127.6(9) . . ? C1 C2 C21 122.9(10) . . ? C2 C3 C4 105.0(9) . . ? C2 C3 C23 129.8(9) . . ? C4 C3 C23 124.9(9) . . ? N1 C4 C5 124.2(9) . . ? N1 C4 C3 111.0(8) . . ? C5 C4 C3 124.7(9) . . ? C4 C5 C6 127.5(9) . . ? C4 C5 H5 116.2 . . ? C6 C5 H5 116.2 . . ? N2 C6 C5 123.3(9) . . ? N2 C6 C7 112.3(8) . . ? C5 C6 C7 124.3(9) . . ? C8 C7 C6 106.4(8) . . ? C8 C7 C25 128.4(9) . . ? C6 C7 C25 125.1(9) . . ? C7 C8 C9 106.0(8) . . ? C7 C8 C27 129.6(9) . . ? C9 C8 C27 124.2(9) . . ? C10 C9 N2 122.7(10) . . ? C10 C9 C8 126.0(9) . . ? N2 C9 C8 111.1(9) . . ? C11 C10 C9 127.4(10) . . ? C11 C10 H10 116.3 . . ? C9 C10 H10 116.3 . . ? C10 C11 N3 125.1(9) . . ? C10 C11 C12 126.7(9) . . ? N3 C11 C12 108.1(9) . . ? C13 C12 C11 109.5(9) . . ? C13 C12 C29 128.4(9) . . ? C11 C12 C29 121.6(9) . . ? C12 C13 C14 104.6(9) . . ? C12 C13 C31 130.2(9) . . ? C14 C13 C31 125.1(9) . . ? N3 C14 C15 124.5(9) . . ? N3 C14 C13 112.1(8) . . ? C15 C14 C13 123.3(9) . . ? C16 C15 C14 125.8(9) . . ? C16 C15 H15 117.1 . . ? C14 C15 H15 117.1 . . ? C15 C16 N4 124.1(9) . . ? C15 C16 C17 126.6(9) . . ? N4 C16 C17 109.3(8) . . ? C18 C17 C16 108.7(9) . . ? C18 C17 C33 127.7(9) . . ? C16 C17 C33 123.6(8) . . ? C17 C18 C19 106.4(9) . . ? C17 C18 C35 127.7(10) . . ? C19 C18 C35 125.9(9) . . ? C20 C19 N4 124.4(10) . . ? C20 C19 C18 124.9(9) . . ? N4 C19 C18 110.3(9) . . ? C1 C20 C19 126.8(9) . . ? C1 C20 H20 116.6 . . ? C19 C20 H20 116.6 . . ? C2 C21 C22 111.9(8) . . ? C2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 114.3(9) . . ? C3 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C3 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 111.3(9) . . ? C7 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C7 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 113.7(8) . . ? C8 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? C8 C27 H27B 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C12 114.2(8) . . ? C30 C29 H29A 108.7 . . ? C12 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? C12 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C13 113.8(8) . . ? C32 C31 H31A 108.8 . . ? C13 C31 H31A 108.8 . . ? C32 C31 H31B 108.8 . . ? C13 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C17 115.4(9) . . ? C34 C33 H33A 108.4 . . ? C17 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? C17 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C18 113.2(8) . . ? C36 C35 H35A 108.9 . . ? C18 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C18 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 119.0(9) . . ? C38 C37 S1 121.2(7) . . ? C42 C37 S1 119.6(8) . . ? N6 C38 C39 123.8(10) . . ? N6 C38 C37 116.5(9) . . ? C39 C38 C37 119.5(10) . . ? C40 C39 C38 119.2(10) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C41 C40 C39 122.6(10) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C40 C41 C42 119.0(10) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C41 C42 N7 121.5(10) . . ? C41 C42 C37 120.5(9) . . ? N7 C42 C37 117.8(9) . . ? O2 C43 N6 127.6(11) . . ? O2 C43 C44 116.4(10) . . ? N6 C43 C44 115.8(10) . . ? F3 C44 F1 105.9(9) . . ? F3 C44 F2 106.6(9) . . ? F1 C44 F2 106.7(9) . . ? F3 C44 C43 112.0(9) . . ? F1 C44 C43 114.0(9) . . ? F2 C44 C43 111.1(9) . . ? O3 C45 N7 128.1(10) . . ? O3 C45 C46 115.9(10) . . ? N7 C45 C46 115.9(10) . . ? F5 C46 F6 108.1(9) . . ? F5 C46 F4 107.6(10) . . ? F6 C46 F4 107.2(10) . . ? F5 C46 C45 111.3(10) . . ? F6 C46 C45 109.9(10) . . ? F4 C46 C45 112.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag #N3 Fe1 N1 C4 -109(11) . . . . ? #N3 Fe1 N1 C1 77(11) . . . . ? #N4 Fe1 N2 C6 113(4) . . . . ? #N4 Fe1 N2 C9 -70(4) . . . . ? #N1 Fe1 N3 C14 -83(11) . . . . ? #N1 Fe1 N3 C11 101(11) . . . . ? #N2 Fe1 N4 C16 79(4) . . . . ? #N2 Fe1 N4 C19 -109(4) . . . . ? N5 Fe1 S1 C37 -113.9(11) . . . . ? N4 Fe1 S1 C37 35.0(4) . . . . ? N1 Fe1 S1 C37 -55.6(4) . . . . ? N2 Fe1 S1 C37 -146.5(4) . . . . ? N3 Fe1 S1 C37 123.9(4) . . . . ? N5 Fe1 N1 C4 76.0(8) . . . . ? N4 Fe1 N1 C4 174.3(7) . . . . ? N2 Fe1 N1 C4 -10.0(7) . . . . ? S1 Fe1 N1 C4 -91.6(7) . . . . ? N5 Fe1 N1 C1 -98.7(8) . . . . ? N4 Fe1 N1 C1 -0.3(8) . . . . ? N2 Fe1 N1 C1 175.3(8) . . . . ? S1 Fe1 N1 C1 93.7(8) . . . . ? N5 Fe1 N2 C6 -78.1(8) . . . . ? N1 Fe1 N2 C6 6.1(8) . . . . ? N3 Fe1 N2 C6 -175.7(7) . . . . ? S1 Fe1 N2 C6 94.1(7) . . . . ? N5 Fe1 N2 C9 98.4(8) . . . . ? N1 Fe1 N2 C9 -177.4(7) . . . . ? N3 Fe1 N2 C9 0.8(8) . . . . ? S1 Fe1 N2 C9 -89.4(7) . . . . ? N5 Fe1 N3 C14 92.4(8) . . . . ? N4 Fe1 N3 C14 -5.9(8) . . . . ? N2 Fe1 N3 C14 178.4(8) . . . . ? S1 Fe1 N3 C14 -100.0(8) . . . . ? N5 Fe1 N3 C11 -84.2(8) . . . . ? N4 Fe1 N3 C11 177.5(8) . . . . ? N2 Fe1 N3 C11 1.8(8) . . . . ? S1 Fe1 N3 C11 83.5(8) . . . . ? N5 Fe1 N4 C16 -89.2(8) . . . . ? N1 Fe1 N4 C16 -173.5(8) . . . . ? N3 Fe1 N4 C16 8.3(8) . . . . ? S1 Fe1 N4 C16 98.3(8) . . . . ? N5 Fe1 N4 C19 82.9(8) . . . . ? N1 Fe1 N4 C19 -1.4(7) . . . . ? N3 Fe1 N4 C19 -179.6(7) . . . . ? S1 Fe1 N4 C19 -89.5(7) . . . . ? N4 Fe1 N5 O1 -133(2) . . . . ? N1 Fe1 N5 O1 -43(2) . . . . ? N2 Fe1 N5 O1 48(2) . . . . ? N3 Fe1 N5 O1 137(2) . . . . ? S1 Fe1 N5 O1 15(3) . . . . ? C4 N1 C1 C20 -172.7(9) . . . . ? Fe1 N1 C1 C20 2.8(14) . . . . ? C4 N1 C1 C2 -1.5(10) . . . . ? Fe1 N1 C1 C2 174.0(6) . . . . ? C20 C1 C2 C3 172.7(10) . . . . ? N1 C1 C2 C3 1.7(11) . . . . ? C20 C1 C2 C21 -10.1(16) . . . . ? N1 C1 C2 C21 178.9(8) . . . . ? C1 C2 C3 C4 -1.1(11) . . . . ? C21 C2 C3 C4 -178.1(9) . . . . ? C1 C2 C3 C23 -174.5(9) . . . . ? C21 C2 C3 C23 8.5(18) . . . . ? C1 N1 C4 C5 -174.9(9) . . . . ? Fe1 N1 C4 C5 9.6(13) . . . . ? C1 N1 C4 C3 0.9(10) . . . . ? Fe1 N1 C4 C3 -174.7(6) . . . . ? C2 C3 C4 N1 0.2(11) . . . . ? C23 C3 C4 N1 174.0(9) . . . . ? C2 C3 C4 C5 175.9(9) . . . . ? C23 C3 C4 C5 -10.3(16) . . . . ? N1 C4 C5 C6 -1.4(16) . . . . ? C3 C4 C5 C6 -176.6(9) . . . . ? C9 N2 C6 C5 -178.2(9) . . . . ? Fe1 N2 C6 C5 -1.0(13) . . . . ? C9 N2 C6 C7 -0.8(10) . . . . ? Fe1 N2 C6 C7 176.5(6) . . . . ? C4 C5 C6 N2 -3.2(16) . . . . ? C4 C5 C6 C7 179.7(9) . . . . ? N2 C6 C7 C8 1.9(11) . . . . ? C5 C6 C7 C8 179.4(9) . . . . ? N2 C6 C7 C25 179.3(9) . . . . ? C5 C6 C7 C25 -3.2(16) . . . . ? C6 C7 C8 C9 -2.2(11) . . . . ? C25 C7 C8 C9 -179.4(9) . . . . ? C6 C7 C8 C27 -176.5(10) . . . . ? C25 C7 C8 C27 6.2(18) . . . . ? C6 N2 C9 C10 176.1(9) . . . . ? Fe1 N2 C9 C10 -1.1(13) . . . . ? C6 N2 C9 C8 -0.6(10) . . . . ? Fe1 N2 C9 C8 -177.8(6) . . . . ? C7 C8 C9 C10 -174.8(9) . . . . ? C27 C8 C9 C10 -0.1(16) . . . . ? C7 C8 C9 N2 1.8(11) . . . . ? C27 C8 C9 N2 176.6(8) . . . . ? N2 C9 C10 C11 -1.7(16) . . . . ? C8 C9 C10 C11 174.6(10) . . . . ? C9 C10 C11 N3 4.7(17) . . . . ? C9 C10 C11 C12 -176.7(9) . . . . ? C14 N3 C11 C10 178.2(9) . . . . ? Fe1 N3 C11 C10 -4.6(14) . . . . ? C14 N3 C11 C12 -0.7(10) . . . . ? Fe1 N3 C11 C12 176.5(6) . . . . ? C10 C11 C12 C13 -178.8(10) . . . . ? N3 C11 C12 C13 0.1(11) . . . . ? C10 C11 C12 C29 8.4(15) . . . . ? N3 C11 C12 C29 -172.7(8) . . . . ? C11 C12 C13 C14 0.5(11) . . . . ? C29 C12 C13 C14 172.7(9) . . . . ? C11 C12 C13 C31 -176.3(9) . . . . ? C29 C12 C13 C31 -4.1(18) . . . . ? C11 N3 C14 C15 -178.8(9) . . . . ? Fe1 N3 C14 C15 4.0(14) . . . . ? C11 N3 C14 C13 1.0(10) . . . . ? Fe1 N3 C14 C13 -176.1(6) . . . . ? C12 C13 C14 N3 -1.0(11) . . . . ? C31 C13 C14 N3 176.0(9) . . . . ? C12 C13 C14 C15 178.9(9) . . . . ? C31 C13 C14 C15 -4.1(15) . . . . ? N3 C14 C15 C16 -1.9(16) . . . . ? C13 C14 C15 C16 178.3(9) . . . . ? C14 C15 C16 N4 4.4(16) . . . . ? C14 C15 C16 C17 -178.0(10) . . . . ? C19 N4 C16 C15 177.5(9) . . . . ? Fe1 N4 C16 C15 -9.1(14) . . . . ? C19 N4 C16 C17 -0.4(10) . . . . ? Fe1 N4 C16 C17 173.0(6) . . . . ? C15 C16 C17 C18 -178.4(10) . . . . ? N4 C16 C17 C18 -0.5(11) . . . . ? C15 C16 C17 C33 2.8(16) . . . . ? N4 C16 C17 C33 -179.3(8) . . . . ? C16 C17 C18 C19 1.2(11) . . . . ? C33 C17 C18 C19 179.9(9) . . . . ? C16 C17 C18 C35 -179.8(9) . . . . ? C33 C17 C18 C35 -1.1(17) . . . . ? C16 N4 C19 C20 174.5(9) . . . . ? Fe1 N4 C19 C20 0.9(13) . . . . ? C16 N4 C19 C18 1.2(10) . . . . ? Fe1 N4 C19 C18 -172.4(6) . . . . ? C17 C18 C19 C20 -174.8(9) . . . . ? C35 C18 C19 C20 6.2(16) . . . . ? C17 C18 C19 N4 -1.5(11) . . . . ? C35 C18 C19 N4 179.5(9) . . . . ? N1 C1 C20 C19 -3.8(17) . . . . ? C2 C1 C20 C19 -173.3(9) . . . . ? N4 C19 C20 C1 1.8(16) . . . . ? C18 C19 C20 C1 174.2(10) . . . . ? C3 C2 C21 C22 104.1(12) . . . . ? C1 C2 C21 C22 -72.6(12) . . . . ? C2 C3 C23 C24 95.1(13) . . . . ? C4 C3 C23 C24 -77.1(13) . . . . ? C8 C7 C25 C26 -100.3(12) . . . . ? C6 C7 C25 C26 82.9(12) . . . . ? C7 C8 C27 C28 97.4(13) . . . . ? C9 C8 C27 C28 -76.1(13) . . . . ? C13 C12 C29 C30 -99.2(12) . . . . ? C11 C12 C29 C30 72.2(12) . . . . ? C12 C13 C31 C32 104.7(12) . . . . ? C14 C13 C31 C32 -71.6(12) . . . . ? C18 C17 C33 C34 94.2(13) . . . . ? C16 C17 C33 C34 -87.3(12) . . . . ? C17 C18 C35 C36 -88.4(13) . . . . ? C19 C18 C35 C36 90.4(12) . . . . ? Fe1 S1 C37 C38 95.2(8) . . . . ? Fe1 S1 C37 C42 -88.4(8) . . . . ? C43 N6 C38 C39 -7.6(16) . . . . ? C43 N6 C38 C37 167.8(9) . . . . ? C42 C37 C38 N6 -171.8(8) . . . . ? S1 C37 C38 N6 4.6(13) . . . . ? C42 C37 C38 C39 3.8(14) . . . . ? S1 C37 C38 C39 -179.7(7) . . . . ? N6 C38 C39 C40 173.4(9) . . . . ? C37 C38 C39 C40 -1.9(15) . . . . ? C38 C39 C40 C41 0.4(16) . . . . ? C39 C40 C41 C42 -1.0(16) . . . . ? C40 C41 C42 N7 -172.7(9) . . . . ? C40 C41 C42 C37 3.0(14) . . . . ? C45 N7 C42 C41 10.7(15) . . . . ? C45 N7 C42 C37 -165.1(10) . . . . ? C38 C37 C42 C41 -4.4(14) . . . . ? S1 C37 C42 C41 179.1(7) . . . . ? C38 C37 C42 N7 171.5(8) . . . . ? S1 C37 C42 N7 -5.1(12) . . . . ? C38 N6 C43 O2 5.7(17) . . . . ? C38 N6 C43 C44 -169.6(9) . . . . ? O2 C43 C44 F3 -55.9(12) . . . . ? N6 C43 C44 F3 120.0(10) . . . . ? O2 C43 C44 F1 -176.2(9) . . . . ? N6 C43 C44 F1 -0.3(13) . . . . ? O2 C43 C44 F2 63.2(12) . . . . ? N6 C43 C44 F2 -120.9(10) . . . . ? C42 N7 C45 O3 -8.7(19) . . . . ? C42 N7 C45 C46 166.5(9) . . . . ? O3 C45 C46 F5 -59.1(14) . . . . ? N7 C45 C46 F5 125.2(11) . . . . ? O3 C45 C46 F6 60.7(14) . . . . ? N7 C45 C46 F6 -115.1(11) . . . . ? O3 C45 C46 F4 -179.9(10) . . . . ? N7 C45 C46 F4 4.3(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6 S1 0.88 2.47 2.980(9) 117.0 . N6 H6 F1 0.88 2.22 2.655(10) 110.2 . N7 H7 S1 0.88 2.50 2.982(9) 115.4 . N7 H7 F4 0.88 2.23 2.660(10) 110.1 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.520 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.100 #===END # Attachment '(P)Fe(SR)_1.cif' data_gr5135 _database_code_depnum_ccdc_archive 'CCDC 298939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H49 F6 Fe N6 O2 S, 0.5(C6 H14)' _chemical_formula_sum 'C49 H56 F6 Fe N6 O2 S' _chemical_formula_weight 962.91 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' S S 0.1246 0.1234 '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 8.9881(14) _cell_length_b 13.208(2) _cell_length_c 19.879(3) _cell_angle_alpha 100.889(5) _cell_angle_beta 91.761(5) _cell_angle_gamma 101.373(5) _cell_volume 2266.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7774 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.24 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8765 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18050 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8813 _reflns_number_gt 6779 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _refine_special_details ; The solvent, which sat on an inversion center, was severely disordered and was best modeled using the Squeeze program. ; _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^)+(0.1000P)^2^+1.1000P] 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 8813 _refine_ls_number_parameters 584 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.32499(4) 0.36001(3) 0.29710(2) 0.02440(14) Uani 1 1 d . . . S1 S 0.39744(8) 0.22743(6) 0.21544(4) 0.03073(19) Uani 1 1 d . . . F1 F 0.4616(3) 0.41500(19) 0.06669(11) 0.0637(7) Uani 1 1 d . . . F2 F 0.3159(3) 0.43792(18) -0.01409(12) 0.0600(6) Uani 1 1 d . . . F3 F 0.4596(3) 0.3266(2) -0.03561(12) 0.0638(6) Uani 1 1 d . . . F4 F 0.3963(2) 0.02574(18) 0.35736(12) 0.0550(6) Uani 1 1 d . . . F5 F 0.2131(3) -0.0602(2) 0.39993(12) 0.0810(9) Uani 1 1 d . . . F6 F 0.3297(4) -0.1401(2) 0.32272(18) 0.1007(11) Uani 1 1 d . . . O1 O 0.1470(4) 0.2380(3) -0.02288(14) 0.0744(10) Uani 1 1 d . . . O2 O 0.0503(3) -0.1103(2) 0.27116(13) 0.0507(7) Uani 1 1 d . . . N1 N 0.1917(3) 0.42318(19) 0.23742(13) 0.0303(6) Uani 1 1 d . . . N2 N 0.5028(3) 0.4816(2) 0.28983(13) 0.0318(6) Uani 1 1 d . . . N3 N 0.4391(3) 0.34610(18) 0.38553(12) 0.0256(5) Uani 1 1 d . . . N4 N 0.1287(3) 0.28575(18) 0.33252(12) 0.0253(5) Uani 1 1 d . A . N5 N 0.2522(3) 0.2579(2) 0.08775(14) 0.0391(7) Uani 1 1 d . . . H5N H 0.335(4) 0.295(3) 0.117(2) 0.047 Uiso 1 1 d . . . N6 N 0.2105(3) 0.0402(2) 0.25641(14) 0.0325(6) Uani 1 1 d . . . H6N H 0.299(4) 0.090(3) 0.2756(18) 0.039 Uiso 1 1 d . . . C1 C 0.0381(3) 0.3860(2) 0.21839(16) 0.0310(7) Uani 1 1 d . . . C2 C -0.0080(4) 0.4374(3) 0.16509(17) 0.0379(8) Uani 1 1 d . . . C3 C 0.1181(4) 0.5057(3) 0.15191(17) 0.0388(8) Uani 1 1 d . . . C4 C 0.2434(4) 0.4964(2) 0.19702(16) 0.0348(7) Uani 1 1 d . . . C5 C 0.3909(4) 0.5509(3) 0.19895(17) 0.0371(8) Uani 1 1 d . . . H5 H 0.4117 0.5976 0.1679 0.044 Uiso 1 1 calc R . . C6 C 0.5124(4) 0.5448(2) 0.24151(16) 0.0330(7) Uani 1 1 d . . . C7 C 0.6662(4) 0.6045(3) 0.24255(16) 0.0359(7) Uani 1 1 d . . . C8 C 0.7513(4) 0.5761(3) 0.29102(16) 0.0347(7) Uani 1 1 d . . . C9 C 0.6485(3) 0.5002(2) 0.32035(15) 0.0315(7) Uani 1 1 d . . . C10 C 0.6879(3) 0.4547(2) 0.37378(16) 0.0310(7) Uani 1 1 d . . . H10 H 0.7915 0.4732 0.3908 0.037 Uiso 1 1 calc R . . C11 C 0.5910(3) 0.3845(2) 0.40503(14) 0.0261(6) Uani 1 1 d . . . C12 C 0.6361(3) 0.3426(2) 0.46247(14) 0.0271(6) Uani 1 1 d . A . C13 C 0.5104(4) 0.2771(2) 0.47731(14) 0.0318(7) Uani 1 1 d DU . . C14 C 0.3867(3) 0.2805(2) 0.42987(14) 0.0279(6) Uani 1 1 d . A . C15 C 0.2375(4) 0.2280(2) 0.43002(15) 0.0298(7) Uani 1 1 d . . . H15 H 0.2155 0.1856 0.4636 0.036 Uiso 1 1 calc R A . C16 C 0.1165(3) 0.2314(2) 0.38569(15) 0.0273(6) Uani 1 1 d . A . C17 C -0.0401(3) 0.1784(2) 0.38831(16) 0.0308(7) Uani 1 1 d . . . C18 C -0.1212(3) 0.2012(2) 0.33594(16) 0.0310(7) Uani 1 1 d . A . C19 C -0.0159(3) 0.2688(2) 0.30177(16) 0.0281(6) Uani 1 1 d . . . C20 C -0.0560(3) 0.3136(2) 0.24850(16) 0.0320(7) Uani 1 1 d . A . H20 H -0.1590 0.2925 0.2305 0.038 Uiso 1 1 calc R . . C21 C -0.1662(4) 0.4139(3) 0.13126(19) 0.0457(9) Uani 1 1 d . . . H21A H -0.1818 0.4748 0.1116 0.055 Uiso 1 1 calc R . . H21B H -0.2409 0.4040 0.1663 0.055 Uiso 1 1 calc R . . C22 C -0.1944(5) 0.3156(3) 0.0746(2) 0.0611(12) Uani 1 1 d . . . H22A H -0.1235 0.3263 0.0389 0.092 Uiso 1 1 d R . . H22B H -0.2991 0.3021 0.0546 0.092 Uiso 1 1 d R . . H22C H -0.1787 0.2552 0.0939 0.092 Uiso 1 1 d R . . C23 C 0.1319(4) 0.5802(3) 0.10184(19) 0.0477(9) Uani 1 1 d . . . H23A H 0.0421 0.5585 0.0684 0.057 Uiso 1 1 calc R . . H23B H 0.2234 0.5747 0.0761 0.057 Uiso 1 1 calc R . . C24 C 0.1434(6) 0.6947(3) 0.1375(2) 0.0639(12) Uani 1 1 d . . . H24A H 0.0554 0.7002 0.1648 0.096 Uiso 1 1 d R . . H24B H 0.1451 0.7388 0.1029 0.096 Uiso 1 1 d R . . H24C H 0.2370 0.7187 0.1677 0.096 Uiso 1 1 d R . . C25 C 0.7153(4) 0.6825(3) 0.19687(19) 0.0460(9) Uani 1 1 d . . . H25A H 0.8274 0.6956 0.1957 0.055 Uiso 1 1 calc R . . H25B H 0.6707 0.6515 0.1495 0.055 Uiso 1 1 calc R . . C26 C 0.6677(5) 0.7855(3) 0.2206(2) 0.0574(11) Uani 1 1 d . . . H26A H 0.5574 0.7726 0.2244 0.086 Uiso 1 1 d R . . H26B H 0.6950 0.8310 0.1874 0.086 Uiso 1 1 d R . . H26C H 0.7197 0.8201 0.2655 0.086 Uiso 1 1 d R . . C27 C 0.9189(4) 0.6173(3) 0.31271(17) 0.0402(8) Uani 1 1 d . . . H27A H 0.9651 0.5585 0.3214 0.048 Uiso 1 1 calc R . . H27B H 0.9707 0.6455 0.2749 0.048 Uiso 1 1 calc R . . C28 C 0.9438(4) 0.7029(3) 0.37654(19) 0.0469(9) Uani 1 1 d . . . H28A H 0.8927 0.7593 0.3691 0.070 Uiso 1 1 d R . . H28B H 1.0530 0.7314 0.3867 0.070 Uiso 1 1 d R . . H28C H 0.9017 0.6734 0.4153 0.070 Uiso 1 1 d R . . C29 C 0.7911(4) 0.3711(2) 0.49906(16) 0.0318(7) Uani 1 1 d . . . H29A H 0.8689 0.3762 0.4650 0.038 Uiso 1 1 calc R A . H29B H 0.8051 0.3146 0.5236 0.038 Uiso 1 1 calc R . . C30 C 0.8146(4) 0.4758(3) 0.55053(17) 0.0402(8) Uani 1 1 d . A . H30A H 0.8112 0.5330 0.5259 0.060 Uiso 1 1 d R . . H30B H 0.9138 0.4889 0.5761 0.060 Uiso 1 1 d R . . H30C H 0.7340 0.4725 0.5826 0.060 Uiso 1 1 d R . . C31 C 0.5056(11) 0.2084(5) 0.5308(3) 0.0300(19) Uani 0.727(8) 1 d PDU A 1 H31A H 0.4289 0.1424 0.5154 0.036 Uiso 0.727(8) 1 calc PR A 1 H31B H 0.6060 0.1899 0.5368 0.036 Uiso 0.727(8) 1 calc PR A 1 C32 C 0.4652(6) 0.2678(4) 0.5983(2) 0.0456(15) Uani 0.727(8) 1 d PDU A 1 H32A H 0.5465 0.3295 0.6156 0.068 Uiso 0.727(8) 1 d PR A 1 H32B H 0.4532 0.2215 0.6318 0.068 Uiso 0.727(8) 1 d PR A 1 H32C H 0.3696 0.2907 0.5913 0.068 Uiso 0.727(8) 1 d PR A 1 C31' C 0.472(3) 0.2287(10) 0.5400(6) 0.035(5) Uani 0.273(8) 1 d PDU A 2 H31C H 0.5481 0.2638 0.5787 0.042 Uiso 0.273(8) 1 calc PR A 2 H31D H 0.3707 0.2388 0.5541 0.042 Uiso 0.273(8) 1 calc PR A 2 C32' C 0.4734(16) 0.1118(8) 0.5222(7) 0.048(4) Uani 0.273(8) 1 d PDU A 2 H32D H 0.3993 0.0777 0.4833 0.071 Uiso 0.273(8) 1 d PR A 2 H32E H 0.4464 0.0798 0.5620 0.071 Uiso 0.273(8) 1 d PR A 2 H32F H 0.5752 0.1024 0.5097 0.071 Uiso 0.273(8) 1 d PR A 2 C33 C -0.0987(4) 0.1152(3) 0.44086(17) 0.0378(8) Uani 1 1 d . A . H33A H -0.1898 0.1391 0.4592 0.045 Uiso 1 1 calc R . . H33B H -0.0202 0.1302 0.4795 0.045 Uiso 1 1 calc R . . C34 C -0.1399(6) -0.0020(3) 0.4146(2) 0.0641(13) Uani 1 1 d . . . H34A H -0.2248 -0.0186 0.3796 0.096 Uiso 1 1 d R A . H34B H -0.1698 -0.0374 0.4527 0.096 Uiso 1 1 d R . . H34C H -0.0519 -0.0264 0.3945 0.096 Uiso 1 1 d R . . C35 C -0.2871(3) 0.1639(3) 0.31469(19) 0.0380(8) Uani 1 1 d . . . H35A H -0.3285 0.2229 0.3029 0.046 Uiso 1 1 calc R A . H35B H -0.3413 0.1413 0.3537 0.046 Uiso 1 1 calc R . . C36 C -0.3161(4) 0.0719(3) 0.25283(19) 0.0437(8) Uani 1 1 d . A . H36A H -0.2681 0.0952 0.2133 0.066 Uiso 1 1 d R . . H36B H -0.4259 0.0476 0.2418 0.066 Uiso 1 1 d R . . H36C H -0.2729 0.0139 0.2639 0.066 Uiso 1 1 d R . . C37 C 0.2226(3) 0.1515(2) 0.17343(15) 0.0302(7) Uani 1 1 d . . . C38 C 0.1653(4) 0.1730(3) 0.11251(16) 0.0345(7) Uani 1 1 d . . . C39 C 0.0324(4) 0.1110(3) 0.07764(17) 0.0401(8) Uani 1 1 d . . . H39 H -0.0063 0.1268 0.0367 0.048 Uiso 1 1 calc R . . C40 C -0.0422(4) 0.0269(3) 0.10269(17) 0.0419(8) Uani 1 1 d . . . H40 H -0.1331 -0.0153 0.0787 0.050 Uiso 1 1 calc R . . C41 C 0.0113(4) 0.0015(3) 0.16240(17) 0.0389(8) Uani 1 1 d . . . H41 H -0.0420 -0.0573 0.1790 0.047 Uiso 1 1 calc R . . C42 C 0.1448(4) 0.0640(2) 0.19744(16) 0.0319(7) Uani 1 1 d . . . C43 C 0.2427(5) 0.2799(3) 0.02455(18) 0.0488(9) Uani 1 1 d . . . C44 C 0.3717(4) 0.3668(3) 0.01163(17) 0.0447(9) Uani 1 1 d . . . C45 C 0.1652(4) -0.0434(3) 0.28527(17) 0.0358(7) Uani 1 1 d . . . C46 C 0.2811(4) -0.0534(3) 0.34136(19) 0.0441(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 Fe1 0.0235(2) 0.0217(2) 0.0262(2) 0.00946(17) -0.00898(16) -0.00246(16) S1 0.0277(4) 0.0341(4) 0.0297(4) 0.0114(3) -0.0048(3) 0.0010(3) F1 0.0778(17) 0.0683(16) 0.0364(12) 0.0213(11) -0.0017(11) -0.0148(13) F2 0.0771(16) 0.0580(14) 0.0570(14) 0.0314(12) 0.0128(12) 0.0223(12) F3 0.0702(16) 0.0794(17) 0.0480(13) 0.0214(12) 0.0092(12) 0.0210(13) F4 0.0377(11) 0.0651(15) 0.0666(14) 0.0377(12) -0.0054(10) -0.0010(10) F5 0.0636(16) 0.122(2) 0.0541(15) 0.0534(16) -0.0041(12) -0.0223(15) F6 0.129(3) 0.071(2) 0.112(2) 0.0123(17) -0.034(2) 0.058(2) O1 0.084(2) 0.088(2) 0.0398(15) 0.0285(15) -0.0270(15) -0.0196(18) O2 0.0508(16) 0.0422(15) 0.0526(15) 0.0148(12) -0.0013(12) -0.0099(12) N1 0.0311(14) 0.0240(13) 0.0334(14) 0.0095(11) -0.0129(11) -0.0017(10) N2 0.0322(14) 0.0292(14) 0.0320(14) 0.0153(11) -0.0119(11) -0.0046(11) N3 0.0264(12) 0.0234(12) 0.0252(12) 0.0083(10) -0.0073(10) -0.0006(10) N4 0.0224(12) 0.0211(12) 0.0298(13) 0.0042(10) -0.0047(10) 0.0004(10) N5 0.0445(17) 0.0412(17) 0.0292(14) 0.0112(12) -0.0091(12) 0.0013(13) N6 0.0311(14) 0.0308(14) 0.0342(14) 0.0078(12) -0.0009(11) 0.0026(11) C1 0.0279(16) 0.0266(16) 0.0369(16) 0.0055(13) -0.0097(13) 0.0047(12) C2 0.0404(19) 0.0323(17) 0.0400(18) 0.0083(14) -0.0173(15) 0.0069(14) C3 0.0435(19) 0.0356(18) 0.0368(18) 0.0113(14) -0.0157(15) 0.0059(15) C4 0.0398(18) 0.0288(16) 0.0338(16) 0.0113(13) -0.0135(14) -0.0001(13) C5 0.0437(19) 0.0336(17) 0.0337(17) 0.0170(14) -0.0078(14) -0.0008(14) C6 0.0337(17) 0.0303(16) 0.0333(16) 0.0103(13) -0.0073(13) 0.0003(13) C7 0.0386(18) 0.0365(18) 0.0312(16) 0.0104(14) -0.0012(13) 0.0011(14) C8 0.0321(17) 0.0354(18) 0.0335(16) 0.0080(14) -0.0037(13) -0.0003(14) C9 0.0322(16) 0.0307(16) 0.0291(15) 0.0096(13) -0.0077(12) -0.0016(13) C10 0.0267(15) 0.0300(16) 0.0334(16) 0.0092(13) -0.0091(12) -0.0022(12) C11 0.0302(15) 0.0213(14) 0.0247(14) 0.0047(12) -0.0073(12) 0.0012(12) C12 0.0337(16) 0.0207(14) 0.0251(14) 0.0038(12) -0.0089(12) 0.0036(12) C13 0.0418(18) 0.0244(15) 0.0260(15) 0.0076(12) -0.0122(13) -0.0010(13) C14 0.0360(16) 0.0206(14) 0.0242(14) 0.0054(11) -0.0083(12) -0.0003(12) C15 0.0399(17) 0.0229(15) 0.0244(14) 0.0089(12) -0.0020(12) -0.0024(13) C16 0.0301(15) 0.0192(14) 0.0292(15) 0.0018(12) 0.0000(12) 0.0002(12) C17 0.0297(16) 0.0223(15) 0.0358(16) -0.0008(13) 0.0059(13) 0.0000(12) C18 0.0244(15) 0.0255(15) 0.0394(17) -0.0016(13) 0.0035(13) 0.0036(12) C19 0.0233(14) 0.0223(15) 0.0355(16) 0.0013(12) -0.0024(12) 0.0023(11) C20 0.0216(15) 0.0291(16) 0.0424(18) 0.0019(14) -0.0093(13) 0.0048(12) C21 0.0398(19) 0.045(2) 0.052(2) 0.0106(17) -0.0219(16) 0.0108(16) C22 0.050(2) 0.060(3) 0.066(3) -0.005(2) -0.031(2) 0.016(2) C23 0.048(2) 0.049(2) 0.047(2) 0.0206(17) -0.0177(17) 0.0051(17) C24 0.082(3) 0.058(3) 0.067(3) 0.033(2) 0.011(2) 0.028(2) C25 0.0407(19) 0.050(2) 0.045(2) 0.0196(17) -0.0019(16) -0.0059(16) C26 0.057(2) 0.044(2) 0.067(3) 0.022(2) -0.016(2) -0.0054(19) C27 0.0399(19) 0.044(2) 0.0359(17) 0.0151(15) 0.0022(14) 0.0003(15) C28 0.047(2) 0.038(2) 0.052(2) 0.0192(17) -0.0126(17) -0.0059(16) C29 0.0342(16) 0.0294(16) 0.0321(16) 0.0076(13) -0.0106(13) 0.0083(13) C30 0.0346(18) 0.0404(19) 0.0399(18) -0.0011(15) -0.0162(14) 0.0054(15) C31 0.035(5) 0.029(3) 0.029(3) 0.013(2) -0.002(2) 0.007(2) C32 0.063(3) 0.055(3) 0.029(3) 0.016(2) 0.012(2) 0.026(3) C31' 0.023(10) 0.035(8) 0.049(11) 0.024(8) -0.024(7) 0.001(7) C32' 0.045(8) 0.047(7) 0.054(8) 0.032(6) -0.006(6) 0.000(6) C33 0.0339(17) 0.0335(18) 0.0408(18) 0.0049(15) 0.0073(14) -0.0036(14) C34 0.103(4) 0.034(2) 0.052(2) 0.0129(18) 0.026(2) -0.001(2) C35 0.0239(16) 0.0345(18) 0.053(2) 0.0037(15) 0.0068(14) 0.0041(13) C36 0.0244(16) 0.042(2) 0.057(2) -0.0008(17) -0.0032(15) 0.0003(14) C37 0.0309(16) 0.0316(16) 0.0272(15) 0.0051(13) -0.0025(12) 0.0055(13) C38 0.0392(18) 0.0349(18) 0.0290(16) 0.0068(13) -0.0035(13) 0.0071(14) C39 0.0425(19) 0.043(2) 0.0325(17) 0.0051(15) -0.0090(14) 0.0078(16) C40 0.0404(19) 0.042(2) 0.0371(18) 0.0014(15) -0.0072(15) 0.0016(15) C41 0.0349(18) 0.0370(18) 0.0398(18) 0.0041(15) 0.0014(14) -0.0007(14) C42 0.0327(16) 0.0316(16) 0.0312(16) 0.0059(13) 0.0026(13) 0.0067(13) C43 0.060(2) 0.051(2) 0.0362(19) 0.0174(17) -0.0069(17) 0.0075(19) C44 0.058(2) 0.051(2) 0.0291(17) 0.0162(16) 0.0001(16) 0.0129(18) C45 0.0394(18) 0.0359(18) 0.0353(17) 0.0138(14) 0.0110(14) 0.0077(15) C46 0.048(2) 0.0352(19) 0.054(2) 0.0257(17) 0.0043(17) 0.0038(16) _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 Fe1 N1 2.054(2) . ? Fe1 N4 2.055(2) . ? Fe1 N2 2.060(2) . ? Fe1 N3 2.064(2) . ? Fe1 S1 2.3593(10) . ? S1 C37 1.776(3) . ? F1 C44 1.318(4) . ? F2 C44 1.322(4) . ? F3 C44 1.345(4) . ? F4 C46 1.301(4) . ? F5 C46 1.341(4) . ? F6 C46 1.299(4) . ? O1 C43 1.225(4) . ? O2 C45 1.207(4) . ? N1 C1 1.385(4) . ? N1 C4 1.391(4) . ? N2 C6 1.381(4) . ? N2 C9 1.383(4) . ? N3 C11 1.376(4) . ? N3 C14 1.380(4) . ? N4 C19 1.378(4) . ? N4 C16 1.382(4) . ? N5 C43 1.346(4) . ? N5 C38 1.412(4) . ? N5 H5N 0.92(4) . ? N6 C45 1.338(4) . ? N6 C42 1.411(4) . ? N6 H6N 0.95(4) . ? C1 C20 1.385(4) . ? C1 C2 1.452(4) . ? C2 C3 1.368(5) . ? C2 C21 1.503(4) . ? C3 C4 1.456(4) . ? C3 C23 1.518(5) . ? C4 C5 1.374(5) . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C7 1.447(4) . ? C7 C8 1.363(4) . ? C7 C25 1.509(4) . ? C8 C9 1.445(4) . ? C8 C27 1.517(4) . ? C9 C10 1.384(4) . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.440(4) . ? C12 C13 1.358(4) . ? C12 C29 1.497(4) . ? C13 C14 1.448(4) . ? C13 C31 1.518(3) . ? C13 C31' 1.522(4) . ? C14 C15 1.384(4) . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C17 1.451(4) . ? C17 C18 1.365(4) . ? C17 C33 1.502(4) . ? C18 C19 1.446(4) . ? C18 C35 1.496(4) . ? C19 C20 1.378(4) . ? C20 H20 0.9500 . ? C21 C22 1.523(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.526(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.502(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.509(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.530(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.515(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31' C32' 1.521(4) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C33 C34 1.504(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.532(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.401(4) . ? C37 C38 1.401(4) . ? C38 C39 1.388(5) . ? C39 C40 1.366(5) . ? C39 H39 0.9500 . ? C40 C41 1.390(5) . ? C40 H40 0.9500 . ? C41 C42 1.396(4) . ? C41 H41 0.9500 . ? C43 C44 1.527(5) . ? C45 C46 1.544(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 87.97(10) . . ? N1 Fe1 N2 87.99(10) . . ? N4 Fe1 N2 157.48(11) . . ? N1 Fe1 N3 156.74(10) . . ? N4 Fe1 N3 87.75(9) . . ? N2 Fe1 N3 87.27(9) . . ? N1 Fe1 S1 102.01(8) . . ? N4 Fe1 S1 104.66(7) . . ? N2 Fe1 S1 97.85(8) . . ? N3 Fe1 S1 101.19(7) . . ? C37 S1 Fe1 104.22(11) . . ? C1 N1 C4 106.2(2) . . ? C1 N1 Fe1 126.4(2) . . ? C4 N1 Fe1 126.1(2) . . ? C6 N2 C9 105.1(2) . . ? C6 N2 Fe1 126.4(2) . . ? C9 N2 Fe1 126.82(19) . . ? C11 N3 C14 105.7(2) . . ? C11 N3 Fe1 126.63(19) . . ? C14 N3 Fe1 126.67(19) . . ? C19 N4 C16 106.2(2) . . ? C19 N4 Fe1 126.01(19) . . ? C16 N4 Fe1 127.34(19) . . ? C43 N5 C38 128.1(3) . . ? C43 N5 H5N 117(2) . . ? C38 N5 H5N 114(2) . . ? C45 N6 C42 128.1(3) . . ? C45 N6 H6N 119(2) . . ? C42 N6 H6N 113(2) . . ? C20 C1 N1 123.9(3) . . ? C20 C1 C2 126.1(3) . . ? N1 C1 C2 109.9(3) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 C21 128.6(3) . . ? C1 C2 C21 124.2(3) . . ? C2 C3 C4 106.8(3) . . ? C2 C3 C23 128.8(3) . . ? C4 C3 C23 124.4(3) . . ? C5 C4 N1 125.0(3) . . ? C5 C4 C3 125.2(3) . . ? N1 C4 C3 109.8(3) . . ? C4 C5 C6 126.8(3) . . ? C4 C5 H5 116.6 . . ? C6 C5 H5 116.6 . . ? N2 C6 C5 124.4(3) . . ? N2 C6 C7 110.4(3) . . ? C5 C6 C7 125.1(3) . . ? C8 C7 C6 107.1(3) . . ? C8 C7 C25 128.8(3) . . ? C6 C7 C25 124.0(3) . . ? C7 C8 C9 106.3(3) . . ? C7 C8 C27 127.9(3) . . ? C9 C8 C27 125.8(3) . . ? N2 C9 C10 123.9(3) . . ? N2 C9 C8 111.0(3) . . ? C10 C9 C8 125.0(3) . . ? C9 C10 C11 126.6(3) . . ? C9 C10 H10 116.7 . . ? C11 C10 H10 116.7 . . ? N3 C11 C10 124.7(3) . . ? N3 C11 C12 110.8(2) . . ? C10 C11 C12 124.6(3) . . ? C13 C12 C11 106.5(2) . . ? C13 C12 C29 128.1(3) . . ? C11 C12 C29 125.3(3) . . ? C12 C13 C14 107.2(2) . . ? C12 C13 C31 125.5(5) . . ? C14 C13 C31 127.2(5) . . ? C12 C13 C31' 132.3(10) . . ? C14 C13 C31' 118.5(10) . . ? N3 C14 C15 125.0(3) . . ? N3 C14 C13 109.8(2) . . ? C15 C14 C13 125.2(3) . . ? C14 C15 C16 126.2(3) . . ? C14 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? N4 C16 C15 124.7(3) . . ? N4 C16 C17 110.1(3) . . ? C15 C16 C17 125.2(3) . . ? C18 C17 C16 106.4(3) . . ? C18 C17 C33 127.9(3) . . ? C16 C17 C33 125.6(3) . . ? C17 C18 C19 107.3(3) . . ? C17 C18 C35 128.3(3) . . ? C19 C18 C35 124.4(3) . . ? N4 C19 C20 125.2(3) . . ? N4 C19 C18 109.9(3) . . ? C20 C19 C18 124.8(3) . . ? C19 C20 C1 126.8(3) . . ? C19 C20 H20 116.6 . . ? C1 C20 H20 116.6 . . ? C2 C21 C22 111.9(3) . . ? C2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 112.6(3) . . ? C3 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C3 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C7 112.7(3) . . ? C26 C25 H25A 109.0 . . ? C7 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C7 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C8 111.9(3) . . ? C28 C27 H27A 109.2 . . ? C8 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? C8 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 111.9(3) . . ? C12 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C12 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C13 109.3(4) . . ? C32 C31 H31A 109.8 . . ? C13 C31 H31A 109.8 . . ? C32 C31 H31B 109.8 . . ? C13 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C32' C31' C13 109.1(6) . . ? C32' C31' H31C 109.9 . . ? C13 C31' H31C 109.9 . . ? C32' C31' H31D 109.9 . . ? C13 C31' H31D 109.9 . . ? H31C C31' H31D 108.3 . . ? C31' C32' H32D 109.5 . . ? C31' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C31' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C17 C33 C34 114.8(3) . . ? C17 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? C17 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 111.9(3) . . ? C18 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C18 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 118.4(3) . . ? C42 C37 S1 120.9(2) . . ? C38 C37 S1 120.6(2) . . ? C39 C38 C37 120.9(3) . . ? C39 C38 N5 122.4(3) . . ? C37 C38 N5 116.6(3) . . ? C40 C39 C38 119.4(3) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 121.8(3) . . ? C39 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? C40 C41 C42 118.7(3) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? C41 C42 C37 120.7(3) . . ? C41 C42 N6 122.1(3) . . ? C37 C42 N6 117.2(3) . . ? O1 C43 N5 128.3(4) . . ? O1 C43 C44 117.5(3) . . ? N5 C43 C44 114.1(3) . . ? F1 C44 F2 108.6(3) . . ? F1 C44 F3 107.2(3) . . ? F2 C44 F3 106.3(3) . . ? F1 C44 C43 114.0(3) . . ? F2 C44 C43 110.2(3) . . ? F3 C44 C43 110.2(3) . . ? O2 C45 N6 127.9(3) . . ? O2 C45 C46 118.7(3) . . ? N6 C45 C46 113.4(3) . . ? F6 C46 F4 109.7(3) . . ? F6 C46 F5 106.7(3) . . ? F4 C46 F5 105.6(3) . . ? F6 C46 C45 109.5(3) . . ? F4 C46 C45 115.0(3) . . ? F5 C46 C45 110.0(3) . . ? 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 Fe1 S1 C37 -53.37(13) . . . . ? N4 Fe1 S1 C37 37.68(13) . . . . ? N2 Fe1 S1 C37 -142.97(12) . . . . ? N3 Fe1 S1 C37 128.28(12) . . . . ? N4 Fe1 N1 C1 -19.6(3) . . . . ? N2 Fe1 N1 C1 -177.5(3) . . . . ? N3 Fe1 N1 C1 -99.2(3) . . . . ? S1 Fe1 N1 C1 84.9(3) . . . . ? N4 Fe1 N1 C4 174.8(3) . . . . ? N2 Fe1 N1 C4 17.0(3) . . . . ? N3 Fe1 N1 C4 95.3(3) . . . . ? S1 Fe1 N1 C4 -80.6(3) . . . . ? N1 Fe1 N2 C6 -18.5(3) . . . . ? N4 Fe1 N2 C6 -98.3(3) . . . . ? N3 Fe1 N2 C6 -175.7(3) . . . . ? S1 Fe1 N2 C6 83.3(3) . . . . ? N1 Fe1 N2 C9 178.3(3) . . . . ? N4 Fe1 N2 C9 98.5(3) . . . . ? N3 Fe1 N2 C9 21.1(3) . . . . ? S1 Fe1 N2 C9 -79.9(3) . . . . ? N1 Fe1 N3 C11 -97.1(3) . . . . ? N4 Fe1 N3 C11 -176.7(2) . . . . ? N2 Fe1 N3 C11 -18.7(2) . . . . ? S1 Fe1 N3 C11 78.8(2) . . . . ? N1 Fe1 N3 C14 96.1(3) . . . . ? N4 Fe1 N3 C14 16.6(2) . . . . ? N2 Fe1 N3 C14 174.6(3) . . . . ? S1 Fe1 N3 C14 -87.9(2) . . . . ? N1 Fe1 N4 C19 18.2(2) . . . . ? N2 Fe1 N4 C19 98.0(3) . . . . ? N3 Fe1 N4 C19 175.3(2) . . . . ? S1 Fe1 N4 C19 -83.7(2) . . . . ? N1 Fe1 N4 C16 -171.0(2) . . . . ? N2 Fe1 N4 C16 -91.2(3) . . . . ? N3 Fe1 N4 C16 -13.9(2) . . . . ? S1 Fe1 N4 C16 87.1(2) . . . . ? C4 N1 C1 C20 -178.0(3) . . . . ? Fe1 N1 C1 C20 14.1(5) . . . . ? C4 N1 C1 C2 -0.3(4) . . . . ? Fe1 N1 C1 C2 -168.2(2) . . . . ? C20 C1 C2 C3 177.7(3) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C20 C1 C2 C21 -3.9(6) . . . . ? N1 C1 C2 C21 178.4(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C21 C2 C3 C4 -178.1(3) . . . . ? C1 C2 C3 C23 -178.6(4) . . . . ? C21 C2 C3 C23 3.0(7) . . . . ? C1 N1 C4 C5 -178.9(3) . . . . ? Fe1 N1 C4 C5 -11.0(5) . . . . ? C1 N1 C4 C3 0.4(4) . . . . ? Fe1 N1 C4 C3 168.4(2) . . . . ? C2 C3 C4 C5 178.9(3) . . . . ? C23 C3 C4 C5 -2.1(6) . . . . ? C2 C3 C4 N1 -0.4(4) . . . . ? C23 C3 C4 N1 178.5(3) . . . . ? N1 C4 C5 C6 -1.4(6) . . . . ? C3 C4 C5 C6 179.4(4) . . . . ? C9 N2 C6 C5 -179.8(3) . . . . ? Fe1 N2 C6 C5 14.1(5) . . . . ? C9 N2 C6 C7 -0.7(4) . . . . ? Fe1 N2 C6 C7 -166.8(2) . . . . ? C4 C5 C6 N2 -0.3(6) . . . . ? C4 C5 C6 C7 -179.3(3) . . . . ? N2 C6 C7 C8 1.0(4) . . . . ? C5 C6 C7 C8 -179.9(3) . . . . ? N2 C6 C7 C25 -179.0(3) . . . . ? C5 C6 C7 C25 0.1(6) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C25 C7 C8 C9 179.2(3) . . . . ? C6 C7 C8 C27 -178.9(3) . . . . ? C25 C7 C8 C27 1.2(6) . . . . ? C6 N2 C9 C10 177.7(3) . . . . ? Fe1 N2 C9 C10 -16.3(5) . . . . ? C6 N2 C9 C8 0.1(4) . . . . ? Fe1 N2 C9 C8 166.1(2) . . . . ? C7 C8 C9 N2 0.6(4) . . . . ? C27 C8 C9 N2 178.6(3) . . . . ? C7 C8 C9 C10 -177.0(3) . . . . ? C27 C8 C9 C10 1.0(6) . . . . ? N2 C9 C10 C11 0.1(5) . . . . ? C8 C9 C10 C11 177.4(3) . . . . ? C14 N3 C11 C10 -179.6(3) . . . . ? Fe1 N3 C11 C10 11.4(4) . . . . ? C14 N3 C11 C12 0.2(3) . . . . ? Fe1 N3 C11 C12 -168.81(19) . . . . ? C9 C10 C11 N3 2.4(5) . . . . ? C9 C10 C11 C12 -177.3(3) . . . . ? N3 C11 C12 C13 0.7(3) . . . . ? C10 C11 C12 C13 -179.5(3) . . . . ? N3 C11 C12 C29 -177.1(3) . . . . ? C10 C11 C12 C29 2.7(5) . . . . ? C11 C12 C13 C14 -1.2(3) . . . . ? C29 C12 C13 C14 176.5(3) . . . . ? C11 C12 C13 C31 175.1(3) . . . . ? C29 C12 C13 C31 -7.2(6) . . . . ? C11 C12 C13 C31' -164.2(7) . . . . ? C29 C12 C13 C31' 13.5(8) . . . . ? C11 N3 C14 C15 177.5(3) . . . . ? Fe1 N3 C14 C15 -13.5(4) . . . . ? C11 N3 C14 C13 -0.9(3) . . . . ? Fe1 N3 C14 C13 168.0(2) . . . . ? C12 C13 C14 N3 1.4(4) . . . . ? C31 C13 C14 N3 -174.9(3) . . . . ? C31' C13 C14 N3 167.1(5) . . . . ? C12 C13 C14 C15 -177.1(3) . . . . ? C31 C13 C14 C15 6.7(5) . . . . ? C31' C13 C14 C15 -11.3(6) . . . . ? N3 C14 C15 C16 0.7(5) . . . . ? C13 C14 C15 C16 178.9(3) . . . . ? C19 N4 C16 C15 -180.0(3) . . . . ? Fe1 N4 C16 C15 7.8(4) . . . . ? C19 N4 C16 C17 0.2(3) . . . . ? Fe1 N4 C16 C17 -172.07(19) . . . . ? C14 C15 C16 N4 2.4(5) . . . . ? C14 C15 C16 C17 -177.8(3) . . . . ? N4 C16 C17 C18 0.4(3) . . . . ? C15 C16 C17 C18 -179.5(3) . . . . ? N4 C16 C17 C33 -177.4(3) . . . . ? C15 C16 C17 C33 2.7(5) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C33 C17 C18 C19 177.0(3) . . . . ? C16 C17 C18 C35 178.2(3) . . . . ? C33 C17 C18 C35 -4.1(5) . . . . ? C16 N4 C19 C20 176.4(3) . . . . ? Fe1 N4 C19 C20 -11.2(4) . . . . ? C16 N4 C19 C18 -0.7(3) . . . . ? Fe1 N4 C19 C18 171.73(19) . . . . ? C17 C18 C19 N4 0.9(3) . . . . ? C35 C18 C19 N4 -178.1(3) . . . . ? C17 C18 C19 C20 -176.2(3) . . . . ? C35 C18 C19 C20 4.8(5) . . . . ? N4 C19 C20 C1 -2.9(5) . . . . ? C18 C19 C20 C1 173.8(3) . . . . ? N1 C1 C20 C19 1.4(5) . . . . ? C2 C1 C20 C19 -176.0(3) . . . . ? C3 C2 C21 C22 96.8(5) . . . . ? C1 C2 C21 C22 -81.3(5) . . . . ? C2 C3 C23 C24 104.1(5) . . . . ? C4 C3 C23 C24 -74.6(5) . . . . ? C8 C7 C25 C26 -103.2(4) . . . . ? C6 C7 C25 C26 76.9(4) . . . . ? C7 C8 C27 C28 97.3(4) . . . . ? C9 C8 C27 C28 -80.3(4) . . . . ? C13 C12 C29 C30 -97.1(4) . . . . ? C11 C12 C29 C30 80.2(4) . . . . ? C12 C13 C31 C32 92.6(7) . . . . ? C14 C13 C31 C32 -91.8(7) . . . . ? C31' C13 C31 C32 -27(4) . . . . ? C12 C13 C31' C32' -107.7(14) . . . . ? C14 C13 C31' C32' 90.8(15) . . . . ? C31 C13 C31' C32' -34(3) . . . . ? C18 C17 C33 C34 75.1(5) . . . . ? C16 C17 C33 C34 -107.6(4) . . . . ? C17 C18 C35 C36 -99.8(4) . . . . ? C19 C18 C35 C36 79.0(4) . . . . ? Fe1 S1 C37 C42 -90.9(3) . . . . ? Fe1 S1 C37 C38 94.0(3) . . . . ? C42 C37 C38 C39 1.7(5) . . . . ? S1 C37 C38 C39 177.0(3) . . . . ? C42 C37 C38 N5 -176.1(3) . . . . ? S1 C37 C38 N5 -0.9(4) . . . . ? C43 N5 C38 C39 -14.2(6) . . . . ? C43 N5 C38 C37 163.6(4) . . . . ? C37 C38 C39 C40 -0.9(5) . . . . ? N5 C38 C39 C40 176.8(3) . . . . ? C38 C39 C40 C41 0.0(5) . . . . ? C39 C40 C41 C42 0.1(5) . . . . ? C40 C41 C42 C37 0.7(5) . . . . ? C40 C41 C42 N6 -176.7(3) . . . . ? C38 C37 C42 C41 -1.6(5) . . . . ? S1 C37 C42 C41 -176.9(3) . . . . ? C38 C37 C42 N6 176.0(3) . . . . ? S1 C37 C42 N6 0.7(4) . . . . ? C45 N6 C42 C41 3.8(5) . . . . ? C45 N6 C42 C37 -173.8(3) . . . . ? C38 N5 C43 O1 8.3(7) . . . . ? C38 N5 C43 C44 -170.0(3) . . . . ? O1 C43 C44 F1 173.7(4) . . . . ? N5 C43 C44 F1 -7.7(5) . . . . ? O1 C43 C44 F2 51.3(5) . . . . ? N5 C43 C44 F2 -130.2(3) . . . . ? O1 C43 C44 F3 -65.7(5) . . . . ? N5 C43 C44 F3 112.8(4) . . . . ? C42 N6 C45 O2 -8.3(6) . . . . ? C42 N6 C45 C46 169.5(3) . . . . ? O2 C45 C46 F6 61.0(4) . . . . ? N6 C45 C46 F6 -117.0(4) . . . . ? O2 C45 C46 F4 -175.0(3) . . . . ? N6 C45 C46 F4 7.0(5) . . . . ? O2 C45 C46 F5 -55.9(4) . . . . ? N6 C45 C46 F5 126.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5N S1 0.92(4) 2.40(4) 2.949(3) 118(3) . N5 H5N F1 0.92(4) 2.18(4) 2.620(4) 108(3) . N6 H6N S1 0.95(4) 2.40(3) 2.968(3) 118(3) . N6 H6N F4 0.95(4) 2.20(3) 2.630(3) 106(3) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.959 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.075 #===END