data_CCDC-875224 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'iron(II) TBC triflate' _chemical_formula_moiety 'C46 H57 F6 Fe N7 O6 S2' _chemical_formula_sum 'C46 H57 F6 Fe N7 O6 S2' _chemical_formula_weight 1037.96 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 12.1461(18) _cell_length_b 13.876(2) _cell_length_c 17.131(3) _cell_angle_alpha 67.041(8) _cell_angle_beta 72.676(9) _cell_angle_gamma 67.039(8) _cell_volume 2411.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8280 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.25 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8700 _exptl_absorpt_correction_T_max 0.8700 _exptl_absorpt_process_details ? _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22851 _diffrn_reflns_av_R_equivalents 0.1296 _diffrn_reflns_av_sigmaI/netI 0.1596 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8905 _reflns_number_gt 5438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^2^+0.6546P] 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 8905 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2378 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.3209 _refine_ls_wR_factor_gt 0.2050 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 0.41867(6) 0.40012(6) 0.29921(4) 0.0173(3) Uani 1 1 d . . . S1 S 0.68370(13) 0.90562(12) 0.36664(9) 0.0278(4) Uani 1 1 d . . . S2 S 0.14012(12) 0.24146(12) 0.19406(9) 0.0303(4) Uani 1 1 d . . . F1 F 0.9077(4) 0.7727(4) 0.3629(3) 0.0642(15) Uani 1 1 d . . . O5 O 0.6483(3) 0.8236(3) 0.4418(3) 0.0343(11) Uani 1 1 d . . . F3 F 0.8608(3) 0.8772(4) 0.4382(3) 0.0552(13) Uani 1 1 d . . . F4 F 0.8929(5) 0.9440(6) 0.3017(4) 0.0858(19) Uani 1 1 d . . . O6 O 0.6333(5) 1.0158(4) 0.3711(4) 0.0554(15) Uani 1 1 d . . . O4 O 0.6874(5) 0.8928(5) 0.2872(3) 0.0560(15) Uani 1 1 d . . . F7 F 0.2503(4) 0.1456(4) 0.0748(2) 0.0490(11) Uani 1 1 d . . . F8 F 0.1466(5) 0.0575(4) 0.1818(4) 0.0784(18) Uani 1 1 d . . . F9 F 0.3166(4) 0.0573(4) 0.1937(3) 0.0626(15) Uani 1 1 d . . . O1 O 0.0354(4) 0.2953(4) 0.1535(3) 0.0409(12) Uani 1 1 d . . . O2 O 0.1165(5) 0.1965(5) 0.2858(3) 0.066(2) Uani 1 1 d . . . O3 O 0.2289(4) 0.2977(5) 0.1601(5) 0.0649(18) Uani 1 1 d . . . N1 N 0.5804(4) 0.3488(4) 0.3508(3) 0.0202(10) Uani 1 1 d . . . C50 C 0.4267(4) 0.4264(4) 0.4601(3) 0.0210(11) Uani 1 1 d . . . H2A H 0.4260 0.3512 0.4971 0.025 Uiso 1 1 calc R . . H2B H 0.4101 0.4710 0.4979 0.025 Uiso 1 1 calc R . . N3 N 0.3307(4) 0.4756(3) 0.4069(3) 0.0184(9) Uani 1 1 d . . . N4 N 0.3159(4) 0.5362(3) 0.2081(3) 0.0202(10) Uani 1 1 d . . . N5 N 0.5222(4) 0.3417(4) 0.1818(3) 0.0198(10) Uani 1 1 d . . . N6 N 0.3426(4) 0.2741(4) 0.3512(3) 0.0215(10) Uani 1 1 d . . . N7 N 0.3691(5) 0.3643(5) 0.9037(4) 0.0508(17) Uani 1 1 d . . . N8 N 0.4721(6) 0.2728(7) 0.7297(5) 0.062(2) Uani 1 1 d . . . C1 C 0.6049(4) 0.2290(4) 0.4067(3) 0.0198(11) Uani 1 1 d . . . H1A H 0.5273 0.2185 0.4425 0.024 Uiso 1 1 calc R . . H1B H 0.6346 0.1823 0.3687 0.024 Uiso 1 1 calc R . . C2 C 0.6952(5) 0.1897(4) 0.4648(3) 0.0218(12) Uani 1 1 d . . . C3 C 0.8205(5) 0.1598(5) 0.4351(4) 0.0285(13) Uani 1 1 d . . . H3 H 0.8505 0.1632 0.3765 0.034 Uiso 1 1 calc R . . C4 C 0.9009(5) 0.1254(5) 0.4904(4) 0.0343(15) Uani 1 1 d . . . H4 H 0.9856 0.1074 0.4690 0.041 Uiso 1 1 calc R . . C5 C 0.8594(5) 0.1167(5) 0.5763(4) 0.0332(14) Uani 1 1 d . . . H5 H 0.9152 0.0921 0.6141 0.040 Uiso 1 1 calc R . . C6 C 0.7358(5) 0.1442(5) 0.6071(4) 0.0281(13) Uani 1 1 d . . . H6 H 0.7065 0.1376 0.6663 0.034 Uiso 1 1 calc R . . C7 C 0.6549(5) 0.1812(4) 0.5517(3) 0.0243(12) Uani 1 1 d . . . H7 H 0.5702 0.2012 0.5733 0.029 Uiso 1 1 calc R . . C8 C 0.5506(4) 0.4212(4) 0.4044(3) 0.0210(11) Uani 1 1 d . . . H8A H 0.5513 0.4962 0.3666 0.025 Uiso 1 1 calc R . . H8B H 0.6127 0.3920 0.4414 0.025 Uiso 1 1 calc R . . C9 C 0.3037(4) 0.5976(4) 0.3756(3) 0.0225(12) Uani 1 1 d . . . H9A H 0.3816 0.6141 0.3558 0.027 Uiso 1 1 calc R . . H9B H 0.2594 0.6260 0.4249 0.027 Uiso 1 1 calc R . . C10 C 0.2310(4) 0.6592(4) 0.3043(3) 0.0222(12) Uani 1 1 d . . . H10A H 0.2030 0.7386 0.2982 0.027 Uiso 1 1 calc R . . H10B H 0.1580 0.6354 0.3211 0.027 Uiso 1 1 calc R . . C11 C 0.2972(5) 0.6447(4) 0.2165(3) 0.0224(12) Uani 1 1 d . . . H11A H 0.2505 0.7035 0.1720 0.027 Uiso 1 1 calc R . . H11B H 0.3775 0.6550 0.2045 0.027 Uiso 1 1 calc R . . C12 C 0.3936(4) 0.5330(4) 0.1228(3) 0.0217(12) Uani 1 1 d . . . H12A H 0.4618 0.5604 0.1140 0.026 Uiso 1 1 calc R . . H12B H 0.3452 0.5819 0.0766 0.026 Uiso 1 1 calc R . . C13 C 0.4433(5) 0.4165(4) 0.1176(3) 0.0235(12) Uani 1 1 d . . . H13A H 0.3750 0.3890 0.1271 0.028 Uiso 1 1 calc R . . H13B H 0.4901 0.4172 0.0593 0.028 Uiso 1 1 calc R . . C14 C 0.6424(4) 0.3604(5) 0.1508(3) 0.0259(13) Uani 1 1 d . . . H14A H 0.6289 0.4408 0.1287 0.031 Uiso 1 1 calc R . . H14B H 0.6848 0.3310 0.1019 0.031 Uiso 1 1 calc R . . C15 C 0.7249(4) 0.3097(5) 0.2166(3) 0.0235(12) Uani 1 1 d . . . H15A H 0.8083 0.3094 0.1862 0.028 Uiso 1 1 calc R . . H15B H 0.7268 0.2321 0.2465 0.028 Uiso 1 1 calc R . . C16 C 0.6880(4) 0.3687(4) 0.2840(3) 0.0223(12) Uani 1 1 d . . . H16A H 0.7578 0.3445 0.3131 0.027 Uiso 1 1 calc R . . H16B H 0.6699 0.4488 0.2541 0.027 Uiso 1 1 calc R . . C17 C 0.5356(5) 0.2241(4) 0.1960(3) 0.0212(12) Uani 1 1 d . . . H17A H 0.4535 0.2161 0.2126 0.025 Uiso 1 1 calc R . . H17B H 0.5788 0.1767 0.2453 0.025 Uiso 1 1 calc R . . C18 C 0.6026(5) 0.1810(4) 0.1200(3) 0.0227(12) Uani 1 1 d . . . C19 C 0.5450(5) 0.1975(5) 0.0563(4) 0.0285(13) Uani 1 1 d . . . H19 H 0.4608 0.2372 0.0597 0.034 Uiso 1 1 calc R . . C20 C 0.6057(6) 0.1580(5) -0.0140(4) 0.0335(15) Uani 1 1 d . . . H20 H 0.5637 0.1693 -0.0571 0.040 Uiso 1 1 calc R . . C21 C 0.7291(6) 0.1017(5) -0.0187(4) 0.0318(15) Uani 1 1 d . . . H21 H 0.7727 0.0751 -0.0661 0.038 Uiso 1 1 calc R . . C22 C 0.7889(5) 0.0843(5) 0.0448(4) 0.0321(15) Uani 1 1 d . . . H22 H 0.8733 0.0456 0.0408 0.038 Uiso 1 1 calc R . . C23 C 0.7270(5) 0.1225(5) 0.1149(4) 0.0295(14) Uani 1 1 d . . . H23 H 0.7687 0.1092 0.1588 0.035 Uiso 1 1 calc R . . C24 C 0.1950(4) 0.5211(4) 0.2149(3) 0.0218(12) Uani 1 1 d . . . H24A H 0.2116 0.4519 0.2030 0.026 Uiso 1 1 calc R . . H24B H 0.1507 0.5130 0.2747 0.026 Uiso 1 1 calc R . . C25 C 0.1151(4) 0.6136(5) 0.1548(3) 0.0230(12) Uani 1 1 d . . . C26 C 0.1279(5) 0.6206(5) 0.0688(4) 0.0304(14) Uani 1 1 d . . . H26 H 0.1875 0.5631 0.0481 0.037 Uiso 1 1 calc R . . C27 C 0.0568(5) 0.7083(6) 0.0135(4) 0.0383(16) Uani 1 1 d . . . H27 H 0.0677 0.7108 -0.0445 0.046 Uiso 1 1 calc R . . C28 C -0.0313(5) 0.7934(6) 0.0425(5) 0.0375(15) Uani 1 1 d . . . H28 H -0.0782 0.8558 0.0040 0.045 Uiso 1 1 calc R . . C29 C -0.0495(5) 0.7862(5) 0.1271(4) 0.0366(16) Uani 1 1 d . . . H29 H -0.1132 0.8413 0.1482 0.044 Uiso 1 1 calc R . . C30 C 0.0239(5) 0.6993(5) 0.1822(4) 0.0275(13) Uani 1 1 d . . . H30 H 0.0121 0.6977 0.2400 0.033 Uiso 1 1 calc R . . C31 C 0.2182(4) 0.4451(4) 0.4590(3) 0.0199(11) Uani 1 1 d . . . H31A H 0.2378 0.3641 0.4767 0.024 Uiso 1 1 calc R . . H31B H 0.1556 0.4783 0.4219 0.024 Uiso 1 1 calc R . . C32 C 0.1655(5) 0.4820(5) 0.5390(3) 0.0246(12) Uani 1 1 d . . . C33 C 0.0731(5) 0.5820(5) 0.5357(4) 0.0277(13) Uani 1 1 d . . . H33 H 0.0418 0.6261 0.4839 0.033 Uiso 1 1 calc R . . C34 C 0.0269(5) 0.6174(5) 0.6080(4) 0.0285(13) Uani 1 1 d . . . H34 H -0.0365 0.6851 0.6057 0.034 Uiso 1 1 calc R . . C35 C 0.0727(5) 0.5544(5) 0.6827(4) 0.0305(14) Uani 1 1 d . . . H35 H 0.0416 0.5796 0.7316 0.037 Uiso 1 1 calc R . . C36 C 0.1633(5) 0.4548(5) 0.6877(4) 0.0285(13) Uani 1 1 d . . . H36 H 0.1944 0.4115 0.7397 0.034 Uiso 1 1 calc R . . C37 C 0.2090(5) 0.4181(4) 0.6156(3) 0.0250(12) Uani 1 1 d . . . H37 H 0.2703 0.3490 0.6191 0.030 Uiso 1 1 calc R . . C38 C 0.3340(4) 0.1881(4) 0.3761(3) 0.0219(12) Uani 1 1 d . . . C39 C 0.3277(5) 0.0773(5) 0.4037(4) 0.0308(14) Uani 1 1 d . . . H39A H 0.3832 0.0394 0.3624 0.046 Uiso 1 1 calc R . . H39B H 0.2446 0.0804 0.4066 0.046 Uiso 1 1 calc R . . H39C H 0.3511 0.0370 0.4606 0.046 Uiso 1 1 calc R . . C40 C 0.2649(5) 0.3955(5) 0.9193(4) 0.0333(15) Uani 1 1 d . . . C41 C 0.1344(6) 0.4373(6) 0.9375(5) 0.0446(18) Uani 1 1 d . . . H41A H 0.1091 0.5165 0.9287 0.067 Uiso 1 1 calc R . . H41B H 0.1054 0.3993 0.9973 0.067 Uiso 1 1 calc R . . H41C H 0.1000 0.4244 0.8988 0.067 Uiso 1 1 calc R . . C42 C 0.4426(6) 0.2056(6) 0.7859(5) 0.0423(17) Uani 1 1 d . . . C43 C 0.4028(6) 0.1192(6) 0.8581(4) 0.0373(15) Uani 1 1 d . . . H43A H 0.3312 0.1529 0.8950 0.056 Uiso 1 1 calc R . . H43B H 0.4683 0.0727 0.8916 0.056 Uiso 1 1 calc R . . H43C H 0.3821 0.0740 0.8361 0.056 Uiso 1 1 calc R . . C44 C 0.8433(6) 0.8748(6) 0.3672(4) 0.0400(16) Uani 1 1 d . . . C45 C 0.2172(6) 0.1186(6) 0.1606(4) 0.0404(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 0.0180(4) 0.0161(4) 0.0164(4) -0.0084(3) 0.0005(3) -0.0032(3) S1 0.0358(7) 0.0219(7) 0.0265(7) -0.0059(6) -0.0087(6) -0.0090(6) S2 0.0272(7) 0.0326(8) 0.0343(8) -0.0229(7) -0.0054(6) -0.0001(6) F1 0.037(2) 0.075(3) 0.075(3) -0.052(3) 0.003(2) 0.007(2) O5 0.032(2) 0.029(2) 0.033(2) -0.011(2) 0.0050(17) -0.0071(17) F3 0.0351(19) 0.087(3) 0.053(3) -0.041(3) -0.0110(18) -0.007(2) F4 0.069(3) 0.118(5) 0.070(3) 0.002(4) 0.000(3) -0.069(3) O6 0.055(3) 0.021(2) 0.091(4) -0.018(3) -0.029(3) 0.001(2) O4 0.076(3) 0.075(4) 0.031(3) -0.014(3) -0.009(2) -0.039(3) F7 0.054(2) 0.059(3) 0.035(2) -0.031(2) 0.0026(17) -0.009(2) F8 0.089(4) 0.060(3) 0.100(4) -0.053(3) 0.032(3) -0.044(3) F9 0.063(3) 0.045(2) 0.053(3) -0.024(2) -0.012(2) 0.021(2) O1 0.0272(19) 0.056(3) 0.039(2) -0.026(2) -0.0079(18) 0.001(2) O2 0.082(4) 0.057(3) 0.033(3) -0.026(3) -0.015(3) 0.020(3) O3 0.035(2) 0.056(3) 0.124(5) -0.062(4) 0.003(3) -0.013(2) N1 0.0201(19) 0.018(2) 0.021(2) -0.0098(19) 0.0027(17) -0.0047(16) C50 0.026(2) 0.019(2) 0.018(2) -0.010(2) 0.003(2) -0.007(2) N3 0.0192(18) 0.020(2) 0.020(2) -0.0117(19) -0.0032(16) -0.0041(16) N4 0.0205(18) 0.017(2) 0.018(2) -0.0072(18) 0.0039(16) -0.0037(16) N5 0.0200(19) 0.021(2) 0.0158(19) -0.0106(19) -0.0011(16) -0.0004(17) N6 0.0209(19) 0.026(3) 0.017(2) -0.012(2) 0.0018(16) -0.0053(18) N7 0.038(3) 0.044(4) 0.061(4) -0.015(3) -0.001(3) -0.010(3) N8 0.059(4) 0.070(5) 0.065(4) -0.029(4) 0.015(4) -0.040(4) C1 0.022(2) 0.015(2) 0.021(2) -0.008(2) -0.0025(19) -0.0035(18) C2 0.027(2) 0.014(2) 0.025(3) -0.008(2) -0.002(2) -0.006(2) C3 0.026(2) 0.023(3) 0.032(3) -0.010(3) -0.005(2) -0.002(2) C4 0.024(2) 0.026(3) 0.049(4) -0.013(3) -0.007(3) -0.004(2) C5 0.033(3) 0.024(3) 0.047(4) -0.009(3) -0.021(3) -0.005(2) C6 0.039(3) 0.022(3) 0.027(3) -0.007(3) -0.011(2) -0.010(2) C7 0.027(2) 0.018(3) 0.025(3) -0.008(2) -0.003(2) -0.005(2) C8 0.022(2) 0.022(3) 0.023(3) -0.014(2) -0.002(2) -0.005(2) C9 0.022(2) 0.021(3) 0.024(2) -0.015(2) 0.004(2) -0.0041(19) C10 0.020(2) 0.021(3) 0.026(3) -0.014(2) 0.001(2) -0.0035(19) C11 0.025(2) 0.018(3) 0.021(3) -0.008(2) 0.003(2) -0.007(2) C12 0.021(2) 0.022(3) 0.015(2) -0.006(2) 0.0007(19) -0.0014(19) C13 0.026(2) 0.022(3) 0.015(2) -0.009(2) 0.0047(19) -0.004(2) C14 0.021(2) 0.027(3) 0.022(3) -0.013(2) 0.008(2) -0.003(2) C15 0.018(2) 0.028(3) 0.025(3) -0.014(2) 0.0020(19) -0.006(2) C16 0.021(2) 0.022(3) 0.024(3) -0.010(2) 0.004(2) -0.009(2) C17 0.026(2) 0.021(3) 0.016(2) -0.010(2) -0.0004(19) -0.005(2) C18 0.026(2) 0.020(3) 0.022(3) -0.013(2) 0.004(2) -0.007(2) C19 0.034(3) 0.027(3) 0.026(3) -0.015(3) -0.004(2) -0.004(2) C20 0.053(4) 0.029(3) 0.018(3) -0.013(3) -0.006(2) -0.007(3) C21 0.045(3) 0.023(3) 0.022(3) -0.013(3) 0.005(2) -0.007(2) C22 0.028(3) 0.021(3) 0.040(3) -0.019(3) 0.006(2) -0.001(2) C23 0.036(3) 0.020(3) 0.026(3) -0.011(3) -0.001(2) -0.002(2) C24 0.021(2) 0.023(3) 0.021(2) -0.011(2) 0.0006(19) -0.005(2) C25 0.019(2) 0.026(3) 0.022(3) -0.010(2) -0.002(2) -0.003(2) C26 0.026(2) 0.039(3) 0.026(3) -0.019(3) 0.001(2) -0.005(2) C27 0.033(3) 0.049(4) 0.030(3) -0.019(3) -0.004(3) -0.005(3) C28 0.032(3) 0.030(3) 0.045(4) -0.009(3) -0.008(3) -0.006(2) C29 0.029(3) 0.032(3) 0.043(4) -0.017(3) -0.006(3) 0.002(2) C30 0.023(2) 0.031(3) 0.028(3) -0.015(3) -0.002(2) -0.004(2) C31 0.022(2) 0.022(3) 0.016(2) -0.010(2) 0.0020(19) -0.007(2) C32 0.026(2) 0.026(3) 0.023(3) -0.016(2) 0.006(2) -0.009(2) C33 0.025(2) 0.025(3) 0.029(3) -0.013(3) 0.004(2) -0.005(2) C34 0.021(2) 0.030(3) 0.036(3) -0.021(3) 0.006(2) -0.006(2) C35 0.034(3) 0.035(3) 0.030(3) -0.023(3) 0.010(2) -0.018(2) C36 0.029(3) 0.038(3) 0.022(3) -0.018(3) 0.003(2) -0.013(2) C37 0.029(2) 0.022(3) 0.021(3) -0.011(2) 0.004(2) -0.007(2) C38 0.023(2) 0.022(3) 0.019(2) -0.010(2) 0.0035(19) -0.007(2) C39 0.037(3) 0.020(3) 0.034(3) -0.012(3) 0.001(2) -0.010(2) C40 0.037(3) 0.028(3) 0.036(3) -0.010(3) 0.001(3) -0.015(3) C41 0.032(3) 0.050(4) 0.040(4) -0.012(3) 0.002(3) -0.009(3) C42 0.037(3) 0.048(4) 0.045(4) -0.021(4) 0.005(3) -0.019(3) C43 0.044(3) 0.039(4) 0.036(3) -0.013(3) -0.006(3) -0.019(3) C44 0.035(3) 0.052(4) 0.037(3) -0.022(3) 0.006(3) -0.018(3) C45 0.044(3) 0.038(4) 0.038(3) -0.022(3) 0.004(3) -0.010(3) _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 N6 2.063(5) . ? Fe1 N1 2.145(5) . ? Fe1 N4 2.141(4) . ? Fe1 N3 2.258(4) . ? Fe1 N5 2.293(3) . ? S1 O4 1.426(5) . ? S1 O6 1.432(5) . ? S1 O5 1.431(5) . ? S1 C44 1.817(7) . ? S2 O1 1.428(5) . ? S2 O3 1.428(6) . ? S2 O2 1.431(5) . ? S2 C45 1.819(6) . ? F1 C44 1.344(8) . ? F3 C44 1.309(8) . ? F4 C44 1.324(9) . ? F7 C45 1.340(7) . ? F8 C45 1.315(9) . ? F9 C45 1.316(8) . ? N1 C8 1.491(6) . ? N1 C16 1.496(6) . ? N1 C1 1.519(7) . ? C50 N3 1.478(7) . ? C50 C8 1.514(6) . ? C50 H2A 0.9900 . ? C50 H2B 0.9900 . ? N3 C9 1.492(7) . ? N3 C31 1.508(6) . ? N4 C12 1.492(5) . ? N4 C11 1.490(6) . ? N4 C24 1.528(7) . ? N5 C13 1.472(7) . ? N5 C14 1.486(7) . ? N5 C17 1.502(7) . ? N6 C38 1.136(7) . ? N7 C40 1.150(8) . ? N8 C42 1.131(10) . ? C1 C2 1.501(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.395(7) . ? C2 C3 1.399(7) . ? C3 C4 1.384(9) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.385(9) . ? C5 H5 0.9500 . ? C6 C7 1.381(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.497(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.529(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.518(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.507(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.532(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.521(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.367(8) . ? C18 C23 1.403(8) . ? C19 C20 1.401(6) . ? C19 H19 0.9500 . ? C20 C21 1.388(9) . ? C20 H20 0.9500 . ? C21 C22 1.377(9) . ? C21 H21 0.9500 . ? C22 C23 1.391(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.497(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.399(7) . ? C25 C26 1.404(7) . ? C26 C27 1.375(9) . ? C26 H26 0.9500 . ? C27 C28 1.394(8) . ? C27 H27 0.9500 . ? C28 C29 1.367(9) . ? C28 H28 0.9500 . ? C29 C30 1.384(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.522(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.389(8) . ? C32 C33 1.397(7) . ? C33 C34 1.392(7) . ? C33 H33 0.9500 . ? C34 C35 1.372(9) . ? C34 H34 0.9500 . ? C35 C36 1.381(8) . ? C35 H35 0.9500 . ? C36 C37 1.397(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.448(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.441(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.464(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? 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 N6 Fe1 N1 108.96(18) . . ? N6 Fe1 N4 110.53(18) . . ? N1 Fe1 N4 140.44(18) . . ? N6 Fe1 N3 96.61(15) . . ? N1 Fe1 N3 83.69(15) . . ? N4 Fe1 N3 93.93(15) . . ? N6 Fe1 N5 91.49(15) . . ? N1 Fe1 N5 93.11(14) . . ? N4 Fe1 N5 83.77(14) . . ? N3 Fe1 N5 171.88(17) . . ? O4 S1 O6 116.3(4) . . ? O4 S1 O5 114.7(3) . . ? O6 S1 O5 115.2(3) . . ? O4 S1 C44 102.3(3) . . ? O6 S1 C44 102.1(3) . . ? O5 S1 C44 103.3(3) . . ? O1 S2 O3 114.4(4) . . ? O1 S2 O2 115.4(3) . . ? O3 S2 O2 115.7(4) . . ? O1 S2 C45 104.0(3) . . ? O3 S2 C45 102.3(3) . . ? O2 S2 C45 102.4(3) . . ? C8 N1 C16 106.8(4) . . ? C8 N1 C1 110.4(4) . . ? C16 N1 C1 112.4(4) . . ? C8 N1 Fe1 104.3(3) . . ? C16 N1 Fe1 113.8(3) . . ? C1 N1 Fe1 108.9(3) . . ? N3 C50 C8 111.1(4) . . ? N3 C50 H2A 109.4 . . ? C8 C50 H2A 109.4 . . ? N3 C50 H2B 109.4 . . ? C8 C50 H2B 109.4 . . ? H2A C50 H2B 108.0 . . ? C50 N3 C9 108.5(4) . . ? C50 N3 C31 110.2(4) . . ? C9 N3 C31 110.4(3) . . ? C50 N3 Fe1 102.4(2) . . ? C9 N3 Fe1 112.4(3) . . ? C31 N3 Fe1 112.6(3) . . ? C12 N4 C11 107.2(4) . . ? C12 N4 C24 110.8(4) . . ? C11 N4 C24 111.2(4) . . ? C12 N4 Fe1 104.3(3) . . ? C11 N4 Fe1 112.9(3) . . ? C24 N4 Fe1 110.2(3) . . ? C13 N5 C14 108.8(4) . . ? C13 N5 C17 110.3(4) . . ? C14 N5 C17 110.7(4) . . ? C13 N5 Fe1 101.5(2) . . ? C14 N5 Fe1 111.5(3) . . ? C17 N5 Fe1 113.7(3) . . ? C38 N6 Fe1 160.8(4) . . ? C2 C1 N1 115.0(4) . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? N1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 117.9(5) . . ? C7 C2 C1 119.9(4) . . ? C3 C2 C1 122.2(5) . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.5(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 121.3(5) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? N1 C8 C50 110.2(4) . . ? N1 C8 H8A 109.6 . . ? C50 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C50 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N3 C9 C10 115.8(4) . . ? N3 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? N3 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 115.6(4) . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? N4 C11 C10 115.2(4) . . ? N4 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? N4 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N4 C12 C13 110.8(4) . . ? N4 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N5 C13 C12 111.7(4) . . ? N5 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? N5 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N5 C14 C15 115.8(4) . . ? N5 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? N5 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 114.4(4) . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? N1 C16 C15 114.6(5) . . ? N1 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? N1 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N5 C17 C18 116.0(4) . . ? N5 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? N5 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C23 118.9(4) . . ? C19 C18 C17 121.8(4) . . ? C23 C18 C17 119.3(5) . . ? C18 C19 C20 122.3(5) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C21 C20 C19 118.1(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 119.4(6) . . ? C22 C23 H23 120.3 . . ? C18 C23 H23 120.3 . . ? C25 C24 N4 114.2(5) . . ? C25 C24 H24A 108.7 . . ? N4 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? N4 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C30 C25 C26 116.5(5) . . ? C30 C25 C24 120.9(5) . . ? C26 C25 C24 122.6(4) . . ? C27 C26 C25 122.0(5) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.9(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.3(6) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 120.7(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 121.5(5) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? N3 C31 C32 114.2(4) . . ? N3 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N3 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C37 C32 C33 119.0(4) . . ? C37 C32 C31 121.0(4) . . ? C33 C32 C31 120.0(5) . . ? C34 C33 C32 120.2(6) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 120.1(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.8(5) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C37 119.5(6) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C32 C37 C36 120.5(5) . . ? C32 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? N6 C38 C39 176.7(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C41 178.6(8) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N8 C42 C43 179.2(9) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? F3 C44 F4 107.8(7) . . ? F3 C44 F1 105.6(6) . . ? F4 C44 F1 107.3(5) . . ? F3 C44 S1 112.2(4) . . ? F4 C44 S1 112.4(5) . . ? F1 C44 S1 111.3(5) . . ? F8 C45 F9 108.3(6) . . ? F8 C45 F7 106.4(6) . . ? F9 C45 F7 106.9(5) . . ? F8 C45 S2 111.9(4) . . ? F9 C45 S2 112.3(5) . . ? F7 C45 S2 110.8(5) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.186 _refine_diff_density_min -3.930 _refine_diff_density_rms 0.243