# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Betley, Theodore' 'Eames, Emily' 'Harris, David' _publ_contact_author_name 'Betley, Theodore' _publ_contact_author_email betley@chemistry.harvard.edu _publ_section_title ; Modulation of Magnetic Behavior via Ligand-Field Effects in the Trigonal Clusters (PhL)Fe3L*3 (L* = thf, py, PMe2Ph) ; data_100K _database_code_depnum_ccdc_archive 'CCDC 789355' #TrackingRef '2147_web_deposit_cif_file_0_EmilyEames_1281822379.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H51 Fe3 N9, 2(C6 H6)' _chemical_formula_sum 'C68 H63 Fe3 N9' _chemical_formula_weight 1173.82 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' 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 11.805(2) _cell_length_b 12.980(2) _cell_length_c 19.363(4) _cell_angle_alpha 73.794(3) _cell_angle_beta 86.132(3) _cell_angle_gamma 75.907(3) _cell_volume 2763.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6533 _cell_measurement_theta_min 2.1905 _cell_measurement_theta_max 27.301 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6914 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39842 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.83 _reflns_number_total 12740 _reflns_number_gt 8927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 XP _computing_publication_material XCIF _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^)+(0.0442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12740 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 0.62922(3) 0.23713(3) 0.230378(19) 0.02226(10) Uani 1 1 d . . . Fe2 Fe 0.69003(3) 0.06363(3) 0.181413(19) 0.02057(9) Uani 1 1 d . . . Fe3 Fe 0.77251(3) 0.06500(3) 0.300871(19) 0.01979(9) Uani 1 1 d . . . N1 N 0.68969(16) -0.05313(16) 0.28899(10) 0.0192(4) Uani 1 1 d . . . N1L N 0.50683(17) 0.38602(16) 0.22423(11) 0.0217(5) Uani 1 1 d . . . N2 N 0.61765(17) 0.14284(16) 0.34279(11) 0.0201(4) Uani 1 1 d . . . N2L N 0.65137(18) -0.03865(16) 0.12268(11) 0.0244(5) Uani 1 1 d . . . N3 N 0.51855(16) 0.14471(15) 0.20504(10) 0.0187(4) Uani 1 1 d . . . N3L N 0.91215(17) -0.00517(16) 0.37551(11) 0.0222(5) Uani 1 1 d . . . N4 N 0.86651(16) -0.01033(15) 0.21409(11) 0.0198(4) Uani 1 1 d . . . N5 N 0.77629(16) 0.24026(15) 0.28520(11) 0.0195(4) Uani 1 1 d . . . N6 N 0.65865(17) 0.23146(16) 0.11651(10) 0.0197(4) Uani 1 1 d . . . C1 C 0.3859(2) -0.0211(2) 0.36945(14) 0.0245(6) Uani 1 1 d . . . H1A H 0.4125 -0.0701 0.4168 0.037 Uiso 1 1 calc R . . H1B H 0.3573 -0.0622 0.3417 0.037 Uiso 1 1 calc R . . H1C H 0.3227 0.0406 0.3754 0.037 Uiso 1 1 calc R . . C2 C 0.4878(2) 0.02358(19) 0.32938(13) 0.0205(5) Uani 1 1 d . . . C3 C 0.5818(2) -0.07665(19) 0.32278(13) 0.0216(5) Uani 1 1 d . . . H3A H 0.6003 -0.1270 0.3715 0.026 Uiso 1 1 calc R . . H3B H 0.5497 -0.1162 0.2948 0.026 Uiso 1 1 calc R . . C4 C 0.5260(2) 0.0875(2) 0.37417(13) 0.0211(5) Uani 1 1 d . . . H4A H 0.4571 0.1434 0.3830 0.025 Uiso 1 1 calc R . . H4B H 0.5533 0.0360 0.4214 0.025 Uiso 1 1 calc R . . C5 C 0.4380(2) 0.09806(19) 0.25722(13) 0.0204(5) Uani 1 1 d . . . H5A H 0.3995 0.0553 0.2350 0.025 Uiso 1 1 calc R . . H5B H 0.3765 0.1598 0.2664 0.025 Uiso 1 1 calc R . . C6 C 0.7710(2) -0.14679(19) 0.28112(13) 0.0197(5) Uani 1 1 d . . . C7 C 0.7619(2) -0.25532(19) 0.30714(13) 0.0243(6) Uani 1 1 d . . . H7A H 0.6941 -0.2717 0.3327 0.029 Uiso 1 1 calc R . . C8 C 0.8527(2) -0.3406(2) 0.29571(15) 0.0289(6) Uani 1 1 d . . . H8A H 0.8462 -0.4149 0.3135 0.035 Uiso 1 1 calc R . . C9 C 0.9503(2) -0.3181(2) 0.25934(14) 0.0280(6) Uani 1 1 d . . . H9A H 1.0119 -0.3769 0.2525 0.034 Uiso 1 1 calc R . . C10 C 0.9606(2) -0.2103(2) 0.23226(14) 0.0232(6) Uani 1 1 d . . . H10A H 1.0289 -0.1954 0.2067 0.028 Uiso 1 1 calc R . . C11 C 0.8712(2) -0.12387(19) 0.24237(13) 0.0195(5) Uani 1 1 d . . . C12 C 0.9716(2) 0.01105(18) 0.17953(13) 0.0205(5) Uani 1 1 d . . . C13 C 0.9796(2) 0.0464(2) 0.10575(14) 0.0249(6) Uani 1 1 d . . . H13A H 0.9135 0.0565 0.0771 0.030 Uiso 1 1 calc R . . C14 C 1.0819(2) 0.0675(2) 0.07289(15) 0.0314(7) Uani 1 1 d . . . H14A H 1.0854 0.0921 0.0219 0.038 Uiso 1 1 calc R . . C15 C 1.1788(2) 0.0533(2) 0.11289(16) 0.0312(6) Uani 1 1 d . . . H15A H 1.2488 0.0692 0.0902 0.037 Uiso 1 1 calc R . . C16 C 1.1727(2) 0.0154(2) 0.18662(15) 0.0296(6) Uani 1 1 d . . . H16A H 1.2396 0.0039 0.2150 0.036 Uiso 1 1 calc R . . C17 C 1.0708(2) -0.0060(2) 0.21958(14) 0.0242(6) Uani 1 1 d . . . H17A H 1.0684 -0.0327 0.2705 0.029 Uiso 1 1 calc R . . C18 C 0.6431(2) 0.21063(19) 0.38124(13) 0.0195(5) Uani 1 1 d . . . C19 C 0.5896(2) 0.2302(2) 0.44369(13) 0.0232(6) Uani 1 1 d . . . H19A H 0.5299 0.1940 0.4652 0.028 Uiso 1 1 calc R . . C20 C 0.6226(2) 0.3023(2) 0.47513(14) 0.0248(6) Uani 1 1 d . . . H20A H 0.5846 0.3163 0.5175 0.030 Uiso 1 1 calc R . . C21 C 0.7102(2) 0.3534(2) 0.44507(13) 0.0249(6) Uani 1 1 d . . . H21A H 0.7331 0.4021 0.4670 0.030 Uiso 1 1 calc R . . C22 C 0.7654(2) 0.33417(19) 0.38266(13) 0.0227(6) Uani 1 1 d . . . H22A H 0.8269 0.3687 0.3626 0.027 Uiso 1 1 calc R . . C23 C 0.7311(2) 0.26484(19) 0.34947(12) 0.0194(5) Uani 1 1 d . . . C24 C 0.8473(2) 0.30884(19) 0.24326(13) 0.0195(5) Uani 1 1 d . . . C25 C 0.9573(2) 0.2630(2) 0.22170(14) 0.0252(6) Uani 1 1 d . . . H25A H 0.9868 0.1852 0.2365 0.030 Uiso 1 1 calc R . . C26 C 1.0249(2) 0.3287(2) 0.17900(15) 0.0311(6) Uani 1 1 d . . . H26A H 1.1003 0.2956 0.1645 0.037 Uiso 1 1 calc R . . C27 C 0.9848(2) 0.4412(2) 0.15714(15) 0.0316(6) Uani 1 1 d . . . H27A H 1.0320 0.4860 0.1277 0.038 Uiso 1 1 calc R . . C28 C 0.8749(2) 0.4888(2) 0.17845(14) 0.0298(6) Uani 1 1 d . . . H28A H 0.8463 0.5667 0.1640 0.036 Uiso 1 1 calc R . . C29 C 0.8070(2) 0.42279(19) 0.22080(13) 0.0238(6) Uani 1 1 d . . . H29A H 0.7313 0.4559 0.2349 0.029 Uiso 1 1 calc R . . C30 C 0.4637(2) 0.22109(19) 0.14378(13) 0.0189(5) Uani 1 1 d . . . C31 C 0.3448(2) 0.2547(2) 0.12926(13) 0.0222(5) Uani 1 1 d . . . H31A H 0.2919 0.2194 0.1607 0.027 Uiso 1 1 calc R . . C32 C 0.3030(2) 0.3403(2) 0.06849(13) 0.0231(6) Uani 1 1 d . . . H32A H 0.2214 0.3638 0.0592 0.028 Uiso 1 1 calc R . . C33 C 0.3783(2) 0.3908(2) 0.02217(13) 0.0222(5) Uani 1 1 d . . . H33A H 0.3489 0.4501 -0.0186 0.027 Uiso 1 1 calc R . . C34 C 0.4978(2) 0.35539(19) 0.03474(13) 0.0201(5) Uani 1 1 d . . . H34A H 0.5500 0.3901 0.0023 0.024 Uiso 1 1 calc R . . C35 C 0.54142(19) 0.26934(19) 0.09462(13) 0.0184(5) Uani 1 1 d . . . C36 C 0.7401(2) 0.25519(19) 0.06048(13) 0.0203(5) Uani 1 1 d . . . C37 C 0.8156(2) 0.32125(19) 0.06050(13) 0.0220(5) Uani 1 1 d . . . H37A H 0.8124 0.3549 0.0986 0.026 Uiso 1 1 calc R . . C38 C 0.8956(2) 0.3390(2) 0.00580(14) 0.0279(6) Uani 1 1 d . . . H38A H 0.9469 0.3849 0.0066 0.033 Uiso 1 1 calc R . . C39 C 0.9021(2) 0.2910(2) -0.04989(14) 0.0277(6) Uani 1 1 d . . . H39A H 0.9578 0.3031 -0.0872 0.033 Uiso 1 1 calc R . . C40 C 0.8269(2) 0.2254(2) -0.05077(13) 0.0260(6) Uani 1 1 d . . . H40A H 0.8307 0.1916 -0.0888 0.031 Uiso 1 1 calc R . . C41 C 0.7463(2) 0.2085(2) 0.00325(13) 0.0225(5) Uani 1 1 d . . . H41A H 0.6938 0.1642 0.0016 0.027 Uiso 1 1 calc R . . C45 C 0.4951(2) 0.4724(2) 0.16633(14) 0.0289(6) Uani 1 1 d . . . H1LA H 0.5576 0.4757 0.1328 0.035 Uiso 1 1 calc R . . C46 C 0.3969(3) 0.5565(2) 0.15313(15) 0.0374(7) Uani 1 1 d . . . H2LA H 0.3922 0.6175 0.1117 0.045 Uiso 1 1 calc R . . C47 C 0.3057(2) 0.5517(2) 0.20041(15) 0.0341(7) Uani 1 1 d . . . H3LA H 0.2360 0.6084 0.1917 0.041 Uiso 1 1 calc R . . C48 C 0.3161(2) 0.4646(2) 0.26010(15) 0.0313(6) Uani 1 1 d . . . H4LA H 0.2541 0.4595 0.2939 0.038 Uiso 1 1 calc R . . C49 C 0.4181(2) 0.3843(2) 0.27037(14) 0.0273(6) Uani 1 1 d . . . H5LA H 0.4257 0.3243 0.3126 0.033 Uiso 1 1 calc R . . C50 C 0.7322(2) -0.1134(2) 0.09931(14) 0.0282(6) Uani 1 1 d . . . H6LA H 0.8123 -0.1185 0.1069 0.034 Uiso 1 1 calc R . . C51 C 0.7039(2) -0.1832(2) 0.06462(15) 0.0338(7) Uani 1 1 d . . . H7LA H 0.7634 -0.2345 0.0479 0.041 Uiso 1 1 calc R . . C52 C 0.5879(3) -0.1771(3) 0.05464(17) 0.0439(8) Uani 1 1 d . . . H8LA H 0.5654 -0.2244 0.0313 0.053 Uiso 1 1 calc R . . C53 C 0.5059(3) -0.1013(3) 0.07918(19) 0.0494(9) Uani 1 1 d . . . H9LA H 0.4252 -0.0954 0.0729 0.059 Uiso 1 1 calc R . . C54 C 0.5397(2) -0.0344(2) 0.11253(16) 0.0357(7) Uani 1 1 d . . . H10B H 0.4812 0.0176 0.1293 0.043 Uiso 1 1 calc R . . C55 C 0.9833(2) 0.0528(2) 0.38891(13) 0.0228(6) Uani 1 1 d . . . H11A H 0.9634 0.1308 0.3703 0.027 Uiso 1 1 calc R . . C56 C 1.0838(2) 0.0044(2) 0.42845(14) 0.0262(6) Uani 1 1 d . . . H12A H 1.1325 0.0483 0.4365 0.031 Uiso 1 1 calc R . . C57 C 1.1135(2) -0.1088(2) 0.45643(14) 0.0286(6) Uani 1 1 d . . . H13B H 1.1836 -0.1444 0.4830 0.034 Uiso 1 1 calc R . . C58 C 1.0390(2) -0.1684(2) 0.44479(14) 0.0296(6) Uani 1 1 d . . . H14B H 1.0556 -0.2462 0.4646 0.036 Uiso 1 1 calc R . . C59 C 0.9401(2) -0.1147(2) 0.40429(14) 0.0259(6) Uani 1 1 d . . . H15B H 0.8894 -0.1570 0.3963 0.031 Uiso 1 1 calc R . . C60 C 0.2254(2) 0.2408(2) 0.44172(16) 0.0368(7) Uani 1 1 d . . . H60A H 0.2778 0.1701 0.4512 0.044 Uiso 1 1 calc R . . C61 C 0.2225(3) 0.3062(3) 0.48632(17) 0.0437(8) Uani 1 1 d . . . H61A H 0.2728 0.2813 0.5269 0.052 Uiso 1 1 calc R . . C62 C 0.1465(3) 0.4084(3) 0.47236(18) 0.0464(8) Uani 1 1 d . . . H62A H 0.1445 0.4541 0.5034 0.056 Uiso 1 1 calc R . . C63 C 0.0740(3) 0.4447(3) 0.41421(17) 0.0418(8) Uani 1 1 d . . . H63A H 0.0215 0.5153 0.4050 0.050 Uiso 1 1 calc R . . C64 C 0.0765(2) 0.3796(2) 0.36923(17) 0.0385(7) Uani 1 1 d . . . H64A H 0.0262 0.4047 0.3287 0.046 Uiso 1 1 calc R . . C65 C 0.1531(3) 0.2770(2) 0.38335(17) 0.0385(7) Uani 1 1 d . . . H65A H 0.1554 0.2314 0.3523 0.046 Uiso 1 1 calc R . . C70 C 0.4858(3) 0.6794(3) 0.2726(2) 0.0555(10) Uani 1 1 d . . . H70A H 0.5487 0.6929 0.2409 0.067 Uiso 1 1 calc R . . C71 C 0.3774(3) 0.7511(3) 0.2603(2) 0.0498(9) Uani 1 1 d . . . H71A H 0.3655 0.8141 0.2199 0.060 Uiso 1 1 calc R . . C72 C 0.2870(3) 0.7315(2) 0.30619(17) 0.0425(8) Uani 1 1 d . . . H72A H 0.2124 0.7812 0.2976 0.051 Uiso 1 1 calc R . . C73 C 0.3033(3) 0.6405(3) 0.36435(17) 0.0510(9) Uani 1 1 d . . . H73A H 0.2405 0.6267 0.3962 0.061 Uiso 1 1 calc R . . C74 C 0.4120(4) 0.5693(3) 0.37610(19) 0.0607(11) Uani 1 1 d . . . H74A H 0.4243 0.5059 0.4163 0.073 Uiso 1 1 calc R . . C75 C 0.5022(3) 0.5890(3) 0.3305(2) 0.0631(12) Uani 1 1 d . . . H75A H 0.5769 0.5395 0.3392 0.076 Uiso 1 1 calc R . . 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 0.0251(2) 0.02135(19) 0.0216(2) -0.00509(15) -0.00296(15) -0.00793(15) Fe2 0.01727(18) 0.02186(19) 0.0215(2) -0.00589(15) -0.00075(15) -0.00228(14) Fe3 0.01623(18) 0.01990(18) 0.0242(2) -0.00700(15) -0.00057(15) -0.00473(14) N1 0.0158(10) 0.0209(10) 0.0215(11) -0.0059(9) 0.0027(8) -0.0059(8) N1L 0.0249(11) 0.0221(11) 0.0207(11) -0.0078(9) 0.0020(9) -0.0084(9) N2 0.0200(11) 0.0197(10) 0.0232(11) -0.0070(9) 0.0017(9) -0.0086(8) N2L 0.0262(12) 0.0233(11) 0.0261(12) -0.0090(9) 0.0027(9) -0.0086(9) N3 0.0169(10) 0.0194(10) 0.0182(11) -0.0019(8) 0.0001(8) -0.0051(8) N3L 0.0200(11) 0.0254(11) 0.0201(11) -0.0046(9) -0.0004(9) -0.0052(9) N4 0.0136(10) 0.0187(10) 0.0269(12) -0.0058(9) -0.0010(9) -0.0038(8) N5 0.0163(10) 0.0203(10) 0.0222(11) -0.0056(9) 0.0002(8) -0.0054(8) N6 0.0191(10) 0.0222(11) 0.0193(11) -0.0057(9) 0.0008(8) -0.0080(8) C1 0.0205(13) 0.0264(13) 0.0261(14) -0.0049(11) 0.0004(11) -0.0069(10) C2 0.0184(12) 0.0219(12) 0.0208(13) -0.0036(10) 0.0029(10) -0.0076(10) C3 0.0202(13) 0.0215(12) 0.0227(14) -0.0041(10) 0.0008(10) -0.0064(10) C4 0.0197(12) 0.0237(13) 0.0188(13) -0.0024(10) 0.0004(10) -0.0073(10) C5 0.0161(12) 0.0239(13) 0.0231(13) -0.0076(11) 0.0013(10) -0.0071(10) C6 0.0199(12) 0.0200(12) 0.0200(13) -0.0065(10) -0.0031(10) -0.0041(10) C7 0.0236(13) 0.0230(13) 0.0253(14) -0.0044(11) 0.0004(11) -0.0063(10) C8 0.0328(15) 0.0172(12) 0.0362(16) -0.0046(11) -0.0005(13) -0.0079(11) C9 0.0259(14) 0.0231(13) 0.0346(16) -0.0118(12) -0.0010(12) -0.0002(11) C10 0.0197(13) 0.0241(13) 0.0278(14) -0.0098(11) 0.0003(11) -0.0059(10) C11 0.0220(13) 0.0189(12) 0.0197(13) -0.0046(10) -0.0042(10) -0.0083(10) C12 0.0182(12) 0.0152(12) 0.0281(14) -0.0059(10) 0.0014(11) -0.0044(10) C13 0.0184(13) 0.0261(13) 0.0277(15) -0.0048(11) 0.0001(11) -0.0036(10) C14 0.0287(15) 0.0283(14) 0.0304(16) -0.0014(12) 0.0064(12) -0.0032(12) C15 0.0201(14) 0.0280(14) 0.0450(18) -0.0084(13) 0.0069(13) -0.0082(11) C16 0.0173(13) 0.0333(15) 0.0419(18) -0.0156(13) -0.0018(12) -0.0061(11) C17 0.0201(13) 0.0258(13) 0.0274(14) -0.0090(11) 0.0003(11) -0.0044(10) C18 0.0174(12) 0.0174(12) 0.0211(13) -0.0027(10) -0.0032(10) -0.0010(10) C19 0.0189(13) 0.0254(13) 0.0234(14) -0.0040(11) -0.0009(10) -0.0046(10) C20 0.0253(14) 0.0259(13) 0.0217(14) -0.0078(11) -0.0037(11) -0.0006(11) C21 0.0296(14) 0.0217(13) 0.0246(14) -0.0090(11) -0.0076(11) -0.0034(11) C22 0.0206(13) 0.0220(13) 0.0240(14) -0.0024(11) -0.0046(11) -0.0052(10) C23 0.0191(12) 0.0202(12) 0.0160(12) -0.0042(10) -0.0016(10) 0.0004(10) C24 0.0200(12) 0.0223(12) 0.0196(13) -0.0073(10) -0.0034(10) -0.0083(10) C25 0.0230(13) 0.0229(13) 0.0282(15) -0.0053(11) 0.0005(11) -0.0045(11) C26 0.0204(14) 0.0341(15) 0.0352(16) -0.0053(13) 0.0034(12) -0.0050(12) C27 0.0318(15) 0.0358(16) 0.0311(16) -0.0050(13) 0.0031(13) -0.0207(13) C28 0.0386(16) 0.0230(13) 0.0309(16) -0.0084(12) -0.0017(13) -0.0112(12) C29 0.0238(13) 0.0225(13) 0.0254(14) -0.0086(11) 0.0004(11) -0.0036(10) C30 0.0195(12) 0.0196(12) 0.0187(13) -0.0074(10) 0.0005(10) -0.0044(10) C31 0.0186(12) 0.0249(13) 0.0228(14) -0.0057(11) 0.0020(10) -0.0057(10) C32 0.0158(12) 0.0278(14) 0.0249(14) -0.0087(11) -0.0023(10) -0.0012(10) C33 0.0240(13) 0.0212(12) 0.0197(13) -0.0057(10) -0.0016(11) -0.0017(10) C34 0.0215(13) 0.0191(12) 0.0208(13) -0.0060(10) 0.0015(10) -0.0064(10) C35 0.0153(12) 0.0231(12) 0.0215(13) -0.0121(10) 0.0012(10) -0.0065(10) C36 0.0186(12) 0.0202(12) 0.0189(13) -0.0021(10) -0.0022(10) -0.0018(10) C37 0.0206(13) 0.0239(13) 0.0229(14) -0.0075(11) 0.0001(10) -0.0065(10) C38 0.0233(14) 0.0304(14) 0.0311(16) -0.0059(12) 0.0026(12) -0.0120(11) C39 0.0211(13) 0.0325(15) 0.0233(14) 0.0002(12) 0.0054(11) -0.0051(11) C40 0.0270(14) 0.0271(14) 0.0192(14) -0.0044(11) -0.0008(11) 0.0000(11) C41 0.0201(13) 0.0229(13) 0.0230(14) -0.0039(11) -0.0024(10) -0.0045(10) C45 0.0391(16) 0.0264(14) 0.0220(14) -0.0098(12) 0.0054(12) -0.0067(12) C46 0.0485(18) 0.0311(15) 0.0235(15) -0.0039(12) 0.0003(13) 0.0033(13) C47 0.0303(15) 0.0357(16) 0.0351(17) -0.0157(13) -0.0063(13) 0.0034(12) C48 0.0284(15) 0.0332(15) 0.0369(17) -0.0166(13) 0.0053(12) -0.0093(12) C49 0.0323(15) 0.0237(13) 0.0280(15) -0.0090(11) 0.0055(12) -0.0099(11) C50 0.0259(14) 0.0319(15) 0.0286(15) -0.0115(12) -0.0002(12) -0.0063(12) C51 0.0384(17) 0.0308(15) 0.0342(16) -0.0166(13) 0.0017(13) -0.0032(13) C52 0.0441(19) 0.0477(19) 0.055(2) -0.0334(17) 0.0019(16) -0.0165(15) C53 0.0268(16) 0.067(2) 0.075(3) -0.047(2) 0.0024(16) -0.0184(16) C54 0.0244(15) 0.0446(17) 0.0490(19) -0.0282(15) 0.0049(13) -0.0116(13) C55 0.0205(13) 0.0254(13) 0.0217(14) -0.0048(11) 0.0030(11) -0.0063(11) C56 0.0192(13) 0.0351(15) 0.0252(14) -0.0087(12) 0.0011(11) -0.0077(11) C57 0.0217(14) 0.0330(15) 0.0274(15) -0.0062(12) -0.0029(11) -0.0011(11) C58 0.0314(15) 0.0250(14) 0.0282(15) -0.0033(12) -0.0021(12) -0.0027(12) C59 0.0276(14) 0.0251(14) 0.0256(14) -0.0055(11) 0.0000(11) -0.0087(11) C60 0.0295(16) 0.0331(16) 0.0412(18) -0.0034(14) 0.0064(14) -0.0045(12) C61 0.0341(17) 0.058(2) 0.0351(18) -0.0047(16) -0.0016(14) -0.0116(15) C62 0.050(2) 0.0474(19) 0.047(2) -0.0224(16) 0.0088(17) -0.0136(16) C63 0.0348(17) 0.0367(17) 0.048(2) -0.0098(15) 0.0067(15) -0.0019(13) C64 0.0288(16) 0.0442(18) 0.0398(18) -0.0024(15) 0.0045(13) -0.0151(14) C65 0.0387(17) 0.0402(17) 0.0417(19) -0.0154(15) 0.0137(15) -0.0174(14) C70 0.040(2) 0.056(2) 0.086(3) -0.043(2) -0.0101(19) -0.0085(17) C71 0.048(2) 0.0355(18) 0.068(2) -0.0193(17) -0.0129(18) -0.0041(15) C72 0.0417(19) 0.0373(17) 0.051(2) -0.0241(16) -0.0121(16) 0.0033(14) C73 0.069(2) 0.047(2) 0.0370(19) -0.0236(16) -0.0107(17) 0.0024(17) C74 0.089(3) 0.042(2) 0.045(2) -0.0223(17) -0.031(2) 0.017(2) C75 0.053(2) 0.061(2) 0.081(3) -0.049(2) -0.038(2) 0.0201(19) _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 N1L 2.091(2) . ? Fe1 N5 2.109(2) . ? Fe1 N3 2.137(2) . ? Fe1 N2 2.193(2) . ? Fe1 N6 2.228(2) . ? Fe1 Fe3 2.5466(6) . ? Fe1 Fe2 2.6074(6) . ? Fe2 N2L 2.115(2) . ? Fe2 N3 2.1263(19) . ? Fe2 N4 2.1277(19) . ? Fe2 N6 2.146(2) . ? Fe2 N1 2.208(2) . ? Fe2 Fe3 2.5756(6) . ? Fe3 N1 2.078(2) . ? Fe3 N2 2.0928(19) . ? Fe3 N3L 2.119(2) . ? Fe3 N5 2.221(2) . ? Fe3 N4 2.269(2) . ? N1 C6 1.392(3) . ? N1 C3 1.452(3) . ? N1L C49 1.331(3) . ? N1L C45 1.333(3) . ? N2 C18 1.394(3) . ? N2 C4 1.450(3) . ? N2L C54 1.332(3) . ? N2L C50 1.338(3) . ? N3 C30 1.394(3) . ? N3 C5 1.449(3) . ? N3L C55 1.336(3) . ? N3L C59 1.340(3) . ? N4 C11 1.410(3) . ? N4 C12 1.420(3) . ? N5 C23 1.409(3) . ? N5 C24 1.422(3) . ? N6 C35 1.403(3) . ? N6 C36 1.419(3) . ? C1 C2 1.532(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.510(3) . ? C2 C3 1.520(3) . ? C2 C5 1.521(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.385(3) . ? C6 C11 1.407(3) . ? C7 C8 1.396(3) . ? C7 H7A 0.9500 . ? C8 C9 1.359(3) . ? C8 H8A 0.9500 . ? C9 C10 1.383(3) . ? C9 H9A 0.9500 . ? C10 C11 1.389(3) . ? C10 H10A 0.9500 . ? C12 C13 1.377(3) . ? C12 C17 1.387(3) . ? C13 C14 1.378(3) . ? C13 H13A 0.9500 . ? C14 C15 1.370(4) . ? C14 H14A 0.9500 . ? C15 C16 1.377(4) . ? C15 H15A 0.9500 . ? C16 C17 1.375(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.384(3) . ? C18 C23 1.408(3) . ? C19 C20 1.388(3) . ? C19 H19A 0.9500 . ? C20 C21 1.373(3) . ? C20 H20A 0.9500 . ? C21 C22 1.389(3) . ? C21 H21A 0.9500 . ? C22 C23 1.386(3) . ? C22 H22A 0.9500 . ? C24 C25 1.380(3) . ? C24 C29 1.389(3) . ? C25 C26 1.377(3) . ? C25 H25A 0.9500 . ? C26 C27 1.372(4) . ? C26 H26A 0.9500 . ? C27 C28 1.384(4) . ? C27 H27A 0.9500 . ? C28 C29 1.379(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.387(3) . ? C30 C35 1.404(3) . ? C31 C32 1.395(3) . ? C31 H31A 0.9500 . ? C32 C33 1.369(3) . ? C32 H32A 0.9500 . ? C33 C34 1.388(3) . ? C33 H33A 0.9500 . ? C34 C35 1.391(3) . ? C34 H34A 0.9500 . ? C36 C37 1.379(3) . ? C36 C41 1.394(3) . ? C37 C38 1.380(3) . ? C37 H37A 0.9500 . ? C38 C39 1.377(4) . ? C38 H38A 0.9500 . ? C39 C40 1.377(4) . ? C39 H39A 0.9500 . ? C40 C41 1.373(3) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C45 C46 1.366(4) . ? C45 H1LA 0.9500 . ? C46 C47 1.367(4) . ? C46 H2LA 0.9500 . ? C47 C48 1.361(4) . ? C47 H3LA 0.9500 . ? C48 C49 1.371(3) . ? C48 H4LA 0.9500 . ? C49 H5LA 0.9500 . ? C50 C51 1.379(4) . ? C50 H6LA 0.9500 . ? C51 C52 1.377(4) . ? C51 H7LA 0.9500 . ? C52 C53 1.366(4) . ? C52 H8LA 0.9500 . ? C53 C54 1.359(4) . ? C53 H9LA 0.9500 . ? C54 H10B 0.9500 . ? C55 C56 1.371(3) . ? C55 H11A 0.9500 . ? C56 C57 1.380(3) . ? C56 H12A 0.9500 . ? C57 C58 1.371(4) . ? C57 H13B 0.9500 . ? C58 C59 1.373(3) . ? C58 H14B 0.9500 . ? C59 H15B 0.9500 . ? C60 C61 1.363(4) . ? C60 C65 1.366(4) . ? C60 H60A 0.9500 . ? C61 C62 1.375(4) . ? C61 H61A 0.9500 . ? C62 C63 1.364(4) . ? C62 H62A 0.9500 . ? C63 C64 1.366(4) . ? C63 H63A 0.9500 . ? C64 C65 1.381(4) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C70 C75 1.362(5) . ? C70 C71 1.377(4) . ? C70 H70A 0.9500 . ? C71 C72 1.368(4) . ? C71 H71A 0.9500 . ? C72 C73 1.370(4) . ? C72 H72A 0.9500 . ? C73 C74 1.378(5) . ? C73 H73A 0.9500 . ? C74 C75 1.363(5) . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? 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 N1L Fe1 N5 107.14(8) . . ? N1L Fe1 N3 99.43(8) . . ? N5 Fe1 N3 149.16(7) . . ? N1L Fe1 N2 103.33(8) . . ? N5 Fe1 N2 72.22(7) . . ? N3 Fe1 N2 86.83(7) . . ? N1L Fe1 N6 104.51(8) . . ? N5 Fe1 N6 115.84(7) . . ? N3 Fe1 N6 70.75(7) . . ? N2 Fe1 N6 146.60(7) . . ? N1L Fe1 Fe3 151.48(6) . . ? N5 Fe1 Fe3 56.03(5) . . ? N3 Fe1 Fe3 93.27(5) . . ? N2 Fe1 Fe3 51.75(5) . . ? N6 Fe1 Fe3 103.76(5) . . ? N1L Fe1 Fe2 145.57(6) . . ? N5 Fe1 Fe2 106.19(5) . . ? N3 Fe1 Fe2 52.11(5) . . ? N2 Fe1 Fe2 94.76(5) . . ? N6 Fe1 Fe2 51.97(5) . . ? Fe3 Fe1 Fe2 59.952(17) . . ? N2L Fe2 N3 100.49(8) . . ? N2L Fe2 N4 103.77(8) . . ? N3 Fe2 N4 149.30(8) . . ? N2L Fe2 N6 110.31(8) . . ? N3 Fe2 N6 72.55(7) . . ? N4 Fe2 N6 115.12(7) . . ? N2L Fe2 N1 96.64(8) . . ? N3 Fe2 N1 87.00(7) . . ? N4 Fe2 N1 71.85(7) . . ? N6 Fe2 N1 148.44(7) . . ? N2L Fe2 Fe3 144.31(6) . . ? N3 Fe2 Fe3 92.69(6) . . ? N4 Fe2 Fe3 56.73(5) . . ? N6 Fe2 Fe3 105.26(6) . . ? N1 Fe2 Fe3 50.77(5) . . ? N2L Fe2 Fe1 150.50(6) . . ? N3 Fe2 Fe1 52.47(5) . . ? N4 Fe2 Fe1 105.70(6) . . ? N6 Fe2 Fe1 54.86(5) . . ? N1 Fe2 Fe1 93.64(5) . . ? Fe3 Fe2 Fe1 58.853(14) . . ? N1 Fe3 N2 89.27(7) . . ? N1 Fe3 N3L 111.69(8) . . ? N2 Fe3 N3L 114.46(8) . . ? N1 Fe3 N5 150.53(7) . . ? N2 Fe3 N5 71.97(7) . . ? N3L Fe3 N5 96.94(8) . . ? N1 Fe3 N4 71.51(7) . . ? N2 Fe3 N4 149.70(8) . . ? N3L Fe3 N4 94.69(7) . . ? N5 Fe3 N4 114.29(7) . . ? N1 Fe3 Fe1 98.71(6) . . ? N2 Fe3 Fe1 55.38(6) . . ? N3L Fe3 Fe1 148.32(6) . . ? N5 Fe3 Fe1 51.98(5) . . ? N4 Fe3 Fe1 103.48(5) . . ? N1 Fe3 Fe2 55.42(6) . . ? N2 Fe3 Fe2 98.23(6) . . ? N3L Fe3 Fe2 145.43(6) . . ? N5 Fe3 Fe2 103.91(5) . . ? N4 Fe3 Fe2 51.63(5) . . ? Fe1 Fe3 Fe2 61.196(16) . . ? C6 N1 C3 113.28(19) . . ? C6 N1 Fe3 110.87(15) . . ? C3 N1 Fe3 127.27(15) . . ? C6 N1 Fe2 102.41(14) . . ? C3 N1 Fe2 121.33(15) . . ? Fe3 N1 Fe2 73.81(6) . . ? C49 N1L C45 117.1(2) . . ? C49 N1L Fe1 117.45(16) . . ? C45 N1L Fe1 122.81(16) . . ? C18 N2 C4 114.29(19) . . ? C18 N2 Fe3 109.23(14) . . ? C4 N2 Fe3 123.46(15) . . ? C18 N2 Fe1 103.27(14) . . ? C4 N2 Fe1 126.40(15) . . ? Fe3 N2 Fe1 72.87(6) . . ? C54 N2L C50 117.6(2) . . ? C54 N2L Fe2 118.28(17) . . ? C50 N2L Fe2 123.98(18) . . ? C30 N3 C5 113.46(18) . . ? C30 N3 Fe2 111.32(14) . . ? C5 N3 Fe2 127.05(14) . . ? C30 N3 Fe1 99.67(14) . . ? C5 N3 Fe1 121.78(15) . . ? Fe2 N3 Fe1 75.42(6) . . ? C55 N3L C59 117.5(2) . . ? C55 N3L Fe3 122.89(16) . . ? C59 N3L Fe3 119.06(17) . . ? C11 N4 C12 113.13(18) . . ? C11 N4 Fe2 105.26(14) . . ? C12 N4 Fe2 129.79(15) . . ? C11 N4 Fe3 103.51(14) . . ? C12 N4 Fe3 125.50(15) . . ? Fe2 N4 Fe3 71.64(6) . . ? C23 N5 C24 116.30(19) . . ? C23 N5 Fe1 104.70(14) . . ? C24 N5 Fe1 114.28(15) . . ? C23 N5 Fe3 105.01(14) . . ? C24 N5 Fe3 133.46(15) . . ? Fe1 N5 Fe3 71.99(6) . . ? C35 N6 C36 114.32(19) . . ? C35 N6 Fe2 110.13(14) . . ? C36 N6 Fe2 116.08(14) . . ? C35 N6 Fe1 97.09(13) . . ? C36 N6 Fe1 138.75(16) . . ? Fe2 N6 Fe1 73.17(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C3 112.9(2) . . ? C4 C2 C5 111.8(2) . . ? C3 C2 C5 113.2(2) . . ? C4 C2 C1 106.67(19) . . ? C3 C2 C1 106.17(19) . . ? C5 C2 C1 105.40(19) . . ? N1 C3 C2 115.36(19) . . ? N1 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N2 C4 C2 115.21(19) . . ? N2 C4 H4A 108.5 . . ? C2 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C2 117.46(19) . . ? N3 C5 H5A 107.9 . . ? C2 C5 H5A 107.9 . . ? N3 C5 H5B 107.9 . . ? C2 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C7 C6 N1 126.9(2) . . ? C7 C6 C11 119.3(2) . . ? N1 C6 C11 113.8(2) . . ? C6 C7 C8 119.9(2) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.5(2) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C11 120.1(2) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C6 119.6(2) . . ? C10 C11 N4 126.3(2) . . ? C6 C11 N4 114.1(2) . . ? C13 C12 C17 117.9(2) . . ? C13 C12 N4 121.6(2) . . ? C17 C12 N4 120.5(2) . . ? C12 C13 C14 121.0(2) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 118.7(2) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C12 120.9(2) . . ? C16 C17 H17A 119.6 . . ? C12 C17 H17A 119.6 . . ? C19 C18 N2 127.0(2) . . ? C19 C18 C23 119.5(2) . . ? N2 C18 C23 113.5(2) . . ? C18 C19 C20 120.4(2) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.3(2) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C18 119.3(2) . . ? C22 C23 N5 126.7(2) . . ? C18 C23 N5 114.0(2) . . ? C25 C24 C29 118.1(2) . . ? C25 C24 N5 120.4(2) . . ? C29 C24 N5 121.4(2) . . ? C26 C25 C24 120.7(2) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 120.9(2) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 119.2(2) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C24 121.2(2) . . ? C28 C29 H29A 119.4 . . ? C24 C29 H29A 119.4 . . ? C31 C30 N3 127.2(2) . . ? C31 C30 C35 119.4(2) . . ? N3 C30 C35 113.3(2) . . ? C30 C31 C32 120.0(2) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 120.0(2) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 120.3(2) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? C34 C35 N6 126.0(2) . . ? C34 C35 C30 119.6(2) . . ? N6 C35 C30 114.0(2) . . ? C37 C36 C41 118.0(2) . . ? C37 C36 N6 122.9(2) . . ? C41 C36 N6 119.1(2) . . ? C36 C37 C38 120.7(2) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C39 C38 C37 120.8(2) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C40 C39 C38 119.2(2) . . ? C40 C39 H39A 120.4 . . ? C38 C39 H39A 120.4 . . ? C41 C40 C39 120.1(2) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C40 C41 C36 121.2(2) . . ? C40 C41 H41A 119.4 . . ? C36 C41 H41A 119.4 . . ? N1L C45 C46 122.8(2) . . ? N1L C45 H1LA 118.6 . . ? C46 C45 H1LA 118.6 . . ? C45 C46 C47 119.0(3) . . ? C45 C46 H2LA 120.5 . . ? C47 C46 H2LA 120.5 . . ? C48 C47 C46 119.1(3) . . ? C48 C47 H3LA 120.4 . . ? C46 C47 H3LA 120.4 . . ? C47 C48 C49 118.5(3) . . ? C47 C48 H4LA 120.8 . . ? C49 C48 H4LA 120.8 . . ? N1L C49 C48 123.3(2) . . ? N1L C49 H5LA 118.3 . . ? C48 C49 H5LA 118.3 . . ? N2L C50 C51 122.7(3) . . ? N2L C50 H6LA 118.7 . . ? C51 C50 H6LA 118.7 . . ? C52 C51 C50 118.7(3) . . ? C52 C51 H7LA 120.6 . . ? C50 C51 H7LA 120.7 . . ? C53 C52 C51 118.3(3) . . ? C53 C52 H8LA 120.8 . . ? C51 C52 H8LA 120.8 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H9LA 120.0 . . ? C52 C53 H9LA 120.0 . . ? N2L C54 C53 122.7(3) . . ? N2L C54 H10B 118.6 . . ? C53 C54 H10B 118.6 . . ? N3L C55 C56 122.7(2) . . ? N3L C55 H11A 118.7 . . ? C56 C55 H11A 118.7 . . ? C55 C56 C57 119.4(3) . . ? C55 C56 H12A 120.3 . . ? C57 C56 H12A 120.3 . . ? C58 C57 C56 118.2(2) . . ? C58 C57 H13B 120.9 . . ? C56 C57 H13B 120.9 . . ? C57 C58 C59 119.4(2) . . ? C57 C58 H14B 120.3 . . ? C59 C58 H14B 120.3 . . ? N3L C59 C58 122.7(2) . . ? N3L C59 H15B 118.6 . . ? C58 C59 H15B 118.6 . . ? C61 C60 C65 119.9(3) . . ? C61 C60 H60A 120.0 . . ? C65 C60 H60A 120.0 . . ? C60 C61 C62 119.8(3) . . ? C60 C61 H61A 120.1 . . ? C62 C61 H61A 120.1 . . ? C63 C62 C61 120.4(3) . . ? C63 C62 H62A 119.8 . . ? C61 C62 H62A 119.8 . . ? C62 C63 C64 120.2(3) . . ? C62 C63 H63A 119.9 . . ? C64 C63 H63A 119.9 . . ? C63 C64 C65 119.3(3) . . ? C63 C64 H64A 120.3 . . ? C65 C64 H64A 120.3 . . ? C60 C65 C64 120.4(3) . . ? C60 C65 H65A 119.8 . . ? C64 C65 H65A 119.8 . . ? C75 C70 C71 119.7(4) . . ? C75 C70 H70A 120.2 . . ? C71 C70 H70A 120.2 . . ? C72 C71 C70 120.0(3) . . ? C72 C71 H71A 120.0 . . ? C70 C71 H71A 120.0 . . ? C71 C72 C73 120.4(3) . . ? C71 C72 H72A 119.8 . . ? C73 C72 H72A 119.8 . . ? C72 C73 C74 119.1(4) . . ? C72 C73 H73A 120.5 . . ? C74 C73 H73A 120.5 . . ? C75 C74 C73 120.5(3) . . ? C75 C74 H74A 119.7 . . ? C73 C74 H74A 119.7 . . ? C70 C75 C74 120.3(3) . . ? C70 C75 H75A 119.8 . . ? C74 C75 H75A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.478 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.075 #=============the end of compound 100K=================== #============compound 150K================================ data_150K _database_code_depnum_ccdc_archive 'CCDC 789356' #TrackingRef '2147_web_deposit_cif_file_0_EmilyEames_1281822379.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H51 Fe3 N9, 2(C6 H6)' _chemical_formula_sum 'C68 H63 Fe3 N9' _chemical_formula_weight 1173.82 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' 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 11.839(4) _cell_length_b 13.026(5) _cell_length_c 19.436(7) _cell_angle_alpha 73.818(6) _cell_angle_beta 86.197(7) _cell_angle_gamma 75.893(7) _cell_volume 2791.6(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7490 _cell_measurement_theta_min 2.167 _cell_measurement_theta_max 25.5875 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6938 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19903 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.93 _reflns_number_total 10629 _reflns_number_gt 7731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 XP _computing_publication_material XCIF _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^)+(0.0494P)^2^+0.0088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10629 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 0.63112(4) 0.23625(3) 0.22953(2) 0.02767(12) Uani 1 1 d . . . Fe2 Fe 0.69044(3) 0.06373(3) 0.18112(2) 0.02633(12) Uani 1 1 d . . . Fe3 Fe 0.77310(3) 0.06547(3) 0.29942(2) 0.02622(12) Uani 1 1 d . . . N1 N 0.69037(19) -0.05261(18) 0.28796(12) 0.0256(5) Uani 1 1 d . . . N1L N 0.5072(2) 0.38525(19) 0.22385(13) 0.0298(6) Uani 1 1 d . . . N2 N 0.61921(19) 0.14315(18) 0.34169(12) 0.0250(5) Uani 1 1 d . . . N2L N 0.6510(2) -0.03796(19) 0.12208(13) 0.0317(6) Uani 1 1 d . . . N3 N 0.51904(19) 0.14525(18) 0.20469(12) 0.0247(5) Uani 1 1 d . . . N3L N 0.9116(2) -0.00435(19) 0.37489(12) 0.0305(6) Uani 1 1 d . . . N4 N 0.86690(19) -0.01021(17) 0.21347(12) 0.0258(5) Uani 1 1 d . . . N5 N 0.77751(19) 0.24035(18) 0.28425(12) 0.0256(5) Uani 1 1 d . . . N6 N 0.65845(19) 0.23110(18) 0.11610(12) 0.0252(5) Uani 1 1 d . . . C1 C 0.3878(2) -0.0210(2) 0.36891(16) 0.0326(7) Uani 1 1 d . . . H1A H 0.4148 -0.0697 0.4160 0.049 Uiso 1 1 calc R . . H1B H 0.3593 -0.0622 0.3414 0.049 Uiso 1 1 calc R . . H1C H 0.3246 0.0403 0.3750 0.049 Uiso 1 1 calc R . . C2 C 0.4891(2) 0.0242(2) 0.32856(15) 0.0258(6) Uani 1 1 d . . . C3 C 0.5829(2) -0.0758(2) 0.32182(15) 0.0275(6) Uani 1 1 d . . . H3A H 0.6016 -0.1260 0.3704 0.033 Uiso 1 1 calc R . . H3B H 0.5506 -0.1152 0.2940 0.033 Uiso 1 1 calc R . . C4 C 0.5281(2) 0.0878(2) 0.37351(15) 0.0269(6) Uani 1 1 d . . . H4A H 0.4597 0.1435 0.3827 0.032 Uiso 1 1 calc R . . H4B H 0.5561 0.0363 0.4204 0.032 Uiso 1 1 calc R . . C5 C 0.4384(2) 0.0986(2) 0.25698(14) 0.0270(6) Uani 1 1 d . . . H5A H 0.3997 0.0561 0.2349 0.032 Uiso 1 1 calc R . . H5B H 0.3773 0.1600 0.2664 0.032 Uiso 1 1 calc R . . C6 C 0.7717(2) -0.1462(2) 0.28037(15) 0.0269(6) Uani 1 1 d . . . C7 C 0.7623(3) -0.2539(2) 0.30607(16) 0.0329(7) Uani 1 1 d . . . H7A H 0.6946 -0.2700 0.3315 0.039 Uiso 1 1 calc R . . C8 C 0.8530(3) -0.3395(2) 0.29456(18) 0.0395(8) Uani 1 1 d . . . H8A H 0.8462 -0.4135 0.3119 0.047 Uiso 1 1 calc R . . C9 C 0.9507(3) -0.3173(2) 0.25875(18) 0.0398(8) Uani 1 1 d . . . H9A H 1.0123 -0.3759 0.2521 0.048 Uiso 1 1 calc R . . C10 C 0.9604(3) -0.2098(2) 0.23204(16) 0.0315(7) Uani 1 1 d . . . H10A H 1.0287 -0.1948 0.2068 0.038 Uiso 1 1 calc R . . C11 C 0.8718(2) -0.1238(2) 0.24167(14) 0.0257(6) Uani 1 1 d . . . C12 C 0.9720(2) 0.0111(2) 0.17951(15) 0.0266(6) Uani 1 1 d . . . C13 C 0.9798(2) 0.0473(2) 0.10576(16) 0.0334(7) Uani 1 1 d . . . H13A H 0.9137 0.0579 0.0772 0.040 Uiso 1 1 calc R . . C14 C 1.0819(3) 0.0681(3) 0.07296(18) 0.0426(8) Uani 1 1 d . . . H14A H 1.0855 0.0924 0.0222 0.051 Uiso 1 1 calc R . . C15 C 1.1782(3) 0.0541(3) 0.11316(19) 0.0424(8) Uani 1 1 d . . . H15A H 1.2477 0.0707 0.0907 0.051 Uiso 1 1 calc R . . C16 C 1.1728(3) 0.0155(2) 0.18653(19) 0.0389(8) Uani 1 1 d . . . H16A H 1.2396 0.0038 0.2148 0.047 Uiso 1 1 calc R . . C17 C 1.0712(2) -0.0062(2) 0.21925(16) 0.0304(7) Uani 1 1 d . . . H17A H 1.0691 -0.0334 0.2699 0.037 Uiso 1 1 calc R . . C18 C 0.6453(2) 0.2102(2) 0.38005(14) 0.0266(6) Uani 1 1 d . . . C19 C 0.5924(2) 0.2296(2) 0.44261(15) 0.0298(7) Uani 1 1 d . . . H19A H 0.5331 0.1934 0.4641 0.036 Uiso 1 1 calc R . . C20 C 0.6252(3) 0.3010(2) 0.47398(16) 0.0358(7) Uani 1 1 d . . . H20A H 0.5874 0.3149 0.5162 0.043 Uiso 1 1 calc R . . C21 C 0.7126(3) 0.3519(2) 0.44393(16) 0.0349(7) Uani 1 1 d . . . H21A H 0.7361 0.3998 0.4660 0.042 Uiso 1 1 calc R . . C22 C 0.7664(3) 0.3336(2) 0.38174(15) 0.0309(7) Uani 1 1 d . . . H22A H 0.8275 0.3684 0.3617 0.037 Uiso 1 1 calc R . . C23 C 0.7320(2) 0.2649(2) 0.34834(14) 0.0256(6) Uani 1 1 d . . . C24 C 0.8475(2) 0.3086(2) 0.24260(15) 0.0273(6) Uani 1 1 d . . . C25 C 0.9574(3) 0.2637(2) 0.22107(16) 0.0331(7) Uani 1 1 d . . . H25A H 0.9872 0.1863 0.2359 0.040 Uiso 1 1 calc R . . C26 C 1.0246(3) 0.3294(3) 0.17839(17) 0.0412(8) Uani 1 1 d . . . H26A H 1.0995 0.2965 0.1636 0.049 Uiso 1 1 calc R . . C27 C 0.9854(3) 0.4408(3) 0.15720(18) 0.0450(9) Uani 1 1 d . . . H27A H 1.0328 0.4855 0.1285 0.054 Uiso 1 1 calc R . . C28 C 0.8751(3) 0.4881(3) 0.17815(17) 0.0400(8) Uani 1 1 d . . . H28A H 0.8464 0.5656 0.1635 0.048 Uiso 1 1 calc R . . C29 C 0.8073(3) 0.4227(2) 0.22003(16) 0.0320(7) Uani 1 1 d . . . H29A H 0.7318 0.4559 0.2338 0.038 Uiso 1 1 calc R . . C30 C 0.4637(2) 0.2212(2) 0.14373(14) 0.0252(6) Uani 1 1 d . . . C31 C 0.3457(2) 0.2548(2) 0.12931(16) 0.0296(7) Uani 1 1 d . . . H31A H 0.2930 0.2201 0.1609 0.036 Uiso 1 1 calc R . . C32 C 0.3034(3) 0.3396(2) 0.06864(16) 0.0319(7) Uani 1 1 d . . . H32A H 0.2220 0.3630 0.0594 0.038 Uiso 1 1 calc R . . C33 C 0.3786(2) 0.3892(2) 0.02228(15) 0.0305(7) Uani 1 1 d . . . H33A H 0.3492 0.4478 -0.0185 0.037 Uiso 1 1 calc R . . C34 C 0.4976(2) 0.3542(2) 0.03476(14) 0.0261(6) Uani 1 1 d . . . H34A H 0.5495 0.3886 0.0023 0.031 Uiso 1 1 calc R . . C35 C 0.5415(2) 0.2687(2) 0.09464(14) 0.0247(6) Uani 1 1 d . . . C36 C 0.7392(2) 0.2550(2) 0.05996(15) 0.0259(6) Uani 1 1 d . . . C37 C 0.8144(2) 0.3209(2) 0.06022(16) 0.0307(7) Uani 1 1 d . . . H37A H 0.8111 0.3543 0.0982 0.037 Uiso 1 1 calc R . . C38 C 0.8946(3) 0.3386(3) 0.00559(17) 0.0371(7) Uani 1 1 d . . . H38A H 0.9459 0.3840 0.0065 0.045 Uiso 1 1 calc R . . C39 C 0.9007(3) 0.2913(3) -0.05000(16) 0.0375(8) Uani 1 1 d . . . H39A H 0.9556 0.3040 -0.0875 0.045 Uiso 1 1 calc R . . C40 C 0.8264(3) 0.2252(2) -0.05065(16) 0.0350(7) Uani 1 1 d . . . H40A H 0.8308 0.1912 -0.0884 0.042 Uiso 1 1 calc R . . C41 C 0.7459(2) 0.2081(2) 0.00296(15) 0.0283(6) Uani 1 1 d . . . H41A H 0.6940 0.1637 0.0012 0.034 Uiso 1 1 calc R . . C45 C 0.4948(3) 0.4711(2) 0.16642(16) 0.0374(8) Uani 1 1 d . . . H45A H 0.5571 0.4749 0.1331 0.045 Uiso 1 1 calc R . . C46 C 0.3961(3) 0.5543(3) 0.15321(18) 0.0514(10) Uani 1 1 d . . . H46A H 0.3905 0.6145 0.1116 0.062 Uiso 1 1 calc R . . C47 C 0.3058(3) 0.5498(3) 0.20032(18) 0.0470(9) Uani 1 1 d . . . H47A H 0.2360 0.6060 0.1917 0.056 Uiso 1 1 calc R . . C48 C 0.3177(3) 0.4634(3) 0.25983(18) 0.0415(8) Uani 1 1 d . . . H48A H 0.2564 0.4581 0.2938 0.050 Uiso 1 1 calc R . . C49 C 0.4196(3) 0.3839(2) 0.27009(17) 0.0352(7) Uani 1 1 d . . . H49A H 0.4280 0.3248 0.3125 0.042 Uiso 1 1 calc R . . C50 C 0.7319(3) -0.1132(2) 0.09902(16) 0.0378(8) Uani 1 1 d . . . H50A H 0.8119 -0.1181 0.1062 0.045 Uiso 1 1 calc R . . C51 C 0.7026(3) -0.1832(3) 0.06538(18) 0.0458(9) Uani 1 1 d . . . H51A H 0.7616 -0.2352 0.0493 0.055 Uiso 1 1 calc R . . C52 C 0.5877(3) -0.1770(3) 0.0554(2) 0.0582(10) Uani 1 1 d . . . H52A H 0.5652 -0.2243 0.0323 0.070 Uiso 1 1 calc R . . C53 C 0.5061(3) -0.1011(3) 0.0795(2) 0.0635(12) Uani 1 1 d . . . H53A H 0.4256 -0.0950 0.0733 0.076 Uiso 1 1 calc R . . C54 C 0.5402(3) -0.0342(3) 0.11230(19) 0.0461(9) Uani 1 1 d . . . H54A H 0.4819 0.0177 0.1290 0.055 Uiso 1 1 calc R . . C55 C 0.9834(3) 0.0530(3) 0.38814(15) 0.0319(7) Uani 1 1 d . . . H55A H 0.9644 0.1306 0.3691 0.038 Uiso 1 1 calc R . . C56 C 1.0831(3) 0.0045(3) 0.42794(16) 0.0342(7) Uani 1 1 d . . . H56A H 1.1320 0.0480 0.4360 0.041 Uiso 1 1 calc R . . C57 C 1.1118(3) -0.1075(3) 0.45610(17) 0.0384(8) Uani 1 1 d . . . H57A H 1.1813 -0.1429 0.4831 0.046 Uiso 1 1 calc R . . C58 C 1.0375(3) -0.1673(3) 0.44427(17) 0.0414(8) Uani 1 1 d . . . H58A H 1.0542 -0.2448 0.4638 0.050 Uiso 1 1 calc R . . C59 C 0.9391(3) -0.1134(2) 0.40379(16) 0.0350(7) Uani 1 1 d . . . H59A H 0.8882 -0.1553 0.3959 0.042 Uiso 1 1 calc R . . C60 C 0.2264(3) 0.2419(3) 0.4418(2) 0.0547(10) Uani 1 1 d . . . H60A H 0.2783 0.1713 0.4510 0.066 Uiso 1 1 calc R . . C61 C 0.2237(3) 0.3067(4) 0.4864(2) 0.0629(11) Uani 1 1 d . . . H61A H 0.2740 0.2818 0.5267 0.075 Uiso 1 1 calc R . . C62 C 0.1472(4) 0.4088(4) 0.4724(2) 0.0685(12) Uani 1 1 d . . . H62A H 0.1449 0.4547 0.5031 0.082 Uiso 1 1 calc R . . C63 C 0.0754(3) 0.4434(3) 0.4148(2) 0.0606(11) Uani 1 1 d . . . H63A H 0.0223 0.5134 0.4054 0.073 Uiso 1 1 calc R . . C64 C 0.0790(3) 0.3785(3) 0.3707(2) 0.0570(10) Uani 1 1 d . . . H64A H 0.0286 0.4029 0.3303 0.068 Uiso 1 1 calc R . . C65 C 0.1547(3) 0.2786(3) 0.3842(2) 0.0538(10) Uani 1 1 d . . . H65A H 0.1575 0.2338 0.3528 0.065 Uiso 1 1 calc R . . C70 C 0.4856(4) 0.6787(4) 0.2727(3) 0.0800(15) Uani 1 1 d . . . H70A H 0.5478 0.6922 0.2406 0.096 Uiso 1 1 calc R . . C71 C 0.3778(4) 0.7496(3) 0.2612(3) 0.0667(12) Uani 1 1 d . . . H71A H 0.3655 0.8127 0.2211 0.080 Uiso 1 1 calc R . . C72 C 0.2883(4) 0.7302(3) 0.3065(2) 0.0607(11) Uani 1 1 d . . . H72A H 0.2136 0.7792 0.2977 0.073 Uiso 1 1 calc R . . C73 C 0.3055(4) 0.6406(4) 0.3645(2) 0.0718(13) Uani 1 1 d . . . H73A H 0.2433 0.6275 0.3966 0.086 Uiso 1 1 calc R . . C74 C 0.4132(5) 0.5695(4) 0.3761(3) 0.0885(17) Uani 1 1 d . . . H74A H 0.4254 0.5064 0.4161 0.106 Uiso 1 1 calc R . . C75 C 0.5028(5) 0.5890(4) 0.3304(3) 0.0847(17) Uani 1 1 d . . . H75A H 0.5775 0.5398 0.3390 0.102 Uiso 1 1 calc R . . 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 0.0310(2) 0.0286(2) 0.0248(2) -0.00736(18) -0.00115(18) -0.00907(18) Fe2 0.0250(2) 0.0279(2) 0.0249(2) -0.00650(18) 0.00045(17) -0.00484(17) Fe3 0.0240(2) 0.0266(2) 0.0288(2) -0.00853(18) 0.00056(17) -0.00633(17) N1 0.0228(12) 0.0242(12) 0.0290(13) -0.0057(10) 0.0020(10) -0.0062(10) N1L 0.0371(14) 0.0281(13) 0.0257(13) -0.0092(11) 0.0031(11) -0.0092(11) N2 0.0244(13) 0.0278(12) 0.0257(13) -0.0080(10) 0.0018(10) -0.0110(10) N2L 0.0356(15) 0.0337(14) 0.0273(14) -0.0098(11) 0.0020(11) -0.0098(11) N3 0.0224(12) 0.0261(12) 0.0234(13) -0.0046(10) 0.0011(10) -0.0046(10) N3L 0.0316(14) 0.0338(14) 0.0239(13) -0.0053(11) -0.0009(11) -0.0065(11) N4 0.0222(12) 0.0252(12) 0.0294(13) -0.0073(10) 0.0018(10) -0.0053(10) N5 0.0249(13) 0.0283(12) 0.0253(13) -0.0088(10) 0.0029(10) -0.0082(10) N6 0.0255(13) 0.0267(12) 0.0221(13) -0.0034(10) 0.0021(10) -0.0076(10) C1 0.0293(16) 0.0384(17) 0.0283(17) -0.0030(13) 0.0050(13) -0.0131(13) C2 0.0231(15) 0.0291(15) 0.0249(15) -0.0051(12) 0.0036(12) -0.0090(12) C3 0.0246(15) 0.0303(15) 0.0265(16) -0.0042(12) 0.0002(12) -0.0083(12) C4 0.0252(15) 0.0326(15) 0.0222(15) -0.0067(12) 0.0025(12) -0.0066(12) C5 0.0248(15) 0.0329(16) 0.0230(15) -0.0061(12) 0.0018(12) -0.0081(12) C6 0.0283(16) 0.0276(15) 0.0256(16) -0.0089(12) -0.0019(12) -0.0054(12) C7 0.0335(17) 0.0290(16) 0.0364(18) -0.0082(13) 0.0035(14) -0.0097(13) C8 0.043(2) 0.0238(15) 0.051(2) -0.0078(14) -0.0007(16) -0.0101(14) C9 0.0363(19) 0.0277(16) 0.055(2) -0.0171(15) -0.0002(16) -0.0004(14) C10 0.0299(16) 0.0325(16) 0.0337(17) -0.0124(14) 0.0002(13) -0.0064(13) C11 0.0313(16) 0.0227(14) 0.0242(15) -0.0062(12) -0.0040(12) -0.0079(12) C12 0.0232(15) 0.0229(14) 0.0342(17) -0.0091(12) 0.0022(13) -0.0054(12) C13 0.0243(16) 0.0357(17) 0.0356(18) -0.0078(14) 0.0010(13) -0.0008(13) C14 0.0364(19) 0.0426(19) 0.039(2) -0.0032(15) 0.0096(15) -0.0026(15) C15 0.0294(18) 0.0369(18) 0.058(2) -0.0107(16) 0.0118(16) -0.0083(14) C16 0.0272(17) 0.0390(18) 0.054(2) -0.0170(16) -0.0007(15) -0.0095(14) C17 0.0250(16) 0.0321(16) 0.0357(18) -0.0130(14) -0.0001(13) -0.0050(13) C18 0.0256(15) 0.0295(15) 0.0220(15) -0.0064(12) -0.0016(12) -0.0017(12) C19 0.0300(16) 0.0319(16) 0.0259(16) -0.0054(13) 0.0017(13) -0.0074(13) C20 0.0416(19) 0.0384(17) 0.0257(17) -0.0124(14) -0.0020(14) -0.0012(15) C21 0.0445(19) 0.0340(17) 0.0292(17) -0.0152(14) -0.0055(14) -0.0052(14) C22 0.0328(17) 0.0295(15) 0.0316(17) -0.0089(13) -0.0042(13) -0.0077(13) C23 0.0219(15) 0.0266(14) 0.0244(15) -0.0065(12) -0.0028(12) 0.0018(12) C24 0.0295(16) 0.0307(15) 0.0234(15) -0.0073(12) -0.0008(12) -0.0099(13) C25 0.0309(17) 0.0311(16) 0.0341(18) -0.0052(13) 0.0017(13) -0.0061(13) C26 0.0316(18) 0.046(2) 0.043(2) -0.0071(16) 0.0107(15) -0.0114(15) C27 0.049(2) 0.049(2) 0.041(2) -0.0072(16) 0.0094(17) -0.0278(17) C28 0.058(2) 0.0293(16) 0.0345(19) -0.0076(14) 0.0021(16) -0.0151(15) C29 0.0350(17) 0.0305(16) 0.0317(17) -0.0101(13) 0.0022(14) -0.0085(13) C30 0.0271(15) 0.0285(15) 0.0225(15) -0.0108(12) 0.0014(12) -0.0069(12) C31 0.0248(16) 0.0339(16) 0.0304(17) -0.0086(13) 0.0034(13) -0.0084(13) C32 0.0259(16) 0.0348(16) 0.0324(17) -0.0087(14) -0.0004(13) -0.0023(13) C33 0.0354(17) 0.0298(16) 0.0222(15) -0.0056(12) -0.0031(13) -0.0012(13) C34 0.0314(16) 0.0245(14) 0.0215(15) -0.0053(12) 0.0019(12) -0.0065(12) C35 0.0217(15) 0.0315(15) 0.0245(15) -0.0123(12) 0.0029(12) -0.0083(12) C36 0.0253(15) 0.0261(14) 0.0237(15) -0.0030(12) 0.0003(12) -0.0053(12) C37 0.0307(16) 0.0323(16) 0.0299(17) -0.0084(13) 0.0007(13) -0.0090(13) C38 0.0336(18) 0.0397(18) 0.0376(19) -0.0042(15) 0.0053(14) -0.0162(14) C39 0.0326(18) 0.0459(19) 0.0282(17) -0.0029(15) 0.0077(14) -0.0088(15) C40 0.0415(19) 0.0358(17) 0.0228(16) -0.0060(13) 0.0015(14) -0.0023(14) C41 0.0309(16) 0.0277(15) 0.0253(16) -0.0059(12) 0.0006(12) -0.0064(12) C45 0.047(2) 0.0332(17) 0.0293(18) -0.0101(14) 0.0072(15) -0.0042(15) C46 0.073(3) 0.0394(19) 0.0288(19) -0.0054(15) 0.0011(18) 0.0057(18) C47 0.042(2) 0.050(2) 0.043(2) -0.0186(17) -0.0066(17) 0.0073(16) C48 0.0353(19) 0.0444(19) 0.046(2) -0.0153(17) 0.0099(15) -0.0101(15) C49 0.0386(18) 0.0317(16) 0.0351(18) -0.0096(14) 0.0048(14) -0.0083(14) C50 0.0341(18) 0.0437(19) 0.0367(19) -0.0153(15) -0.0001(14) -0.0060(15) C51 0.053(2) 0.046(2) 0.042(2) -0.0208(17) -0.0014(17) -0.0072(17) C52 0.066(3) 0.056(2) 0.071(3) -0.042(2) 0.000(2) -0.018(2) C53 0.041(2) 0.082(3) 0.092(3) -0.057(3) 0.008(2) -0.025(2) C54 0.038(2) 0.055(2) 0.055(2) -0.0306(18) -0.0002(17) -0.0112(16) C55 0.0308(17) 0.0359(17) 0.0287(17) -0.0073(14) 0.0042(13) -0.0098(14) C56 0.0276(16) 0.0455(19) 0.0309(17) -0.0103(15) 0.0003(13) -0.0116(14) C57 0.0306(17) 0.0458(19) 0.0333(18) -0.0082(15) -0.0035(14) -0.0009(15) C58 0.050(2) 0.0322(17) 0.0359(19) -0.0036(14) -0.0098(16) -0.0012(15) C59 0.0410(19) 0.0347(17) 0.0291(17) -0.0070(14) 0.0001(14) -0.0108(14) C60 0.046(2) 0.051(2) 0.060(3) -0.011(2) 0.013(2) -0.0066(18) C61 0.052(2) 0.078(3) 0.055(3) -0.007(2) -0.003(2) -0.020(2) C62 0.079(3) 0.070(3) 0.064(3) -0.032(2) 0.011(3) -0.019(2) C63 0.052(2) 0.054(2) 0.068(3) -0.015(2) 0.008(2) -0.0029(19) C64 0.045(2) 0.065(3) 0.058(3) -0.004(2) 0.0066(19) -0.022(2) C65 0.061(3) 0.057(2) 0.051(2) -0.018(2) 0.016(2) -0.027(2) C70 0.059(3) 0.083(3) 0.121(4) -0.062(3) -0.016(3) -0.017(3) C71 0.069(3) 0.046(2) 0.089(3) -0.025(2) -0.014(3) -0.009(2) C72 0.066(3) 0.049(2) 0.070(3) -0.032(2) -0.016(2) 0.004(2) C73 0.097(4) 0.071(3) 0.051(3) -0.037(2) -0.011(2) -0.001(3) C74 0.136(5) 0.060(3) 0.060(3) -0.031(2) -0.036(3) 0.022(3) C75 0.079(4) 0.078(3) 0.103(4) -0.061(3) -0.050(3) 0.026(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 N1L 2.108(2) . ? Fe1 N5 2.111(2) . ? Fe1 N3 2.138(2) . ? Fe1 N2 2.194(2) . ? Fe1 N6 2.224(2) . ? Fe1 Fe3 2.5327(8) . ? Fe1 Fe2 2.5981(10) . ? Fe2 N2L 2.124(2) . ? Fe2 N4 2.131(2) . ? Fe2 N3 2.134(2) . ? Fe2 N6 2.149(2) . ? Fe2 N1 2.203(2) . ? Fe2 Fe3 2.5658(10) . ? Fe3 N1 2.081(2) . ? Fe3 N2 2.094(2) . ? Fe3 N3L 2.125(2) . ? Fe3 N5 2.227(2) . ? Fe3 N4 2.266(2) . ? N1 C6 1.395(3) . ? N1 C3 1.452(3) . ? N1L C49 1.327(4) . ? N1L C45 1.328(4) . ? N2 C18 1.392(3) . ? N2 C4 1.452(3) . ? N2L C54 1.325(4) . ? N2L C50 1.345(4) . ? N3 C30 1.395(3) . ? N3 C5 1.457(3) . ? N3L C59 1.339(4) . ? N3L C55 1.339(4) . ? N4 C11 1.416(3) . ? N4 C12 1.421(3) . ? N5 C23 1.412(3) . ? N5 C24 1.415(3) . ? N6 C35 1.402(3) . ? N6 C36 1.421(3) . ? C1 C2 1.537(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.519(4) . ? C2 C5 1.520(4) . ? C2 C3 1.522(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.381(4) . ? C6 C11 1.409(4) . ? C7 C8 1.403(4) . ? C7 H7A 0.9500 . ? C8 C9 1.359(4) . ? C8 H8A 0.9500 . ? C9 C10 1.383(4) . ? C9 H9A 0.9500 . ? C10 C11 1.381(4) . ? C10 H10A 0.9500 . ? C12 C13 1.383(4) . ? C12 C17 1.386(4) . ? C13 C14 1.379(4) . ? C13 H13A 0.9500 . ? C14 C15 1.371(5) . ? C14 H14A 0.9500 . ? C15 C16 1.376(5) . ? C15 H15A 0.9500 . ? C16 C17 1.376(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.388(4) . ? C18 C23 1.403(4) . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.374(4) . ? C20 H20A 0.9500 . ? C21 C22 1.381(4) . ? C21 H21A 0.9500 . ? C22 C23 1.388(4) . ? C22 H22A 0.9500 . ? C24 C25 1.379(4) . ? C24 C29 1.396(4) . ? C25 C26 1.380(4) . ? C25 H25A 0.9500 . ? C26 C27 1.361(4) . ? C26 H26A 0.9500 . ? C27 C28 1.388(4) . ? C27 H27A 0.9500 . ? C28 C29 1.375(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.382(4) . ? C30 C35 1.405(4) . ? C31 C32 1.394(4) . ? C31 H31A 0.9500 . ? C32 C33 1.368(4) . ? C32 H32A 0.9500 . ? C33 C34 1.386(4) . ? C33 H33A 0.9500 . ? C34 C35 1.393(4) . ? C34 H34A 0.9500 . ? C36 C37 1.379(4) . ? C36 C41 1.396(4) . ? C37 C38 1.385(4) . ? C37 H37A 0.9500 . ? C38 C39 1.376(4) . ? C38 H38A 0.9500 . ? C39 C40 1.375(4) . ? C39 H39A 0.9500 . ? C40 C41 1.373(4) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C45 C46 1.369(4) . ? C45 H45A 0.9500 . ? C46 C47 1.361(5) . ? C46 H46A 0.9500 . ? C47 C48 1.358(5) . ? C47 H47A 0.9500 . ? C48 C49 1.370(4) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C51 1.377(4) . ? C50 H50A 0.9500 . ? C51 C52 1.366(5) . ? C51 H51A 0.9500 . ? C52 C53 1.364(5) . ? C52 H52A 0.9500 . ? C53 C54 1.359(5) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.370(4) . ? C55 H55A 0.9500 . ? C56 C57 1.371(4) . ? C56 H56A 0.9500 . ? C57 C58 1.377(4) . ? C57 H57A 0.9500 . ? C58 C59 1.373(4) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 C65 1.353(5) . ? C60 C61 1.362(5) . ? C60 H60A 0.9500 . ? C61 C62 1.381(6) . ? C61 H61A 0.9500 . ? C62 C63 1.356(6) . ? C62 H62A 0.9500 . ? C63 C64 1.354(5) . ? C63 H63A 0.9500 . ? C64 C65 1.355(5) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C70 C75 1.361(7) . ? C70 C71 1.371(6) . ? C70 H70A 0.9500 . ? C71 C72 1.358(6) . ? C71 H71A 0.9500 . ? C72 C73 1.362(6) . ? C72 H72A 0.9500 . ? C73 C74 1.371(6) . ? C73 H73A 0.9500 . ? C74 C75 1.363(7) . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? 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 N1L Fe1 N5 106.94(9) . . ? N1L Fe1 N3 98.59(9) . . ? N5 Fe1 N3 149.82(9) . . ? N1L Fe1 N2 102.68(9) . . ? N5 Fe1 N2 72.29(9) . . ? N3 Fe1 N2 86.82(9) . . ? N1L Fe1 N6 104.36(9) . . ? N5 Fe1 N6 116.49(9) . . ? N3 Fe1 N6 70.79(8) . . ? N2 Fe1 N6 147.00(8) . . ? N1L Fe1 Fe3 151.30(7) . . ? N5 Fe1 Fe3 56.44(6) . . ? N3 Fe1 Fe3 93.58(7) . . ? N2 Fe1 Fe3 51.99(6) . . ? N6 Fe1 Fe3 104.18(6) . . ? N1L Fe1 Fe2 145.34(7) . . ? N5 Fe1 Fe2 106.77(6) . . ? N3 Fe1 Fe2 52.46(6) . . ? N2 Fe1 Fe2 94.96(6) . . ? N6 Fe1 Fe2 52.23(6) . . ? Fe3 Fe1 Fe2 59.99(3) . . ? N2L Fe2 N4 103.93(9) . . ? N2L Fe2 N3 100.40(9) . . ? N4 Fe2 N3 149.41(9) . . ? N2L Fe2 N6 109.85(9) . . ? N4 Fe2 N6 115.28(9) . . ? N3 Fe2 N6 72.34(8) . . ? N2L Fe2 N1 96.73(9) . . ? N4 Fe2 N1 71.92(8) . . ? N3 Fe2 N1 87.14(8) . . ? N6 Fe2 N1 148.67(8) . . ? N2L Fe2 Fe3 144.68(7) . . ? N4 Fe2 Fe3 56.78(6) . . ? N3 Fe2 Fe3 92.75(7) . . ? N6 Fe2 Fe3 105.35(7) . . ? N1 Fe2 Fe3 51.04(6) . . ? N2L Fe2 Fe1 150.44(7) . . ? N4 Fe2 Fe1 105.59(6) . . ? N3 Fe2 Fe1 52.61(6) . . ? N6 Fe2 Fe1 54.90(6) . . ? N1 Fe2 Fe1 93.86(6) . . ? Fe3 Fe2 Fe1 58.739(19) . . ? N1 Fe3 N2 89.41(9) . . ? N1 Fe3 N3L 111.54(9) . . ? N2 Fe3 N3L 113.53(9) . . ? N1 Fe3 N5 150.91(9) . . ? N2 Fe3 N5 71.94(8) . . ? N3L Fe3 N5 96.56(9) . . ? N1 Fe3 N4 71.58(8) . . ? N2 Fe3 N4 150.18(9) . . ? N3L Fe3 N4 95.08(9) . . ? N5 Fe3 N4 114.57(8) . . ? N1 Fe3 Fe1 98.91(7) . . ? N2 Fe3 Fe1 55.63(7) . . ? N3L Fe3 Fe1 148.06(7) . . ? N5 Fe3 Fe1 52.19(6) . . ? N4 Fe3 Fe1 103.72(6) . . ? N1 Fe3 Fe2 55.44(6) . . ? N2 Fe3 Fe2 98.45(7) . . ? N3L Fe3 Fe2 146.01(7) . . ? N5 Fe3 Fe2 104.34(6) . . ? N4 Fe3 Fe2 51.90(6) . . ? Fe1 Fe3 Fe2 61.27(2) . . ? C6 N1 C3 113.4(2) . . ? C6 N1 Fe3 110.81(18) . . ? C3 N1 Fe3 127.16(17) . . ? C6 N1 Fe2 102.69(17) . . ? C3 N1 Fe2 121.41(17) . . ? Fe3 N1 Fe2 73.52(7) . . ? C49 N1L C45 117.0(3) . . ? C49 N1L Fe1 117.93(19) . . ? C45 N1L Fe1 122.66(19) . . ? C18 N2 C4 114.1(2) . . ? C18 N2 Fe3 109.22(17) . . ? C4 N2 Fe3 123.41(17) . . ? C18 N2 Fe1 103.59(16) . . ? C4 N2 Fe1 126.84(17) . . ? Fe3 N2 Fe1 72.37(7) . . ? C54 N2L C50 117.5(3) . . ? C54 N2L Fe2 118.5(2) . . ? C50 N2L Fe2 123.7(2) . . ? C30 N3 C5 113.2(2) . . ? C30 N3 Fe2 111.55(16) . . ? C5 N3 Fe2 126.93(17) . . ? C30 N3 Fe1 100.07(16) . . ? C5 N3 Fe1 122.11(17) . . ? Fe2 N3 Fe1 74.93(8) . . ? C59 N3L C55 117.3(3) . . ? C59 N3L Fe3 119.0(2) . . ? C55 N3L Fe3 123.1(2) . . ? C11 N4 C12 113.1(2) . . ? C11 N4 Fe2 105.30(16) . . ? C12 N4 Fe2 130.14(18) . . ? C11 N4 Fe3 103.81(16) . . ? C12 N4 Fe3 125.12(17) . . ? Fe2 N4 Fe3 71.32(7) . . ? C23 N5 C24 116.4(2) . . ? C23 N5 Fe1 104.66(17) . . ? C24 N5 Fe1 114.24(17) . . ? C23 N5 Fe3 105.07(16) . . ? C24 N5 Fe3 133.57(17) . . ? Fe1 N5 Fe3 71.37(7) . . ? C35 N6 C36 114.3(2) . . ? C35 N6 Fe2 110.19(16) . . ? C36 N6 Fe2 116.25(16) . . ? C35 N6 Fe1 97.37(15) . . ? C36 N6 Fe1 138.54(18) . . ? Fe2 N6 Fe1 72.87(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C5 112.0(2) . . ? C4 C2 C3 112.7(2) . . ? C5 C2 C3 113.5(2) . . ? C4 C2 C1 106.7(2) . . ? C5 C2 C1 105.3(2) . . ? C3 C2 C1 106.0(2) . . ? N1 C3 C2 115.5(2) . . ? N1 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N2 C4 C2 114.9(2) . . ? N2 C4 H4A 108.5 . . ? C2 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C2 117.1(2) . . ? N3 C5 H5A 108.0 . . ? C2 C5 H5A 108.0 . . ? N3 C5 H5B 108.0 . . ? C2 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C7 C6 N1 126.8(3) . . ? C7 C6 C11 119.2(2) . . ? N1 C6 C11 113.9(2) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C6 119.6(3) . . ? C10 C11 N4 126.5(3) . . ? C6 C11 N4 113.8(2) . . ? C13 C12 C17 117.7(3) . . ? C13 C12 N4 121.3(3) . . ? C17 C12 N4 121.0(3) . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 119.1(3) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C12 121.1(3) . . ? C16 C17 H17A 119.5 . . ? C12 C17 H17A 119.5 . . ? C19 C18 N2 127.0(3) . . ? C19 C18 C23 119.2(3) . . ? N2 C18 C23 113.8(2) . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 119.3(3) . . ? C22 C23 N5 126.6(3) . . ? C18 C23 N5 114.1(2) . . ? C25 C24 C29 117.6(3) . . ? C25 C24 N5 120.7(3) . . ? C29 C24 N5 121.7(2) . . ? C24 C25 C26 121.0(3) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 119.0(3) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C24 121.2(3) . . ? C28 C29 H29A 119.4 . . ? C24 C29 H29A 119.4 . . ? C31 C30 N3 127.5(3) . . ? C31 C30 C35 119.4(3) . . ? N3 C30 C35 113.0(2) . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 120.1(3) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C33 C34 C35 120.4(3) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? C34 C35 N6 125.9(2) . . ? C34 C35 C30 119.3(2) . . ? N6 C35 C30 114.4(2) . . ? C37 C36 C41 118.0(3) . . ? C37 C36 N6 122.6(3) . . ? C41 C36 N6 119.3(2) . . ? C36 C37 C38 120.5(3) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C40 C39 C38 119.1(3) . . ? C40 C39 H39A 120.4 . . ? C38 C39 H39A 120.4 . . ? C41 C40 C39 120.4(3) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C40 C41 C36 121.1(3) . . ? C40 C41 H41A 119.4 . . ? C36 C41 H41A 119.4 . . ? N1L C45 C46 122.8(3) . . ? N1L C45 H45A 118.6 . . ? C46 C45 H45A 118.6 . . ? C47 C46 C45 119.3(3) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C48 C47 C46 118.6(3) . . ? C48 C47 H47A 120.7 . . ? C46 C47 H47A 120.7 . . ? C47 C48 C49 118.9(3) . . ? C47 C48 H48A 120.6 . . ? C49 C48 H48A 120.6 . . ? N1L C49 C48 123.4(3) . . ? N1L C49 H49A 118.3 . . ? C48 C49 H49A 118.3 . . ? N2L C50 C51 122.1(3) . . ? N2L C50 H50A 118.9 . . ? C51 C50 H50A 118.9 . . ? C52 C51 C50 119.2(3) . . ? C52 C51 H51A 120.4 . . ? C50 C51 H51A 120.4 . . ? C53 C52 C51 118.3(3) . . ? C53 C52 H52A 120.8 . . ? C51 C52 H52A 120.8 . . ? C54 C53 C52 119.8(4) . . ? C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? N2L C54 C53 123.0(3) . . ? N2L C54 H54A 118.5 . . ? C53 C54 H54A 118.5 . . ? N3L C55 C56 122.8(3) . . ? N3L C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C55 C56 C57 119.5(3) . . ? C55 C56 H56A 120.3 . . ? C57 C56 H56A 120.3 . . ? C56 C57 C58 118.4(3) . . ? C56 C57 H57A 120.8 . . ? C58 C57 H57A 120.8 . . ? C59 C58 C57 119.1(3) . . ? C59 C58 H58A 120.4 . . ? C57 C58 H58A 120.4 . . ? N3L C59 C58 122.9(3) . . ? N3L C59 H59A 118.6 . . ? C58 C59 H59A 118.6 . . ? C65 C60 C61 119.6(4) . . ? C65 C60 H60A 120.2 . . ? C61 C60 H60A 120.2 . . ? C60 C61 C62 119.5(4) . . ? C60 C61 H61A 120.2 . . ? C62 C61 H61A 120.2 . . ? C63 C62 C61 119.8(4) . . ? C63 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? C64 C63 C62 120.2(4) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C63 C64 C65 119.9(4) . . ? C63 C64 H64A 120.1 . . ? C65 C64 H64A 120.1 . . ? C60 C65 C64 121.0(4) . . ? C60 C65 H65A 119.5 . . ? C64 C65 H65A 119.5 . . ? C75 C70 C71 119.5(5) . . ? C75 C70 H70A 120.3 . . ? C71 C70 H70A 120.3 . . ? C72 C71 C70 120.5(5) . . ? C72 C71 H71A 119.7 . . ? C70 C71 H71A 119.7 . . ? C71 C72 C73 120.1(4) . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 119.9 . . ? C72 C73 C74 119.5(5) . . ? C72 C73 H73A 120.3 . . ? C74 C73 H73A 120.3 . . ? C75 C74 C73 120.3(5) . . ? C75 C74 H74A 119.8 . . ? C73 C74 H74A 119.8 . . ? C70 C75 C74 120.1(4) . . ? C70 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.529 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.069 #=============the end of compound 150K=================== #============compound 200K================================ data_200k _database_code_depnum_ccdc_archive 'CCDC 789357' #TrackingRef '2147_web_deposit_cif_file_0_EmilyEames_1281822379.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H51 Fe3 N9, 2(C6 H6)' _chemical_formula_sum 'C68 H63 Fe3 N9' _chemical_formula_weight 1173.82 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' 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 11.8394(18) _cell_length_b 13.037(2) _cell_length_c 19.508(3) _cell_angle_alpha 73.852(3) _cell_angle_beta 86.214(3) _cell_angle_gamma 75.811(3) _cell_volume 2804.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9446 _cell_measurement_theta_min 2.1735 _cell_measurement_theta_max 25.7165 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6949 _exptl_absorpt_correction_T_max 0.9227 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34422 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.93 _reflns_number_total 10693 _reflns_number_gt 8140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 XP _computing_publication_material XCIF _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^)+(0.0472P)^2^+1.0520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10693 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.63201(3) 0.23565(3) 0.228958(18) 0.03057(10) Uani 1 1 d . . . Fe2 Fe 0.69082(3) 0.06387(3) 0.180714(18) 0.02937(10) Uani 1 1 d . . . Fe3 Fe 0.77409(3) 0.06565(3) 0.298349(19) 0.02959(10) Uani 1 1 d . . . N1 N 0.69092(16) -0.05253(15) 0.28695(11) 0.0295(4) Uani 1 1 d . . . N1L N 0.50816(18) 0.38495(16) 0.22319(11) 0.0343(5) Uani 1 1 d . . . N2 N 0.62065(16) 0.14262(15) 0.34092(10) 0.0286(4) Uani 1 1 d . . . N2L N 0.65124(19) -0.03781(17) 0.12182(11) 0.0365(5) Uani 1 1 d . . . N3 N 0.51932(16) 0.14493(15) 0.20455(10) 0.0280(4) Uani 1 1 d . . . N3L N 0.91204(17) -0.00374(17) 0.37428(11) 0.0347(5) Uani 1 1 d . . . N4 N 0.86771(16) -0.00972(15) 0.21302(11) 0.0302(4) Uani 1 1 d . . . N5 N 0.77764(16) 0.24077(15) 0.28287(10) 0.0283(4) Uani 1 1 d . . . N6 N 0.65865(16) 0.23003(15) 0.11580(10) 0.0285(4) Uani 1 1 d . . . C1 C 0.3904(2) -0.0210(2) 0.36869(14) 0.0405(6) Uani 1 1 d . . . H1A H 0.4183 -0.0699 0.4154 0.061 Uiso 1 1 calc R . . H1B H 0.3612 -0.0621 0.3415 0.061 Uiso 1 1 calc R . . H1C H 0.3274 0.0401 0.3752 0.061 Uiso 1 1 calc R . . C2 C 0.4908(2) 0.02413(19) 0.32789(13) 0.0303(5) Uani 1 1 d . . . C3 C 0.5844(2) -0.07507(19) 0.32060(13) 0.0329(6) Uani 1 1 d . . . H3A H 0.6035 -0.1255 0.3688 0.039 Uiso 1 1 calc R . . H3B H 0.5518 -0.1142 0.2929 0.039 Uiso 1 1 calc R . . C4 C 0.5302(2) 0.0876(2) 0.37251(12) 0.0312(5) Uani 1 1 d . . . H4A H 0.4619 0.1432 0.3819 0.037 Uiso 1 1 calc R . . H4B H 0.5585 0.0361 0.4191 0.037 Uiso 1 1 calc R . . C5 C 0.4398(2) 0.0988(2) 0.25673(13) 0.0317(5) Uani 1 1 d . . . H5A H 0.4005 0.0567 0.2349 0.038 Uiso 1 1 calc R . . H5B H 0.3790 0.1604 0.2663 0.038 Uiso 1 1 calc R . . C6 C 0.7728(2) -0.14556(19) 0.27945(13) 0.0306(5) Uani 1 1 d . . . C7 C 0.7639(2) -0.2532(2) 0.30519(14) 0.0378(6) Uani 1 1 d . . . H7A H 0.6963 -0.2693 0.3306 0.045 Uiso 1 1 calc R . . C8 C 0.8543(3) -0.3383(2) 0.29390(16) 0.0482(7) Uani 1 1 d . . . H8A H 0.8478 -0.4123 0.3116 0.058 Uiso 1 1 calc R . . C9 C 0.9512(3) -0.3164(2) 0.25801(16) 0.0479(7) Uani 1 1 d . . . H9A H 1.0126 -0.3750 0.2511 0.057 Uiso 1 1 calc R . . C10 C 0.9612(2) -0.2090(2) 0.23139(14) 0.0368(6) Uani 1 1 d . . . H10A H 1.0294 -0.1943 0.2062 0.044 Uiso 1 1 calc R . . C11 C 0.8725(2) -0.12290(19) 0.24111(12) 0.0297(5) Uani 1 1 d . . . C12 C 0.9725(2) 0.01157(18) 0.17915(13) 0.0308(5) Uani 1 1 d . . . C13 C 0.9798(2) 0.0475(2) 0.10600(14) 0.0388(6) Uani 1 1 d . . . H13A H 0.9136 0.0580 0.0776 0.047 Uiso 1 1 calc R . . C14 C 1.0816(2) 0.0686(2) 0.07336(17) 0.0512(8) Uani 1 1 d . . . H14A H 1.0848 0.0933 0.0228 0.061 Uiso 1 1 calc R . . C15 C 1.1780(2) 0.0543(2) 0.11301(18) 0.0523(8) Uani 1 1 d . . . H15A H 1.2475 0.0708 0.0906 0.063 Uiso 1 1 calc R . . C16 C 1.1724(2) 0.0158(2) 0.18588(18) 0.0482(7) Uani 1 1 d . . . H16A H 1.2393 0.0040 0.2140 0.058 Uiso 1 1 calc R . . C17 C 1.0717(2) -0.0057(2) 0.21851(15) 0.0386(6) Uani 1 1 d . . . H17A H 1.0698 -0.0330 0.2690 0.046 Uiso 1 1 calc R . . C18 C 0.6469(2) 0.20967(19) 0.37888(12) 0.0303(5) Uani 1 1 d . . . C19 C 0.5956(2) 0.2279(2) 0.44154(13) 0.0354(6) Uani 1 1 d . . . H19A H 0.5370 0.1912 0.4633 0.043 Uiso 1 1 calc R . . C20 C 0.6288(2) 0.2989(2) 0.47297(14) 0.0413(6) Uani 1 1 d . . . H20A H 0.5918 0.3119 0.5155 0.050 Uiso 1 1 calc R . . C21 C 0.7148(2) 0.3501(2) 0.44279(14) 0.0417(6) Uani 1 1 d . . . H21A H 0.7382 0.3980 0.4649 0.050 Uiso 1 1 calc R . . C22 C 0.7680(2) 0.3328(2) 0.38024(13) 0.0352(6) Uani 1 1 d . . . H22A H 0.8285 0.3680 0.3600 0.042 Uiso 1 1 calc R . . C23 C 0.7333(2) 0.26427(18) 0.34720(12) 0.0287(5) Uani 1 1 d . . . C24 C 0.8480(2) 0.30904(19) 0.24171(13) 0.0314(5) Uani 1 1 d . . . C25 C 0.9576(2) 0.2636(2) 0.22006(14) 0.0391(6) Uani 1 1 d . . . H25A H 0.9872 0.1862 0.2344 0.047 Uiso 1 1 calc R . . C26 C 1.0246(3) 0.3293(3) 0.17792(16) 0.0526(8) Uani 1 1 d . . . H26A H 1.0997 0.2966 0.1632 0.063 Uiso 1 1 calc R . . C27 C 0.9848(3) 0.4403(3) 0.15709(17) 0.0564(8) Uani 1 1 d . . . H27A H 1.0321 0.4850 0.1284 0.068 Uiso 1 1 calc R . . C28 C 0.8754(3) 0.4876(2) 0.17781(16) 0.0502(7) Uani 1 1 d . . . H28A H 0.8469 0.5651 0.1633 0.060 Uiso 1 1 calc R . . C29 C 0.8077(2) 0.4226(2) 0.21935(14) 0.0383(6) Uani 1 1 d . . . H29A H 0.7321 0.4558 0.2331 0.046 Uiso 1 1 calc R . . C30 C 0.4643(2) 0.22071(18) 0.14379(12) 0.0277(5) Uani 1 1 d . . . C31 C 0.3461(2) 0.2547(2) 0.12968(13) 0.0341(6) Uani 1 1 d . . . H31A H 0.2935 0.2206 0.1615 0.041 Uiso 1 1 calc R . . C32 C 0.3039(2) 0.3385(2) 0.06911(14) 0.0385(6) Uani 1 1 d . . . H32A H 0.2225 0.3617 0.0600 0.046 Uiso 1 1 calc R . . C33 C 0.3784(2) 0.3879(2) 0.02266(13) 0.0360(6) Uani 1 1 d . . . H33A H 0.3487 0.4463 -0.0180 0.043 Uiso 1 1 calc R . . C34 C 0.4978(2) 0.35267(19) 0.03487(13) 0.0307(5) Uani 1 1 d . . . H34A H 0.5498 0.3865 0.0023 0.037 Uiso 1 1 calc R . . C35 C 0.54113(19) 0.26771(18) 0.09485(12) 0.0266(5) Uani 1 1 d . . . C36 C 0.7389(2) 0.25429(19) 0.05985(12) 0.0297(5) Uani 1 1 d . . . C37 C 0.8128(2) 0.3207(2) 0.05996(13) 0.0356(6) Uani 1 1 d . . . H37A H 0.8092 0.3544 0.0977 0.043 Uiso 1 1 calc R . . C38 C 0.8925(2) 0.3387(2) 0.00535(15) 0.0454(7) Uani 1 1 d . . . H38A H 0.9432 0.3848 0.0060 0.054 Uiso 1 1 calc R . . C39 C 0.8994(2) 0.2911(2) -0.04959(15) 0.0460(7) Uani 1 1 d . . . H39A H 0.9548 0.3035 -0.0866 0.055 Uiso 1 1 calc R . . C40 C 0.8256(2) 0.2255(2) -0.05059(14) 0.0420(7) Uani 1 1 d . . . H40A H 0.8296 0.1922 -0.0885 0.050 Uiso 1 1 calc R . . C41 C 0.7458(2) 0.2077(2) 0.00317(13) 0.0347(6) Uani 1 1 d . . . H41A H 0.6943 0.1627 0.0016 0.042 Uiso 1 1 calc R . . C45 C 0.4947(3) 0.4702(2) 0.16585(14) 0.0453(7) Uani 1 1 d . . . H45A H 0.5564 0.4740 0.1322 0.054 Uiso 1 1 calc R . . C46 C 0.3960(3) 0.5525(2) 0.15316(16) 0.0612(9) Uani 1 1 d . . . H46A H 0.3895 0.6123 0.1114 0.073 Uiso 1 1 calc R . . C47 C 0.3070(3) 0.5484(3) 0.20049(17) 0.0576(8) Uani 1 1 d . . . H47A H 0.2371 0.6046 0.1921 0.069 Uiso 1 1 calc R . . C48 C 0.3194(2) 0.4628(2) 0.25992(17) 0.0494(7) Uani 1 1 d . . . H48A H 0.2586 0.4578 0.2941 0.059 Uiso 1 1 calc R . . C49 C 0.4212(2) 0.3838(2) 0.26964(15) 0.0428(7) Uani 1 1 d . . . H49A H 0.4302 0.3248 0.3119 0.051 Uiso 1 1 calc R . . C50 C 0.7308(3) -0.1128(2) 0.09930(15) 0.0460(7) Uani 1 1 d . . . H50A H 0.8108 -0.1182 0.1067 0.055 Uiso 1 1 calc R . . C51 C 0.7022(3) -0.1825(3) 0.06578(17) 0.0557(8) Uani 1 1 d . . . H51A H 0.7613 -0.2343 0.0496 0.067 Uiso 1 1 calc R . . C52 C 0.5881(3) -0.1766(3) 0.0560(2) 0.0713(10) Uani 1 1 d . . . H52A H 0.5661 -0.2245 0.0333 0.086 Uiso 1 1 calc R . . C53 C 0.5057(3) -0.1006(3) 0.0794(2) 0.0756(11) Uani 1 1 d . . . H53A H 0.4252 -0.0946 0.0732 0.091 Uiso 1 1 calc R . . C54 C 0.5406(3) -0.0335(3) 0.11191(17) 0.0531(8) Uani 1 1 d . . . H54A H 0.4825 0.0189 0.1282 0.064 Uiso 1 1 calc R . . C55 C 0.9833(2) 0.0533(2) 0.38711(14) 0.0373(6) Uani 1 1 d . . . H55A H 0.9645 0.1309 0.3676 0.045 Uiso 1 1 calc R . . C56 C 1.0822(2) 0.0052(2) 0.42709(14) 0.0437(7) Uani 1 1 d . . . H56A H 1.1309 0.0488 0.4351 0.052 Uiso 1 1 calc R . . C57 C 1.1106(2) -0.1060(3) 0.45544(16) 0.0503(7) Uani 1 1 d . . . H57A H 1.1800 -0.1414 0.4825 0.060 Uiso 1 1 calc R . . C58 C 1.0369(3) -0.1653(2) 0.44393(16) 0.0522(8) Uani 1 1 d . . . H58A H 1.0533 -0.2427 0.4639 0.063 Uiso 1 1 calc R . . C59 C 0.9391(2) -0.1122(2) 0.40336(14) 0.0425(6) Uani 1 1 d . . . H59A H 0.8884 -0.1542 0.3956 0.051 Uiso 1 1 calc R . . C60 C 0.2286(3) 0.2431(3) 0.4420(2) 0.0747(11) Uani 1 1 d . . . H60A H 0.2811 0.1728 0.4509 0.090 Uiso 1 1 calc R . . C61 C 0.2258(4) 0.3064(4) 0.4865(2) 0.0868(12) Uani 1 1 d . . . H61A H 0.2763 0.2813 0.5267 0.104 Uiso 1 1 calc R . . C62 C 0.1479(4) 0.4091(4) 0.4730(3) 0.0943(14) Uani 1 1 d . . . H62A H 0.1446 0.4552 0.5035 0.113 Uiso 1 1 calc R . . C63 C 0.0766(4) 0.4418(4) 0.4151(3) 0.0849(12) Uani 1 1 d . . . H63A H 0.0227 0.5113 0.4054 0.102 Uiso 1 1 calc R . . C64 C 0.0813(3) 0.3780(4) 0.3719(2) 0.0764(11) Uani 1 1 d . . . H64A H 0.0310 0.4020 0.3317 0.092 Uiso 1 1 calc R . . C65 C 0.1576(4) 0.2790(3) 0.3853(2) 0.0755(11) Uani 1 1 d . . . H65A H 0.1610 0.2341 0.3539 0.091 Uiso 1 1 calc R . . C70 C 0.4864(4) 0.6780(4) 0.2734(3) 0.0999(16) Uani 1 1 d . . . H70A H 0.5485 0.6916 0.2414 0.120 Uiso 1 1 calc R . . C71 C 0.3793(4) 0.7475(3) 0.2618(3) 0.0880(13) Uani 1 1 d . . . H71A H 0.3666 0.8097 0.2213 0.106 Uiso 1 1 calc R . . C72 C 0.2909(4) 0.7291(3) 0.3068(2) 0.0797(12) Uani 1 1 d . . . H72A H 0.2164 0.7785 0.2981 0.096 Uiso 1 1 calc R . . C73 C 0.3077(4) 0.6404(4) 0.3647(2) 0.0919(13) Uani 1 1 d . . . H73A H 0.2454 0.6270 0.3965 0.110 Uiso 1 1 calc R . . C74 C 0.4163(6) 0.5702(4) 0.3765(3) 0.1094(19) Uani 1 1 d . . . H74A H 0.4299 0.5080 0.4170 0.131 Uiso 1 1 calc R . . C75 C 0.5041(5) 0.5901(4) 0.3302(4) 0.110(2) Uani 1 1 d . . . H75A H 0.5790 0.5412 0.3382 0.132 Uiso 1 1 calc R . . 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 0.0319(2) 0.03127(19) 0.0304(2) -0.00966(15) -0.00347(15) -0.00832(15) Fe2 0.02693(19) 0.03031(19) 0.0307(2) -0.00864(15) -0.00209(14) -0.00537(14) Fe3 0.02574(18) 0.02954(18) 0.0350(2) -0.01076(15) -0.00182(15) -0.00650(14) N1 0.0284(11) 0.0253(10) 0.0357(11) -0.0082(8) 0.0011(9) -0.0080(8) N1L 0.0370(12) 0.0325(11) 0.0344(12) -0.0119(9) 0.0026(9) -0.0074(9) N2 0.0294(11) 0.0315(11) 0.0279(11) -0.0089(8) -0.0003(8) -0.0115(9) N2L 0.0392(12) 0.0399(12) 0.0345(12) -0.0142(10) 0.0016(10) -0.0127(10) N3 0.0235(10) 0.0310(10) 0.0298(11) -0.0076(8) -0.0005(8) -0.0077(8) N3L 0.0329(12) 0.0394(12) 0.0297(11) -0.0062(9) -0.0038(9) -0.0073(10) N4 0.0243(10) 0.0285(10) 0.0379(12) -0.0101(9) 0.0007(9) -0.0053(8) N5 0.0267(10) 0.0304(10) 0.0307(11) -0.0113(8) -0.0008(8) -0.0081(8) N6 0.0262(10) 0.0318(10) 0.0276(11) -0.0063(8) -0.0006(8) -0.0087(8) C1 0.0382(15) 0.0457(15) 0.0378(15) -0.0067(12) 0.0031(12) -0.0162(12) C2 0.0271(12) 0.0343(13) 0.0297(13) -0.0058(10) 0.0024(10) -0.0117(10) C3 0.0313(13) 0.0322(13) 0.0359(14) -0.0062(11) -0.0009(11) -0.0120(11) C4 0.0307(13) 0.0362(13) 0.0264(13) -0.0064(10) 0.0018(10) -0.0097(11) C5 0.0274(13) 0.0369(13) 0.0321(13) -0.0085(11) -0.0002(10) -0.0111(11) C6 0.0323(13) 0.0273(12) 0.0330(13) -0.0083(10) -0.0064(11) -0.0069(10) C7 0.0383(15) 0.0311(13) 0.0446(16) -0.0080(11) -0.0003(12) -0.0117(11) C8 0.0542(18) 0.0263(13) 0.064(2) -0.0088(13) -0.0002(15) -0.0119(13) C9 0.0456(17) 0.0327(15) 0.0634(19) -0.0180(13) 0.0009(15) -0.0001(12) C10 0.0314(14) 0.0353(14) 0.0454(16) -0.0152(12) 0.0009(12) -0.0063(11) C11 0.0322(13) 0.0280(12) 0.0292(13) -0.0066(10) -0.0081(10) -0.0069(10) C12 0.0255(12) 0.0247(12) 0.0425(15) -0.0104(10) -0.0024(11) -0.0041(10) C13 0.0292(14) 0.0414(15) 0.0412(16) -0.0082(12) -0.0010(11) -0.0029(11) C14 0.0406(17) 0.0504(17) 0.0493(18) -0.0011(14) 0.0074(14) -0.0022(13) C15 0.0302(15) 0.0445(16) 0.078(2) -0.0133(16) 0.0144(15) -0.0091(13) C16 0.0293(15) 0.0505(17) 0.071(2) -0.0238(15) -0.0020(14) -0.0109(13) C17 0.0298(14) 0.0434(15) 0.0444(16) -0.0160(12) -0.0027(12) -0.0065(11) C18 0.0276(13) 0.0309(12) 0.0302(13) -0.0083(10) -0.0051(10) -0.0016(10) C19 0.0344(14) 0.0394(14) 0.0306(14) -0.0085(11) -0.0017(11) -0.0060(11) C20 0.0469(16) 0.0458(16) 0.0298(14) -0.0149(12) -0.0047(12) -0.0019(13) C21 0.0525(17) 0.0384(14) 0.0365(15) -0.0169(12) -0.0107(13) -0.0042(13) C22 0.0369(14) 0.0334(13) 0.0371(14) -0.0109(11) -0.0074(11) -0.0083(11) C23 0.0266(12) 0.0289(12) 0.0276(13) -0.0075(10) -0.0049(10) 0.0002(10) C24 0.0306(13) 0.0339(13) 0.0337(14) -0.0125(11) -0.0029(10) -0.0104(11) C25 0.0347(14) 0.0384(14) 0.0431(16) -0.0105(12) 0.0018(12) -0.0075(12) C26 0.0398(16) 0.0584(19) 0.0584(19) -0.0124(15) 0.0097(14) -0.0157(14) C27 0.062(2) 0.060(2) 0.055(2) -0.0126(16) 0.0128(16) -0.0364(17) C28 0.069(2) 0.0352(15) 0.0510(18) -0.0121(13) 0.0038(15) -0.0217(15) C29 0.0422(15) 0.0337(14) 0.0413(15) -0.0133(12) 0.0004(12) -0.0099(12) C30 0.0277(12) 0.0285(12) 0.0278(12) -0.0096(10) -0.0029(10) -0.0055(10) C31 0.0279(13) 0.0374(14) 0.0359(14) -0.0082(11) 0.0010(11) -0.0077(11) C32 0.0263(13) 0.0429(15) 0.0422(15) -0.0107(12) -0.0062(11) 0.0002(11) C33 0.0366(14) 0.0346(13) 0.0326(14) -0.0069(11) -0.0064(11) -0.0015(11) C34 0.0338(13) 0.0292(12) 0.0296(13) -0.0091(10) 0.0013(10) -0.0076(10) C35 0.0245(12) 0.0315(12) 0.0279(12) -0.0143(10) -0.0006(10) -0.0068(10) C36 0.0267(12) 0.0304(12) 0.0285(13) -0.0038(10) -0.0018(10) -0.0048(10) C37 0.0363(14) 0.0361(14) 0.0341(14) -0.0071(11) 0.0024(11) -0.0114(11) C38 0.0410(16) 0.0494(16) 0.0455(17) -0.0045(13) 0.0060(13) -0.0213(13) C39 0.0375(15) 0.0548(17) 0.0366(16) -0.0026(13) 0.0068(12) -0.0073(13) C40 0.0431(16) 0.0461(16) 0.0305(14) -0.0096(12) 0.0013(12) -0.0002(13) C41 0.0342(14) 0.0367(14) 0.0314(14) -0.0071(11) -0.0014(11) -0.0069(11) C45 0.0588(19) 0.0391(15) 0.0349(15) -0.0129(12) 0.0079(13) -0.0045(13) C46 0.083(2) 0.0463(18) 0.0369(17) -0.0066(14) -0.0038(16) 0.0120(16) C47 0.0539(19) 0.0583(19) 0.0513(19) -0.0208(16) -0.0118(15) 0.0139(15) C48 0.0372(16) 0.0533(18) 0.0594(19) -0.0226(15) 0.0079(14) -0.0075(13) C49 0.0452(16) 0.0383(15) 0.0434(16) -0.0116(12) 0.0056(13) -0.0081(12) C50 0.0437(16) 0.0540(17) 0.0446(17) -0.0228(14) -0.0011(13) -0.0084(14) C51 0.063(2) 0.0518(18) 0.058(2) -0.0319(15) -0.0018(16) -0.0051(15) C52 0.078(3) 0.071(2) 0.090(3) -0.054(2) 0.000(2) -0.028(2) C53 0.051(2) 0.099(3) 0.107(3) -0.067(3) -0.001(2) -0.029(2) C54 0.0438(17) 0.0612(19) 0.067(2) -0.0373(17) -0.0015(15) -0.0124(15) C55 0.0337(14) 0.0398(14) 0.0370(15) -0.0071(12) -0.0017(11) -0.0094(12) C56 0.0340(15) 0.0565(18) 0.0408(16) -0.0118(13) -0.0026(12) -0.0123(13) C57 0.0370(16) 0.0595(19) 0.0458(17) -0.0090(14) -0.0096(13) 0.0009(14) C58 0.0564(19) 0.0413(16) 0.0489(18) -0.0028(13) -0.0127(15) -0.0002(14) C59 0.0472(17) 0.0392(15) 0.0394(15) -0.0066(12) -0.0062(13) -0.0102(13) C60 0.065(2) 0.065(2) 0.081(3) -0.012(2) 0.018(2) -0.0038(19) C61 0.073(3) 0.107(4) 0.072(3) -0.009(3) -0.006(2) -0.021(3) C62 0.113(4) 0.094(3) 0.086(3) -0.045(3) 0.015(3) -0.025(3) C63 0.075(3) 0.078(3) 0.089(3) -0.020(2) 0.014(2) 0.001(2) C64 0.052(2) 0.094(3) 0.080(3) -0.010(2) 0.0068(19) -0.027(2) C65 0.084(3) 0.072(3) 0.078(3) -0.024(2) 0.018(2) -0.034(2) C70 0.070(3) 0.099(4) 0.156(5) -0.074(4) -0.018(3) -0.017(3) C71 0.094(3) 0.062(2) 0.111(4) -0.029(2) -0.022(3) -0.013(2) C72 0.082(3) 0.064(2) 0.095(3) -0.045(2) -0.023(2) 0.013(2) C73 0.120(4) 0.091(3) 0.071(3) -0.051(3) -0.008(3) -0.003(3) C74 0.168(6) 0.073(3) 0.079(3) -0.040(3) -0.053(3) 0.024(3) C75 0.102(4) 0.094(4) 0.143(5) -0.078(4) -0.071(4) 0.030(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 N5 2.1020(19) . ? Fe1 N1L 2.110(2) . ? Fe1 N3 2.1392(19) . ? Fe1 N2 2.1972(19) . ? Fe1 N6 2.2281(19) . ? Fe1 Fe3 2.5254(5) . ? Fe1 Fe2 2.5898(6) . ? Fe2 N2L 2.126(2) . ? Fe2 N3 2.1337(18) . ? Fe2 N4 2.1346(19) . ? Fe2 N6 2.1388(19) . ? Fe2 N1 2.202(2) . ? Fe2 Fe3 2.5648(6) . ? Fe3 N1 2.0871(19) . ? Fe3 N2 2.0899(19) . ? Fe3 N3L 2.128(2) . ? Fe3 N5 2.2287(19) . ? Fe3 N4 2.2578(19) . ? N1 C6 1.392(3) . ? N1 C3 1.439(3) . ? N1L C45 1.326(3) . ? N1L C49 1.326(3) . ? N2 C18 1.390(3) . ? N2 C4 1.444(3) . ? N2L C54 1.323(3) . ? N2L C50 1.330(3) . ? N3 C30 1.393(3) . ? N3 C5 1.448(3) . ? N3L C55 1.329(3) . ? N3L C59 1.334(3) . ? N4 C11 1.412(3) . ? N4 C12 1.419(3) . ? N5 C23 1.411(3) . ? N5 C24 1.417(3) . ? N6 C35 1.404(3) . ? N6 C36 1.419(3) . ? C1 C2 1.533(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.517(3) . ? C2 C4 1.518(3) . ? C2 C5 1.520(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.381(3) . ? C6 C11 1.403(3) . ? C7 C8 1.396(4) . ? C7 H7A 0.9500 . ? C8 C9 1.353(4) . ? C8 H8A 0.9500 . ? C9 C10 1.383(4) . ? C9 H9A 0.9500 . ? C10 C11 1.383(3) . ? C10 H10A 0.9500 . ? C12 C13 1.377(4) . ? C12 C17 1.382(3) . ? C13 C14 1.377(4) . ? C13 H13A 0.9500 . ? C14 C15 1.367(4) . ? C14 H14A 0.9500 . ? C15 C16 1.372(4) . ? C15 H15A 0.9500 . ? C16 C17 1.368(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.383(3) . ? C18 C23 1.401(3) . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.366(4) . ? C20 H20A 0.9500 . ? C21 C22 1.385(4) . ? C21 H21A 0.9500 . ? C22 C23 1.385(3) . ? C22 H22A 0.9500 . ? C24 C25 1.380(3) . ? C24 C29 1.390(3) . ? C25 C26 1.376(4) . ? C25 H25A 0.9500 . ? C26 C27 1.358(4) . ? C26 H26A 0.9500 . ? C27 C28 1.378(4) . ? C27 H27A 0.9500 . ? C28 C29 1.371(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.381(3) . ? C30 C35 1.396(3) . ? C31 C32 1.390(3) . ? C31 H31A 0.9500 . ? C32 C33 1.364(4) . ? C32 H32A 0.9500 . ? C33 C34 1.390(3) . ? C33 H33A 0.9500 . ? C34 C35 1.392(3) . ? C34 H34A 0.9500 . ? C36 C37 1.374(3) . ? C36 C41 1.391(3) . ? C37 C38 1.385(3) . ? C37 H37A 0.9500 . ? C38 C39 1.369(4) . ? C38 H38A 0.9500 . ? C39 C40 1.369(4) . ? C39 H39A 0.9500 . ? C40 C41 1.374(3) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C45 C46 1.362(4) . ? C45 H45A 0.9500 . ? C46 C47 1.355(4) . ? C46 H46A 0.9500 . ? C47 C48 1.354(4) . ? C47 H47A 0.9500 . ? C48 C49 1.365(4) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C51 1.372(4) . ? C50 H50A 0.9500 . ? C51 C52 1.356(5) . ? C51 H51A 0.9500 . ? C52 C53 1.365(5) . ? C52 H52A 0.9500 . ? C53 C54 1.363(4) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.365(4) . ? C55 H55A 0.9500 . ? C56 C57 1.364(4) . ? C56 H56A 0.9500 . ? C57 C58 1.364(4) . ? C57 H57A 0.9500 . ? C58 C59 1.367(4) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 C65 1.339(5) . ? C60 C61 1.348(6) . ? C60 H60A 0.9500 . ? C61 C62 1.394(6) . ? C61 H61A 0.9500 . ? C62 C63 1.360(6) . ? C62 H62A 0.9500 . ? C63 C64 1.329(6) . ? C63 H63A 0.9500 . ? C64 C65 1.349(5) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C70 C75 1.338(7) . ? C70 C71 1.357(6) . ? C70 H70A 0.9500 . ? C71 C72 1.345(6) . ? C71 H71A 0.9500 . ? C72 C73 1.358(6) . ? C72 H72A 0.9500 . ? C73 C74 1.374(6) . ? C73 H73A 0.9500 . ? C74 C75 1.357(7) . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? 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 N1L 106.58(8) . . ? N5 Fe1 N3 150.24(7) . . ? N1L Fe1 N3 98.51(8) . . ? N5 Fe1 N2 72.43(7) . . ? N1L Fe1 N2 102.80(8) . . ? N3 Fe1 N2 86.79(7) . . ? N5 Fe1 N6 116.65(7) . . ? N1L Fe1 N6 104.30(8) . . ? N3 Fe1 N6 70.77(7) . . ? N2 Fe1 N6 146.91(7) . . ? N5 Fe1 Fe3 56.70(5) . . ? N1L Fe1 Fe3 151.32(6) . . ? N3 Fe1 Fe3 93.76(5) . . ? N2 Fe1 Fe3 51.96(5) . . ? N6 Fe1 Fe3 104.20(5) . . ? N5 Fe1 Fe2 107.15(5) . . ? N1L Fe1 Fe2 145.26(6) . . ? N3 Fe1 Fe2 52.59(5) . . ? N2 Fe1 Fe2 95.05(5) . . ? N6 Fe1 Fe2 52.05(5) . . ? Fe3 Fe1 Fe2 60.170(16) . . ? N2L Fe2 N3 100.35(8) . . ? N2L Fe2 N4 104.13(8) . . ? N3 Fe2 N4 149.20(8) . . ? N2L Fe2 N6 109.53(8) . . ? N3 Fe2 N6 72.62(7) . . ? N4 Fe2 N6 115.22(7) . . ? N2L Fe2 N1 96.62(8) . . ? N3 Fe2 N1 86.97(7) . . ? N4 Fe2 N1 72.00(7) . . ? N6 Fe2 N1 149.05(7) . . ? N2L Fe2 Fe3 144.73(6) . . ? N3 Fe2 Fe3 92.79(5) . . ? N4 Fe2 Fe3 56.54(5) . . ? N6 Fe2 Fe3 105.61(5) . . ? N1 Fe2 Fe3 51.24(5) . . ? N2L Fe2 Fe1 150.53(6) . . ? N3 Fe2 Fe1 52.79(5) . . ? N4 Fe2 Fe1 105.29(5) . . ? N6 Fe2 Fe1 55.23(5) . . ? N1 Fe2 Fe1 93.93(5) . . ? Fe3 Fe2 Fe1 58.670(14) . . ? N1 Fe3 N2 89.26(7) . . ? N1 Fe3 N3L 111.69(8) . . ? N2 Fe3 N3L 112.80(8) . . ? N1 Fe3 N5 150.58(7) . . ? N2 Fe3 N5 72.00(7) . . ? N3L Fe3 N5 96.67(8) . . ? N1 Fe3 N4 71.73(7) . . ? N2 Fe3 N4 150.41(7) . . ? N3L Fe3 N4 95.53(8) . . ? N5 Fe3 N4 114.48(7) . . ? N1 Fe3 Fe1 98.75(6) . . ? N2 Fe3 Fe1 55.90(5) . . ? N3L Fe3 Fe1 147.91(6) . . ? N5 Fe3 Fe1 52.02(5) . . ? N4 Fe3 Fe1 103.71(5) . . ? N1 Fe3 Fe2 55.36(6) . . ? N2 Fe3 Fe2 98.53(6) . . ? N3L Fe3 Fe2 146.56(6) . . ? N5 Fe3 Fe2 104.13(5) . . ? N4 Fe3 Fe2 52.07(5) . . ? Fe1 Fe3 Fe2 61.160(15) . . ? C6 N1 C3 113.95(19) . . ? C6 N1 Fe3 110.25(15) . . ? C3 N1 Fe3 127.00(15) . . ? C6 N1 Fe2 102.68(14) . . ? C3 N1 Fe2 121.48(15) . . ? Fe3 N1 Fe2 73.40(6) . . ? C45 N1L C49 116.9(2) . . ? C45 N1L Fe1 122.83(17) . . ? C49 N1L Fe1 117.76(17) . . ? C18 N2 C4 114.28(18) . . ? C18 N2 Fe3 109.11(14) . . ? C4 N2 Fe3 123.54(15) . . ? C18 N2 Fe1 103.51(14) . . ? C4 N2 Fe1 126.76(15) . . ? Fe3 N2 Fe1 72.14(6) . . ? C54 N2L C50 117.3(2) . . ? C54 N2L Fe2 118.46(18) . . ? C50 N2L Fe2 124.00(19) . . ? C30 N3 C5 113.72(18) . . ? C30 N3 Fe2 111.18(14) . . ? C5 N3 Fe2 127.06(15) . . ? C30 N3 Fe1 99.96(14) . . ? C5 N3 Fe1 121.94(15) . . ? Fe2 N3 Fe1 74.62(6) . . ? C55 N3L C59 117.5(2) . . ? C55 N3L Fe3 122.95(17) . . ? C59 N3L Fe3 118.90(18) . . ? C11 N4 C12 113.25(18) . . ? C11 N4 Fe2 105.03(14) . . ? C12 N4 Fe2 130.15(15) . . ? C11 N4 Fe3 103.65(14) . . ? C12 N4 Fe3 125.21(15) . . ? Fe2 N4 Fe3 71.39(6) . . ? C23 N5 C24 116.26(19) . . ? C23 N5 Fe1 105.15(14) . . ? C24 N5 Fe1 114.86(15) . . ? C23 N5 Fe3 104.60(14) . . ? C24 N5 Fe3 133.68(15) . . ? Fe1 N5 Fe3 71.28(6) . . ? C35 N6 C36 114.45(18) . . ? C35 N6 Fe2 110.14(14) . . ? C36 N6 Fe2 116.61(14) . . ? C35 N6 Fe1 97.19(13) . . ? C36 N6 Fe1 138.30(15) . . ? Fe2 N6 Fe1 72.72(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C4 112.6(2) . . ? C3 C2 C5 113.2(2) . . ? C4 C2 C5 111.8(2) . . ? C3 C2 C1 106.2(2) . . ? C4 C2 C1 106.49(19) . . ? C5 C2 C1 105.85(19) . . ? N1 C3 C2 115.98(19) . . ? N1 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? N1 C3 H3B 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C2 115.13(19) . . ? N2 C4 H4A 108.5 . . ? C2 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C2 117.38(19) . . ? N3 C5 H5A 108.0 . . ? C2 C5 H5A 108.0 . . ? N3 C5 H5B 108.0 . . ? C2 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C7 C6 N1 126.6(2) . . ? C7 C6 C11 119.4(2) . . ? N1 C6 C11 114.1(2) . . ? C6 C7 C8 119.9(2) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C11 120.5(2) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C6 119.3(2) . . ? C10 C11 N4 126.5(2) . . ? C6 C11 N4 114.1(2) . . ? C13 C12 C17 117.8(2) . . ? C13 C12 N4 121.2(2) . . ? C17 C12 N4 121.0(2) . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 118.8(3) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C12 121.0(3) . . ? C16 C17 H17A 119.5 . . ? C12 C17 H17A 119.5 . . ? C19 C18 N2 126.9(2) . . ? C19 C18 C23 119.2(2) . . ? N2 C18 C23 113.9(2) . . ? C18 C19 C20 120.8(2) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C21 C20 C19 119.9(2) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 120.5(2) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C18 119.5(2) . . ? C22 C23 N5 126.4(2) . . ? C18 C23 N5 114.1(2) . . ? C25 C24 C29 117.9(2) . . ? C25 C24 N5 120.5(2) . . ? C29 C24 N5 121.6(2) . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 119.5(3) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C24 121.1(3) . . ? C28 C29 H29A 119.5 . . ? C24 C29 H29A 119.5 . . ? C31 C30 N3 127.3(2) . . ? C31 C30 C35 119.3(2) . . ? N3 C30 C35 113.4(2) . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 119.9(2) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 119.9(2) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C30 119.9(2) . . ? C34 C35 N6 125.4(2) . . ? C30 C35 N6 114.4(2) . . ? C37 C36 C41 118.1(2) . . ? C37 C36 N6 122.5(2) . . ? C41 C36 N6 119.4(2) . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C39 C38 C37 120.9(3) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 119.3(3) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.4 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C36 121.2(2) . . ? C40 C41 H41A 119.4 . . ? C36 C41 H41A 119.4 . . ? N1L C45 C46 122.6(3) . . ? N1L C45 H45A 118.7 . . ? C46 C45 H45A 118.7 . . ? C47 C46 C45 119.5(3) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C48 C47 C46 118.9(3) . . ? C48 C47 H47A 120.6 . . ? C46 C47 H47A 120.6 . . ? C47 C48 C49 118.5(3) . . ? C47 C48 H48A 120.7 . . ? C49 C48 H48A 120.7 . . ? N1L C49 C48 123.5(3) . . ? N1L C49 H49A 118.2 . . ? C48 C49 H49A 118.2 . . ? N2L C50 C51 122.7(3) . . ? N2L C50 H50A 118.7 . . ? C51 C50 H50A 118.7 . . ? C52 C51 C50 119.1(3) . . ? C52 C51 H51A 120.5 . . ? C50 C51 H51A 120.5 . . ? C51 C52 C53 118.7(3) . . ? C51 C52 H52A 120.7 . . ? C53 C52 H52A 120.7 . . ? C54 C53 C52 119.0(3) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? N2L C54 C53 123.2(3) . . ? N2L C54 H54A 118.4 . . ? C53 C54 H54A 118.4 . . ? N3L C55 C56 122.7(3) . . ? N3L C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C57 C56 C55 119.5(3) . . ? C57 C56 H56A 120.3 . . ? C55 C56 H56A 120.3 . . ? C58 C57 C56 118.4(3) . . ? C58 C57 H57A 120.8 . . ? C56 C57 H57A 120.8 . . ? C57 C58 C59 119.3(3) . . ? C57 C58 H58A 120.3 . . ? C59 C58 H58A 120.3 . . ? N3L C59 C58 122.6(3) . . ? N3L C59 H59A 118.7 . . ? C58 C59 H59A 118.7 . . ? C65 C60 C61 120.1(4) . . ? C65 C60 H60A 119.9 . . ? C61 C60 H60A 119.9 . . ? C60 C61 C62 119.3(4) . . ? C60 C61 H61A 120.4 . . ? C62 C61 H61A 120.4 . . ? C63 C62 C61 118.5(4) . . ? C63 C62 H62A 120.7 . . ? C61 C62 H62A 120.7 . . ? C64 C63 C62 121.0(4) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? C63 C64 C65 119.9(4) . . ? C63 C64 H64A 120.1 . . ? C65 C64 H64A 120.1 . . ? C60 C65 C64 121.1(4) . . ? C60 C65 H65A 119.5 . . ? C64 C65 H65A 119.5 . . ? C75 C70 C71 119.6(5) . . ? C75 C70 H70A 120.2 . . ? C71 C70 H70A 120.2 . . ? C72 C71 C70 120.7(5) . . ? C72 C71 H71A 119.7 . . ? C70 C71 H71A 119.7 . . ? C71 C72 C73 120.3(4) . . ? C71 C72 H72A 119.8 . . ? C73 C72 H72A 119.8 . . ? C72 C73 C74 118.9(5) . . ? C72 C73 H73A 120.6 . . ? C74 C73 H73A 120.6 . . ? C75 C74 C73 119.8(5) . . ? C75 C74 H74A 120.1 . . ? C73 C74 H74A 120.1 . . ? C70 C75 C74 120.7(5) . . ? C70 C75 H75A 119.6 . . ? C74 C75 H75A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.440 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.056 #=============the end of compound 200K=================== #============compound 250K================================ data_250 _database_code_depnum_ccdc_archive 'CCDC 789358' #TrackingRef '2147_web_deposit_cif_file_0_EmilyEames_1281822379.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H51 Fe3 N9, 2(C6 H6)' _chemical_formula_sum 'C68 H63 Fe3 N9' _chemical_formula_weight 1173.82 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' 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 11.888(3) _cell_length_b 13.106(3) _cell_length_c 19.649(4) _cell_angle_alpha 73.904(4) _cell_angle_beta 86.251(4) _cell_angle_gamma 75.708(4) _cell_volume 2850.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 10043 _cell_measurement_theta_min 2.2155 _cell_measurement_theta_max 25.6165 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6987 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34608 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.90 _reflns_number_total 10822 _reflns_number_gt 8108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0536P)^2^+1.4556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10822 _refine_ls_number_parameters 697 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.63248(3) 0.23530(3) 0.22843(2) 0.03596(11) Uani 1 1 d . . . Fe2 Fe 0.69135(3) 0.06394(3) 0.180296(19) 0.03472(11) Uani 1 1 d . . . Fe3 Fe 0.77544(3) 0.06573(3) 0.29738(2) 0.03546(11) Uani 1 1 d . . . N1 N 0.69231(18) -0.05173(16) 0.28592(11) 0.0352(5) Uani 1 1 d . . . N1L N 0.5088(2) 0.38468(17) 0.22254(12) 0.0408(5) Uani 1 1 d . . . N2 N 0.62219(18) 0.14280(17) 0.33981(11) 0.0349(5) Uani 1 1 d . . . N2L N 0.6515(2) -0.03770(19) 0.12166(12) 0.0450(6) Uani 1 1 d . . . N3 N 0.51977(17) 0.14500(16) 0.20449(11) 0.0328(5) Uani 1 1 d . . . N3L N 0.91243(19) -0.00291(19) 0.37307(12) 0.0422(5) Uani 1 1 d . . . N4 N 0.86867(17) -0.00961(16) 0.21241(11) 0.0351(5) Uani 1 1 d . . . N5 N 0.77819(17) 0.24119(16) 0.28157(11) 0.0342(5) Uani 1 1 d . . . N6 N 0.65860(17) 0.22919(17) 0.11547(11) 0.0342(5) Uani 1 1 d . . . C1 C 0.3931(2) -0.0208(2) 0.36793(16) 0.0493(7) Uani 1 1 d . . . H1A H 0.4211 -0.0688 0.4138 0.074 Uiso 1 1 calc R . . H1B H 0.3646 -0.0615 0.3413 0.074 Uiso 1 1 calc R . . H1C H 0.3307 0.0393 0.3744 0.074 Uiso 1 1 calc R . . C2 C 0.4928(2) 0.0246(2) 0.32716(14) 0.0368(6) Uani 1 1 d . . . C3 C 0.5858(2) -0.0743(2) 0.31975(15) 0.0398(6) Uani 1 1 d . . . H3A H 0.6050 -0.1240 0.3671 0.048 Uiso 1 1 calc R . . H3B H 0.5534 -0.1127 0.2926 0.048 Uiso 1 1 calc R . . C4 C 0.5325(2) 0.0874(2) 0.37141(14) 0.0394(6) Uani 1 1 d . . . H4A H 0.4651 0.1418 0.3811 0.047 Uiso 1 1 calc R . . H4B H 0.5611 0.0363 0.4170 0.047 Uiso 1 1 calc R . . C5 C 0.4410(2) 0.0987(2) 0.25655(14) 0.0380(6) Uani 1 1 d . . . H5A H 0.4024 0.0569 0.2353 0.046 Uiso 1 1 calc R . . H5B H 0.3808 0.1592 0.2661 0.046 Uiso 1 1 calc R . . C6 C 0.7741(2) -0.1447(2) 0.27850(14) 0.0369(6) Uani 1 1 d . . . C7 C 0.7655(3) -0.2519(2) 0.30426(16) 0.0473(7) Uani 1 1 d . . . H7A H 0.6989 -0.2675 0.3293 0.057 Uiso 1 1 calc R . . C8 C 0.8554(3) -0.3370(2) 0.29317(19) 0.0597(9) Uani 1 1 d . . . H8A H 0.8491 -0.4098 0.3105 0.072 Uiso 1 1 calc R . . C9 C 0.9521(3) -0.3148(2) 0.25732(19) 0.0601(9) Uani 1 1 d . . . H9A H 1.0128 -0.3724 0.2505 0.072 Uiso 1 1 calc R . . C10 C 0.9621(2) -0.2080(2) 0.23078(16) 0.0454(7) Uani 1 1 d . . . H10A H 1.0293 -0.1936 0.2061 0.055 Uiso 1 1 calc R . . C11 C 0.8733(2) -0.1219(2) 0.24042(14) 0.0357(6) Uani 1 1 d . . . C12 C 0.9729(2) 0.0122(2) 0.17881(15) 0.0372(6) Uani 1 1 d . . . C13 C 0.9800(2) 0.0481(2) 0.10586(16) 0.0477(7) Uani 1 1 d . . . H13A H 0.9148 0.0581 0.0779 0.057 Uiso 1 1 calc R . . C14 C 1.0810(3) 0.0692(3) 0.07365(19) 0.0634(9) Uani 1 1 d . . . H14A H 1.0841 0.0939 0.0240 0.076 Uiso 1 1 calc R . . C15 C 1.1774(3) 0.0548(3) 0.1131(2) 0.0656(10) Uani 1 1 d . . . H15A H 1.2459 0.0710 0.0910 0.079 Uiso 1 1 calc R . . C16 C 1.1723(3) 0.0163(3) 0.1851(2) 0.0577(8) Uani 1 1 d . . . H16A H 1.2383 0.0047 0.2127 0.069 Uiso 1 1 calc R . . C17 C 1.0719(2) -0.0055(2) 0.21764(17) 0.0472(7) Uani 1 1 d . . . H17A H 1.0705 -0.0330 0.2672 0.057 Uiso 1 1 calc R . . C18 C 0.6493(2) 0.2092(2) 0.37764(13) 0.0357(6) Uani 1 1 d . . . C19 C 0.5992(2) 0.2265(2) 0.44042(14) 0.0439(7) Uani 1 1 d . . . H19A H 0.5418 0.1902 0.4620 0.053 Uiso 1 1 calc R . . C20 C 0.6329(3) 0.2971(3) 0.47169(16) 0.0524(8) Uani 1 1 d . . . H20A H 0.5976 0.3092 0.5139 0.063 Uiso 1 1 calc R . . C21 C 0.7173(3) 0.3486(2) 0.44129(16) 0.0513(8) Uani 1 1 d . . . H21A H 0.7402 0.3959 0.4629 0.062 Uiso 1 1 calc R . . C22 C 0.7699(2) 0.3321(2) 0.37878(15) 0.0438(7) Uani 1 1 d . . . H22A H 0.8294 0.3667 0.3588 0.053 Uiso 1 1 calc R . . C23 C 0.7344(2) 0.2641(2) 0.34578(13) 0.0349(6) Uani 1 1 d . . . C24 C 0.8485(2) 0.3089(2) 0.24059(14) 0.0377(6) Uani 1 1 d . . . C25 C 0.9570(2) 0.2639(2) 0.21918(16) 0.0485(7) Uani 1 1 d . . . H25A H 0.9862 0.1877 0.2332 0.058 Uiso 1 1 calc R . . C26 C 1.0239(3) 0.3294(3) 0.17727(19) 0.0649(9) Uani 1 1 d . . . H26A H 1.0977 0.2969 0.1627 0.078 Uiso 1 1 calc R . . C27 C 0.9849(3) 0.4395(3) 0.1568(2) 0.0719(10) Uani 1 1 d . . . H27A H 1.0316 0.4833 0.1288 0.086 Uiso 1 1 calc R . . C28 C 0.8760(3) 0.4866(3) 0.17746(19) 0.0647(9) Uani 1 1 d . . . H28A H 0.8481 0.5630 0.1634 0.078 Uiso 1 1 calc R . . C29 C 0.8081(3) 0.4223(2) 0.21856(16) 0.0489(7) Uani 1 1 d . . . H29A H 0.7335 0.4551 0.2320 0.059 Uiso 1 1 calc R . . C30 C 0.4648(2) 0.2201(2) 0.14389(13) 0.0331(5) Uani 1 1 d . . . C31 C 0.3468(2) 0.2541(2) 0.13011(15) 0.0418(6) Uani 1 1 d . . . H31A H 0.2950 0.2209 0.1615 0.050 Uiso 1 1 calc R . . C32 C 0.3047(2) 0.3373(2) 0.06980(15) 0.0458(7) Uani 1 1 d . . . H32A H 0.2243 0.3604 0.0610 0.055 Uiso 1 1 calc R . . C33 C 0.3786(2) 0.3858(2) 0.02316(15) 0.0440(7) Uani 1 1 d . . . H33A H 0.3491 0.4428 -0.0170 0.053 Uiso 1 1 calc R . . C34 C 0.4972(2) 0.3508(2) 0.03510(14) 0.0375(6) Uani 1 1 d . . . H34A H 0.5482 0.3839 0.0028 0.045 Uiso 1 1 calc R . . C35 C 0.5415(2) 0.2666(2) 0.09483(13) 0.0325(5) Uani 1 1 d . . . C36 C 0.7382(2) 0.2536(2) 0.05973(13) 0.0359(6) Uani 1 1 d . . . C37 C 0.8111(2) 0.3205(2) 0.05952(15) 0.0438(7) Uani 1 1 d . . . H37A H 0.8070 0.3540 0.0965 0.053 Uiso 1 1 calc R . . C38 C 0.8904(3) 0.3389(3) 0.00541(17) 0.0568(8) Uani 1 1 d . . . H38A H 0.9400 0.3844 0.0062 0.068 Uiso 1 1 calc R . . C39 C 0.8976(3) 0.2916(3) -0.04939(17) 0.0567(8) Uani 1 1 d . . . H39A H 0.9518 0.3043 -0.0859 0.068 Uiso 1 1 calc R . . C40 C 0.8247(3) 0.2256(2) -0.05007(15) 0.0513(8) Uani 1 1 d . . . H40A H 0.8290 0.1927 -0.0873 0.062 Uiso 1 1 calc R . . C41 C 0.7454(2) 0.2071(2) 0.00329(14) 0.0420(6) Uani 1 1 d . . . H41A H 0.6953 0.1624 0.0017 0.050 Uiso 1 1 calc R . . C45 C 0.4945(3) 0.4690(2) 0.16518(16) 0.0557(8) Uani 1 1 d . . . H45A H 0.5547 0.4724 0.1317 0.067 Uiso 1 1 calc R . . C46 C 0.3958(4) 0.5509(3) 0.15293(18) 0.0770(12) Uani 1 1 d . . . H46A H 0.3888 0.6095 0.1118 0.092 Uiso 1 1 calc R . . C47 C 0.3083(3) 0.5473(3) 0.2001(2) 0.0720(11) Uani 1 1 d . . . H47A H 0.2391 0.6025 0.1919 0.086 Uiso 1 1 calc R . . C48 C 0.3219(3) 0.4629(3) 0.25946(19) 0.0609(9) Uani 1 1 d . . . H48A H 0.2626 0.4587 0.2935 0.073 Uiso 1 1 calc R . . C49 C 0.4231(3) 0.3841(2) 0.26905(16) 0.0500(7) Uani 1 1 d . . . H49A H 0.4324 0.3263 0.3108 0.060 Uiso 1 1 calc R . . C50 C 0.7308(3) -0.1129(3) 0.09965(17) 0.0564(8) Uani 1 1 d . . . H50A H 0.8096 -0.1186 0.1071 0.068 Uiso 1 1 calc R . . C51 C 0.7019(4) -0.1825(3) 0.06650(19) 0.0699(10) Uani 1 1 d . . . H51A H 0.7601 -0.2341 0.0509 0.084 Uiso 1 1 calc R . . C52 C 0.5877(4) -0.1756(3) 0.0566(2) 0.0864(13) Uani 1 1 d . . . H52A H 0.5656 -0.2223 0.0341 0.104 Uiso 1 1 calc R . . C53 C 0.5066(4) -0.1001(4) 0.0795(3) 0.0928(14) Uani 1 1 d . . . H53A H 0.4272 -0.0939 0.0734 0.111 Uiso 1 1 calc R . . C54 C 0.5414(3) -0.0333(3) 0.11170(19) 0.0632(9) Uani 1 1 d . . . H54A H 0.4841 0.0186 0.1276 0.076 Uiso 1 1 calc R . . C55 C 0.9833(2) 0.0541(3) 0.38599(15) 0.0467(7) Uani 1 1 d . . . H55A H 0.9650 0.1304 0.3667 0.056 Uiso 1 1 calc R . . C56 C 1.0817(3) 0.0061(3) 0.42628(17) 0.0564(8) Uani 1 1 d . . . H56A H 1.1298 0.0489 0.4342 0.068 Uiso 1 1 calc R . . C57 C 1.1093(3) -0.1042(3) 0.45484(18) 0.0651(9) Uani 1 1 d . . . H57A H 1.1773 -0.1388 0.4820 0.078 Uiso 1 1 calc R . . C58 C 1.0367(3) -0.1634(3) 0.44332(18) 0.0639(9) Uani 1 1 d . . . H58A H 1.0529 -0.2395 0.4632 0.077 Uiso 1 1 calc R . . C59 C 0.9393(3) -0.1103(2) 0.40225(16) 0.0534(8) Uani 1 1 d . . . H59A H 0.8896 -0.1517 0.3945 0.064 Uiso 1 1 calc R . . C60 C 0.2354(2) 0.2427(2) 0.4432(2) 0.1012(15) Uani 1 1 d G . . H60A H 0.2897 0.1749 0.4517 0.121 Uiso 1 1 calc R . . C61 C 0.2280(3) 0.3075(3) 0.48937(15) 0.1188(18) Uani 1 1 d G . . H61A H 0.2773 0.2836 0.5291 0.143 Uiso 1 1 calc R . . C62 C 0.1476(3) 0.4078(3) 0.47681(17) 0.132(2) Uani 1 1 d G . . H62A H 0.1426 0.4517 0.5080 0.159 Uiso 1 1 calc R . . C63 C 0.0747(2) 0.4433(2) 0.4181(2) 0.1190(19) Uani 1 1 d G . . H63A H 0.0204 0.5111 0.4096 0.143 Uiso 1 1 calc R . . C64 C 0.0821(3) 0.3784(3) 0.37197(18) 0.1039(16) Uani 1 1 d G . . H64A H 0.0328 0.4024 0.3323 0.125 Uiso 1 1 calc R . . C65 C 0.1625(3) 0.2781(3) 0.38453(18) 0.1028(15) Uani 1 1 d G . . H65A H 0.1675 0.2342 0.3533 0.123 Uiso 1 1 calc R . . C70 C 0.4902(4) 0.6786(4) 0.2712(3) 0.127(2) Uani 1 1 d G . . H70A H 0.5508 0.6918 0.2394 0.152 Uiso 1 1 calc R . . C71 C 0.3806(4) 0.7492(3) 0.2593(2) 0.1159(18) Uani 1 1 d G . . H71A H 0.3672 0.8100 0.2194 0.139 Uiso 1 1 calc R . . C72 C 0.2910(3) 0.7298(3) 0.3065(2) 0.1034(16) Uani 1 1 d G . . H72A H 0.2169 0.7776 0.2984 0.124 Uiso 1 1 calc R . . C73 C 0.3109(4) 0.6398(4) 0.3655(2) 0.1190(18) Uani 1 1 d G . . H73A H 0.2503 0.6267 0.3974 0.143 Uiso 1 1 calc R . . C74 C 0.4205(5) 0.5692(3) 0.37736(19) 0.132(3) Uani 1 1 d G . . H74A H 0.4339 0.5083 0.4173 0.159 Uiso 1 1 calc R . . C75 C 0.5101(3) 0.5885(3) 0.3302(3) 0.131(3) Uani 1 1 d G . . H75A H 0.5842 0.5407 0.3382 0.157 Uiso 1 1 calc R . . 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 0.0364(2) 0.0366(2) 0.0365(2) -0.01121(16) -0.00381(16) -0.00912(16) Fe2 0.0317(2) 0.0354(2) 0.0365(2) -0.00979(16) -0.00226(15) -0.00620(15) Fe3 0.0309(2) 0.0348(2) 0.0420(2) -0.01265(16) -0.00238(16) -0.00704(15) N1 0.0331(11) 0.0299(11) 0.0423(13) -0.0082(9) 0.0013(9) -0.0091(9) N1L 0.0455(13) 0.0369(12) 0.0404(13) -0.0135(10) 0.0012(10) -0.0072(10) N2 0.0338(11) 0.0390(12) 0.0341(12) -0.0108(9) 0.0003(9) -0.0113(9) N2L 0.0489(14) 0.0480(14) 0.0434(14) -0.0179(11) -0.0009(11) -0.0147(11) N3 0.0268(10) 0.0364(11) 0.0341(12) -0.0065(9) -0.0001(9) -0.0090(9) N3L 0.0402(13) 0.0463(13) 0.0369(13) -0.0070(10) -0.0059(10) -0.0077(11) N4 0.0277(11) 0.0337(11) 0.0437(13) -0.0111(9) 0.0000(9) -0.0061(9) N5 0.0313(11) 0.0350(11) 0.0388(12) -0.0127(9) -0.0005(9) -0.0092(9) N6 0.0312(11) 0.0378(11) 0.0330(12) -0.0068(9) -0.0005(9) -0.0104(9) C1 0.0432(16) 0.0551(18) 0.0489(18) -0.0064(14) 0.0075(13) -0.0212(14) C2 0.0331(14) 0.0410(14) 0.0370(14) -0.0071(11) 0.0043(11) -0.0150(11) C3 0.0391(15) 0.0372(14) 0.0430(16) -0.0062(12) -0.0003(12) -0.0141(12) C4 0.0375(14) 0.0447(15) 0.0331(14) -0.0066(12) 0.0026(11) -0.0095(12) C5 0.0304(13) 0.0450(15) 0.0393(15) -0.0094(12) -0.0007(11) -0.0121(11) C6 0.0386(14) 0.0330(13) 0.0397(15) -0.0103(11) -0.0048(12) -0.0078(11) C7 0.0480(17) 0.0371(15) 0.0564(19) -0.0095(13) 0.0016(14) -0.0131(13) C8 0.066(2) 0.0314(15) 0.081(2) -0.0121(15) 0.0003(18) -0.0140(15) C9 0.057(2) 0.0392(17) 0.082(2) -0.0221(16) 0.0020(18) 0.0001(14) C10 0.0427(16) 0.0398(15) 0.0550(18) -0.0173(13) 0.0017(13) -0.0074(12) C11 0.0392(14) 0.0310(13) 0.0376(14) -0.0083(11) -0.0078(11) -0.0087(11) C12 0.0308(13) 0.0309(13) 0.0491(17) -0.0130(12) -0.0006(12) -0.0033(11) C13 0.0349(15) 0.0512(17) 0.0505(18) -0.0091(14) -0.0007(13) -0.0039(13) C14 0.051(2) 0.062(2) 0.059(2) -0.0004(16) 0.0115(16) -0.0026(16) C15 0.0356(17) 0.0549(19) 0.099(3) -0.0133(19) 0.0153(18) -0.0103(14) C16 0.0329(16) 0.061(2) 0.084(3) -0.0261(18) -0.0029(16) -0.0129(14) C17 0.0353(15) 0.0529(17) 0.0559(18) -0.0199(14) -0.0030(13) -0.0084(13) C18 0.0371(14) 0.0371(14) 0.0317(14) -0.0106(11) -0.0058(11) -0.0040(11) C19 0.0427(16) 0.0500(16) 0.0361(15) -0.0106(13) -0.0044(12) -0.0056(13) C20 0.0592(19) 0.0592(19) 0.0377(16) -0.0199(14) -0.0067(14) -0.0028(16) C21 0.063(2) 0.0488(17) 0.0459(18) -0.0231(14) -0.0129(15) -0.0063(15) C22 0.0461(16) 0.0397(15) 0.0473(17) -0.0134(13) -0.0095(13) -0.0087(13) C23 0.0338(14) 0.0350(13) 0.0324(14) -0.0091(11) -0.0060(11) -0.0003(11) C24 0.0377(14) 0.0393(14) 0.0412(15) -0.0144(12) -0.0032(12) -0.0133(12) C25 0.0405(16) 0.0462(16) 0.0566(19) -0.0125(14) 0.0048(14) -0.0092(13) C26 0.0462(19) 0.072(2) 0.075(2) -0.0148(19) 0.0127(17) -0.0206(17) C27 0.079(3) 0.074(3) 0.073(2) -0.013(2) 0.012(2) -0.046(2) C28 0.087(3) 0.0424(17) 0.070(2) -0.0158(16) 0.006(2) -0.0261(18) C29 0.0529(18) 0.0406(16) 0.0558(18) -0.0168(14) 0.0030(14) -0.0125(14) C30 0.0305(13) 0.0356(13) 0.0349(14) -0.0123(11) -0.0026(11) -0.0073(11) C31 0.0320(14) 0.0493(16) 0.0429(16) -0.0104(13) 0.0000(12) -0.0097(12) C32 0.0317(14) 0.0530(17) 0.0468(17) -0.0121(14) -0.0065(12) 0.0009(13) C33 0.0446(16) 0.0419(15) 0.0388(15) -0.0086(12) -0.0087(13) 0.0017(13) C34 0.0417(15) 0.0349(13) 0.0338(14) -0.0070(11) 0.0003(11) -0.0080(11) C35 0.0287(13) 0.0375(13) 0.0342(14) -0.0156(11) -0.0010(10) -0.0061(11) C36 0.0305(13) 0.0371(14) 0.0336(14) -0.0026(11) -0.0011(11) -0.0039(11) C37 0.0430(16) 0.0452(16) 0.0434(16) -0.0087(13) 0.0019(13) -0.0148(13) C38 0.0503(19) 0.062(2) 0.057(2) -0.0049(16) 0.0057(15) -0.0246(16) C39 0.0451(17) 0.068(2) 0.0449(18) -0.0010(16) 0.0117(14) -0.0105(16) C40 0.0527(18) 0.0559(18) 0.0366(16) -0.0098(14) 0.0033(13) -0.0010(15) C41 0.0430(15) 0.0437(15) 0.0372(15) -0.0078(12) -0.0011(12) -0.0096(12) C45 0.072(2) 0.0439(17) 0.0440(18) -0.0120(14) 0.0098(15) -0.0023(15) C46 0.106(3) 0.055(2) 0.0444(19) -0.0046(16) -0.004(2) 0.020(2) C47 0.065(2) 0.073(2) 0.064(2) -0.026(2) -0.0112(18) 0.0216(18) C48 0.0476(18) 0.064(2) 0.071(2) -0.0260(18) 0.0099(16) -0.0075(16) C49 0.0511(18) 0.0464(16) 0.0502(18) -0.0135(14) 0.0068(14) -0.0086(14) C50 0.0540(19) 0.064(2) 0.058(2) -0.0274(16) -0.0005(15) -0.0123(16) C51 0.081(3) 0.067(2) 0.070(2) -0.0410(19) -0.003(2) -0.0076(19) C52 0.090(3) 0.086(3) 0.112(3) -0.064(3) -0.004(3) -0.031(2) C53 0.065(2) 0.115(3) 0.136(4) -0.085(3) -0.003(2) -0.031(2) C54 0.052(2) 0.074(2) 0.080(2) -0.045(2) -0.0035(17) -0.0160(17) C55 0.0405(16) 0.0558(18) 0.0428(17) -0.0096(14) -0.0031(13) -0.0130(14) C56 0.0425(17) 0.072(2) 0.0534(19) -0.0122(17) -0.0069(14) -0.0150(16) C57 0.0460(19) 0.077(2) 0.059(2) -0.0075(18) -0.0154(16) 0.0020(17) C58 0.072(2) 0.0496(18) 0.057(2) -0.0028(16) -0.0158(18) 0.0001(17) C59 0.060(2) 0.0477(17) 0.0490(18) -0.0053(14) -0.0111(15) -0.0116(15) C60 0.088(3) 0.090(3) 0.103(4) -0.011(3) 0.027(3) -0.004(3) C61 0.099(4) 0.150(5) 0.091(4) -0.012(4) -0.003(3) -0.024(4) C62 0.153(6) 0.123(5) 0.128(5) -0.059(4) 0.010(4) -0.019(4) C63 0.109(4) 0.101(4) 0.125(5) -0.023(4) 0.022(4) 0.002(3) C64 0.069(3) 0.125(4) 0.110(4) -0.009(3) 0.013(3) -0.038(3) C65 0.116(4) 0.096(4) 0.106(4) -0.029(3) 0.024(3) -0.049(3) C70 0.094(4) 0.129(5) 0.190(7) -0.091(5) -0.024(4) -0.026(4) C71 0.118(4) 0.082(3) 0.151(5) -0.039(3) -0.032(4) -0.013(3) C72 0.115(4) 0.079(3) 0.119(4) -0.054(3) -0.038(3) 0.013(3) C73 0.148(5) 0.124(5) 0.098(4) -0.071(4) -0.008(4) -0.008(4) C74 0.191(7) 0.096(4) 0.102(4) -0.053(3) -0.067(4) 0.029(4) C75 0.121(5) 0.117(5) 0.169(6) -0.087(5) -0.078(5) 0.024(4) _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 2.108(2) . ? Fe1 N1L 2.117(2) . ? Fe1 N3 2.143(2) . ? Fe1 N2 2.200(2) . ? Fe1 N6 2.242(2) . ? Fe1 Fe3 2.5357(6) . ? Fe1 Fe2 2.5967(7) . ? Fe2 N2L 2.136(2) . ? Fe2 N6 2.141(2) . ? Fe2 N3 2.144(2) . ? Fe2 N4 2.146(2) . ? Fe2 N1 2.204(2) . ? Fe2 Fe3 2.5757(7) . ? Fe3 N1 2.090(2) . ? Fe3 N2 2.096(2) . ? Fe3 N3L 2.127(2) . ? Fe3 N5 2.242(2) . ? Fe3 N4 2.263(2) . ? N1 C6 1.395(3) . ? N1 C3 1.448(3) . ? N1L C49 1.324(3) . ? N1L C45 1.328(4) . ? N2 C18 1.393(3) . ? N2 C4 1.448(3) . ? N2L C54 1.321(4) . ? N2L C50 1.331(4) . ? N3 C30 1.396(3) . ? N3 C5 1.451(3) . ? N3L C59 1.329(4) . ? N3L C55 1.334(4) . ? N4 C11 1.409(3) . ? N4 C12 1.420(3) . ? N5 C23 1.414(3) . ? N5 C24 1.420(3) . ? N6 C35 1.404(3) . ? N6 C36 1.420(3) . ? C1 C2 1.536(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C4 1.516(4) . ? C2 C3 1.516(4) . ? C2 C5 1.522(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.383(4) . ? C6 C11 1.405(4) . ? C7 C8 1.397(4) . ? C7 H7A 0.9400 . ? C8 C9 1.360(4) . ? C8 H8A 0.9400 . ? C9 C10 1.383(4) . ? C9 H9A 0.9400 . ? C10 C11 1.388(4) . ? C10 H10A 0.9400 . ? C12 C17 1.380(4) . ? C12 C13 1.383(4) . ? C13 C14 1.374(4) . ? C13 H13A 0.9400 . ? C14 C15 1.370(5) . ? C14 H14A 0.9400 . ? C15 C16 1.367(5) . ? C15 H15A 0.9400 . ? C16 C17 1.372(4) . ? C16 H16A 0.9400 . ? C17 H17A 0.9400 . ? C18 C19 1.386(4) . ? C18 C23 1.400(4) . ? C19 C20 1.387(4) . ? C19 H19A 0.9400 . ? C20 C21 1.360(4) . ? C20 H20A 0.9400 . ? C21 C22 1.388(4) . ? C21 H21A 0.9400 . ? C22 C23 1.390(4) . ? C22 H22A 0.9400 . ? C24 C25 1.372(4) . ? C24 C29 1.395(4) . ? C25 C26 1.380(4) . ? C25 H25A 0.9400 . ? C26 C27 1.353(5) . ? C26 H26A 0.9400 . ? C27 C28 1.377(5) . ? C27 H27A 0.9400 . ? C28 C29 1.374(4) . ? C28 H28A 0.9400 . ? C29 H29A 0.9400 . ? C30 C31 1.384(4) . ? C30 C35 1.402(3) . ? C31 C32 1.391(4) . ? C31 H31A 0.9400 . ? C32 C33 1.365(4) . ? C32 H32A 0.9400 . ? C33 C34 1.385(4) . ? C33 H33A 0.9400 . ? C34 C35 1.396(4) . ? C34 H34A 0.9400 . ? C36 C37 1.376(4) . ? C36 C41 1.395(4) . ? C37 C38 1.384(4) . ? C37 H37A 0.9400 . ? C38 C39 1.372(5) . ? C38 H38A 0.9400 . ? C39 C40 1.371(4) . ? C39 H39A 0.9400 . ? C40 C41 1.375(4) . ? C40 H40A 0.9400 . ? C41 H41A 0.9400 . ? C45 C46 1.363(4) . ? C45 H45A 0.9400 . ? C46 C47 1.348(5) . ? C46 H46A 0.9400 . ? C47 C48 1.353(5) . ? C47 H47A 0.9400 . ? C48 C49 1.363(4) . ? C48 H48A 0.9400 . ? C49 H49A 0.9400 . ? C50 C51 1.374(4) . ? C50 H50A 0.9400 . ? C51 C52 1.362(5) . ? C51 H51A 0.9400 . ? C52 C53 1.354(5) . ? C52 H52A 0.9400 . ? C53 C54 1.363(5) . ? C53 H53A 0.9400 . ? C54 H54A 0.9400 . ? C55 C56 1.368(4) . ? C55 H55A 0.9400 . ? C56 C57 1.361(5) . ? C56 H56A 0.9400 . ? C57 C58 1.361(5) . ? C57 H57A 0.9400 . ? C58 C59 1.375(4) . ? C58 H58A 0.9400 . ? C59 H59A 0.9400 . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C60 H60A 0.9400 . ? C61 C62 1.3900 . ? C61 H61A 0.9400 . ? C62 C63 1.3900 . ? C62 H62A 0.9400 . ? C63 C64 1.3900 . ? C63 H63A 0.9400 . ? C64 C65 1.3900 . ? C64 H64A 0.9400 . ? C65 H65A 0.9400 . ? C70 C71 1.390(6) . ? C70 C75 1.390(6) . ? C70 H70A 0.9400 . ? C71 C72 1.3900 . ? C71 H71A 0.9400 . ? C72 C73 1.3900 . ? C72 H72A 0.9400 . ? C73 C74 1.3900 . ? C73 H73A 0.9400 . ? C74 C75 1.3900 . ? C74 H74A 0.9400 . ? C75 H75A 0.9400 . ? 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 N1L 106.34(9) . . ? N5 Fe1 N3 150.53(8) . . ? N1L Fe1 N3 98.53(9) . . ? N5 Fe1 N2 72.50(8) . . ? N1L Fe1 N2 103.01(8) . . ? N3 Fe1 N2 86.87(8) . . ? N5 Fe1 N6 116.58(8) . . ? N1L Fe1 N6 104.25(8) . . ? N3 Fe1 N6 70.77(7) . . ? N2 Fe1 N6 146.85(8) . . ? N5 Fe1 Fe3 56.84(6) . . ? N1L Fe1 Fe3 151.42(7) . . ? N3 Fe1 Fe3 93.92(6) . . ? N2 Fe1 Fe3 51.96(5) . . ? N6 Fe1 Fe3 104.12(6) . . ? N5 Fe1 Fe2 107.27(6) . . ? N1L Fe1 Fe2 145.27(7) . . ? N3 Fe1 Fe2 52.75(5) . . ? N2 Fe1 Fe2 95.14(6) . . ? N6 Fe1 Fe2 51.89(5) . . ? Fe3 Fe1 Fe2 60.232(19) . . ? N2L Fe2 N6 109.30(9) . . ? N2L Fe2 N3 100.38(9) . . ? N6 Fe2 N3 72.71(8) . . ? N2L Fe2 N4 104.23(9) . . ? N6 Fe2 N4 115.32(8) . . ? N3 Fe2 N4 149.03(8) . . ? N2L Fe2 N1 96.72(9) . . ? N6 Fe2 N1 149.19(8) . . ? N3 Fe2 N1 86.92(8) . . ? N4 Fe2 N1 71.89(8) . . ? N2L Fe2 Fe3 144.72(7) . . ? N6 Fe2 Fe3 105.85(6) . . ? N3 Fe2 Fe3 92.75(6) . . ? N4 Fe2 Fe3 56.40(6) . . ? N1 Fe2 Fe3 51.15(6) . . ? N2L Fe2 Fe1 150.48(7) . . ? N6 Fe2 Fe1 55.48(6) . . ? N3 Fe2 Fe1 52.69(6) . . ? N4 Fe2 Fe1 105.26(6) . . ? N1 Fe2 Fe1 93.82(6) . . ? Fe3 Fe2 Fe1 58.710(15) . . ? N1 Fe3 N2 89.25(8) . . ? N1 Fe3 N3L 111.89(9) . . ? N2 Fe3 N3L 112.47(9) . . ? N1 Fe3 N5 150.22(8) . . ? N2 Fe3 N5 71.88(8) . . ? N3L Fe3 N5 96.79(8) . . ? N1 Fe3 N4 71.70(8) . . ? N2 Fe3 N4 150.39(8) . . ? N3L Fe3 N4 95.88(8) . . ? N5 Fe3 N4 114.45(8) . . ? N1 Fe3 Fe1 98.47(6) . . ? N2 Fe3 Fe1 55.75(6) . . ? N3L Fe3 Fe1 147.84(7) . . ? N5 Fe3 Fe1 51.93(6) . . ? N4 Fe3 Fe1 103.75(6) . . ? N1 Fe3 Fe2 55.18(6) . . ? N2 Fe3 Fe2 98.41(6) . . ? N3L Fe3 Fe2 146.98(6) . . ? N5 Fe3 Fe2 103.92(6) . . ? N4 Fe3 Fe2 52.16(6) . . ? Fe1 Fe3 Fe2 61.058(17) . . ? C6 N1 C3 113.9(2) . . ? C6 N1 Fe3 110.20(16) . . ? C3 N1 Fe3 126.95(17) . . ? C6 N1 Fe2 102.78(16) . . ? C3 N1 Fe2 121.46(16) . . ? Fe3 N1 Fe2 73.67(7) . . ? C49 N1L C45 116.9(3) . . ? C49 N1L Fe1 117.70(19) . . ? C45 N1L Fe1 122.83(19) . . ? C18 N2 C4 114.6(2) . . ? C18 N2 Fe3 108.76(16) . . ? C4 N2 Fe3 123.19(16) . . ? C18 N2 Fe1 103.75(15) . . ? C4 N2 Fe1 126.69(16) . . ? Fe3 N2 Fe1 72.29(7) . . ? C54 N2L C50 117.2(3) . . ? C54 N2L Fe2 118.6(2) . . ? C50 N2L Fe2 123.9(2) . . ? C30 N3 C5 114.02(19) . . ? C30 N3 Fe1 100.07(15) . . ? C5 N3 Fe1 122.07(16) . . ? C30 N3 Fe2 110.80(15) . . ? C5 N3 Fe2 126.91(16) . . ? Fe1 N3 Fe2 74.56(7) . . ? C59 N3L C55 117.4(3) . . ? C59 N3L Fe3 119.0(2) . . ? C55 N3L Fe3 123.01(19) . . ? C11 N4 C12 113.8(2) . . ? C11 N4 Fe2 104.87(15) . . ? C12 N4 Fe2 130.05(17) . . ? C11 N4 Fe3 103.47(15) . . ? C12 N4 Fe3 124.81(16) . . ? Fe2 N4 Fe3 71.43(6) . . ? C23 N5 C24 116.5(2) . . ? C23 N5 Fe1 105.14(15) . . ? C24 N5 Fe1 115.24(16) . . ? C23 N5 Fe3 104.26(15) . . ? C24 N5 Fe3 133.51(16) . . ? Fe1 N5 Fe3 71.24(6) . . ? C35 N6 C36 114.4(2) . . ? C35 N6 Fe2 110.22(15) . . ? C36 N6 Fe2 116.83(15) . . ? C35 N6 Fe1 97.20(14) . . ? C36 N6 Fe1 138.20(17) . . ? Fe2 N6 Fe1 72.63(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C3 112.6(2) . . ? C4 C2 C5 112.2(2) . . ? C3 C2 C5 113.2(2) . . ? C4 C2 C1 106.6(2) . . ? C3 C2 C1 105.8(2) . . ? C5 C2 C1 105.7(2) . . ? N1 C3 C2 115.8(2) . . ? N1 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? N1 C3 H3B 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C2 115.3(2) . . ? N2 C4 H4A 108.5 . . ? C2 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C2 117.2(2) . . ? N3 C5 H5A 108.0 . . ? C2 C5 H5A 108.0 . . ? N3 C5 H5B 108.0 . . ? C2 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C7 C6 N1 126.6(2) . . ? C7 C6 C11 119.6(2) . . ? N1 C6 C11 113.8(2) . . ? C6 C7 C8 120.1(3) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C6 119.2(2) . . ? C10 C11 N4 126.3(2) . . ? C6 C11 N4 114.5(2) . . ? C17 C12 C13 117.7(3) . . ? C17 C12 N4 121.2(3) . . ? C13 C12 N4 121.1(2) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C16 C15 C14 118.8(3) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 120.8(3) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C16 C17 C12 121.1(3) . . ? C16 C17 H17A 119.5 . . ? C12 C17 H17A 119.5 . . ? C19 C18 N2 126.7(2) . . ? C19 C18 C23 119.2(2) . . ? N2 C18 C23 114.1(2) . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.8(3) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C21 C22 C23 119.8(3) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C18 119.6(2) . . ? C22 C23 N5 126.2(2) . . ? C18 C23 N5 114.2(2) . . ? C25 C24 C29 117.9(3) . . ? C25 C24 N5 120.6(2) . . ? C29 C24 N5 121.4(2) . . ? C24 C25 C26 120.7(3) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C27 C26 C25 121.1(3) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 119.3(3) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 120.2(3) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C24 120.7(3) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? C31 C30 N3 127.1(2) . . ? C31 C30 C35 119.3(2) . . ? N3 C30 C35 113.6(2) . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C33 C34 C35 120.3(2) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C30 119.5(2) . . ? C34 C35 N6 125.7(2) . . ? C30 C35 N6 114.4(2) . . ? C37 C36 C41 117.9(2) . . ? C37 C36 N6 122.5(2) . . ? C41 C36 N6 119.6(2) . . ? C36 C37 C38 120.6(3) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C39 C38 C37 120.9(3) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C40 C39 C38 119.0(3) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? C39 C40 C41 120.5(3) . . ? C39 C40 H40A 119.7 . . ? C41 C40 H40A 119.7 . . ? C40 C41 C36 121.0(3) . . ? C40 C41 H41A 119.5 . . ? C36 C41 H41A 119.5 . . ? N1L C45 C46 122.5(3) . . ? N1L C45 H45A 118.8 . . ? C46 C45 H45A 118.8 . . ? C47 C46 C45 119.7(3) . . ? C47 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C46 C47 C48 118.7(3) . . ? C46 C47 H47A 120.6 . . ? C48 C47 H47A 120.6 . . ? C47 C48 C49 118.8(3) . . ? C47 C48 H48A 120.6 . . ? C49 C48 H48A 120.6 . . ? N1L C49 C48 123.3(3) . . ? N1L C49 H49A 118.3 . . ? C48 C49 H49A 118.3 . . ? N2L C50 C51 122.6(3) . . ? N2L C50 H50A 118.7 . . ? C51 C50 H50A 118.7 . . ? C52 C51 C50 118.8(3) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? C53 C52 C51 118.8(3) . . ? C53 C52 H52A 120.6 . . ? C51 C52 H52A 120.6 . . ? C52 C53 C54 119.2(4) . . ? C52 C53 H53A 120.4 . . ? C54 C53 H53A 120.4 . . ? N2L C54 C53 123.3(3) . . ? N2L C54 H54A 118.4 . . ? C53 C54 H54A 118.4 . . ? N3L C55 C56 122.6(3) . . ? N3L C55 H55A 118.7 . . ? C56 C55 H55A 118.7 . . ? C57 C56 C55 119.4(3) . . ? C57 C56 H56A 120.3 . . ? C55 C56 H56A 120.3 . . ? C56 C57 C58 118.7(3) . . ? C56 C57 H57A 120.7 . . ? C58 C57 H57A 120.7 . . ? C57 C58 C59 119.1(3) . . ? C57 C58 H58A 120.5 . . ? C59 C58 H58A 120.5 . . ? N3L C59 C58 122.8(3) . . ? N3L C59 H59A 118.6 . . ? C58 C59 H59A 118.6 . . ? C61 C60 C65 120.0 . . ? C61 C60 H60A 120.0 . . ? C65 C60 H60A 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61A 120.0 . . ? C62 C61 H61A 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 H65A 120.0 . . ? C60 C65 H65A 120.0 . . ? C71 C70 C75 120.0(4) . . ? C71 C70 H70A 120.0 . . ? C75 C70 H70A 120.0 . . ? C70 C71 C72 120.0(2) . . ? C70 C71 H71A 120.0 . . ? C72 C71 H71A 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C74 C75 C70 120.0(2) . . ? C74 C75 H75A 120.0 . . ? C70 C75 H75A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.452 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.054 #=============the end of compound 250K=================== #============compound 300K================================ data_300k _database_code_depnum_ccdc_archive 'CCDC 789359' #TrackingRef '2147_web_deposit_cif_file_0_EmilyEames_1281822379.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H51 Fe3 N9, 2(C6 H6)' _chemical_formula_sum 'C68 H63 Fe3 N9' _chemical_formula_weight 1173.82 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' 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 11.881(3) _cell_length_b 13.093(4) _cell_length_c 19.706(6) _cell_angle_alpha 73.971(5) _cell_angle_beta 86.265(5) _cell_angle_gamma 75.654(5) _cell_volume 2854.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 8810 _cell_measurement_theta_min 2.2135 _cell_measurement_theta_max 24.701 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6990 _exptl_absorpt_correction_T_max 0.9240 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34991 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.95 _reflns_number_total 10868 _reflns_number_gt 7622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0598P)^2^+1.1292P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10868 _refine_ls_number_parameters 697 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.006 _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 0.63283(3) 0.23516(3) 0.22786(2) 0.04316(12) Uani 1 1 d . . . Fe2 Fe 0.69197(3) 0.06392(3) 0.17990(2) 0.04189(12) Uani 1 1 d . . . Fe3 Fe 0.77713(3) 0.06594(3) 0.29634(2) 0.04321(12) Uani 1 1 d . . . N1 N 0.69372(19) -0.05105(18) 0.28475(13) 0.0427(5) Uani 1 1 d . . . N1L N 0.5091(2) 0.38478(19) 0.22147(13) 0.0492(6) Uani 1 1 d . . . N2 N 0.62394(19) 0.14324(18) 0.33839(12) 0.0420(5) Uani 1 1 d . . . N2L N 0.6521(2) -0.0378(2) 0.12154(14) 0.0540(6) Uani 1 1 d . . . N3 N 0.52076(18) 0.14500(18) 0.20425(12) 0.0397(5) Uani 1 1 d . . . N3L N 0.9133(2) -0.0019(2) 0.37216(13) 0.0513(6) Uani 1 1 d . . . N4 N 0.86954(19) -0.00911(18) 0.21202(13) 0.0433(6) Uani 1 1 d . . . N5 N 0.77866(19) 0.24210(18) 0.27985(12) 0.0414(5) Uani 1 1 d . . . N6 N 0.65847(19) 0.22830(18) 0.11503(12) 0.0413(5) Uani 1 1 d . . . C1 C 0.3956(3) -0.0202(3) 0.36752(18) 0.0603(9) Uani 1 1 d . . . H1A H 0.4240 -0.0679 0.4126 0.090 Uiso 1 1 calc R . . H1B H 0.3664 -0.0602 0.3414 0.090 Uiso 1 1 calc R . . H1C H 0.3343 0.0394 0.3743 0.090 Uiso 1 1 calc R . . C2 C 0.4949(2) 0.0249(2) 0.32627(15) 0.0448(7) Uani 1 1 d . . . C3 C 0.5876(3) -0.0732(2) 0.31882(17) 0.0488(7) Uani 1 1 d . . . H3A H 0.6070 -0.1221 0.3656 0.059 Uiso 1 1 calc R . . H3B H 0.5552 -0.1116 0.2923 0.059 Uiso 1 1 calc R . . C4 C 0.5350(3) 0.0879(2) 0.37008(15) 0.0480(7) Uani 1 1 d . . . H4A H 0.4682 0.1418 0.3798 0.058 Uiso 1 1 calc R . . H4B H 0.5638 0.0375 0.4150 0.058 Uiso 1 1 calc R . . C5 C 0.4424(2) 0.0988(2) 0.25644(15) 0.0456(7) Uani 1 1 d . . . H5A H 0.4038 0.0576 0.2356 0.055 Uiso 1 1 calc R . . H5B H 0.3831 0.1588 0.2661 0.055 Uiso 1 1 calc R . . C6 C 0.7757(3) -0.1435(2) 0.27766(16) 0.0456(7) Uani 1 1 d . . . C7 C 0.7669(3) -0.2505(2) 0.30325(18) 0.0582(8) Uani 1 1 d . . . H7A H 0.7009 -0.2661 0.3277 0.070 Uiso 1 1 calc R . . C8 C 0.8570(3) -0.3348(3) 0.2923(2) 0.0731(11) Uani 1 1 d . . . H8A H 0.8510 -0.4069 0.3096 0.088 Uiso 1 1 calc R . . C9 C 0.9534(3) -0.3133(3) 0.2567(2) 0.0735(11) Uani 1 1 d . . . H9A H 1.0137 -0.3706 0.2502 0.088 Uiso 1 1 calc R . . C10 C 0.9625(3) -0.2069(2) 0.23004(18) 0.0561(8) Uani 1 1 d . . . H10A H 1.0287 -0.1925 0.2053 0.067 Uiso 1 1 calc R . . C11 C 0.8744(2) -0.1214(2) 0.23979(15) 0.0431(7) Uani 1 1 d . . . C12 C 0.9734(2) 0.0124(2) 0.17811(16) 0.0448(7) Uani 1 1 d . . . C13 C 0.9802(3) 0.0484(3) 0.10605(18) 0.0579(8) Uani 1 1 d . . . H13A H 0.9155 0.0585 0.0786 0.069 Uiso 1 1 calc R . . C14 C 1.0809(3) 0.0696(3) 0.0739(2) 0.0742(11) Uani 1 1 d . . . H14A H 1.0835 0.0941 0.0249 0.089 Uiso 1 1 calc R . . C15 C 1.1770(3) 0.0553(3) 0.1125(3) 0.0797(12) Uani 1 1 d . . . H15A H 1.2446 0.0713 0.0905 0.096 Uiso 1 1 calc R . . C16 C 1.1724(3) 0.0172(3) 0.1840(2) 0.0700(10) Uani 1 1 d . . . H16A H 1.2380 0.0059 0.2109 0.084 Uiso 1 1 calc R . . C17 C 1.0726(3) -0.0048(3) 0.21676(19) 0.0566(8) Uani 1 1 d . . . H17A H 1.0715 -0.0317 0.2656 0.068 Uiso 1 1 calc R . . C18 C 0.6515(2) 0.2087(2) 0.37629(15) 0.0439(7) Uani 1 1 d . . . C19 C 0.6027(3) 0.2253(3) 0.43909(16) 0.0546(8) Uani 1 1 d . . . H19A H 0.5461 0.1890 0.4606 0.066 Uiso 1 1 calc R . . C20 C 0.6368(3) 0.2949(3) 0.47026(18) 0.0648(9) Uani 1 1 d . . . H20A H 0.6027 0.3063 0.5122 0.078 Uiso 1 1 calc R . . C21 C 0.7204(3) 0.3471(3) 0.43960(18) 0.0639(9) Uani 1 1 d . . . H21A H 0.7432 0.3939 0.4609 0.077 Uiso 1 1 calc R . . C22 C 0.7718(3) 0.3311(2) 0.37710(17) 0.0545(8) Uani 1 1 d . . . H22A H 0.8305 0.3656 0.3572 0.065 Uiso 1 1 calc R . . C23 C 0.7359(2) 0.2637(2) 0.34409(14) 0.0430(7) Uani 1 1 d . . . C24 C 0.8483(2) 0.3094(2) 0.23896(16) 0.0454(7) Uani 1 1 d . . . C25 C 0.9566(3) 0.2646(3) 0.21795(18) 0.0597(9) Uani 1 1 d . . . H25A H 0.9855 0.1891 0.2318 0.072 Uiso 1 1 calc R . . C26 C 1.0231(3) 0.3295(4) 0.1767(2) 0.0812(12) Uani 1 1 d . . . H26A H 1.0961 0.2973 0.1622 0.097 Uiso 1 1 calc R . . C27 C 0.9844(4) 0.4391(4) 0.1568(2) 0.0896(13) Uani 1 1 d . . . H27A H 1.0311 0.4824 0.1297 0.108 Uiso 1 1 calc R . . C28 C 0.8761(4) 0.4862(3) 0.1767(2) 0.0800(12) Uani 1 1 d . . . H28A H 0.8482 0.5619 0.1625 0.096 Uiso 1 1 calc R . . C29 C 0.8084(3) 0.4221(3) 0.21755(18) 0.0597(8) Uani 1 1 d . . . H29A H 0.7348 0.4546 0.2311 0.072 Uiso 1 1 calc R . . C30 C 0.4652(2) 0.2195(2) 0.14423(14) 0.0392(6) Uani 1 1 d . . . C31 C 0.3477(3) 0.2536(3) 0.13025(17) 0.0512(7) Uani 1 1 d . . . H31A H 0.2964 0.2210 0.1613 0.061 Uiso 1 1 calc R . . C32 C 0.3054(3) 0.3360(3) 0.07030(17) 0.0573(8) Uani 1 1 d . . . H32A H 0.2258 0.3591 0.0618 0.069 Uiso 1 1 calc R . . C33 C 0.3790(3) 0.3836(3) 0.02376(17) 0.0535(8) Uani 1 1 d . . . H33A H 0.3497 0.4397 -0.0159 0.064 Uiso 1 1 calc R . . C34 C 0.4975(3) 0.3487(2) 0.03532(15) 0.0460(7) Uani 1 1 d . . . H34A H 0.5478 0.3810 0.0033 0.055 Uiso 1 1 calc R . . C35 C 0.5416(2) 0.2650(2) 0.09507(14) 0.0391(6) Uani 1 1 d . . . C36 C 0.7376(2) 0.2527(2) 0.05945(15) 0.0433(7) Uani 1 1 d . . . C37 C 0.8095(3) 0.3202(3) 0.05921(17) 0.0550(8) Uani 1 1 d . . . H37A H 0.8053 0.3536 0.0956 0.066 Uiso 1 1 calc R . . C38 C 0.8879(3) 0.3387(3) 0.0053(2) 0.0676(10) Uani 1 1 d . . . H38A H 0.9366 0.3841 0.0060 0.081 Uiso 1 1 calc R . . C39 C 0.8956(3) 0.2919(3) -0.04887(19) 0.0695(10) Uani 1 1 d . . . H39A H 0.9490 0.3050 -0.0849 0.083 Uiso 1 1 calc R . . C40 C 0.8243(3) 0.2256(3) -0.04963(17) 0.0629(9) Uani 1 1 d . . . H40A H 0.8288 0.1931 -0.0865 0.076 Uiso 1 1 calc R . . C41 C 0.7454(3) 0.2064(2) 0.00370(16) 0.0509(7) Uani 1 1 d . . . H41A H 0.6965 0.1614 0.0023 0.061 Uiso 1 1 calc R . . C45 C 0.4947(3) 0.4679(3) 0.16435(18) 0.0678(10) Uani 1 1 d . . . H45A H 0.5540 0.4711 0.1311 0.081 Uiso 1 1 calc R . . C46 C 0.3957(4) 0.5493(3) 0.1527(2) 0.0948(15) Uani 1 1 d . . . H46A H 0.3878 0.6070 0.1119 0.114 Uiso 1 1 calc R . . C47 C 0.3092(4) 0.5463(4) 0.2001(2) 0.0891(13) Uani 1 1 d . . . H47A H 0.2405 0.6007 0.1921 0.107 Uiso 1 1 calc R . . C48 C 0.3238(3) 0.4636(3) 0.2591(2) 0.0750(11) Uani 1 1 d . . . H48A H 0.2659 0.4600 0.2933 0.090 Uiso 1 1 calc R . . C49 C 0.4247(3) 0.3850(3) 0.26810(18) 0.0601(9) Uani 1 1 d . . . H49A H 0.4347 0.3283 0.3095 0.072 Uiso 1 1 calc R . . C50 C 0.7311(3) -0.1128(3) 0.09998(19) 0.0695(10) Uani 1 1 d . . . H50A H 0.8092 -0.1185 0.1075 0.083 Uiso 1 1 calc R . . C51 C 0.7028(4) -0.1821(3) 0.0672(2) 0.0828(12) Uani 1 1 d . . . H51A H 0.7605 -0.2330 0.0518 0.099 Uiso 1 1 calc R . . C52 C 0.5886(5) -0.1755(4) 0.0576(3) 0.1037(16) Uani 1 1 d . . . H52A H 0.5669 -0.2224 0.0358 0.124 Uiso 1 1 calc R . . C53 C 0.5073(4) -0.0997(4) 0.0801(3) 0.1110(18) Uani 1 1 d . . . H53A H 0.4286 -0.0933 0.0739 0.133 Uiso 1 1 calc R . . C54 C 0.5425(3) -0.0335(3) 0.1116(2) 0.0765(11) Uani 1 1 d . . . H54A H 0.4860 0.0181 0.1272 0.092 Uiso 1 1 calc R . . C55 C 0.9837(3) 0.0548(3) 0.38475(17) 0.0576(8) Uani 1 1 d . . . H55A H 0.9658 0.1302 0.3651 0.069 Uiso 1 1 calc R . . C56 C 1.0812(3) 0.0076(3) 0.4252(2) 0.0715(10) Uani 1 1 d . . . H56A H 1.1285 0.0503 0.4329 0.086 Uiso 1 1 calc R . . C57 C 1.1087(3) -0.1014(4) 0.4540(2) 0.0818(12) Uani 1 1 d . . . H57A H 1.1755 -0.1351 0.4813 0.098 Uiso 1 1 calc R . . C58 C 1.0375(4) -0.1608(3) 0.4426(2) 0.0828(12) Uani 1 1 d . . . H58A H 1.0540 -0.2361 0.4624 0.099 Uiso 1 1 calc R . . C59 C 0.9405(3) -0.1085(3) 0.40149(18) 0.0662(9) Uani 1 1 d . . . H59A H 0.8917 -0.1499 0.3939 0.079 Uiso 1 1 calc R . . C60 C 0.2383(4) 0.2427(3) 0.4446(4) 0.132(2) Uani 1 1 d G . . H60A H 0.2916 0.1752 0.4531 0.159 Uiso 1 1 calc R . . C61 C 0.2325(4) 0.3083(6) 0.4901(2) 0.151(2) Uani 1 1 d G . . H61A H 0.2819 0.2846 0.5290 0.181 Uiso 1 1 calc R . . C62 C 0.1529(6) 0.4092(5) 0.4775(3) 0.176(3) Uani 1 1 d G . . H62A H 0.1490 0.4530 0.5079 0.211 Uiso 1 1 calc R . . C63 C 0.0791(4) 0.4446(3) 0.4193(4) 0.158(3) Uani 1 1 d G . . H63A H 0.0258 0.5121 0.4109 0.190 Uiso 1 1 calc R . . C64 C 0.0849(4) 0.3790(6) 0.3738(2) 0.139(2) Uani 1 1 d G . . H64A H 0.0355 0.4027 0.3350 0.167 Uiso 1 1 calc R . . C65 C 0.1645(6) 0.2781(5) 0.3865(3) 0.137(2) Uani 1 1 d G . . H65A H 0.1684 0.2343 0.3560 0.164 Uiso 1 1 calc R . . C70 C 0.4903(4) 0.6774(5) 0.2726(3) 0.157(3) Uani 1 1 d G . . H70A H 0.5502 0.6901 0.2410 0.188 Uiso 1 1 calc R . . C71 C 0.3805(6) 0.7479(3) 0.2606(2) 0.146(3) Uani 1 1 d G . . H71A H 0.3670 0.8077 0.2210 0.175 Uiso 1 1 calc R . . C72 C 0.2910(4) 0.7289(4) 0.3078(3) 0.129(2) Uani 1 1 d G . . H72A H 0.2176 0.7761 0.2998 0.155 Uiso 1 1 calc R . . C73 C 0.3113(5) 0.6394(5) 0.3670(3) 0.152(3) Uani 1 1 d G . . H73A H 0.2515 0.6267 0.3986 0.182 Uiso 1 1 calc R . . C74 C 0.4211(6) 0.5689(3) 0.3789(2) 0.161(3) Uani 1 1 d G . . H74A H 0.4347 0.5091 0.4185 0.194 Uiso 1 1 calc R . . C75 C 0.5106(4) 0.5879(4) 0.3317(4) 0.161(4) Uani 1 1 d G . . H75A H 0.5841 0.5407 0.3397 0.194 Uiso 1 1 calc R . . 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 0.0427(2) 0.0432(2) 0.0450(2) -0.01297(18) -0.00384(18) -0.01071(18) Fe2 0.0382(2) 0.0421(2) 0.0450(2) -0.01155(18) -0.00228(18) -0.00843(17) Fe3 0.0374(2) 0.0420(2) 0.0515(3) -0.01459(19) -0.00285(18) -0.00874(17) N1 0.0375(12) 0.0391(12) 0.0508(14) -0.0101(11) 0.0027(11) -0.0110(10) N1L 0.0543(15) 0.0449(14) 0.0474(15) -0.0146(12) 0.0025(12) -0.0082(11) N2 0.0415(13) 0.0462(13) 0.0410(13) -0.0128(11) 0.0013(10) -0.0146(11) N2L 0.0590(17) 0.0567(16) 0.0526(16) -0.0215(13) 0.0006(13) -0.0175(13) N3 0.0327(12) 0.0448(13) 0.0408(13) -0.0081(10) 0.0004(10) -0.0115(10) N3L 0.0484(15) 0.0537(15) 0.0480(15) -0.0088(12) -0.0075(12) -0.0089(12) N4 0.0338(12) 0.0407(13) 0.0532(15) -0.0108(11) 0.0003(11) -0.0070(10) N5 0.0396(13) 0.0413(12) 0.0466(14) -0.0148(11) -0.0003(10) -0.0121(10) N6 0.0364(12) 0.0464(13) 0.0399(13) -0.0078(10) -0.0002(10) -0.0117(10) C1 0.0509(19) 0.067(2) 0.061(2) -0.0061(17) 0.0088(16) -0.0262(16) C2 0.0395(15) 0.0498(16) 0.0458(17) -0.0086(13) 0.0065(13) -0.0183(13) C3 0.0488(17) 0.0441(16) 0.0532(18) -0.0067(14) 0.0015(14) -0.0181(13) C4 0.0451(17) 0.0541(17) 0.0414(17) -0.0073(14) 0.0060(13) -0.0135(14) C5 0.0367(15) 0.0557(17) 0.0460(17) -0.0118(14) 0.0016(13) -0.0163(13) C6 0.0479(17) 0.0402(15) 0.0497(18) -0.0118(13) -0.0057(14) -0.0111(13) C7 0.059(2) 0.0385(16) 0.074(2) -0.0084(15) 0.0020(17) -0.0143(15) C8 0.077(3) 0.0391(18) 0.102(3) -0.0143(18) 0.003(2) -0.0182(17) C9 0.070(2) 0.0443(19) 0.102(3) -0.0266(19) 0.001(2) 0.0020(17) C10 0.0499(18) 0.0498(18) 0.068(2) -0.0189(16) 0.0016(16) -0.0084(14) C11 0.0451(16) 0.0382(15) 0.0469(17) -0.0103(12) -0.0074(13) -0.0107(12) C12 0.0369(15) 0.0357(14) 0.061(2) -0.0143(13) 0.0003(14) -0.0062(12) C13 0.0399(17) 0.062(2) 0.062(2) -0.0077(16) 0.0011(15) -0.0048(15) C14 0.056(2) 0.077(2) 0.071(2) -0.0007(19) 0.0116(19) -0.0079(19) C15 0.043(2) 0.070(2) 0.116(4) -0.014(2) 0.021(2) -0.0142(17) C16 0.0384(18) 0.077(2) 0.101(3) -0.031(2) -0.0049(19) -0.0158(17) C17 0.0415(17) 0.065(2) 0.065(2) -0.0228(17) -0.0026(15) -0.0094(15) C18 0.0435(16) 0.0458(16) 0.0402(16) -0.0129(13) -0.0070(13) -0.0033(13) C19 0.0550(19) 0.062(2) 0.0437(18) -0.0150(15) -0.0041(14) -0.0072(15) C20 0.075(2) 0.070(2) 0.0464(19) -0.0220(17) -0.0093(17) -0.0018(19) C21 0.079(3) 0.059(2) 0.057(2) -0.0294(17) -0.0163(19) -0.0055(18) C22 0.0573(19) 0.0484(17) 0.060(2) -0.0177(15) -0.0121(16) -0.0104(15) C23 0.0401(15) 0.0442(15) 0.0399(16) -0.0118(13) -0.0079(12) 0.0010(12) C24 0.0436(16) 0.0460(16) 0.0523(18) -0.0185(14) -0.0020(13) -0.0150(13) C25 0.0476(18) 0.0574(19) 0.072(2) -0.0150(17) 0.0062(16) -0.0139(15) C26 0.060(2) 0.085(3) 0.097(3) -0.019(2) 0.018(2) -0.026(2) C27 0.100(3) 0.088(3) 0.094(3) -0.019(3) 0.023(3) -0.059(3) C28 0.108(3) 0.049(2) 0.090(3) -0.0191(19) 0.011(2) -0.033(2) C29 0.066(2) 0.0472(18) 0.069(2) -0.0191(16) 0.0045(17) -0.0153(16) C30 0.0356(14) 0.0432(15) 0.0411(15) -0.0149(12) -0.0012(12) -0.0091(12) C31 0.0394(16) 0.0580(18) 0.0548(19) -0.0128(15) 0.0026(14) -0.0120(14) C32 0.0378(16) 0.067(2) 0.059(2) -0.0136(17) -0.0087(15) -0.0001(15) C33 0.0507(18) 0.0508(18) 0.0493(18) -0.0073(14) -0.0108(15) 0.0011(14) C34 0.0486(17) 0.0434(16) 0.0422(17) -0.0075(13) 0.0001(13) -0.0084(13) C35 0.0335(14) 0.0422(15) 0.0449(16) -0.0175(13) -0.0017(12) -0.0079(12) C36 0.0380(15) 0.0453(16) 0.0399(16) -0.0039(13) 0.0001(12) -0.0060(12) C37 0.0531(19) 0.0561(19) 0.056(2) -0.0109(15) 0.0075(15) -0.0205(15) C38 0.059(2) 0.074(2) 0.068(2) -0.0055(19) 0.0112(18) -0.0314(18) C39 0.054(2) 0.085(3) 0.056(2) -0.0029(19) 0.0179(17) -0.0145(19) C40 0.065(2) 0.068(2) 0.0460(19) -0.0135(16) 0.0047(16) -0.0014(18) C41 0.0506(18) 0.0529(18) 0.0450(18) -0.0084(14) -0.0005(14) -0.0098(14) C45 0.087(3) 0.052(2) 0.055(2) -0.0149(17) 0.0128(18) -0.0020(18) C46 0.124(4) 0.070(3) 0.054(2) -0.0053(19) -0.001(2) 0.029(2) C47 0.083(3) 0.088(3) 0.075(3) -0.028(2) -0.014(2) 0.028(2) C48 0.059(2) 0.077(3) 0.085(3) -0.028(2) 0.010(2) -0.0041(19) C49 0.062(2) 0.0544(19) 0.058(2) -0.0127(16) 0.0076(17) -0.0083(16) C50 0.067(2) 0.079(2) 0.071(2) -0.035(2) -0.0002(19) -0.0149(19) C51 0.097(3) 0.079(3) 0.084(3) -0.050(2) 0.000(2) -0.010(2) C52 0.111(4) 0.104(4) 0.131(4) -0.076(3) -0.004(3) -0.036(3) C53 0.076(3) 0.137(4) 0.163(5) -0.100(4) -0.006(3) -0.037(3) C54 0.060(2) 0.093(3) 0.095(3) -0.052(2) -0.006(2) -0.020(2) C55 0.0477(18) 0.067(2) 0.056(2) -0.0099(16) -0.0055(15) -0.0147(16) C56 0.052(2) 0.092(3) 0.070(2) -0.017(2) -0.0114(18) -0.020(2) C57 0.059(2) 0.095(3) 0.078(3) -0.016(2) -0.021(2) 0.002(2) C58 0.092(3) 0.062(2) 0.077(3) -0.004(2) -0.023(2) 0.002(2) C59 0.075(2) 0.059(2) 0.059(2) -0.0063(17) -0.0134(18) -0.0145(18) C60 0.108(5) 0.119(5) 0.142(6) -0.016(5) 0.032(4) -0.006(4) C61 0.140(6) 0.169(7) 0.118(5) -0.010(5) -0.004(4) -0.022(5) C62 0.213(9) 0.155(7) 0.155(7) -0.065(6) 0.012(6) -0.014(6) C63 0.152(7) 0.135(6) 0.158(7) -0.034(6) 0.030(6) 0.007(5) C64 0.089(4) 0.154(6) 0.158(6) -0.003(5) 0.014(4) -0.046(4) C65 0.154(6) 0.124(6) 0.143(6) -0.032(4) 0.035(5) -0.067(5) C70 0.120(6) 0.156(6) 0.239(9) -0.111(7) -0.021(5) -0.044(5) C71 0.148(6) 0.097(4) 0.196(8) -0.053(4) -0.045(6) -0.009(4) C72 0.138(5) 0.102(4) 0.148(6) -0.069(4) -0.036(5) 0.016(4) C73 0.189(7) 0.156(6) 0.121(5) -0.090(5) -0.015(5) 0.000(5) C74 0.223(9) 0.126(5) 0.124(5) -0.067(4) -0.068(6) 0.034(6) C75 0.163(7) 0.128(6) 0.201(8) -0.094(6) -0.103(7) 0.031(5) _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 2.102(2) . ? Fe1 N1L 2.116(2) . ? Fe1 N3 2.132(2) . ? Fe1 N2 2.188(2) . ? Fe1 N6 2.248(2) . ? Fe1 Fe3 2.5370(7) . ? Fe1 Fe2 2.5917(8) . ? Fe2 N6 2.132(2) . ? Fe2 N2L 2.133(3) . ? Fe2 N3 2.140(2) . ? Fe2 N4 2.146(2) . ? Fe2 N1 2.193(2) . ? Fe2 Fe3 2.5765(8) . ? Fe3 N1 2.087(2) . ? Fe3 N2 2.092(2) . ? Fe3 N3L 2.123(3) . ? Fe3 N5 2.243(2) . ? Fe3 N4 2.250(2) . ? N1 C6 1.387(3) . ? N1 C3 1.445(3) . ? N1L C49 1.315(4) . ? N1L C45 1.318(4) . ? N2 C18 1.387(4) . ? N2 C4 1.441(3) . ? N2L C54 1.314(4) . ? N2L C50 1.323(4) . ? N3 C30 1.390(3) . ? N3 C5 1.449(3) . ? N3L C59 1.319(4) . ? N3L C55 1.323(4) . ? N4 C11 1.408(3) . ? N4 C12 1.417(3) . ? N5 C23 1.408(3) . ? N5 C24 1.411(4) . ? N6 C35 1.396(3) . ? N6 C36 1.417(3) . ? C1 C2 1.535(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.505(4) . ? C2 C4 1.515(4) . ? C2 C5 1.516(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.380(4) . ? C6 C11 1.396(4) . ? C7 C8 1.388(5) . ? C7 H7A 0.9300 . ? C8 C9 1.352(5) . ? C8 H8A 0.9300 . ? C9 C10 1.376(5) . ? C9 H9A 0.9300 . ? C10 C11 1.377(4) . ? C10 H10A 0.9300 . ? C12 C13 1.371(4) . ? C12 C17 1.382(4) . ? C13 C14 1.370(4) . ? C13 H13A 0.9300 . ? C14 C15 1.359(6) . ? C14 H14A 0.9300 . ? C15 C16 1.360(6) . ? C15 H15A 0.9300 . ? C16 C17 1.368(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.381(4) . ? C18 C23 1.395(4) . ? C19 C20 1.378(5) . ? C19 H19A 0.9300 . ? C20 C21 1.359(5) . ? C20 H20A 0.9300 . ? C21 C22 1.384(5) . ? C21 H21A 0.9300 . ? C22 C23 1.388(4) . ? C22 H22A 0.9300 . ? C24 C25 1.364(4) . ? C24 C29 1.384(4) . ? C25 C26 1.369(5) . ? C25 H25A 0.9300 . ? C26 C27 1.346(6) . ? C26 H26A 0.9300 . ? C27 C28 1.365(6) . ? C27 H27A 0.9300 . ? C28 C29 1.370(5) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.377(4) . ? C30 C35 1.397(4) . ? C31 C32 1.385(4) . ? C31 H31A 0.9300 . ? C32 C33 1.358(4) . ? C32 H32A 0.9300 . ? C33 C34 1.380(4) . ? C33 H33A 0.9300 . ? C34 C35 1.395(4) . ? C34 H34A 0.9300 . ? C36 C37 1.372(4) . ? C36 C41 1.382(4) . ? C37 C38 1.377(4) . ? C37 H37A 0.9300 . ? C38 C39 1.357(5) . ? C38 H38A 0.9300 . ? C39 C40 1.358(5) . ? C39 H39A 0.9300 . ? C40 C41 1.374(4) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C45 C46 1.361(5) . ? C45 H45A 0.9300 . ? C46 C47 1.344(6) . ? C46 H46A 0.9300 . ? C47 C48 1.340(5) . ? C47 H47A 0.9300 . ? C48 C49 1.358(5) . ? C48 H48A 0.9300 . ? C49 H49A 0.9300 . ? C50 C51 1.362(5) . ? C50 H50A 0.9300 . ? C51 C52 1.360(6) . ? C51 H51A 0.9300 . ? C52 C53 1.352(6) . ? C52 H52A 0.9300 . ? C53 C54 1.352(5) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C55 C56 1.362(5) . ? C55 H55A 0.9300 . ? C56 C57 1.345(5) . ? C56 H56A 0.9300 . ? C57 C58 1.348(6) . ? C57 H57A 0.9300 . ? C58 C59 1.371(5) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C60 H60A 0.9300 . ? C61 C62 1.3900 . ? C61 H61A 0.9300 . ? C62 C63 1.3900 . ? C62 H62A 0.9300 . ? C63 C64 1.3900 . ? C63 H63A 0.9300 . ? C64 C65 1.3900 . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C70 H70A 0.9300 . ? C71 C72 1.3900 . ? C71 H71A 0.9300 . ? C72 C73 1.3900 . ? C72 H72A 0.9300 . ? C73 C74 1.3900 . ? C73 H73A 0.9300 . ? C74 C75 1.3900 . ? C74 H74A 0.9300 . ? C75 H75A 0.9300 . ? 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 N1L 106.34(9) . . ? N5 Fe1 N3 150.84(9) . . ? N1L Fe1 N3 98.52(9) . . ? N5 Fe1 N2 72.64(9) . . ? N1L Fe1 N2 103.45(9) . . ? N3 Fe1 N2 87.11(9) . . ? N5 Fe1 N6 116.41(9) . . ? N1L Fe1 N6 104.02(9) . . ? N3 Fe1 N6 70.55(8) . . ? N2 Fe1 N6 146.71(8) . . ? N5 Fe1 Fe3 56.91(6) . . ? N1L Fe1 Fe3 151.74(7) . . ? N3 Fe1 Fe3 94.13(6) . . ? N2 Fe1 Fe3 51.92(6) . . ? N6 Fe1 Fe3 104.00(6) . . ? N5 Fe1 Fe2 107.29(6) . . ? N1L Fe1 Fe2 145.10(7) . . ? N3 Fe1 Fe2 52.78(6) . . ? N2 Fe1 Fe2 95.19(6) . . ? N6 Fe1 Fe2 51.69(6) . . ? Fe3 Fe1 Fe2 60.30(2) . . ? N6 Fe2 N2L 108.89(10) . . ? N6 Fe2 N3 72.67(8) . . ? N2L Fe2 N3 100.49(10) . . ? N6 Fe2 N4 115.44(9) . . ? N2L Fe2 N4 104.48(10) . . ? N3 Fe2 N4 148.73(9) . . ? N6 Fe2 N1 149.43(9) . . ? N2L Fe2 N1 96.87(10) . . ? N3 Fe2 N1 86.97(8) . . ? N4 Fe2 N1 71.73(8) . . ? N6 Fe2 Fe3 106.18(7) . . ? N2L Fe2 Fe3 144.77(8) . . ? N3 Fe2 Fe3 92.83(6) . . ? N4 Fe2 Fe3 56.01(6) . . ? N1 Fe2 Fe3 51.13(6) . . ? N6 Fe2 Fe1 55.81(6) . . ? N2L Fe2 Fe1 150.41(8) . . ? N3 Fe2 Fe1 52.52(6) . . ? N4 Fe2 Fe1 105.07(6) . . ? N1 Fe2 Fe1 93.73(6) . . ? Fe3 Fe2 Fe1 58.797(18) . . ? N1 Fe3 N2 89.14(9) . . ? N1 Fe3 N3L 112.21(10) . . ? N2 Fe3 N3L 112.14(10) . . ? N1 Fe3 N5 149.59(9) . . ? N2 Fe3 N5 71.71(8) . . ? N3L Fe3 N5 97.07(9) . . ? N1 Fe3 N4 71.67(9) . . ? N2 Fe3 N4 150.19(9) . . ? N3L Fe3 N4 96.43(9) . . ? N5 Fe3 N4 114.33(8) . . ? N1 Fe3 Fe1 98.00(7) . . ? N2 Fe3 Fe1 55.42(6) . . ? N3L Fe3 Fe1 147.76(7) . . ? N5 Fe3 Fe1 51.74(6) . . ? N4 Fe3 Fe1 103.77(6) . . ? N1 Fe3 Fe2 54.89(7) . . ? N2 Fe3 Fe2 98.09(7) . . ? N3L Fe3 Fe2 147.57(7) . . ? N5 Fe3 Fe2 103.54(6) . . ? N4 Fe3 Fe2 52.27(6) . . ? Fe1 Fe3 Fe2 60.90(2) . . ? C6 N1 C3 114.2(2) . . ? C6 N1 Fe3 109.75(18) . . ? C3 N1 Fe3 126.64(18) . . ? C6 N1 Fe2 102.96(17) . . ? C3 N1 Fe2 121.43(18) . . ? Fe3 N1 Fe2 73.98(7) . . ? C49 N1L C45 117.2(3) . . ? C49 N1L Fe1 117.7(2) . . ? C45 N1L Fe1 122.7(2) . . ? C18 N2 C4 114.3(2) . . ? C18 N2 Fe3 108.47(17) . . ? C4 N2 Fe3 123.14(18) . . ? C18 N2 Fe1 104.28(17) . . ? C4 N2 Fe1 126.62(18) . . ? Fe3 N2 Fe1 72.66(7) . . ? C54 N2L C50 117.2(3) . . ? C54 N2L Fe2 118.7(2) . . ? C50 N2L Fe2 123.8(2) . . ? C30 N3 C5 113.9(2) . . ? C30 N3 Fe1 100.33(16) . . ? C5 N3 Fe1 121.78(18) . . ? C30 N3 Fe2 110.98(16) . . ? C5 N3 Fe2 126.88(17) . . ? Fe1 N3 Fe2 74.70(7) . . ? C59 N3L C55 117.0(3) . . ? C59 N3L Fe3 119.3(2) . . ? C55 N3L Fe3 123.0(2) . . ? C11 N4 C12 113.6(2) . . ? C11 N4 Fe2 104.72(17) . . ? C12 N4 Fe2 129.88(18) . . ? C11 N4 Fe3 103.58(17) . . ? C12 N4 Fe3 125.13(18) . . ? Fe2 N4 Fe3 71.72(7) . . ? C23 N5 C24 117.1(2) . . ? C23 N5 Fe1 105.12(17) . . ? C24 N5 Fe1 115.51(18) . . ? C23 N5 Fe3 103.47(17) . . ? C24 N5 Fe3 133.38(18) . . ? Fe1 N5 Fe3 71.36(7) . . ? C35 N6 C36 114.6(2) . . ? C35 N6 Fe2 110.15(16) . . ? C36 N6 Fe2 116.97(17) . . ? C35 N6 Fe1 97.02(16) . . ? C36 N6 Fe1 138.05(19) . . ? Fe2 N6 Fe1 72.50(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C4 112.4(2) . . ? C3 C2 C5 113.5(2) . . ? C4 C2 C5 112.0(2) . . ? C3 C2 C1 106.1(2) . . ? C4 C2 C1 106.3(2) . . ? C5 C2 C1 105.8(2) . . ? N1 C3 C2 116.2(2) . . ? N1 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? N1 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C2 115.3(2) . . ? N2 C4 H4A 108.4 . . ? C2 C4 H4A 108.4 . . ? N2 C4 H4B 108.4 . . ? C2 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C2 117.2(2) . . ? N3 C5 H5A 108.0 . . ? C2 C5 H5A 108.0 . . ? N3 C5 H5B 108.0 . . ? C2 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C7 C6 N1 126.4(3) . . ? C7 C6 C11 119.4(3) . . ? N1 C6 C11 114.2(2) . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C6 119.5(3) . . ? C10 C11 N4 126.3(3) . . ? C6 C11 N4 114.1(2) . . ? C13 C12 C17 117.6(3) . . ? C13 C12 N4 121.5(3) . . ? C17 C12 N4 120.9(3) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C16 118.8(3) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C16 C17 C12 120.8(3) . . ? C16 C17 H17A 119.6 . . ? C12 C17 H17A 119.6 . . ? C19 C18 N2 126.9(3) . . ? C19 C18 C23 119.5(3) . . ? N2 C18 C23 113.6(2) . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.7(3) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 119.3(3) . . ? C22 C23 N5 126.0(3) . . ? C18 C23 N5 114.8(2) . . ? C25 C24 C29 117.9(3) . . ? C25 C24 N5 120.7(3) . . ? C29 C24 N5 121.4(3) . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C29 C24 120.8(3) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? C31 C30 N3 127.7(3) . . ? C31 C30 C35 119.0(3) . . ? N3 C30 C35 113.2(2) . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 120.1(3) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 N6 125.2(2) . . ? C34 C35 C30 119.6(2) . . ? N6 C35 C30 114.8(2) . . ? C37 C36 C41 118.0(3) . . ? C37 C36 N6 122.2(3) . . ? C41 C36 N6 119.8(3) . . ? C36 C37 C38 120.2(3) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C39 C38 C37 121.3(3) . . ? C39 C38 H38A 119.3 . . ? C37 C38 H38A 119.3 . . ? C38 C39 C40 119.1(3) . . ? C38 C39 H39A 120.5 . . ? C40 C39 H39A 120.5 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C40 C41 C36 121.0(3) . . ? C40 C41 H41A 119.5 . . ? C36 C41 H41A 119.5 . . ? N1L C45 C46 121.8(3) . . ? N1L C45 H45A 119.1 . . ? C46 C45 H45A 119.1 . . ? C47 C46 C45 120.0(4) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C48 C47 C46 118.8(4) . . ? C48 C47 H47A 120.6 . . ? C46 C47 H47A 120.6 . . ? C47 C48 C49 118.6(4) . . ? C47 C48 H48A 120.7 . . ? C49 C48 H48A 120.7 . . ? N1L C49 C48 123.6(3) . . ? N1L C49 H49A 118.2 . . ? C48 C49 H49A 118.2 . . ? N2L C50 C51 122.6(4) . . ? N2L C50 H50A 118.7 . . ? C51 C50 H50A 118.7 . . ? C52 C51 C50 118.8(4) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? C53 C52 C51 118.9(4) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C54 C53 C52 118.7(4) . . ? C54 C53 H53A 120.7 . . ? C52 C53 H53A 120.7 . . ? N2L C54 C53 123.8(4) . . ? N2L C54 H54A 118.1 . . ? C53 C54 H54A 118.1 . . ? N3L C55 C56 122.8(3) . . ? N3L C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C57 C56 C55 119.5(4) . . ? C57 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? C56 C57 C58 118.8(4) . . ? C56 C57 H57A 120.6 . . ? C58 C57 H57A 120.6 . . ? C57 C58 C59 119.0(4) . . ? C57 C58 H58A 120.5 . . ? C59 C58 H58A 120.5 . . ? N3L C59 C58 122.9(4) . . ? N3L C59 H59A 118.5 . . ? C58 C59 H59A 118.5 . . ? C61 C60 C65 120.0 . . ? C61 C60 H60A 120.0 . . ? C65 C60 H60A 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61A 120.0 . . ? C62 C61 H61A 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 H65A 120.0 . . ? C60 C65 H65A 120.0 . . ? C71 C70 C75 120.0 . . ? C71 C70 H70A 120.0 . . ? C75 C70 H70A 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71A 120.0 . . ? C70 C71 H71A 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C74 C75 C70 120.0 . . ? C74 C75 H75A 120.0 . . ? C70 C75 H75A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.385 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.053 #=============the end of compound 300K=================== # Attachment '- combinedcif.txt' #============compound Fe3Lthf3================================ data_Fe3Lthf3 _database_code_depnum_ccdc_archive 'CCDC 836229' #TrackingRef '- combinedcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H74 Fe3 N6 O4.75' _chemical_formula_weight 1122.80 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.1077(18) _cell_length_b 15.5695(13) _cell_length_c 33.842(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.773(6) _cell_angle_gamma 90.00 _cell_volume 10991.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 10337 _cell_measurement_theta_min 4.3365 _cell_measurement_theta_max 24.118 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7419 _exptl_absorpt_correction_T_max 0.9674 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57662 _diffrn_reflns_av_R_equivalents 0.1105 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.21 _reflns_number_total 9764 _reflns_number_gt 5159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 XP _computing_publication_material XCIF _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^)+(0.0798P)^2^+27.8181P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9764 _refine_ls_number_parameters 738 _refine_ls_number_restraints 342 _refine_ls_R_factor_all 0.1473 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.20982(4) 0.41490(5) 0.37129(2) 0.0280(2) Uani 1 1 d . A . Fe2 Fe 0.19459(4) 0.54925(5) 0.40562(2) 0.0262(2) Uani 1 1 d . A . Fe3 Fe 0.22730(4) 0.55401(5) 0.33697(2) 0.0288(2) Uani 1 1 d D . . N1 N 0.1436(2) 0.6153(3) 0.35455(13) 0.0273(11) Uani 1 1 d . A . N2 N 0.1622(2) 0.4488(3) 0.31385(13) 0.0297(11) Uani 1 1 d . A . N3 N 0.1236(2) 0.4502(3) 0.39496(13) 0.0271(11) Uani 1 1 d . . . N4 N 0.2595(2) 0.6432(3) 0.38565(13) 0.0252(11) Uani 1 1 d . A . N5 N 0.2832(2) 0.4374(3) 0.33408(13) 0.0320(12) Uani 1 1 d . A . N6 N 0.2365(2) 0.4372(3) 0.43601(13) 0.0240(11) Uani 1 1 d . . . C1 C -0.0139(3) 0.5056(4) 0.31251(18) 0.0394(16) Uani 1 1 d . B . H1B H -0.0183 0.5352 0.2867 0.059 Uiso 1 1 calc R . . H1A H -0.0392 0.5358 0.3302 0.059 Uiso 1 1 calc R . . H1C H -0.0295 0.4465 0.3085 0.059 Uiso 1 1 calc R . . C2 C 0.0573(2) 0.5046(4) 0.33177(16) 0.0286(14) Uani 1 1 d . . . C3 C 0.0774(3) 0.5986(4) 0.33704(17) 0.0307(14) Uani 1 1 d . A . H3A H 0.0694 0.6266 0.3105 0.037 Uiso 1 1 calc R . . H3B H 0.0491 0.6267 0.3540 0.037 Uiso 1 1 calc R . . C4 C 0.0929(3) 0.4586(4) 0.30218(17) 0.0340(15) Uani 1 1 d . A . H4B H 0.0739 0.4007 0.2973 0.041 Uiso 1 1 calc R . . H4A H 0.0852 0.4902 0.2765 0.041 Uiso 1 1 calc R . . C5 C 0.0603(3) 0.4570(4) 0.37113(16) 0.0291(14) Uani 1 1 d . B . H5B H 0.0315 0.4862 0.3873 0.035 Uiso 1 1 calc R . . H5A H 0.0434 0.3982 0.3654 0.035 Uiso 1 1 calc R . . C6 C 0.1574(3) 0.7025(4) 0.36068(16) 0.0298(14) Uani 1 1 d . . . C7 C 0.1159(3) 0.7714(4) 0.35211(17) 0.0332(14) Uani 1 1 d . B . H7 H 0.0728 0.7616 0.3402 0.040 Uiso 1 1 calc R . . C8 C 0.1374(3) 0.8550(4) 0.36101(19) 0.0391(16) Uani 1 1 d . . . H8 H 0.1086 0.9018 0.3548 0.047 Uiso 1 1 calc R B . C9 C 0.1983(3) 0.8705(4) 0.37825(19) 0.0408(16) Uani 1 1 d . B . H9 H 0.2119 0.9278 0.3845 0.049 Uiso 1 1 calc R . . C10 C 0.2415(3) 0.8022(4) 0.38696(17) 0.0346(15) Uani 1 1 d . . . H10 H 0.2845 0.8130 0.3990 0.041 Uiso 1 1 calc R B . C11 C 0.2212(3) 0.7192(3) 0.37785(15) 0.0255(13) Uani 1 1 d . A . C12 C 0.3267(2) 0.6584(3) 0.39475(16) 0.0251(13) Uani 1 1 d . . . C13 C 0.3596(3) 0.6997(4) 0.36705(18) 0.0372(15) Uani 1 1 d . B . H13 H 0.3363 0.7188 0.3424 0.045 Uiso 1 1 calc R . . C14 C 0.4240(3) 0.7130(4) 0.3747(2) 0.0442(17) Uani 1 1 d . . . H14 H 0.4450 0.7410 0.3554 0.053 Uiso 1 1 calc R B . C15 C 0.4592(3) 0.6864(4) 0.4102(2) 0.0425(17) Uani 1 1 d . B . H15 H 0.5043 0.6950 0.4155 0.051 Uiso 1 1 calc R . . C16 C 0.4276(3) 0.6468(4) 0.43804(19) 0.0404(16) Uani 1 1 d . . . H16 H 0.4514 0.6284 0.4627 0.049 Uiso 1 1 calc R B . C17 C 0.3618(3) 0.6330(4) 0.43092(17) 0.0306(14) Uani 1 1 d . B . H17 H 0.3409 0.6063 0.4507 0.037 Uiso 1 1 calc R . . C18 C 0.1939(3) 0.4129(4) 0.28410(16) 0.0319(14) Uani 1 1 d . . . C19 C 0.1665(3) 0.3878(4) 0.24596(18) 0.0446(17) Uani 1 1 d . B . H19 H 0.1213 0.3905 0.2384 0.053 Uiso 1 1 calc R . . C20 C 0.2050(4) 0.3583(4) 0.21849(19) 0.0479(18) Uani 1 1 d . . . H20 H 0.1860 0.3423 0.1922 0.058 Uiso 1 1 calc R B . C21 C 0.2696(4) 0.3528(4) 0.2295(2) 0.0525(19) Uani 1 1 d . B . H21 H 0.2956 0.3326 0.2109 0.063 Uiso 1 1 calc R . . C22 C 0.2977(3) 0.3762(4) 0.26760(18) 0.0393(16) Uani 1 1 d . . . H22 H 0.3428 0.3720 0.2749 0.047 Uiso 1 1 calc R B . C23 C 0.2605(3) 0.4058(4) 0.29525(17) 0.0308(14) Uani 1 1 d . A . C24 C 0.3476(3) 0.4141(4) 0.34940(16) 0.0308(14) Uani 1 1 d . . . C25 C 0.3642(3) 0.3276(4) 0.35482(17) 0.0365(15) Uani 1 1 d . B . H25 H 0.3329 0.2843 0.3474 0.044 Uiso 1 1 calc R . . C26 C 0.4258(3) 0.3048(4) 0.37087(18) 0.0448(17) Uani 1 1 d . . . H26 H 0.4366 0.2457 0.3737 0.054 Uiso 1 1 calc R B . C27 C 0.4727(3) 0.3662(5) 0.3830(2) 0.0512(19) Uani 1 1 d . B . H27 H 0.5146 0.3495 0.3949 0.061 Uiso 1 1 calc R . . C28 C 0.4570(3) 0.4516(5) 0.3774(2) 0.0495(18) Uani 1 1 d . . . H28 H 0.4886 0.4944 0.3850 0.059 Uiso 1 1 calc R B . C29 C 0.3948(3) 0.4759(4) 0.36068(18) 0.0378(16) Uani 1 1 d . B . H29 H 0.3847 0.5350 0.3569 0.045 Uiso 1 1 calc R . . C30 C 0.1254(3) 0.3996(3) 0.42934(16) 0.0277(13) Uani 1 1 d . B . C31 C 0.0750(3) 0.3565(4) 0.44244(17) 0.0312(14) Uani 1 1 d . . . H31 H 0.0330 0.3621 0.4279 0.037 Uiso 1 1 calc R B . C32 C 0.0847(3) 0.3050(4) 0.47655(17) 0.0352(15) Uani 1 1 d . B . H32 H 0.0498 0.2756 0.4851 0.042 Uiso 1 1 calc R . . C33 C 0.1453(3) 0.2972(4) 0.49764(17) 0.0354(15) Uani 1 1 d . . . H33 H 0.1523 0.2612 0.5206 0.042 Uiso 1 1 calc R B . C34 C 0.1966(3) 0.3413(3) 0.48602(17) 0.0304(14) Uani 1 1 d . B . H34 H 0.2381 0.3356 0.5012 0.036 Uiso 1 1 calc R . . C35 C 0.1875(3) 0.3936(3) 0.45227(16) 0.0272(14) Uani 1 1 d . B . C36 C 0.2952(3) 0.4475(3) 0.46282(16) 0.0266(13) Uani 1 1 d . B . C37 C 0.2962(3) 0.4924(3) 0.49847(16) 0.0293(14) Uani 1 1 d . . . H37 H 0.2574 0.5151 0.5051 0.035 Uiso 1 1 calc R B . C38 C 0.3525(3) 0.5045(4) 0.52428(17) 0.0369(15) Uani 1 1 d . B . H38 H 0.3520 0.5345 0.5487 0.044 Uiso 1 1 calc R . . C39 C 0.4097(3) 0.4731(4) 0.51491(19) 0.0431(17) Uani 1 1 d . . . H39 H 0.4486 0.4820 0.5326 0.052 Uiso 1 1 calc R B . C40 C 0.4097(3) 0.4288(4) 0.47960(19) 0.0406(17) Uani 1 1 d . B . H40 H 0.4488 0.4069 0.4730 0.049 Uiso 1 1 calc R . . C41 C 0.3528(3) 0.4157(4) 0.45353(17) 0.0305(14) Uani 1 1 d . . . H41 H 0.3533 0.3851 0.4293 0.037 Uiso 1 1 calc R B . O1 O 0.2055(2) 0.2770(2) 0.37306(12) 0.0397(11) Uani 1 1 d . . . C1L C 0.1443(3) 0.2372(4) 0.3573(2) 0.0525(19) Uani 0.578(12) 1 d PD A 1 H1LA H 0.1376 0.2383 0.3277 0.063 Uiso 0.578(12) 1 calc PR A 1 H1LB H 0.1088 0.2689 0.3667 0.063 Uiso 0.578(12) 1 calc PR A 1 C2L C 0.1458(8) 0.1454(8) 0.3721(4) 0.056(3) Uani 0.578(12) 1 d PD A 1 H2LA H 0.1645 0.1057 0.3541 0.067 Uiso 0.578(12) 1 calc PR A 1 H2LB H 0.1028 0.1248 0.3759 0.067 Uiso 0.578(12) 1 calc PR A 1 C3L C 0.1911(6) 0.1588(8) 0.4129(4) 0.056(3) Uani 0.578(12) 1 d PD A 1 H3LA H 0.1672 0.1829 0.4333 0.067 Uiso 0.578(12) 1 calc PR A 1 H3LB H 0.2112 0.1039 0.4229 0.067 Uiso 0.578(12) 1 calc PR A 1 C4L C 0.2415(3) 0.2221(4) 0.40282(19) 0.0464(18) Uani 0.578(12) 1 d PD A 1 H4LA H 0.2602 0.2554 0.4267 0.056 Uiso 0.578(12) 1 calc PR A 1 H4LB H 0.2764 0.1920 0.3919 0.056 Uiso 0.578(12) 1 calc PR A 1 C1M C 0.1443(3) 0.2372(4) 0.3573(2) 0.0525(19) Uani 0.422(12) 1 d PD A 2 H1MA H 0.1424 0.2214 0.3288 0.063 Uiso 0.422(12) 1 calc PR A 2 H1MB H 0.1080 0.2757 0.3602 0.063 Uiso 0.422(12) 1 calc PR A 2 C2M C 0.1441(10) 0.1569(10) 0.3839(6) 0.056(3) Uani 0.422(12) 1 d PD A 2 H2MA H 0.1199 0.1096 0.3690 0.067 Uiso 0.422(12) 1 calc PR A 2 H2MB H 0.1245 0.1699 0.4080 0.067 Uiso 0.422(12) 1 calc PR A 2 C3M C 0.2160(8) 0.1322(9) 0.3957(6) 0.056(3) Uani 0.422(12) 1 d PD A 2 H3MA H 0.2236 0.0965 0.4201 0.067 Uiso 0.422(12) 1 calc PR A 2 H3MB H 0.2335 0.1032 0.3737 0.067 Uiso 0.422(12) 1 calc PR A 2 C4M C 0.2415(3) 0.2221(4) 0.40282(19) 0.0464(18) Uani 0.422(12) 1 d PD A 2 H4MA H 0.2363 0.2415 0.4300 0.056 Uiso 0.422(12) 1 calc PR A 2 H4MB H 0.2877 0.2239 0.4004 0.056 Uiso 0.422(12) 1 calc PR A 2 O2 O 0.16055(18) 0.6140(2) 0.45457(11) 0.0360(10) Uani 1 1 d . . . C5L C 0.0910(3) 0.6233(4) 0.4514(2) 0.0490(18) Uani 1 1 d . B . H5LA H 0.0724 0.5743 0.4644 0.059 Uiso 1 1 calc R . . H5LB H 0.0709 0.6259 0.4230 0.059 Uiso 1 1 calc R . . C6L C 0.0808(3) 0.7061(5) 0.4725(2) 0.056(2) Uani 1 1 d . . . H6LA H 0.0423 0.7367 0.4590 0.067 Uiso 1 1 calc R B . H6LB H 0.0760 0.6957 0.5008 0.067 Uiso 1 1 calc R . . C7L C 0.1409(3) 0.7559(4) 0.4695(2) 0.0517(19) Uani 1 1 d . B . H7LA H 0.1385 0.7841 0.4431 0.062 Uiso 1 1 calc R . . H7LB H 0.1490 0.8000 0.4908 0.062 Uiso 1 1 calc R . . C8L C 0.1911(3) 0.6881(4) 0.47483(18) 0.0410(16) Uani 1 1 d . B . H8LA H 0.2289 0.7058 0.4627 0.049 Uiso 1 1 calc R . . H8LB H 0.2050 0.6758 0.5035 0.049 Uiso 1 1 calc R . . O3L O 0.2456(2) 0.6120(3) 0.28379(12) 0.0482(11) Uani 0.43(4) 1 d PDU B 1 C9L C 0.1859(11) 0.627(4) 0.2553(6) 0.057(4) Uani 0.43(4) 1 d PDU B 1 H9LA H 0.1679 0.6846 0.2595 0.068 Uiso 0.43(4) 1 calc PR B 1 H9LB H 0.1532 0.5830 0.2583 0.068 Uiso 0.43(4) 1 calc PR B 1 C10L C 0.2074(16) 0.621(2) 0.2136(7) 0.066(5) Uani 0.43(4) 1 d PDU B 1 H10A H 0.1778 0.5837 0.1957 0.079 Uiso 0.43(4) 1 calc PR B 1 H10B H 0.2077 0.6787 0.2013 0.079 Uiso 0.43(4) 1 calc PR B 1 C11L C 0.2700(15) 0.5857(19) 0.2198(8) 0.071(5) Uani 0.43(4) 1 d PDU B 1 H11A H 0.2957 0.6102 0.2004 0.085 Uiso 0.43(4) 1 calc PR B 1 H11B H 0.2679 0.5226 0.2161 0.085 Uiso 0.43(4) 1 calc PR B 1 C12L C 0.3001(10) 0.608(4) 0.2619(8) 0.052(4) Uani 0.43(4) 1 d PDU B 1 H12A H 0.3307 0.5626 0.2731 0.063 Uiso 0.43(4) 1 calc PR B 1 H12B H 0.3227 0.6634 0.2628 0.063 Uiso 0.43(4) 1 calc PR B 1 O3M O 0.2456(2) 0.6120(3) 0.28379(12) 0.0482(11) Uani 0.57(4) 1 d PDU B 2 C9M C 0.1956(9) 0.629(3) 0.2490(5) 0.057(4) Uani 0.57(4) 1 d PDU B 2 H9MA H 0.1692 0.6797 0.2539 0.068 Uiso 0.57(4) 1 calc PR B 2 H9MB H 0.1673 0.5790 0.2426 0.068 Uiso 0.57(4) 1 calc PR B 2 C10M C 0.2347(13) 0.6478(14) 0.2150(5) 0.063(4) Uani 0.57(4) 1 d PDU B 2 H10C H 0.2116 0.6268 0.1892 0.075 Uiso 0.57(4) 1 calc PR B 2 H10D H 0.2423 0.7102 0.2128 0.075 Uiso 0.57(4) 1 calc PR B 2 C11M C 0.2937(12) 0.6037(15) 0.2250(6) 0.071(4) Uani 0.57(4) 1 d PDU B 2 H11C H 0.3280 0.6320 0.2128 0.085 Uiso 0.57(4) 1 calc PR B 2 H11D H 0.2897 0.5433 0.2158 0.085 Uiso 0.57(4) 1 calc PR B 2 C12M C 0.3079(7) 0.608(3) 0.2698(6) 0.049(4) Uani 0.57(4) 1 d PDU B 2 H12C H 0.3320 0.5564 0.2807 0.059 Uiso 0.57(4) 1 calc PR B 2 H12D H 0.3338 0.6596 0.2785 0.059 Uiso 0.57(4) 1 calc PR B 2 O1S O 0.3714(14) 0.0883(19) 0.3867(8) 0.0778(17) Uani 0.30(3) 1 d PDU C 1 C1S C 0.4225(18) 0.091(3) 0.4183(10) 0.0776(17) Uani 0.30(3) 1 d PDU C 1 H1SB H 0.4222 0.1465 0.4324 0.093 Uiso 0.30(3) 1 calc PR C 1 H1SA H 0.4635 0.0862 0.4077 0.093 Uiso 0.30(3) 1 calc PR C 1 C2S C 0.418(2) 0.018(4) 0.4475(11) 0.0774(17) Uani 0.30(3) 1 d PDU C 1 H2SB H 0.4556 -0.0198 0.4496 0.093 Uiso 0.30(3) 1 calc PR C 1 H2SA H 0.4135 0.0405 0.4743 0.093 Uiso 0.30(3) 1 calc PR C 1 C3S C 0.3573(18) -0.028(2) 0.4288(9) 0.0774(17) Uani 0.30(3) 1 d PDU C 1 H3SA H 0.3204 -0.0129 0.4423 0.093 Uiso 0.30(3) 1 calc PR C 1 H3SB H 0.3634 -0.0914 0.4300 0.093 Uiso 0.30(3) 1 calc PR C 1 C4S C 0.348(2) 0.004(2) 0.3860(8) 0.0775(17) Uani 0.30(3) 1 d PDU C 1 H4SA H 0.3717 -0.0333 0.3695 0.093 Uiso 0.30(3) 1 calc PR C 1 H4SB H 0.3019 0.0024 0.3745 0.093 Uiso 0.30(3) 1 calc PR C 1 O1P O 0.3829(6) 0.0579(9) 0.3864(3) 0.0780(17) Uani 0.70(3) 1 d PDU C 2 C1P C 0.4100(10) 0.0872(12) 0.4242(4) 0.0776(17) Uani 0.70(3) 1 d PDU C 2 H1PB H 0.3833 0.1336 0.4330 0.093 Uiso 0.70(3) 1 calc PR C 2 H1PA H 0.4534 0.1104 0.4232 0.093 Uiso 0.70(3) 1 calc PR C 2 C2P C 0.4140(12) 0.0125(15) 0.4533(5) 0.0773(17) Uani 0.70(3) 1 d PDU C 2 H2PB H 0.4589 -0.0072 0.4607 0.093 Uiso 0.70(3) 1 calc PR C 2 H2PA H 0.3970 0.0289 0.4779 0.093 Uiso 0.70(3) 1 calc PR C 2 C3P C 0.3732(9) -0.0569(10) 0.4308(4) 0.0774(17) Uani 0.70(3) 1 d PDU C 2 H3PA H 0.3936 -0.1140 0.4355 0.093 Uiso 0.70(3) 1 calc PR C 2 H3PB H 0.3300 -0.0588 0.4389 0.093 Uiso 0.70(3) 1 calc PR C 2 C4P C 0.3693(9) -0.0306(11) 0.3880(4) 0.0773(17) Uani 0.70(3) 1 d PDU C 2 H4PA H 0.4005 -0.0639 0.3751 0.093 Uiso 0.70(3) 1 calc PR C 2 H4PB H 0.3258 -0.0424 0.3734 0.093 Uiso 0.70(3) 1 calc PR C 2 O2S O 0.5000 0.2150(6) 0.2500 0.0970(18) Uani 1 2 d SD . . C5S C 0.4569(4) 0.2662(6) 0.2655(3) 0.0970(18) Uani 1 1 d D . . H5SA H 0.4571 0.2517 0.2941 0.116 Uiso 1 1 calc R . . H5SB H 0.4132 0.2558 0.2510 0.116 Uiso 1 1 calc R . . C6S C 0.4738(4) 0.3571(6) 0.2619(3) 0.0970(18) Uani 1 1 d D . . H6SA H 0.4368 0.3901 0.2482 0.116 Uiso 1 1 calc R . . H6SB H 0.4879 0.3827 0.2885 0.116 Uiso 1 1 calc R . . O3S O 0.0000 0.2285(12) 0.2500 0.131(5) Uani 0.50 2 d SPD . . C7S C 0.0178(12) 0.1793(11) 0.2816(6) 0.131(5) Uani 0.50 1 d PD . . H7SA H -0.0083 0.1923 0.3028 0.157 Uiso 0.50 1 calc PR . . H7SB H 0.0635 0.1895 0.2924 0.157 Uiso 0.50 1 calc PR . . C8S C 0.0088(13) 0.0967(11) 0.2694(6) 0.131(5) Uani 0.50 1 d PD . . H8SA H 0.0491 0.0637 0.2764 0.157 Uiso 0.50 1 calc PR . . H8SB H -0.0247 0.0695 0.2827 0.157 Uiso 0.50 1 calc PR . . 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 0.0341(5) 0.0293(5) 0.0203(5) -0.0001(4) 0.0029(4) -0.0015(4) Fe2 0.0303(5) 0.0258(5) 0.0223(5) 0.0022(4) 0.0031(4) -0.0019(4) Fe3 0.0363(5) 0.0282(5) 0.0221(5) -0.0015(4) 0.0049(4) 0.0015(4) N1 0.029(3) 0.027(3) 0.025(3) 0.001(2) 0.001(2) 0.001(2) N2 0.035(3) 0.031(3) 0.022(3) -0.003(2) 0.002(2) -0.002(2) N3 0.028(3) 0.030(3) 0.021(3) 0.001(2) -0.001(2) -0.002(2) N4 0.027(3) 0.023(3) 0.025(3) 0.000(2) 0.003(2) 0.000(2) N5 0.039(3) 0.034(3) 0.022(3) -0.003(2) 0.001(2) 0.003(2) N6 0.026(3) 0.028(3) 0.018(3) 0.004(2) 0.004(2) -0.001(2) C1 0.033(3) 0.051(4) 0.031(4) -0.004(3) -0.005(3) -0.002(3) C2 0.026(3) 0.036(4) 0.023(3) 0.000(3) -0.002(2) -0.004(3) C3 0.032(3) 0.031(3) 0.028(3) 0.002(3) 0.002(3) 0.003(3) C4 0.034(3) 0.042(4) 0.023(3) -0.006(3) -0.006(3) -0.002(3) C5 0.029(3) 0.027(3) 0.031(3) -0.002(3) 0.003(3) -0.002(3) C6 0.033(3) 0.033(4) 0.023(3) 0.002(3) 0.002(3) 0.006(3) C7 0.033(3) 0.032(4) 0.035(4) 0.005(3) 0.006(3) 0.000(3) C8 0.042(4) 0.029(4) 0.050(4) 0.007(3) 0.018(3) 0.013(3) C9 0.051(4) 0.023(3) 0.051(5) 0.001(3) 0.018(3) -0.001(3) C10 0.040(4) 0.028(4) 0.036(4) -0.003(3) 0.006(3) 0.000(3) C11 0.033(4) 0.026(3) 0.018(3) 0.001(2) 0.006(3) 0.004(3) C12 0.025(3) 0.023(3) 0.027(3) 0.001(3) 0.004(3) -0.004(2) C13 0.042(4) 0.043(4) 0.027(4) 0.008(3) 0.004(3) -0.006(3) C14 0.046(4) 0.039(4) 0.052(5) 0.001(3) 0.022(4) -0.013(3) C15 0.024(3) 0.045(4) 0.057(5) -0.003(4) 0.002(3) -0.009(3) C16 0.042(4) 0.035(4) 0.040(4) -0.006(3) -0.008(3) 0.000(3) C17 0.030(3) 0.034(4) 0.027(4) -0.001(3) 0.004(3) -0.007(3) C18 0.051(4) 0.028(3) 0.015(3) 0.000(3) 0.001(3) 0.002(3) C19 0.068(5) 0.038(4) 0.025(4) -0.007(3) -0.003(3) 0.005(3) C20 0.080(6) 0.042(4) 0.019(4) -0.009(3) -0.001(4) 0.012(4) C21 0.086(6) 0.046(4) 0.030(4) 0.001(3) 0.022(4) 0.021(4) C22 0.052(4) 0.036(4) 0.032(4) 0.002(3) 0.012(3) 0.012(3) C23 0.043(4) 0.024(3) 0.026(4) 0.002(3) 0.007(3) 0.005(3) C24 0.042(4) 0.035(4) 0.018(3) 0.003(3) 0.012(3) 0.008(3) C25 0.041(4) 0.040(4) 0.029(4) 0.001(3) 0.007(3) 0.002(3) C26 0.060(5) 0.042(4) 0.035(4) 0.005(3) 0.020(3) 0.019(4) C27 0.046(4) 0.064(5) 0.045(5) 0.004(4) 0.011(3) 0.015(4) C28 0.041(4) 0.066(5) 0.043(4) -0.011(4) 0.012(3) -0.005(4) C29 0.040(4) 0.039(4) 0.036(4) 0.001(3) 0.010(3) 0.009(3) C30 0.038(4) 0.024(3) 0.021(3) -0.004(3) 0.005(3) -0.002(3) C31 0.032(3) 0.029(3) 0.031(4) -0.001(3) 0.001(3) -0.009(3) C32 0.035(4) 0.041(4) 0.033(4) 0.005(3) 0.013(3) -0.010(3) C33 0.048(4) 0.035(4) 0.024(3) 0.008(3) 0.007(3) -0.008(3) C34 0.032(3) 0.031(3) 0.028(3) 0.004(3) 0.004(3) 0.000(3) C35 0.037(4) 0.025(3) 0.019(3) -0.005(3) 0.001(3) 0.000(3) C36 0.030(3) 0.024(3) 0.024(3) 0.005(3) -0.001(3) -0.005(3) C37 0.037(3) 0.028(3) 0.023(3) 0.002(3) 0.005(3) -0.004(3) C38 0.048(4) 0.038(4) 0.022(3) 0.002(3) -0.002(3) -0.011(3) C39 0.039(4) 0.055(4) 0.031(4) 0.010(3) -0.010(3) -0.011(3) C40 0.029(3) 0.050(4) 0.043(4) 0.014(3) 0.005(3) -0.003(3) C41 0.038(4) 0.032(3) 0.021(3) 0.001(3) 0.003(3) -0.003(3) O1 0.053(3) 0.028(2) 0.036(3) 0.002(2) -0.001(2) 0.000(2) C1L 0.057(5) 0.041(4) 0.055(5) -0.017(4) -0.006(4) -0.009(4) C2L 0.089(5) 0.038(4) 0.044(7) -0.003(4) 0.019(4) -0.015(4) C3L 0.089(5) 0.038(4) 0.044(7) -0.003(4) 0.019(4) -0.015(4) C4L 0.063(5) 0.033(4) 0.043(4) 0.006(3) 0.006(4) 0.010(3) C1M 0.057(5) 0.041(4) 0.055(5) -0.017(4) -0.006(4) -0.009(4) C2M 0.089(5) 0.038(4) 0.044(7) -0.003(4) 0.019(4) -0.015(4) C3M 0.089(5) 0.038(4) 0.044(7) -0.003(4) 0.019(4) -0.015(4) C4M 0.063(5) 0.033(4) 0.043(4) 0.006(3) 0.006(4) 0.010(3) O2 0.039(3) 0.035(2) 0.035(3) -0.0129(19) 0.0079(19) -0.0056(19) C5L 0.038(4) 0.056(5) 0.054(5) -0.016(4) 0.012(3) -0.007(3) C6L 0.056(5) 0.062(5) 0.053(5) -0.004(4) 0.015(4) 0.008(4) C7L 0.065(5) 0.043(4) 0.049(5) -0.015(3) 0.016(4) -0.005(4) C8L 0.047(4) 0.040(4) 0.035(4) -0.018(3) 0.003(3) -0.011(3) O3L 0.065(3) 0.051(3) 0.030(2) 0.011(2) 0.012(2) 0.001(2) C9L 0.079(8) 0.059(8) 0.029(8) 0.019(8) 0.003(7) 0.003(9) C10L 0.088(10) 0.077(10) 0.033(7) 0.018(8) 0.011(8) -0.013(9) C11L 0.097(11) 0.079(10) 0.039(8) 0.008(8) 0.021(9) -0.016(9) C12L 0.070(7) 0.063(8) 0.028(8) 0.010(9) 0.020(7) -0.007(8) O3M 0.065(3) 0.051(3) 0.030(2) 0.011(2) 0.012(2) 0.001(2) C9M 0.077(7) 0.053(7) 0.039(7) 0.015(8) 0.006(6) 0.004(7) C10M 0.102(10) 0.057(8) 0.030(6) 0.017(6) 0.010(7) -0.002(8) C11M 0.083(9) 0.093(9) 0.039(7) 0.011(7) 0.013(8) -0.021(8) C12M 0.071(7) 0.060(7) 0.021(7) 0.011(8) 0.024(6) -0.001(7) O1S 0.107(4) 0.059(4) 0.067(3) -0.006(3) 0.009(3) -0.018(3) C1S 0.106(4) 0.059(4) 0.067(3) -0.006(3) 0.009(3) -0.018(3) C2S 0.106(4) 0.059(4) 0.067(3) -0.007(3) 0.009(3) -0.018(3) C3S 0.106(4) 0.059(4) 0.066(3) -0.007(3) 0.009(3) -0.018(3) C4S 0.106(4) 0.059(4) 0.066(3) -0.007(3) 0.010(3) -0.018(3) O1P 0.107(4) 0.059(4) 0.067(3) -0.007(3) 0.010(3) -0.017(3) C1P 0.106(4) 0.059(4) 0.067(3) -0.007(3) 0.009(3) -0.018(3) C2P 0.106(4) 0.059(4) 0.066(3) -0.007(3) 0.009(3) -0.018(3) C3P 0.106(4) 0.059(4) 0.067(3) -0.007(3) 0.009(3) -0.018(3) C4P 0.106(4) 0.059(4) 0.066(3) -0.007(3) 0.010(3) -0.018(3) O2S 0.092(4) 0.096(4) 0.110(5) 0.000 0.039(3) 0.000 C5S 0.092(4) 0.096(4) 0.110(5) 0.000 0.039(3) 0.000 C6S 0.092(4) 0.096(4) 0.110(5) 0.000 0.039(3) 0.000 O3S 0.157(11) 0.072(9) 0.150(15) 0.000 -0.024(11) 0.000 C7S 0.157(11) 0.072(9) 0.150(15) 0.000 -0.024(11) 0.000 C8S 0.157(11) 0.072(9) 0.150(15) 0.000 -0.024(11) 0.000 _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 N2 2.114(4) . ? Fe1 O1 2.151(4) . ? Fe1 N3 2.169(5) . ? Fe1 N5 2.169(5) . ? Fe1 N6 2.204(4) . ? Fe1 Fe2 2.4377(11) . ? Fe1 Fe3 2.5114(11) . ? Fe2 N3 2.142(4) . ? Fe2 N6 2.146(4) . ? Fe2 N1 2.153(4) . ? Fe2 O2 2.154(4) . ? Fe2 N4 2.181(4) . ? Fe2 Fe3 2.5235(11) . ? Fe3 O3L 2.101(4) . ? Fe3 N1 2.169(5) . ? Fe3 N5 2.176(5) . ? Fe3 N4 2.182(4) . ? Fe3 N2 2.203(5) . ? N1 C6 1.398(7) . ? N1 C3 1.456(7) . ? N2 C18 1.406(7) . ? N2 C4 1.465(7) . ? N3 C30 1.401(7) . ? N3 C5 1.455(7) . ? N4 C12 1.425(7) . ? N4 C11 1.434(7) . ? N5 C23 1.417(7) . ? N5 C24 1.425(7) . ? N6 C35 1.415(7) . ? N6 C36 1.429(7) . ? C1 C2 1.545(7) . ? C1 H1B 0.9800 . ? C1 H1A 0.9800 . ? C1 H1C 0.9800 . ? C2 C5 1.518(7) . ? C2 C4 1.520(8) . ? C2 C3 1.526(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 H5B 0.9900 . ? C5 H5A 0.9900 . ? C6 C7 1.387(8) . ? C6 C11 1.407(7) . ? C7 C8 1.396(8) . ? C7 H7 0.9500 . ? C8 C9 1.350(8) . ? C8 H8 0.9500 . ? C9 C10 1.404(8) . ? C9 H9 0.9500 . ? C10 C11 1.381(8) . ? C10 H10 0.9500 . ? C12 C17 1.388(7) . ? C12 C13 1.405(8) . ? C13 C14 1.361(8) . ? C13 H13 0.9500 . ? C14 C15 1.377(9) . ? C14 H14 0.9500 . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 C17 1.389(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.388(8) . ? C18 C23 1.404(8) . ? C19 C20 1.402(9) . ? C19 H19 0.9500 . ? C20 C21 1.361(9) . ? C20 H20 0.9500 . ? C21 C22 1.384(9) . ? C21 H21 0.9500 . ? C22 C23 1.388(8) . ? C22 H22 0.9500 . ? C24 C29 1.397(8) . ? C24 C25 1.396(8) . ? C25 C26 1.377(8) . ? C25 H25 0.9500 . ? C26 C27 1.392(9) . ? C26 H26 0.9500 . ? C27 C28 1.377(9) . ? C27 H27 0.9500 . ? C28 C29 1.399(8) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.387(8) . ? C30 C35 1.422(7) . ? C31 C32 1.394(8) . ? C31 H31 0.9500 . ? C32 C33 1.371(8) . ? C32 H32 0.9500 . ? C33 C34 1.388(8) . ? C33 H33 0.9500 . ? C34 C35 1.392(7) . ? C34 H34 0.9500 . ? C36 C37 1.392(8) . ? C36 C41 1.392(8) . ? C37 C38 1.376(8) . ? C37 H37 0.9500 . ? C38 C39 1.385(9) . ? C38 H38 0.9500 . ? C39 C40 1.380(9) . ? C39 H39 0.9500 . ? C40 C41 1.392(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? O1 C4L 1.445(7) . ? O1 C1L 1.459(7) . ? C1L C2L 1.514(12) . ? C1L H1LA 0.9900 . ? C1L H1LB 0.9900 . ? C2L C3L 1.569(14) . ? C2L H2LA 0.9900 . ? C2L H2LB 0.9900 . ? C3L C4L 1.527(12) . ? C3L H3LA 0.9900 . ? C3L H3LB 0.9900 . ? C4L H4LA 0.9900 . ? C4L H4LB 0.9900 . ? C2M C3M 1.557(17) . ? C2M H2MA 0.9900 . ? C2M H2MB 0.9900 . ? C3M H3MA 0.9900 . ? C3M H3MB 0.9900 . ? O2 C8L 1.442(6) . ? O2 C5L 1.462(7) . ? C5L C6L 1.507(9) . ? C5L H5LA 0.9900 . ? C5L H5LB 0.9900 . ? C6L C7L 1.504(9) . ? C6L H6LA 0.9900 . ? C6L H6LB 0.9900 . ? C7L C8L 1.487(9) . ? C7L H7LA 0.9900 . ? C7L H7LB 0.9900 . ? C8L H8LA 0.9900 . ? C8L H8LB 0.9900 . ? O3L C12L 1.461(14) . ? O3L C9L 1.485(14) . ? C9L C10L 1.550(18) . ? C9L H9LA 0.9900 . ? C9L H9LB 0.9900 . ? C10L C11L 1.416(17) . ? C10L H10A 0.9900 . ? C10L H10B 0.9900 . ? C11L C12L 1.510(17) . ? C11L H11A 0.9900 . ? C11L H11B 0.9900 . ? C12L H12A 0.9900 . ? C12L H12B 0.9900 . ? C9M C10M 1.540(16) . ? C9M H9MA 0.9900 . ? C9M H9MB 0.9900 . ? C10M C11M 1.416(15) . ? C10M H10C 0.9900 . ? C10M H10D 0.9900 . ? C11M C12M 1.501(14) . ? C11M H11C 0.9900 . ? C11M H11D 0.9900 . ? C12M H12C 0.9900 . ? C12M H12D 0.9900 . ? O1S C1S 1.399(16) . ? O1S C4S 1.408(16) . ? C1S C2S 1.513(15) . ? C1S H1SB 0.9900 . ? C1S H1SA 0.9900 . ? C2S C3S 1.52(2) . ? C2S H2SB 0.9900 . ? C2S H2SA 0.9900 . ? C3S C4S 1.516(16) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? O1P C1P 1.396(12) . ? O1P C4P 1.411(10) . ? C1P C2P 1.519(12) . ? C1P H1PB 0.9900 . ? C1P H1PA 0.9900 . ? C2P C3P 1.514(14) . ? C2P H2PB 0.9900 . ? C2P H2PA 0.9900 . ? C3P C4P 1.496(12) . ? C3P H3PA 0.9900 . ? C3P H3PB 0.9900 . ? C4P H4PA 0.9900 . ? C4P H4PB 0.9900 . ? O2S C5S 1.374(9) . ? O2S C5S 1.374(9) 2_655 ? C5S C6S 1.470(11) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S C6S 1.461(16) 2_655 ? C6S H6SA 0.9900 . ? C6S H6SB 0.9900 . ? O3S C7S 1.322(16) . ? O3S C7S 1.323(16) 2 ? C7S C8S 1.356(18) . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C8S C8S 1.31(4) 2 ? C8S H8SA 0.9900 . ? C8S H8SB 0.9900 . ? 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 N2 Fe1 O1 105.03(17) . . ? N2 Fe1 N3 88.19(17) . . ? O1 Fe1 N3 101.64(17) . . ? N2 Fe1 N5 72.98(17) . . ? O1 Fe1 N5 102.37(17) . . ? N3 Fe1 N5 152.59(17) . . ? N2 Fe1 N6 152.57(17) . . ? O1 Fe1 N6 97.75(16) . . ? N3 Fe1 N6 72.20(16) . . ? N5 Fe1 N6 117.05(17) . . ? N2 Fe1 Fe2 98.33(13) . . ? O1 Fe1 Fe2 146.55(12) . . ? N3 Fe1 Fe2 55.05(12) . . ? N5 Fe1 Fe2 107.21(13) . . ? N6 Fe1 Fe2 54.80(11) . . ? N2 Fe1 Fe3 56.08(13) . . ? O1 Fe1 Fe3 152.12(12) . . ? N3 Fe1 Fe3 98.21(12) . . ? N5 Fe1 Fe3 54.82(12) . . ? N6 Fe1 Fe3 106.89(12) . . ? Fe2 Fe1 Fe3 61.29(3) . . ? N3 Fe2 N6 73.87(16) . . ? N3 Fe2 N1 87.55(17) . . ? N6 Fe2 N1 153.12(17) . . ? N3 Fe2 O2 99.18(16) . . ? N6 Fe2 O2 99.98(16) . . ? N1 Fe2 O2 102.07(16) . . ? N3 Fe2 N4 152.52(17) . . ? N6 Fe2 N4 117.51(16) . . ? N1 Fe2 N4 72.02(17) . . ? O2 Fe2 N4 102.88(16) . . ? N3 Fe2 Fe1 56.09(12) . . ? N6 Fe2 Fe1 57.06(12) . . ? N1 Fe2 Fe1 96.51(12) . . ? O2 Fe2 Fe1 148.42(11) . . ? N4 Fe2 Fe1 107.06(12) . . ? N3 Fe2 Fe3 98.57(12) . . ? N6 Fe2 Fe3 108.34(12) . . ? N1 Fe2 Fe3 54.58(12) . . ? O2 Fe2 Fe3 149.80(12) . . ? N4 Fe2 Fe3 54.69(12) . . ? Fe1 Fe2 Fe3 60.79(3) . . ? O3L Fe3 N1 108.04(17) . . ? O3L Fe3 N5 98.52(18) . . ? N1 Fe3 N5 148.16(18) . . ? O3L Fe3 N4 107.23(17) . . ? N1 Fe3 N4 71.68(17) . . ? N5 Fe3 N4 117.16(17) . . ? O3L Fe3 N2 101.62(17) . . ? N1 Fe3 N2 86.25(17) . . ? N5 Fe3 N2 71.16(17) . . ? N4 Fe3 N2 147.84(17) . . ? O3L Fe3 Fe1 145.67(13) . . ? N1 Fe3 Fe1 93.98(12) . . ? N5 Fe3 Fe1 54.56(13) . . ? N4 Fe3 Fe1 104.51(12) . . ? N2 Fe3 Fe1 52.81(12) . . ? O3L Fe3 Fe2 155.91(13) . . ? N1 Fe3 Fe2 53.98(12) . . ? N5 Fe3 Fe2 104.09(13) . . ? N4 Fe3 Fe2 54.63(12) . . ? N2 Fe3 Fe2 93.54(12) . . ? Fe1 Fe3 Fe2 57.92(3) . . ? C6 N1 C3 113.5(4) . . ? C6 N1 Fe2 106.1(3) . . ? C3 N1 Fe2 124.9(3) . . ? C6 N1 Fe3 107.9(3) . . ? C3 N1 Fe3 125.6(3) . . ? Fe2 N1 Fe3 71.44(14) . . ? C18 N2 C4 114.3(4) . . ? C18 N2 Fe1 110.4(3) . . ? C4 N2 Fe1 126.1(4) . . ? C18 N2 Fe3 102.2(3) . . ? C4 N2 Fe3 124.2(4) . . ? Fe1 N2 Fe3 71.11(14) . . ? C30 N3 C5 114.0(4) . . ? C30 N3 Fe2 109.6(3) . . ? C5 N3 Fe2 126.9(3) . . ? C30 N3 Fe1 104.2(3) . . ? C5 N3 Fe1 124.4(3) . . ? Fe2 N3 Fe1 68.86(13) . . ? C12 N4 C11 114.7(4) . . ? C12 N4 Fe2 134.1(3) . . ? C11 N4 Fe2 104.4(3) . . ? C12 N4 Fe3 117.0(3) . . ? C11 N4 Fe3 106.5(3) . . ? Fe2 N4 Fe3 70.68(13) . . ? C23 N5 C24 114.7(5) . . ? C23 N5 Fe1 108.1(4) . . ? C24 N5 Fe1 118.2(3) . . ? C23 N5 Fe3 102.9(3) . . ? C24 N5 Fe3 133.6(4) . . ? Fe1 N5 Fe3 70.61(15) . . ? C35 N6 C36 114.9(4) . . ? C35 N6 Fe2 107.7(3) . . ? C36 N6 Fe2 117.8(3) . . ? C35 N6 Fe1 102.7(3) . . ? C36 N6 Fe1 135.5(4) . . ? Fe2 N6 Fe1 68.14(13) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? C5 C2 C4 112.9(5) . . ? C5 C2 C3 113.1(4) . . ? C4 C2 C3 111.9(5) . . ? C5 C2 C1 106.4(4) . . ? C4 C2 C1 105.9(4) . . ? C3 C2 C1 105.9(5) . . ? N1 C3 C2 116.8(4) . . ? N1 C3 H3A 108.1 . . ? C2 C3 H3A 108.1 . . ? N1 C3 H3B 108.1 . . ? C2 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? N2 C4 C2 116.4(4) . . ? N2 C4 H4B 108.2 . . ? C2 C4 H4B 108.2 . . ? N2 C4 H4A 108.2 . . ? C2 C4 H4A 108.2 . . ? H4B C4 H4A 107.3 . . ? N3 C5 C2 115.7(4) . . ? N3 C5 H5B 108.4 . . ? C2 C5 H5B 108.4 . . ? N3 C5 H5A 108.4 . . ? C2 C5 H5A 108.4 . . ? H5B C5 H5A 107.4 . . ? C7 C6 N1 127.5(5) . . ? C7 C6 C11 118.6(5) . . ? N1 C6 C11 113.9(5) . . ? C6 C7 C8 120.1(6) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 121.1(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.1(6) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C6 120.7(5) . . ? C10 C11 N4 125.7(5) . . ? C6 C11 N4 113.6(5) . . ? C17 C12 C13 117.9(5) . . ? C17 C12 N4 121.5(5) . . ? C13 C12 N4 120.6(5) . . ? C14 C13 C12 121.6(6) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 120.8(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 118.5(6) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C15 C16 C17 121.8(6) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C12 119.6(5) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C19 C18 N2 127.0(6) . . ? C19 C18 C23 119.1(6) . . ? N2 C18 C23 113.9(5) . . ? C18 C19 C20 120.5(6) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 119.8(6) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.5(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 120.7(6) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.4(5) . . ? C22 C23 N5 126.5(6) . . ? C18 C23 N5 113.9(5) . . ? C29 C24 C25 118.3(6) . . ? C29 C24 N5 121.7(5) . . ? C25 C24 N5 120.0(5) . . ? C26 C25 C24 120.2(6) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.7(6) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 118.5(6) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 120.5(6) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120.7(6) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 N3 127.8(5) . . ? C31 C30 C35 118.8(5) . . ? N3 C30 C35 113.3(5) . . ? C30 C31 C32 121.4(5) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C33 C32 C31 119.3(5) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 121.0(5) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C35 120.4(5) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 N6 125.6(5) . . ? C34 C35 C30 119.1(5) . . ? N6 C35 C30 115.1(5) . . ? C37 C36 C41 118.4(5) . . ? C37 C36 N6 120.2(5) . . ? C41 C36 N6 121.3(5) . . ? C38 C37 C36 121.1(6) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.4(6) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.3(6) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 120.6(6) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C36 120.2(6) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? C4L O1 C1L 110.3(5) . . ? C4L O1 Fe1 126.2(4) . . ? C1L O1 Fe1 116.9(4) . . ? O1 C1L C2L 107.9(7) . . ? O1 C1L H1LA 110.1 . . ? C2L C1L H1LA 110.1 . . ? O1 C1L H1LB 110.1 . . ? C2L C1L H1LB 110.1 . . ? H1LA C1L H1LB 108.4 . . ? C1L C2L C3L 98.3(9) . . ? C1L C2L H2LA 112.1 . . ? C3L C2L H2LA 112.1 . . ? C1L C2L H2LB 112.1 . . ? C3L C2L H2LB 112.1 . . ? H2LA C2L H2LB 109.8 . . ? C4L C3L C2L 104.0(10) . . ? C4L C3L H3LA 111.0 . . ? C2L C3L H3LA 111.0 . . ? C4L C3L H3LB 111.0 . . ? C2L C3L H3LB 111.0 . . ? H3LA C3L H3LB 109.0 . . ? O1 C4L C3L 103.1(7) . . ? O1 C4L H4LA 111.1 . . ? C3L C4L H4LA 111.1 . . ? O1 C4L H4LB 111.1 . . ? C3L C4L H4LB 111.1 . . ? H4LA C4L H4LB 109.1 . . ? C3M C2M H2MA 110.7 . . ? C3M C2M H2MB 110.7 . . ? H2MA C2M H2MB 108.8 . . ? C2M C3M H3MA 112.4 . . ? C2M C3M H3MB 112.4 . . ? H3MA C3M H3MB 109.9 . . ? C8L O2 C5L 109.1(4) . . ? C8L O2 Fe2 124.2(3) . . ? C5L O2 Fe2 116.0(3) . . ? O2 C5L C6L 105.3(5) . . ? O2 C5L H5LA 110.7 . . ? C6L C5L H5LA 110.7 . . ? O2 C5L H5LB 110.7 . . ? C6L C5L H5LB 110.7 . . ? H5LA C5L H5LB 108.8 . . ? C7L C6L C5L 103.0(5) . . ? C7L C6L H6LA 111.2 . . ? C5L C6L H6LA 111.2 . . ? C7L C6L H6LB 111.2 . . ? C5L C6L H6LB 111.2 . . ? H6LA C6L H6LB 109.1 . . ? C8L C7L C6L 102.6(6) . . ? C8L C7L H7LA 111.2 . . ? C6L C7L H7LA 111.2 . . ? C8L C7L H7LB 111.2 . . ? C6L C7L H7LB 111.2 . . ? H7LA C7L H7LB 109.2 . . ? O2 C8L C7L 104.6(5) . . ? O2 C8L H8LA 110.8 . . ? C7L C8L H8LA 110.8 . . ? O2 C8L H8LB 110.8 . . ? C7L C8L H8LB 110.8 . . ? H8LA C8L H8LB 108.9 . . ? C12L O3L C9L 109.5(15) . . ? C12L O3L Fe3 132.5(18) . . ? C9L O3L Fe3 112.1(14) . . ? O3L C9L C10L 104.1(16) . . ? O3L C9L H9LA 110.9 . . ? C10L C9L H9LA 110.9 . . ? O3L C9L H9LB 110.9 . . ? C10L C9L H9LB 110.9 . . ? H9LA C9L H9LB 109.0 . . ? C11L C10L C9L 106.6(18) . . ? C11L C10L H10A 110.4 . . ? C9L C10L H10A 110.4 . . ? C11L C10L H10B 110.4 . . ? C9L C10L H10B 110.4 . . ? H10A C10L H10B 108.6 . . ? C10L C11L C12L 107(2) . . ? C10L C11L H11A 110.2 . . ? C12L C11L H11A 110.2 . . ? C10L C11L H11B 110.2 . . ? C12L C11L H11B 110.2 . . ? H11A C11L H11B 108.5 . . ? O3L C12L C11L 103.8(19) . . ? O3L C12L H12A 111.0 . . ? C11L C12L H12A 111.0 . . ? O3L C12L H12B 111.0 . . ? C11L C12L H12B 111.0 . . ? H12A C12L H12B 109.0 . . ? C10M C9M H9MA 111.1 . . ? C10M C9M H9MB 111.1 . . ? H9MA C9M H9MB 109.1 . . ? C11M C10M C9M 106.4(14) . . ? C11M C10M H10C 110.4 . . ? C9M C10M H10C 110.4 . . ? C11M C10M H10D 110.4 . . ? C9M C10M H10D 110.4 . . ? H10C C10M H10D 108.6 . . ? C10M C11M C12M 104.7(15) . . ? C10M C11M H11C 110.8 . . ? C12M C11M H11C 110.8 . . ? C10M C11M H11D 110.8 . . ? C12M C11M H11D 110.8 . . ? H11C C11M H11D 108.9 . . ? C11M C12M H12C 110.5 . . ? C11M C12M H12D 110.5 . . ? H12C C12M H12D 108.7 . . ? C1S O1S C4S 105.4(16) . . ? O1S C1S C2S 111.0(14) . . ? O1S C1S H1SB 109.4 . . ? C2S C1S H1SB 109.4 . . ? O1S C1S H1SA 109.4 . . ? C2S C1S H1SA 109.4 . . ? H1SB C1S H1SA 108.0 . . ? C3S C2S C1S 102.8(13) . . ? C3S C2S H2SB 111.2 . . ? C1S C2S H2SB 111.2 . . ? C3S C2S H2SA 111.2 . . ? C1S C2S H2SA 111.2 . . ? H2SB C2S H2SA 109.1 . . ? C2S C3S C4S 102.6(14) . . ? C2S C3S H3SA 111.2 . . ? C4S C3S H3SA 111.2 . . ? C2S C3S H3SB 111.2 . . ? C4S C3S H3SB 111.2 . . ? H3SA C3S H3SB 109.2 . . ? O1S C4S C3S 107.4(14) . . ? O1S C4S H4SA 110.2 . . ? C3S C4S H4SA 110.2 . . ? O1S C4S H4SB 110.2 . . ? C3S C4S H4SB 110.2 . . ? H4SA C4S H4SB 108.5 . . ? C1P O1P C4P 110.0(9) . . ? O1P C1P C2P 108.6(9) . . ? O1P C1P H1PB 110.0 . . ? C2P C1P H1PB 110.0 . . ? O1P C1P H1PA 110.0 . . ? C2P C1P H1PA 110.0 . . ? H1PB C1P H1PA 108.3 . . ? C3P C2P C1P 104.4(8) . . ? C3P C2P H2PB 110.9 . . ? C1P C2P H2PB 110.9 . . ? C3P C2P H2PA 110.9 . . ? C1P C2P H2PA 110.9 . . ? H2PB C2P H2PA 108.9 . . ? C4P C3P C2P 103.7(8) . . ? C4P C3P H3PA 111.0 . . ? C2P C3P H3PA 111.0 . . ? C4P C3P H3PB 111.0 . . ? C2P C3P H3PB 111.0 . . ? H3PA C3P H3PB 109.0 . . ? O1P C4P C3P 108.8(8) . . ? O1P C4P H4PA 109.9 . . ? C3P C4P H4PA 109.9 . . ? O1P C4P H4PB 109.9 . . ? C3P C4P H4PB 109.9 . . ? H4PA C4P H4PB 108.3 . . ? C5S O2S C5S 109.1(10) . 2_655 ? O2S C5S C6S 110.0(8) . . ? O2S C5S H5SA 109.7 . . ? C6S C5S H5SA 109.7 . . ? O2S C5S H5SB 109.7 . . ? C6S C5S H5SB 109.7 . . ? H5SA C5S H5SB 108.2 . . ? C6S C6S C5S 105.2(5) 2_655 . ? C6S C6S H6SA 110.7 2_655 . ? C5S C6S H6SA 110.7 . . ? C6S C6S H6SB 110.7 2_655 . ? C5S C6S H6SB 110.7 . . ? H6SA C6S H6SB 108.8 . . ? C7S O3S C7S 109(2) . 2 ? O3S C7S C8S 107.1(19) . . ? O3S C7S H7SA 110.3 . . ? C8S C7S H7SA 110.3 . . ? O3S C7S H7SB 110.3 . . ? C8S C7S H7SB 110.3 . . ? H7SA C7S H7SB 108.6 . . ? C8S C8S C7S 108.1(12) 2 . ? C8S C8S H8SA 110.1 2 . ? C7S C8S H8SA 110.1 . . ? C8S C8S H8SB 110.1 2 . ? C7S C8S H8SB 110.1 . . ? H8SA C8S H8SB 108.4 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.293 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.094 #=============the end of compound Fe3Lpy3_300K=================== #============compound Fe3LPMe2Ph3================================ data_Fe3LPMe2Ph3 _database_code_depnum_ccdc_archive 'CCDC 836230' #TrackingRef '- combinedcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H69 Fe3 N6 P3' _chemical_formula_sum 'C65 H69 Fe3 N6 P3' _chemical_formula_weight 1194.72 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.403(3) _cell_length_b 20.060(4) _cell_length_c 22.036(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5483(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5752 _cell_measurement_theta_min 2.235 _cell_measurement_theta_max 23.681 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7893 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53801 _diffrn_reflns_av_R_equivalents 0.1994 _diffrn_reflns_av_sigmaI/netI 0.1514 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9824 _reflns_number_gt 5572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0100P)^2^+3.4700P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9824 _refine_ls_number_parameters 702 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.28885(7) 0.03519(5) 0.15924(4) 0.0215(2) Uani 1 1 d . . . Fe2 Fe 0.44104(7) 0.04295(4) 0.23683(4) 0.0208(2) Uani 1 1 d . . . Fe3 Fe 0.27760(7) -0.03529(4) 0.25798(4) 0.0212(2) Uani 1 1 d . . . P1 P 0.21285(15) 0.07594(9) 0.06202(8) 0.0255(4) Uani 1 1 d . . . P2 P 0.63093(14) 0.07255(9) 0.25470(8) 0.0274(4) Uani 1 1 d . . . P3 P 0.19522(14) -0.12467(8) 0.31335(8) 0.0261(4) Uani 1 1 d . . . N1 N 0.4472(4) -0.0601(2) 0.2542(2) 0.0204(13) Uani 1 1 d . . . N2 N 0.2664(4) -0.0683(2) 0.1650(2) 0.0191(12) Uani 1 1 d . . . N3 N 0.4519(4) 0.0169(2) 0.1398(2) 0.0189(12) Uani 1 1 d . . . N4 N 0.3641(4) 0.0236(2) 0.3248(2) 0.0197(13) Uani 1 1 d . . . N5 N 0.1445(4) 0.0178(2) 0.2118(2) 0.0200(13) Uani 1 1 d . . . N6 N 0.3879(4) 0.1255(2) 0.1858(2) 0.0202(13) Uani 1 1 d . . . C1 C 0.5132(5) -0.1658(3) 0.1165(3) 0.0244(16) Uani 1 1 d . . . H1B H 0.4935 -0.2076 0.1366 0.037 Uiso 1 1 calc R . . H1A H 0.5914 -0.1596 0.1187 0.037 Uiso 1 1 calc R . . H1C H 0.4908 -0.1676 0.0738 0.037 Uiso 1 1 calc R . . C1A C 0.1673(5) 0.0051(3) 0.0188(3) 0.0361(19) Uani 1 1 d . . . H1AA H 0.1054 -0.0154 0.0392 0.054 Uiso 1 1 calc R . . H1AB H 0.2258 -0.0276 0.0156 0.054 Uiso 1 1 calc R . . H1AC H 0.1460 0.0196 -0.0219 0.054 Uiso 1 1 calc R . . C1B C 0.6982(5) 0.1338(3) 0.2085(3) 0.0368(19) Uani 1 1 d . . . H1BA H 0.6943 0.1205 0.1658 0.055 Uiso 1 1 calc R . . H1BB H 0.7739 0.1372 0.2209 0.055 Uiso 1 1 calc R . . H1BC H 0.6630 0.1772 0.2137 0.055 Uiso 1 1 calc R . . C1C C 0.2922(5) -0.1767(3) 0.3518(3) 0.0322(18) Uani 1 1 d . . . H1CA H 0.3464 -0.1922 0.3227 0.048 Uiso 1 1 calc R . . H1CC H 0.2553 -0.2152 0.3696 0.048 Uiso 1 1 calc R . . H1CB H 0.3274 -0.1510 0.3840 0.048 Uiso 1 1 calc R . . C2 C 0.4569(5) -0.1079(3) 0.1478(3) 0.0233(16) Uani 1 1 d . . . C2A C 0.3051(5) 0.1147(3) 0.0098(3) 0.0322(18) Uani 1 1 d . . . H2AB H 0.3633 0.0835 0.0000 0.048 Uiso 1 1 calc R . . H2AA H 0.3355 0.1549 0.0284 0.048 Uiso 1 1 calc R . . H2AC H 0.2666 0.1269 -0.0275 0.048 Uiso 1 1 calc R . . C2B C 0.7178(5) 0.0000(3) 0.2451(3) 0.0341(17) Uani 1 1 d . . . H2BB H 0.6914 -0.0365 0.2706 0.051 Uiso 1 1 calc R . . H2BA H 0.7916 0.0115 0.2571 0.051 Uiso 1 1 calc R . . H2BC H 0.7172 -0.0139 0.2025 0.051 Uiso 1 1 calc R . . C2C C 0.1275(5) -0.1860(3) 0.2667(3) 0.0350(19) Uani 1 1 d . . . H2CA H 0.0658 -0.1652 0.2464 0.052 Uiso 1 1 calc R . . H2CB H 0.1023 -0.2227 0.2923 0.052 Uiso 1 1 calc R . . H2CC H 0.1778 -0.2031 0.2362 0.052 Uiso 1 1 calc R . . C3 C 0.4899(5) -0.1108(3) 0.2136(3) 0.0228(16) Uani 1 1 d . . . H3A H 0.4686 -0.1550 0.2297 0.027 Uiso 1 1 calc R . . H3B H 0.5696 -0.1085 0.2153 0.027 Uiso 1 1 calc R . . C3A C 0.0958(5) 0.1296(3) 0.0590(3) 0.0221(16) Uani 1 1 d . . . C3B C 0.6627(5) 0.1000(3) 0.3308(3) 0.0222(16) Uani 1 1 d . . . C3C C 0.0967(5) -0.1073(3) 0.3720(3) 0.0251(17) Uani 1 1 d . . . C4 C 0.3384(5) -0.1191(3) 0.1393(3) 0.0209(16) Uani 1 1 d . . . H4B H 0.3238 -0.1224 0.0953 0.025 Uiso 1 1 calc R . . H4A H 0.3196 -0.1627 0.1577 0.025 Uiso 1 1 calc R . . C4A C -0.0035(6) 0.1045(4) 0.0749(3) 0.0359(19) Uani 1 1 d . . . H4AA H -0.0083 0.0595 0.0882 0.043 Uiso 1 1 calc R . . C4B C 0.6670(5) 0.1666(3) 0.3455(3) 0.0277(17) Uani 1 1 d . . . H4BA H 0.6592 0.1989 0.3143 0.033 Uiso 1 1 calc R . . C4C C 0.1316(6) -0.0881(3) 0.4289(3) 0.0334(19) Uani 1 1 d . . . H4C H 0.2066 -0.0845 0.4369 0.040 Uiso 1 1 calc R . . C5 C 0.4956(5) -0.0452(3) 0.1164(3) 0.0258(16) Uani 1 1 d . . . H5A H 0.5752 -0.0434 0.1195 0.031 Uiso 1 1 calc R . . H5B H 0.4772 -0.0485 0.0728 0.031 Uiso 1 1 calc R . . C5A C -0.0959(6) 0.1420(4) 0.0724(3) 0.043(2) Uani 1 1 d . . . H5AA H -0.1636 0.1233 0.0830 0.052 Uiso 1 1 calc R . . C5B C 0.6823(5) 0.1874(3) 0.4042(3) 0.0299(18) Uani 1 1 d . . . H5BA H 0.6851 0.2337 0.4131 0.036 Uiso 1 1 calc R . . C5C C 0.0582(7) -0.0743(3) 0.4740(4) 0.046(2) Uani 1 1 d . . . H5C H 0.0825 -0.0632 0.5136 0.056 Uiso 1 1 calc R . . C6 C 0.4788(5) -0.0694(3) 0.3140(3) 0.0194(15) Uani 1 1 d . . . C6A C -0.0882(6) 0.2078(4) 0.0540(3) 0.047(2) Uani 1 1 d . . . H6A H -0.1512 0.2345 0.0520 0.056 Uiso 1 1 calc R . . C6B C 0.6936(5) 0.1418(3) 0.4500(3) 0.0296(17) Uani 1 1 d . . . H6B H 0.7040 0.1559 0.4907 0.035 Uiso 1 1 calc R . . C6C C -0.0496(7) -0.0766(4) 0.4617(4) 0.047(2) Uani 1 1 d . . . H6C H -0.1004 -0.0654 0.4924 0.056 Uiso 1 1 calc R . . C7 C 0.5465(5) -0.1172(3) 0.3372(3) 0.0226(16) Uani 1 1 d . . . H7 H 0.5815 -0.1475 0.3105 0.027 Uiso 1 1 calc R . . C7A C 0.0092(7) 0.2344(4) 0.0389(3) 0.045(2) Uani 1 1 d . . . H7A H 0.0142 0.2796 0.0265 0.054 Uiso 1 1 calc R . . C7B C 0.6895(5) 0.0745(3) 0.4356(3) 0.0289(17) Uani 1 1 d . . . H7B H 0.6984 0.0424 0.4669 0.035 Uiso 1 1 calc R . . C7C C -0.0840(6) -0.0946(3) 0.4061(4) 0.043(2) Uani 1 1 d . . . H7C H -0.1592 -0.0965 0.3982 0.052 Uiso 1 1 calc R . . C8 C 0.5643(5) -0.1214(3) 0.3990(3) 0.0237(16) Uani 1 1 d . . . H8 H 0.6128 -0.1540 0.4144 0.028 Uiso 1 1 calc R . . C8A C 0.1007(6) 0.1951(3) 0.0416(3) 0.0305(18) Uani 1 1 d . . . H8A H 0.1685 0.2140 0.0312 0.037 Uiso 1 1 calc R . . C8B C 0.6729(5) 0.0533(3) 0.3772(3) 0.0223(16) Uani 1 1 d . . . H8B H 0.6684 0.0070 0.3684 0.027 Uiso 1 1 calc R . . C8C C -0.0127(5) -0.1103(3) 0.3607(3) 0.0320(18) Uani 1 1 d . . . H8C H -0.0384 -0.1232 0.3219 0.038 Uiso 1 1 calc R . . C9 C 0.5129(5) -0.0792(3) 0.4381(3) 0.0226(16) Uani 1 1 d . . . H9 H 0.5234 -0.0835 0.4807 0.027 Uiso 1 1 calc R . . C10 C 0.4457(5) -0.0305(3) 0.4156(3) 0.0211(15) Uani 1 1 d . . . H10 H 0.4101 -0.0011 0.4428 0.025 Uiso 1 1 calc R . . C11 C 0.4296(5) -0.0239(3) 0.3547(3) 0.0199(16) Uani 1 1 d . . . C12 C 0.3264(5) 0.0762(3) 0.3635(3) 0.0191(15) Uani 1 1 d . . . C13 C 0.4010(5) 0.1175(3) 0.3924(3) 0.0226(16) Uani 1 1 d . . . H13 H 0.4761 0.1104 0.3867 0.027 Uiso 1 1 calc R . . C14 C 0.3657(6) 0.1685(3) 0.4290(3) 0.0297(18) Uani 1 1 d . . . H14 H 0.4162 0.1958 0.4499 0.036 Uiso 1 1 calc R . . C15 C 0.2572(6) 0.1800(4) 0.4352(3) 0.039(2) Uani 1 1 d . . . H15 H 0.2331 0.2167 0.4589 0.047 Uiso 1 1 calc R . . C16 C 0.1845(6) 0.1402(4) 0.4082(3) 0.041(2) Uani 1 1 d . . . H16 H 0.1096 0.1483 0.4134 0.049 Uiso 1 1 calc R . . C17 C 0.2190(5) 0.0869(3) 0.3727(3) 0.0287(17) Uani 1 1 d . . . H17 H 0.1675 0.0579 0.3547 0.034 Uiso 1 1 calc R . . C18 C 0.1580(5) -0.0811(3) 0.1535(3) 0.0240(16) Uani 1 1 d . . . C19 C 0.1132(5) -0.1315(3) 0.1201(3) 0.0262(17) Uani 1 1 d . . . H19 H 0.1590 -0.1635 0.1015 0.031 Uiso 1 1 calc R . . C20 C 0.0027(5) -0.1370(3) 0.1128(3) 0.0283(17) Uani 1 1 d . . . H20 H -0.0272 -0.1729 0.0902 0.034 Uiso 1 1 calc R . . C21 C -0.0630(6) -0.0898(3) 0.1386(3) 0.0298(18) Uani 1 1 d . . . H21 H -0.1389 -0.0930 0.1336 0.036 Uiso 1 1 calc R . . C22 C -0.0204(5) -0.0376(3) 0.1716(3) 0.0258(16) Uani 1 1 d . . . H22 H -0.0671 -0.0050 0.1885 0.031 Uiso 1 1 calc R . . C23 C 0.0897(5) -0.0326(3) 0.1804(3) 0.0231(15) Uani 1 1 d . . . C24 C 0.0777(4) 0.0614(3) 0.2437(3) 0.0119(13) Uani 1 1 d . . . C25 C 0.0090(5) 0.0398(4) 0.2890(3) 0.0259(16) Uani 1 1 d . . . H25 H 0.0034 -0.0066 0.2972 0.031 Uiso 1 1 calc R . . C26 C -0.0521(5) 0.0843(4) 0.3229(3) 0.0360(19) Uani 1 1 d . . . H26 H -0.1010 0.0684 0.3527 0.043 Uiso 1 1 calc R . . C27 C -0.0412(6) 0.1510(4) 0.3130(4) 0.045(2) Uani 1 1 d . . . H27 H -0.0815 0.1818 0.3366 0.054 Uiso 1 1 calc R . . C28 C 0.0273(6) 0.1738(4) 0.2692(4) 0.044(2) Uani 1 1 d . . . H28 H 0.0351 0.2204 0.2632 0.053 Uiso 1 1 calc R . . C29 C 0.0858(5) 0.1298(3) 0.2332(3) 0.0323(18) Uani 1 1 d . . . H29 H 0.1310 0.1462 0.2018 0.039 Uiso 1 1 calc R . . C30 C 0.4966(5) 0.0732(3) 0.1125(3) 0.0205(15) Uani 1 1 d . . . C31 C 0.5718(5) 0.0749(3) 0.0660(3) 0.0210(15) Uani 1 1 d . . . H31 H 0.5984 0.0344 0.0494 0.025 Uiso 1 1 calc R . . C32 C 0.6084(5) 0.1351(3) 0.0435(3) 0.0240(16) Uani 1 1 d . . . H32 H 0.6591 0.1355 0.0112 0.029 Uiso 1 1 calc R . . C33 C 0.5727(5) 0.1940(3) 0.0671(3) 0.0229(16) Uani 1 1 d . . . H33 H 0.5979 0.2352 0.0513 0.027 Uiso 1 1 calc R . . C34 C 0.4985(5) 0.1930(3) 0.1148(3) 0.0205(15) Uani 1 1 d . . . H34 H 0.4741 0.2338 0.1319 0.025 Uiso 1 1 calc R . . C35 C 0.4602(5) 0.1334(3) 0.1374(3) 0.0180(15) Uani 1 1 d . . . C36 C 0.3362(5) 0.1845(3) 0.2055(3) 0.0192(15) Uani 1 1 d . . . C37 C 0.2762(5) 0.2231(3) 0.1650(3) 0.0241(16) Uani 1 1 d . . . H37 H 0.2735 0.2107 0.1234 0.029 Uiso 1 1 calc R . . C38 C 0.2216(5) 0.2781(3) 0.1840(3) 0.0274(17) Uani 1 1 d . . . H38 H 0.1821 0.3038 0.1554 0.033 Uiso 1 1 calc R . . C39 C 0.2227(5) 0.2971(3) 0.2438(3) 0.0322(17) Uani 1 1 d . . . H39 H 0.1833 0.3351 0.2568 0.039 Uiso 1 1 calc R . . C40 C 0.2822(6) 0.2601(3) 0.2849(3) 0.0322(18) Uani 1 1 d . . . H40 H 0.2827 0.2719 0.3266 0.039 Uiso 1 1 calc R . . C41 C 0.3410(5) 0.2056(3) 0.2649(3) 0.0265(16) Uani 1 1 d . . . H41 H 0.3855 0.1822 0.2928 0.032 Uiso 1 1 calc R . . 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 0.0198(5) 0.0252(5) 0.0196(5) 0.0027(5) 0.0008(4) -0.0010(5) Fe2 0.0206(5) 0.0240(5) 0.0179(5) 0.0007(5) -0.0002(4) -0.0013(5) Fe3 0.0220(5) 0.0250(5) 0.0167(5) 0.0010(5) -0.0002(4) -0.0015(5) P1 0.0272(10) 0.0308(11) 0.0185(10) 0.0003(8) 0.0023(8) 0.0016(9) P2 0.0222(10) 0.0372(11) 0.0228(11) -0.0009(9) 0.0007(9) -0.0038(9) P3 0.0289(11) 0.0260(10) 0.0234(10) 0.0020(8) -0.0006(8) -0.0040(9) N1 0.027(3) 0.024(3) 0.010(3) -0.009(2) -0.002(3) -0.001(2) N2 0.022(3) 0.019(3) 0.017(3) -0.005(2) 0.001(2) -0.002(2) N3 0.023(3) 0.016(3) 0.018(3) -0.006(2) 0.000(2) 0.000(2) N4 0.019(3) 0.024(3) 0.016(3) 0.000(2) 0.004(2) -0.002(3) N5 0.022(3) 0.021(3) 0.017(3) 0.002(2) 0.002(3) -0.005(2) N6 0.023(3) 0.019(3) 0.019(3) -0.003(2) 0.000(3) -0.001(3) C1 0.026(4) 0.031(4) 0.016(4) 0.001(3) 0.000(3) 0.004(3) C1A 0.048(5) 0.033(4) 0.027(4) 0.001(3) -0.006(4) 0.006(4) C1B 0.027(4) 0.058(5) 0.025(4) 0.001(4) -0.003(3) -0.008(4) C1C 0.033(4) 0.032(4) 0.032(5) 0.008(3) -0.001(4) 0.002(4) C2 0.024(4) 0.025(4) 0.021(4) 0.000(3) 0.000(3) 0.008(3) C2A 0.027(4) 0.050(5) 0.020(4) 0.009(3) 0.000(3) 0.006(4) C2B 0.019(4) 0.050(4) 0.033(4) -0.013(4) 0.005(3) 0.001(4) C2C 0.039(5) 0.030(4) 0.036(5) 0.000(4) 0.001(4) -0.009(4) C3 0.029(4) 0.018(4) 0.021(4) 0.002(3) 0.008(3) -0.005(3) C3A 0.022(4) 0.034(4) 0.011(4) -0.003(3) -0.003(3) -0.003(3) C3B 0.018(4) 0.026(4) 0.023(4) -0.005(3) -0.003(3) 0.001(3) C3C 0.030(4) 0.024(4) 0.021(4) 0.002(3) 0.005(3) -0.006(3) C4 0.028(4) 0.022(4) 0.013(4) 0.002(3) 0.006(3) 0.003(3) C4A 0.033(5) 0.047(5) 0.028(5) 0.002(4) -0.004(4) 0.003(4) C4B 0.021(4) 0.036(5) 0.026(4) 0.011(4) 0.000(3) 0.005(3) C4C 0.041(5) 0.030(4) 0.029(5) -0.002(4) 0.004(4) 0.004(4) C5 0.025(4) 0.029(4) 0.024(4) -0.001(3) -0.001(3) 0.000(3) C5A 0.017(4) 0.080(7) 0.033(5) -0.005(4) 0.004(4) 0.001(4) C5B 0.033(5) 0.026(4) 0.031(5) -0.007(3) 0.005(4) -0.006(3) C5C 0.059(6) 0.037(5) 0.043(5) -0.011(4) 0.008(5) 0.008(4) C6 0.021(4) 0.025(4) 0.012(4) -0.006(3) 0.001(3) -0.003(3) C6A 0.039(5) 0.062(6) 0.040(5) -0.014(5) -0.005(4) 0.029(5) C6B 0.036(5) 0.034(4) 0.019(4) -0.002(3) 0.000(3) -0.006(4) C6C 0.049(6) 0.035(5) 0.056(6) -0.007(4) 0.027(5) -0.001(4) C7 0.024(4) 0.022(4) 0.023(4) 0.004(3) 0.000(3) -0.001(3) C7A 0.059(6) 0.034(5) 0.042(5) -0.008(4) -0.018(5) 0.014(5) C7B 0.025(4) 0.036(4) 0.026(4) 0.009(3) 0.003(3) -0.002(3) C7C 0.035(5) 0.035(5) 0.060(6) 0.001(4) 0.010(5) -0.004(4) C8 0.028(4) 0.021(4) 0.022(4) 0.004(3) 0.000(3) -0.001(3) C8A 0.038(5) 0.022(4) 0.032(4) -0.002(3) -0.011(4) -0.006(4) C8B 0.020(4) 0.026(4) 0.021(4) -0.001(3) -0.001(3) 0.000(3) C8C 0.033(5) 0.028(4) 0.035(5) 0.003(4) 0.004(4) -0.010(4) C9 0.029(4) 0.020(4) 0.019(4) 0.004(3) -0.008(3) -0.001(3) C10 0.029(4) 0.023(4) 0.012(4) -0.003(3) -0.001(3) -0.004(3) C11 0.008(3) 0.020(4) 0.031(4) 0.009(3) -0.004(3) 0.001(3) C12 0.030(4) 0.015(3) 0.012(4) 0.001(3) -0.001(3) -0.005(3) C13 0.023(4) 0.029(4) 0.015(4) 0.005(3) 0.003(3) 0.000(3) C14 0.038(5) 0.033(4) 0.018(4) -0.005(3) -0.002(3) -0.002(4) C15 0.047(5) 0.046(5) 0.025(5) -0.008(4) 0.003(4) 0.019(4) C16 0.028(5) 0.069(6) 0.025(5) -0.001(4) 0.002(4) 0.012(4) C17 0.021(4) 0.042(5) 0.023(4) -0.008(3) 0.007(3) 0.001(4) C18 0.033(4) 0.025(4) 0.015(4) 0.000(3) 0.002(3) 0.003(3) C19 0.034(5) 0.030(4) 0.014(4) -0.008(3) 0.001(3) -0.001(3) C20 0.032(4) 0.033(4) 0.019(4) -0.004(3) -0.002(3) -0.008(4) C21 0.028(4) 0.045(5) 0.016(4) 0.000(3) -0.001(3) -0.008(4) C22 0.026(4) 0.027(4) 0.024(4) -0.002(3) 0.001(3) 0.004(4) C23 0.031(4) 0.023(4) 0.016(4) 0.000(3) -0.003(3) -0.005(3) C24 0.007(3) 0.018(4) 0.011(3) 0.003(3) -0.002(3) 0.005(3) C25 0.018(4) 0.040(4) 0.019(4) -0.008(4) -0.004(3) 0.001(4) C26 0.020(4) 0.056(5) 0.032(5) -0.014(4) 0.005(4) 0.001(4) C27 0.018(4) 0.058(6) 0.058(6) -0.021(5) -0.004(4) 0.005(4) C28 0.028(5) 0.035(5) 0.068(6) -0.008(4) -0.011(5) -0.004(4) C29 0.023(4) 0.045(5) 0.028(4) -0.004(4) -0.007(3) 0.006(4) C30 0.019(4) 0.024(4) 0.018(4) -0.006(3) -0.004(3) 0.000(3) C31 0.016(4) 0.035(4) 0.012(4) 0.003(3) -0.005(3) 0.001(3) C32 0.018(4) 0.038(4) 0.016(4) 0.004(3) -0.003(3) -0.003(3) C33 0.017(4) 0.032(4) 0.020(4) 0.009(3) -0.005(3) -0.006(3) C34 0.020(4) 0.022(4) 0.019(4) -0.004(3) -0.005(3) -0.002(3) C35 0.014(3) 0.030(4) 0.010(3) 0.000(3) -0.002(3) -0.002(3) C36 0.019(4) 0.019(4) 0.020(4) -0.003(3) 0.004(3) -0.004(3) C37 0.027(4) 0.022(4) 0.023(4) -0.002(3) 0.003(3) 0.001(3) C38 0.030(4) 0.021(4) 0.032(4) 0.007(3) 0.002(4) 0.006(3) C39 0.031(4) 0.027(4) 0.038(5) -0.003(4) 0.004(4) 0.000(4) C40 0.038(4) 0.034(4) 0.025(4) -0.006(3) 0.005(4) -0.006(4) C41 0.028(4) 0.031(4) 0.021(4) -0.001(3) 0.002(3) -0.007(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 N2 2.098(5) . ? Fe1 N3 2.099(5) . ? Fe1 N5 2.161(5) . ? Fe1 N6 2.265(5) . ? Fe1 P1 2.479(2) . ? Fe1 Fe2 2.5517(13) . ? Fe1 Fe3 2.5986(13) . ? Fe2 N1 2.104(5) . ? Fe2 N6 2.108(5) . ? Fe2 N4 2.196(5) . ? Fe2 N3 2.204(5) . ? Fe2 P2 2.461(2) . ? Fe2 Fe3 2.6057(13) . ? Fe3 N2 2.158(5) . ? Fe3 N1 2.163(5) . ? Fe3 N4 2.171(5) . ? Fe3 N5 2.212(5) . ? Fe3 P3 2.3974(19) . ? P1 C2A 1.800(6) . ? P1 C1A 1.802(6) . ? P1 C3A 1.809(6) . ? P2 C1B 1.801(6) . ? P2 C3B 1.808(6) . ? P2 C2B 1.823(6) . ? P3 C1C 1.804(6) . ? P3 C2C 1.809(6) . ? P3 C3C 1.812(7) . ? N1 C6 1.387(7) . ? N1 C3 1.455(7) . ? N2 C18 1.392(7) . ? N2 C4 1.469(7) . ? N3 C30 1.394(7) . ? N3 C5 1.454(7) . ? N4 C11 1.414(7) . ? N4 C12 1.434(7) . ? N5 C24 1.393(7) . ? N5 C23 1.403(7) . ? N6 C35 1.401(7) . ? N6 C36 1.416(7) . ? C1 C2 1.521(8) . ? C1 H1B 0.9800 . ? C1 H1A 0.9800 . ? C1 H1C 0.9800 . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C1C H1CA 0.9800 . ? C1C H1CC 0.9800 . ? C1C H1CB 0.9800 . ? C2 C4 1.499(8) . ? C2 C3 1.507(8) . ? C2 C5 1.514(8) . ? C2A H2AB 0.9800 . ? C2A H2AA 0.9800 . ? C2A H2AC 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BA 0.9800 . ? C2B H2BC 0.9800 . ? C2C H2CA 0.9800 . ? C2C H2CB 0.9800 . ? C2C H2CC 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3A C8A 1.371(8) . ? C3A C4A 1.376(9) . ? C3B C4B 1.375(8) . ? C3B C8B 1.392(8) . ? C3C C8C 1.380(9) . ? C3C C4C 1.381(9) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C4A C5A 1.372(9) . ? C4A H4AA 0.9500 . ? C4B C5B 1.372(8) . ? C4B H4BA 0.9500 . ? C4C C5C 1.377(9) . ? C4C H4C 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5A C6A 1.382(10) . ? C5A H5AA 0.9500 . ? C5B C6B 1.370(8) . ? C5B H5BA 0.9500 . ? C5C C6C 1.365(10) . ? C5C H5C 0.9500 . ? C6 C7 1.372(8) . ? C6 C11 1.418(8) . ? C6A C7A 1.362(10) . ? C6A H6A 0.9500 . ? C6B C7B 1.387(8) . ? C6B H6B 0.9500 . ? C6C C7C 1.347(10) . ? C6C H6C 0.9500 . ? C7 C8 1.382(8) . ? C7 H7 0.9500 . ? C7A C8A 1.382(9) . ? C7A H7A 0.9500 . ? C7B C8B 1.372(8) . ? C7B H7B 0.9500 . ? C7C C8C 1.372(9) . ? C7C H7C 0.9500 . ? C8 C9 1.368(8) . ? C8 H8 0.9500 . ? C8A H8A 0.9500 . ? C8B H8B 0.9500 . ? C8C H8C 0.9500 . ? C9 C10 1.377(8) . ? C9 H9 0.9500 . ? C10 C11 1.364(8) . ? C10 H10 0.9500 . ? C12 C17 1.365(8) . ? C12 C13 1.395(8) . ? C13 C14 1.375(8) . ? C13 H13 0.9500 . ? C14 C15 1.372(9) . ? C14 H14 0.9500 . ? C15 C16 1.344(9) . ? C15 H15 0.9500 . ? C16 C17 1.391(9) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.369(8) . ? C18 C23 1.420(8) . ? C19 C20 1.385(8) . ? C19 H19 0.9500 . ? C20 C21 1.373(8) . ? C20 H20 0.9500 . ? C21 C22 1.380(8) . ? C21 H21 0.9500 . ? C22 C23 1.383(8) . ? C22 H22 0.9500 . ? C24 C25 1.383(8) . ? C24 C29 1.395(8) . ? C25 C26 1.389(8) . ? C25 H25 0.9500 . ? C26 C27 1.363(9) . ? C26 H26 0.9500 . ? C27 C28 1.363(9) . ? C27 H27 0.9500 . ? C28 C29 1.392(9) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.386(8) . ? C30 C35 1.401(8) . ? C31 C32 1.381(8) . ? C31 H31 0.9500 . ? C32 C33 1.365(8) . ? C32 H32 0.9500 . ? C33 C34 1.397(8) . ? C33 H33 0.9500 . ? C34 C35 1.380(8) . ? C34 H34 0.9500 . ? C36 C41 1.377(8) . ? C36 C37 1.396(8) . ? C37 C38 1.361(8) . ? C37 H37 0.9500 . ? C38 C39 1.372(9) . ? C38 H38 0.9500 . ? C39 C40 1.383(9) . ? C39 H39 0.9500 . ? C40 C41 1.386(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? 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 N2 Fe1 N3 88.13(19) . . ? N2 Fe1 N5 72.45(18) . . ? N3 Fe1 N5 151.54(19) . . ? N2 Fe1 N6 147.94(19) . . ? N3 Fe1 N6 70.70(17) . . ? N5 Fe1 N6 116.10(18) . . ? N2 Fe1 P1 109.13(14) . . ? N3 Fe1 P1 104.35(14) . . ? N5 Fe1 P1 101.64(14) . . ? N6 Fe1 P1 99.53(13) . . ? N2 Fe1 Fe2 96.79(14) . . ? N3 Fe1 Fe2 55.56(13) . . ? N5 Fe1 Fe2 105.26(14) . . ? N6 Fe1 Fe2 51.48(13) . . ? P1 Fe1 Fe2 147.16(6) . . ? N2 Fe1 Fe3 53.44(13) . . ? N3 Fe1 Fe3 97.31(14) . . ? N5 Fe1 Fe3 54.46(13) . . ? N6 Fe1 Fe3 104.37(13) . . ? P1 Fe1 Fe3 151.95(6) . . ? Fe2 Fe1 Fe3 60.78(4) . . ? N1 Fe2 N6 151.70(19) . . ? N1 Fe2 N4 71.41(18) . . ? N6 Fe2 N4 118.33(18) . . ? N1 Fe2 N3 86.65(18) . . ? N6 Fe2 N3 71.78(18) . . ? N4 Fe2 N3 147.23(18) . . ? N1 Fe2 P2 99.98(14) . . ? N6 Fe2 P2 101.25(14) . . ? N4 Fe2 P2 108.52(14) . . ? N3 Fe2 P2 98.86(14) . . ? N1 Fe2 Fe1 95.10(14) . . ? N6 Fe2 Fe1 57.24(13) . . ? N4 Fe2 Fe1 105.02(13) . . ? N3 Fe2 Fe1 51.75(13) . . ? P2 Fe2 Fe1 146.10(6) . . ? N1 Fe2 Fe3 53.40(13) . . ? N6 Fe2 Fe3 108.99(14) . . ? N4 Fe2 Fe3 52.94(13) . . ? N3 Fe2 Fe3 94.49(13) . . ? P2 Fe2 Fe3 149.47(6) . . ? Fe1 Fe2 Fe3 60.50(4) . . ? N2 Fe3 N1 87.45(18) . . ? N2 Fe3 N4 147.43(18) . . ? N1 Fe3 N4 70.79(17) . . ? N2 Fe3 N5 70.32(18) . . ? N1 Fe3 N5 144.97(18) . . ? N4 Fe3 N5 114.73(18) . . ? N2 Fe3 P3 103.10(14) . . ? N1 Fe3 P3 105.16(14) . . ? N4 Fe3 P3 105.79(13) . . ? N5 Fe3 P3 106.04(13) . . ? N2 Fe3 Fe1 51.32(13) . . ? N1 Fe3 Fe1 92.36(13) . . ? N4 Fe3 Fe1 104.21(13) . . ? N5 Fe3 Fe1 52.63(12) . . ? P3 Fe3 Fe1 148.86(6) . . ? N2 Fe3 Fe2 93.72(13) . . ? N1 Fe3 Fe2 51.35(13) . . ? N4 Fe3 Fe2 53.80(12) . . ? N5 Fe3 Fe2 102.01(13) . . ? P3 Fe3 Fe2 150.81(6) . . ? Fe1 Fe3 Fe2 58.72(3) . . ? C2A P1 C1A 101.7(3) . . ? C2A P1 C3A 103.3(3) . . ? C1A P1 C3A 101.4(3) . . ? C2A P1 Fe1 117.0(2) . . ? C1A P1 Fe1 108.4(2) . . ? C3A P1 Fe1 122.2(2) . . ? C1B P2 C3B 102.4(3) . . ? C1B P2 C2B 101.8(3) . . ? C3B P2 C2B 102.8(3) . . ? C1B P2 Fe2 121.2(2) . . ? C3B P2 Fe2 115.5(2) . . ? C2B P2 Fe2 110.8(2) . . ? C1C P3 C2C 100.5(3) . . ? C1C P3 C3C 103.0(3) . . ? C2C P3 C3C 102.9(3) . . ? C1C P3 Fe3 112.8(2) . . ? C2C P3 Fe3 114.7(2) . . ? C3C P3 Fe3 120.4(2) . . ? C6 N1 C3 112.8(5) . . ? C6 N1 Fe2 108.4(4) . . ? C3 N1 Fe2 126.0(4) . . ? C6 N1 Fe3 105.6(4) . . ? C3 N1 Fe3 122.6(4) . . ? Fe2 N1 Fe3 75.24(16) . . ? C18 N2 C4 112.9(5) . . ? C18 N2 Fe1 107.5(4) . . ? C4 N2 Fe1 125.7(4) . . ? C18 N2 Fe3 106.9(4) . . ? C4 N2 Fe3 122.6(4) . . ? Fe1 N2 Fe3 75.24(15) . . ? C30 N3 C5 113.1(5) . . ? C30 N3 Fe1 109.3(4) . . ? C5 N3 Fe1 125.5(4) . . ? C30 N3 Fe2 104.6(4) . . ? C5 N3 Fe2 124.8(4) . . ? Fe1 N3 Fe2 72.69(15) . . ? C11 N4 C12 114.0(5) . . ? C11 N4 Fe3 103.5(4) . . ? C12 N4 Fe3 130.0(4) . . ? C11 N4 Fe2 106.3(4) . . ? C12 N4 Fe2 122.4(4) . . ? Fe3 N4 Fe2 73.27(15) . . ? C24 N5 C23 114.4(5) . . ? C24 N5 Fe1 131.4(4) . . ? C23 N5 Fe1 104.7(4) . . ? C24 N5 Fe3 120.9(4) . . ? C23 N5 Fe3 103.9(4) . . ? Fe1 N5 Fe3 72.91(15) . . ? C35 N6 C36 115.4(5) . . ? C35 N6 Fe2 107.1(4) . . ? C36 N6 Fe2 129.4(4) . . ? C35 N6 Fe1 104.0(4) . . ? C36 N6 Fe1 120.2(4) . . ? Fe2 N6 Fe1 71.29(15) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? P1 C1A H1AA 109.5 . . ? P1 C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? P1 C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? P2 C1B H1BA 109.5 . . ? P2 C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? P2 C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? P3 C1C H1CA 109.5 . . ? P3 C1C H1CC 109.5 . . ? H1CA C1C H1CC 109.5 . . ? P3 C1C H1CB 109.5 . . ? H1CA C1C H1CB 109.5 . . ? H1CC C1C H1CB 109.5 . . ? C4 C2 C3 112.4(5) . . ? C4 C2 C5 112.3(5) . . ? C3 C2 C5 112.7(5) . . ? C4 C2 C1 106.2(5) . . ? C3 C2 C1 106.4(5) . . ? C5 C2 C1 106.3(5) . . ? P1 C2A H2AB 109.5 . . ? P1 C2A H2AA 109.5 . . ? H2AB C2A H2AA 109.5 . . ? P1 C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? P2 C2B H2BB 109.5 . . ? P2 C2B H2BA 109.5 . . ? H2BB C2B H2BA 109.5 . . ? P2 C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? P3 C2C H2CA 109.5 . . ? P3 C2C H2CB 109.5 . . ? H2CA C2C H2CB 109.5 . . ? P3 C2C H2CC 109.5 . . ? H2CA C2C H2CC 109.5 . . ? H2CB C2C H2CC 109.5 . . ? N1 C3 C2 117.8(5) . . ? N1 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? N1 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C8A C3A C4A 117.5(6) . . ? C8A C3A P1 123.0(5) . . ? C4A C3A P1 119.4(5) . . ? C4B C3B C8B 118.5(6) . . ? C4B C3B P2 121.5(5) . . ? C8B C3B P2 119.7(5) . . ? C8C C3C C4C 118.8(6) . . ? C8C C3C P3 121.8(5) . . ? C4C C3C P3 119.3(5) . . ? N2 C4 C2 116.3(5) . . ? N2 C4 H4B 108.2 . . ? C2 C4 H4B 108.2 . . ? N2 C4 H4A 108.2 . . ? C2 C4 H4A 108.2 . . ? H4B C4 H4A 107.4 . . ? C5A C4A C3A 122.4(7) . . ? C5A C4A H4AA 118.8 . . ? C3A C4A H4AA 118.8 . . ? C5B C4B C3B 121.5(6) . . ? C5B C4B H4BA 119.2 . . ? C3B C4B H4BA 119.2 . . ? C5C C4C C3C 120.4(7) . . ? C5C C4C H4C 119.8 . . ? C3C C4C H4C 119.8 . . ? N3 C5 C2 115.6(5) . . ? N3 C5 H5A 108.4 . . ? C2 C5 H5A 108.4 . . ? N3 C5 H5B 108.4 . . ? C2 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C4A C5A C6A 118.5(7) . . ? C4A C5A H5AA 120.7 . . ? C6A C5A H5AA 120.7 . . ? C6B C5B C4B 120.4(6) . . ? C6B C5B H5BA 119.8 . . ? C4B C5B H5BA 119.8 . . ? C6C C5C C4C 119.9(8) . . ? C6C C5C H5C 120.1 . . ? C4C C5C H5C 120.1 . . ? C7 C6 N1 128.3(6) . . ? C7 C6 C11 118.6(6) . . ? N1 C6 C11 113.1(5) . . ? C7A C6A C5A 120.4(7) . . ? C7A C6A H6A 119.8 . . ? C5A C6A H6A 119.8 . . ? C5B C6B C7B 118.5(6) . . ? C5B C6B H6B 120.8 . . ? C7B C6B H6B 120.8 . . ? C7C C6C C5C 119.9(8) . . ? C7C C6C H6C 120.0 . . ? C5C C6C H6C 120.0 . . ? C6 C7 C8 120.5(6) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C6A C7A C8A 119.6(7) . . ? C6A C7A H7A 120.2 . . ? C8A C7A H7A 120.2 . . ? C8B C7B C6B 121.5(6) . . ? C8B C7B H7B 119.2 . . ? C6B C7B H7B 119.2 . . ? C6C C7C C8C 121.4(8) . . ? C6C C7C H7C 119.3 . . ? C8C C7C H7C 119.3 . . ? C9 C8 C7 120.6(6) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C3A C8A C7A 121.4(7) . . ? C3A C8A H8A 119.3 . . ? C7A C8A H8A 119.3 . . ? C7B C8B C3B 119.6(6) . . ? C7B C8B H8B 120.2 . . ? C3B C8B H8B 120.2 . . ? C7C C8C C3C 119.5(7) . . ? C7C C8C H8C 120.2 . . ? C3C C8C H8C 120.2 . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 N4 127.4(6) . . ? C10 C11 C6 119.7(6) . . ? N4 C11 C6 112.8(5) . . ? C17 C12 C13 119.0(6) . . ? C17 C12 N4 121.5(6) . . ? C13 C12 N4 119.5(5) . . ? C14 C13 C12 119.9(6) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 119.7(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.9(7) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.0(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.3(7) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 N2 128.8(6) . . ? C19 C18 C23 119.2(6) . . ? N2 C18 C23 112.0(6) . . ? C18 C19 C20 121.6(6) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 118.9(6) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 121.0(7) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 120.4(6) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 N5 126.9(6) . . ? C22 C23 C18 118.8(6) . . ? N5 C23 C18 114.3(6) . . ? C25 C24 N5 122.3(5) . . ? C25 C24 C29 118.1(6) . . ? N5 C24 C29 119.4(5) . . ? C24 C25 C26 121.6(7) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C27 C26 C25 119.4(7) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 120.3(7) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 121.0(7) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C24 119.5(7) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? C31 C30 N3 127.4(6) . . ? C31 C30 C35 119.0(6) . . ? N3 C30 C35 113.6(5) . . ? C32 C31 C30 120.6(6) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.8(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.2(6) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 120.7(6) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 N6 126.3(6) . . ? C34 C35 C30 119.7(6) . . ? N6 C35 C30 114.0(5) . . ? C41 C36 C37 117.5(6) . . ? C41 C36 N6 121.9(6) . . ? C37 C36 N6 120.6(6) . . ? C38 C37 C36 121.2(6) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 121.1(6) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C38 C39 C40 119.0(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C39 C40 C41 119.8(7) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C36 C41 C40 121.4(7) . . ? C36 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.892 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.101 # start Validation Reply Form _vrf_SYMMS02_1 ; PROBLEM: All angles should not be 90 for a monoclinic cell RESPONSE: Space group checked by Platon; no change suggested ; #=============the end of compound Fe3LPMe2Ph3===================