# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xu-Chun Wang' _publ_contact_author_email WXCHUN2004@163.COM _publ_section_title ; Functionalized ferrocenes and ferroceniums: synthesis, crystal structures and electrochemical properties based on carbazole/ phenothiazine-ferrocene conjugated molecules ; loop_ _publ_author_name 'Xu-Chun Wang.' 'Min-Hua Jiang.' 'Baokang Jin.' 'Yuhe Kan.' 'Xutang Tao.' ; Yu-Peng Tian ; 'Jie-Ying Wu.' 'Jia-Xiang Yang.' 'Sheng-Yi Zhang.' 'Hongping Zhou.' ; Cong-Yu Zuo ; # Attachment 'CIF-ccdc-1-2-3-5-revised.cif' data_ccdc270824 _database_code_depnum_ccdc_archive 'CCDC 270824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H23 Fe N S' _chemical_formula_weight 437.36 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4558(18) _cell_length_b 8.5905(19) _cell_length_c 29.350(3) _cell_angle_alpha 90.710(3) _cell_angle_beta 95.229(2) _cell_angle_gamma 96.165(3) _cell_volume 2110.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2277 _cell_measurement_theta_min 2.385 _cell_measurement_theta_max 23.128 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 1.368 _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6927 _exptl_absorpt_correction_T_max 0.9147 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 11195 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7366 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7366 _refine_ls_number_parameters 523 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.038 _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 1.17859(7) 0.42832(8) 0.35270(2) 0.0495(2) Uani 1 1 d . . . Fe2 Fe 0.72270(8) 0.85913(9) 0.44400(2) 0.0589(2) Uani 1 1 d . . . N1 N 0.4156(4) 0.1386(4) 0.11043(12) 0.0461(9) Uani 1 1 d . . . N2 N 0.0908(4) 0.6561(4) 0.16736(11) 0.0410(9) Uani 1 1 d . . . S1 S 0.61692(13) 0.42372(15) 0.08864(4) 0.0527(3) Uani 1 1 d . . . S2 S -0.00012(13) 0.88492(14) 0.23461(4) 0.0474(3) Uani 1 1 d . . . C1 C 0.5034(5) 0.2132(5) 0.14959(15) 0.0383(10) Uani 1 1 d . . . C2 C 0.4976(5) 0.1550(5) 0.19347(16) 0.0498(12) Uani 1 1 d . . . H2 H 0.4286 0.0660 0.1981 0.060 Uiso 1 1 calc R . . C3 C 0.5919(5) 0.2265(5) 0.23022(15) 0.0476(12) Uani 1 1 d . . . H3 H 0.5868 0.1839 0.2591 0.057 Uiso 1 1 calc R . . C4 C 0.6942(5) 0.3611(5) 0.22477(15) 0.0404(11) Uani 1 1 d . . . C5 C 0.6937(4) 0.4241(5) 0.18135(15) 0.0415(11) Uani 1 1 d . . . H5 H 0.7563 0.5178 0.1773 0.050 Uiso 1 1 calc R . . C6 C 0.6026(5) 0.3511(5) 0.14410(14) 0.0380(10) Uani 1 1 d . . . C7 C 0.3361(5) 0.2340(5) 0.07947(14) 0.0420(11) Uani 1 1 d . . . C8 C 0.1787(5) 0.1961(5) 0.06155(15) 0.0500(12) Uani 1 1 d . . . H8 H 0.1204 0.1062 0.0710 0.060 Uiso 1 1 calc R . . C9 C 0.1084(6) 0.2906(7) 0.02985(17) 0.0643(15) Uani 1 1 d . . . H9 H 0.0043 0.2616 0.0173 0.077 Uiso 1 1 calc R . . C10 C 0.1894(6) 0.4262(6) 0.01659(16) 0.0609(14) Uani 1 1 d . . . H10 H 0.1407 0.4887 -0.0049 0.073 Uiso 1 1 calc R . . C11 C 0.3437(6) 0.4702(5) 0.03525(15) 0.0504(12) Uani 1 1 d . . . H11 H 0.3987 0.5637 0.0270 0.061 Uiso 1 1 calc R . . C12 C 0.4161(5) 0.3739(5) 0.06634(14) 0.0418(11) Uani 1 1 d . . . C13 C 0.3520(6) -0.0260(5) 0.11353(17) 0.0655(15) Uani 1 1 d . . . H13A H 0.2431 -0.0317 0.1218 0.079 Uiso 1 1 calc R . . H13B H 0.4151 -0.0746 0.1375 0.079 Uiso 1 1 calc R . . C14 C 0.3545(6) -0.1159(6) 0.0687(2) 0.0893(19) Uani 1 1 d . . . H14A H 0.3121 -0.2229 0.0721 0.134 Uiso 1 1 calc R . . H14B H 0.4624 -0.1121 0.0607 0.134 Uiso 1 1 calc R . . H14C H 0.2904 -0.0694 0.0450 0.134 Uiso 1 1 calc R . . C15 C 0.8017(5) 0.4397(5) 0.26193(15) 0.0441(11) Uani 1 1 d . . . H15 H 0.8562 0.5347 0.2547 0.053 Uiso 1 1 calc R . . C16 C 0.8320(5) 0.3936(5) 0.30461(16) 0.0515(12) Uani 1 1 d . . . H16 H 0.7759 0.3013 0.3133 0.062 Uiso 1 1 calc R . . C17 C 0.9470(5) 0.4774(5) 0.33876(15) 0.0465(12) Uani 1 1 d . . . C18 C 1.0572(5) 0.6084(5) 0.33122(16) 0.0539(13) Uani 1 1 d . . . H18 H 1.0661 0.6615 0.3021 0.065 Uiso 1 1 calc R . . C19 C 1.1520(6) 0.6504(6) 0.37257(17) 0.0597(14) Uani 1 1 d . . . H19 H 1.2371 0.7376 0.3771 0.072 Uiso 1 1 calc R . . C20 C 1.1031(6) 0.5448(6) 0.40584(16) 0.0604(14) Uani 1 1 d . . . H20 H 1.1481 0.5449 0.4378 0.072 Uiso 1 1 calc R . . C21 C 0.9786(5) 0.4364(6) 0.38496(16) 0.0541(13) Uani 1 1 d . . . H21 H 0.9226 0.3486 0.4001 0.065 Uiso 1 1 calc R . . C22 C 1.2074(7) 0.2457(8) 0.3109(2) 0.0832(19) Uani 1 1 d . . . H22 H 1.1257 0.1893 0.2891 0.100 Uiso 1 1 calc R . . C23 C 1.3140(7) 0.3750(8) 0.3019(2) 0.0790(17) Uani 1 1 d . . . H23 H 1.3179 0.4275 0.2725 0.095 Uiso 1 1 calc R . . C24 C 1.4114(7) 0.4176(7) 0.3411(2) 0.0804(17) Uani 1 1 d . . . H24 H 1.4957 0.5058 0.3441 0.097 Uiso 1 1 calc R . . C25 C 1.3690(7) 0.3194(7) 0.37564(19) 0.0707(16) Uani 1 1 d . . . H25 H 1.4195 0.3245 0.4071 0.085 Uiso 1 1 calc R . . C26 C 1.2426(7) 0.2102(7) 0.3583(2) 0.0813(18) Uani 1 1 d . . . H26 H 1.1902 0.1242 0.3749 0.098 Uiso 1 1 calc R . . C27 C 0.2174(5) 0.7140(5) 0.20006(13) 0.0378(10) Uani 1 1 d . . . C28 C 0.3692(5) 0.6669(5) 0.20026(14) 0.0443(11) Uani 1 1 d . . . H28 H 0.3919 0.6004 0.1771 0.053 Uiso 1 1 calc R . . C29 C 0.4866(5) 0.7175(5) 0.23440(14) 0.0449(11) Uani 1 1 d . . . H29 H 0.5872 0.6837 0.2336 0.054 Uiso 1 1 calc R . . C30 C 0.4609(5) 0.8169(5) 0.26989(14) 0.0404(11) Uani 1 1 d . . . C31 C 0.3105(5) 0.8729(5) 0.26800(13) 0.0391(10) Uani 1 1 d . . . H31 H 0.2906 0.9453 0.2900 0.047 Uiso 1 1 calc R . . C32 C 0.1919(5) 0.8222(5) 0.23410(14) 0.0384(10) Uani 1 1 d . . . C33 C -0.0071(4) 0.7656(5) 0.14731(15) 0.0393(11) Uani 1 1 d . . . C34 C -0.0589(5) 0.7606(5) 0.10106(14) 0.0453(12) Uani 1 1 d . . . H34 H -0.0285 0.6842 0.0819 0.054 Uiso 1 1 calc R . . C35 C -0.1562(5) 0.8698(6) 0.08336(16) 0.0550(13) Uani 1 1 d . . . H35 H -0.1921 0.8643 0.0524 0.066 Uiso 1 1 calc R . . C36 C -0.2005(5) 0.9850(6) 0.11040(17) 0.0588(14) Uani 1 1 d . . . H36 H -0.2653 1.0576 0.0980 0.071 Uiso 1 1 calc R . . C37 C -0.1477(5) 0.9925(5) 0.15647(16) 0.0519(12) Uani 1 1 d . . . H37 H -0.1752 1.0720 0.1750 0.062 Uiso 1 1 calc R . . C38 C -0.0552(4) 0.8833(5) 0.17495(14) 0.0370(10) Uani 1 1 d . . . C39 C 0.1008(5) 0.5080(5) 0.14302(15) 0.0482(12) Uani 1 1 d . . . H39A H 0.1916 0.5201 0.1249 0.058 Uiso 1 1 calc R . . H39B H 0.0052 0.4842 0.1221 0.058 Uiso 1 1 calc R . . C40 C 0.1180(5) 0.3716(5) 0.17479(15) 0.0571(13) Uani 1 1 d . . . H40A H 0.1232 0.2780 0.1570 0.086 Uiso 1 1 calc R . . H40B H 0.0277 0.3577 0.1925 0.086 Uiso 1 1 calc R . . H40C H 0.2141 0.3929 0.1950 0.086 Uiso 1 1 calc R . . C41 C 0.5866(5) 0.8580(5) 0.30732(14) 0.0448(11) Uani 1 1 d . . . H41 H 0.6852 0.8229 0.3038 0.054 Uiso 1 1 calc R . . C42 C 0.5763(5) 0.9382(5) 0.34508(15) 0.0474(12) Uani 1 1 d . . . H42 H 0.4799 0.9779 0.3485 0.057 Uiso 1 1 calc R . . C43 C 0.7036(5) 0.9707(5) 0.38239(14) 0.0471(12) Uani 1 1 d . . . C44 C 0.6995(6) 1.0768(6) 0.41998(16) 0.0625(14) Uani 1 1 d . . . H44 H 0.6127 1.1402 0.4250 0.075 Uiso 1 1 calc R . . C45 C 0.8427(7) 1.0756(7) 0.44807(17) 0.0732(17) Uani 1 1 d . . . H45 H 0.8729 1.1383 0.4763 0.088 Uiso 1 1 calc R . . C46 C 0.9345(6) 0.9704(7) 0.42943(18) 0.0740(17) Uani 1 1 d . . . H46 H 1.0401 0.9466 0.4422 0.089 Uiso 1 1 calc R . . C47 C 0.8491(5) 0.9030(6) 0.38879(16) 0.0605(14) Uani 1 1 d . . . H47 H 0.8848 0.8245 0.3687 0.073 Uiso 1 1 calc R . . C48 C 0.5348(8) 0.7865(8) 0.4795(3) 0.107(2) Uani 1 1 d . . . H48 H 0.4436 0.8446 0.4839 0.129 Uiso 1 1 calc R . . C49 C 0.6748(14) 0.7955(11) 0.5071(3) 0.146(4) Uani 1 1 d U . . H49 H 0.7002 0.8617 0.5348 0.175 Uiso 1 1 calc R . . C50 C 0.7684(9) 0.6993(11) 0.4914(3) 0.138(3) Uani 1 1 d U . . H50 H 0.8747 0.6826 0.5054 0.165 Uiso 1 1 calc R . . C51 C 0.6911(8) 0.6229(7) 0.4502(3) 0.099(2) Uani 1 1 d . . . H51 H 0.7309 0.5433 0.4314 0.118 Uiso 1 1 calc R . . C52 C 0.5443(6) 0.6808(7) 0.44456(18) 0.0669(15) Uani 1 1 d . . . H52 H 0.4610 0.6521 0.4195 0.080 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 0.0537(4) 0.0560(5) 0.0400(4) 0.0024(3) 0.0020(3) 0.0136(3) Fe2 0.0544(4) 0.0749(6) 0.0420(4) 0.0084(4) -0.0088(3) -0.0074(4) N1 0.047(2) 0.032(2) 0.056(3) 0.0085(19) 0.0015(19) -0.0062(18) N2 0.044(2) 0.037(2) 0.040(2) -0.0072(17) -0.0015(18) 0.0048(18) S1 0.0469(7) 0.0583(9) 0.0498(8) 0.0106(6) 0.0043(6) -0.0099(6) S2 0.0447(7) 0.0567(8) 0.0427(7) -0.0068(6) 0.0041(5) 0.0151(6) C1 0.034(2) 0.034(3) 0.048(3) 0.003(2) 0.002(2) 0.009(2) C2 0.047(3) 0.041(3) 0.062(3) 0.013(3) 0.011(3) -0.005(2) C3 0.046(3) 0.052(3) 0.046(3) 0.010(2) 0.004(2) 0.007(2) C4 0.036(2) 0.043(3) 0.044(3) 0.003(2) 0.007(2) 0.008(2) C5 0.033(2) 0.039(3) 0.052(3) 0.005(2) 0.006(2) 0.000(2) C6 0.034(2) 0.033(3) 0.046(3) 0.001(2) 0.005(2) 0.001(2) C7 0.045(3) 0.043(3) 0.038(3) -0.002(2) 0.004(2) 0.005(2) C8 0.044(3) 0.052(3) 0.051(3) -0.005(2) 0.000(2) -0.004(2) C9 0.047(3) 0.084(4) 0.059(4) -0.014(3) -0.011(3) 0.009(3) C10 0.066(4) 0.070(4) 0.046(3) -0.006(3) -0.002(3) 0.013(3) C11 0.063(3) 0.047(3) 0.045(3) 0.001(2) 0.013(3) 0.010(3) C12 0.047(3) 0.042(3) 0.038(3) -0.003(2) 0.011(2) 0.005(2) C13 0.069(3) 0.039(3) 0.083(4) 0.004(3) -0.007(3) -0.008(3) C14 0.094(4) 0.046(4) 0.123(5) -0.025(3) -0.002(4) 0.001(3) C15 0.042(3) 0.045(3) 0.047(3) 0.005(2) 0.006(2) 0.010(2) C16 0.046(3) 0.057(3) 0.052(3) 0.007(3) 0.007(2) 0.002(2) C17 0.047(3) 0.049(3) 0.044(3) 0.007(2) 0.004(2) 0.009(2) C18 0.059(3) 0.052(3) 0.051(3) 0.013(2) 0.000(3) 0.011(3) C19 0.058(3) 0.050(3) 0.068(4) -0.001(3) -0.011(3) 0.007(3) C20 0.069(3) 0.073(4) 0.042(3) -0.005(3) -0.002(3) 0.023(3) C21 0.060(3) 0.057(3) 0.046(3) 0.004(3) 0.012(3) 0.007(3) C22 0.092(5) 0.075(5) 0.084(5) -0.039(4) -0.016(4) 0.038(4) C23 0.087(4) 0.102(5) 0.053(4) -0.009(4) 0.010(4) 0.029(4) C24 0.070(4) 0.096(5) 0.080(5) -0.003(4) 0.020(4) 0.018(3) C25 0.068(4) 0.082(5) 0.067(4) 0.013(4) 0.000(3) 0.035(3) C26 0.086(4) 0.051(4) 0.113(6) 0.013(4) 0.030(4) 0.021(3) C27 0.041(3) 0.034(3) 0.037(3) 0.001(2) 0.000(2) 0.002(2) C28 0.048(3) 0.049(3) 0.036(3) -0.007(2) 0.002(2) 0.009(2) C29 0.047(3) 0.047(3) 0.043(3) -0.001(2) 0.006(2) 0.014(2) C30 0.047(3) 0.039(3) 0.035(3) 0.005(2) 0.000(2) 0.004(2) C31 0.049(3) 0.037(3) 0.033(3) -0.001(2) 0.005(2) 0.006(2) C32 0.046(3) 0.034(3) 0.037(3) 0.001(2) 0.007(2) 0.010(2) C33 0.032(2) 0.041(3) 0.044(3) 0.000(2) 0.001(2) 0.000(2) C34 0.043(3) 0.050(3) 0.043(3) -0.006(2) 0.003(2) 0.003(2) C35 0.047(3) 0.071(4) 0.046(3) 0.005(3) -0.003(2) 0.007(3) C36 0.046(3) 0.069(4) 0.062(4) 0.003(3) -0.009(3) 0.022(3) C37 0.041(3) 0.051(3) 0.064(4) -0.005(3) 0.001(2) 0.008(2) C38 0.029(2) 0.038(3) 0.044(3) -0.004(2) 0.003(2) 0.004(2) C39 0.054(3) 0.039(3) 0.051(3) -0.011(2) 0.006(2) 0.001(2) C40 0.066(3) 0.040(3) 0.067(3) -0.005(3) 0.015(3) 0.007(2) C41 0.041(3) 0.056(3) 0.039(3) 0.003(2) 0.003(2) 0.011(2) C42 0.041(3) 0.060(3) 0.042(3) 0.003(2) 0.002(2) 0.010(2) C43 0.042(3) 0.063(3) 0.035(3) 0.007(2) -0.003(2) 0.008(2) C44 0.072(3) 0.063(4) 0.050(3) 0.000(3) -0.004(3) 0.003(3) C45 0.088(4) 0.078(4) 0.043(3) 0.006(3) -0.013(3) -0.026(3) C46 0.048(3) 0.105(5) 0.061(4) 0.019(3) -0.011(3) -0.014(3) C47 0.047(3) 0.083(4) 0.051(3) 0.008(3) 0.000(3) 0.009(3) C48 0.100(5) 0.109(6) 0.115(6) 0.004(5) 0.058(5) -0.017(5) C49 0.196(8) 0.153(7) 0.065(5) 0.022(5) 0.003(5) -0.088(6) C50 0.099(5) 0.143(7) 0.149(7) 0.096(5) -0.057(5) -0.037(5) C51 0.094(5) 0.071(5) 0.135(6) 0.027(4) 0.023(5) 0.015(4) C52 0.061(4) 0.075(4) 0.059(4) -0.004(3) -0.001(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C26 2.010(5) . ? Fe1 C25 2.016(5) . ? Fe1 C21 2.019(4) . ? Fe1 C18 2.022(4) . ? Fe1 C22 2.028(5) . ? Fe1 C19 2.029(5) . ? Fe1 C20 2.030(4) . ? Fe1 C23 2.037(5) . ? Fe1 C24 2.040(5) . ? Fe1 C17 2.053(4) . ? Fe2 C49 2.001(8) . ? Fe2 C50 2.008(7) . ? Fe2 C45 2.017(5) . ? Fe2 C46 2.022(5) . ? Fe2 C48 2.026(6) . ? Fe2 C44 2.030(5) . ? Fe2 C51 2.031(6) . ? Fe2 C52 2.033(5) . ? Fe2 C47 2.038(5) . ? Fe2 C43 2.059(4) . ? N1 C7 1.406(5) . ? N1 C1 1.417(5) . ? N1 C13 1.464(5) . ? N2 C27 1.415(5) . ? N2 C33 1.417(5) . ? N2 C39 1.466(5) . ? S1 C6 1.760(4) . ? S1 C12 1.769(4) . ? S2 C32 1.766(4) . ? S2 C38 1.770(4) . ? C1 C2 1.390(5) . ? C1 C6 1.396(5) . ? C2 C3 1.377(5) . ? C3 C4 1.388(5) . ? C4 C5 1.390(5) . ? C4 C15 1.463(5) . ? C5 C6 1.381(5) . ? C7 C8 1.388(5) . ? C7 C12 1.391(6) . ? C8 C9 1.378(6) . ? C9 C10 1.366(6) . ? C10 C11 1.380(6) . ? C11 C12 1.385(6) . ? C13 C14 1.520(6) . ? C15 C16 1.329(5) . ? C16 C17 1.457(6) . ? C17 C21 1.414(6) . ? C17 C18 1.415(6) . ? C18 C19 1.413(6) . ? C19 C20 1.401(6) . ? C20 C21 1.417(6) . ? C22 C23 1.397(8) . ? C22 C26 1.438(7) . ? C23 C24 1.373(7) . ? C24 C25 1.376(7) . ? C25 C26 1.398(7) . ? C27 C28 1.386(5) . ? C27 C32 1.403(5) . ? C28 C29 1.377(5) . ? C29 C30 1.386(5) . ? C30 C31 1.404(5) . ? C30 C41 1.469(5) . ? C31 C32 1.378(5) . ? C33 C34 1.387(5) . ? C33 C38 1.405(5) . ? C34 C35 1.388(5) . ? C35 C36 1.365(6) . ? C36 C37 1.383(6) . ? C37 C38 1.371(5) . ? C39 C40 1.517(5) . ? C41 C42 1.312(5) . ? C42 C43 1.466(5) . ? C43 C47 1.415(6) . ? C43 C44 1.428(6) . ? C44 C45 1.403(6) . ? C45 C46 1.391(7) . ? C46 C47 1.420(6) . ? C48 C49 1.366(10) . ? C48 C52 1.375(7) . ? C49 C50 1.312(11) . ? C50 C51 1.436(10) . ? C51 C52 1.383(7) . ? 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 C26 Fe1 C25 40.6(2) . . ? C26 Fe1 C21 107.7(2) . . ? C25 Fe1 C21 125.4(2) . . ? C26 Fe1 C18 160.2(3) . . ? C25 Fe1 C18 157.3(2) . . ? C21 Fe1 C18 68.33(19) . . ? C26 Fe1 C22 41.7(2) . . ? C25 Fe1 C22 68.5(2) . . ? C21 Fe1 C22 121.8(3) . . ? C18 Fe1 C22 122.5(2) . . ? C26 Fe1 C19 157.6(3) . . ? C25 Fe1 C19 122.3(2) . . ? C21 Fe1 C19 68.6(2) . . ? C18 Fe1 C19 40.81(17) . . ? C22 Fe1 C19 159.2(3) . . ? C26 Fe1 C20 122.4(2) . . ? C25 Fe1 C20 109.0(2) . . ? C21 Fe1 C20 40.98(17) . . ? C18 Fe1 C20 68.23(19) . . ? C22 Fe1 C20 158.6(3) . . ? C19 Fe1 C20 40.37(18) . . ? C26 Fe1 C23 68.3(2) . . ? C25 Fe1 C23 67.1(2) . . ? C21 Fe1 C23 157.3(2) . . ? C18 Fe1 C23 107.4(2) . . ? C22 Fe1 C23 40.2(2) . . ? C19 Fe1 C23 123.8(3) . . ? C20 Fe1 C23 160.2(3) . . ? C26 Fe1 C24 67.6(2) . . ? C25 Fe1 C24 39.7(2) . . ? C21 Fe1 C24 161.7(2) . . ? C18 Fe1 C24 122.2(2) . . ? C22 Fe1 C24 67.3(2) . . ? C19 Fe1 C24 108.7(2) . . ? C20 Fe1 C24 125.3(2) . . ? C23 Fe1 C24 39.36(19) . . ? C26 Fe1 C17 123.8(2) . . ? C25 Fe1 C17 161.3(2) . . ? C21 Fe1 C17 40.64(16) . . ? C18 Fe1 C17 40.63(16) . . ? C22 Fe1 C17 106.6(2) . . ? C19 Fe1 C17 68.63(18) . . ? C20 Fe1 C17 68.55(18) . . ? C23 Fe1 C17 121.6(2) . . ? C24 Fe1 C17 156.8(2) . . ? C49 Fe2 C50 38.2(3) . . ? C49 Fe2 C45 108.4(3) . . ? C50 Fe2 C45 121.0(3) . . ? C49 Fe2 C46 123.5(3) . . ? C50 Fe2 C46 107.6(3) . . ? C45 Fe2 C46 40.3(2) . . ? C49 Fe2 C48 39.6(3) . . ? C50 Fe2 C48 65.6(3) . . ? C45 Fe2 C48 125.4(3) . . ? C46 Fe2 C48 160.1(3) . . ? C49 Fe2 C44 123.1(4) . . ? C50 Fe2 C44 156.1(4) . . ? C45 Fe2 C44 40.56(18) . . ? C46 Fe2 C44 68.2(2) . . ? C48 Fe2 C44 109.9(3) . . ? C49 Fe2 C51 67.6(3) . . ? C50 Fe2 C51 41.6(3) . . ? C45 Fe2 C51 156.7(3) . . ? C46 Fe2 C51 121.3(3) . . ? C48 Fe2 C51 67.2(3) . . ? C44 Fe2 C51 161.0(3) . . ? C49 Fe2 C52 66.6(3) . . ? C50 Fe2 C52 66.9(3) . . ? C45 Fe2 C52 161.7(3) . . ? C46 Fe2 C52 157.4(3) . . ? C48 Fe2 C52 39.6(2) . . ? C44 Fe2 C52 125.9(2) . . ? C51 Fe2 C52 39.8(2) . . ? C49 Fe2 C47 159.5(4) . . ? C50 Fe2 C47 124.7(3) . . ? C45 Fe2 C47 68.4(2) . . ? C46 Fe2 C47 40.93(18) . . ? C48 Fe2 C47 158.4(3) . . ? C44 Fe2 C47 68.6(2) . . ? C51 Fe2 C47 106.9(2) . . ? C52 Fe2 C47 122.7(2) . . ? C49 Fe2 C43 159.1(4) . . ? C50 Fe2 C43 161.5(4) . . ? C45 Fe2 C43 68.24(19) . . ? C46 Fe2 C43 68.17(19) . . ? C48 Fe2 C43 124.2(3) . . ? C44 Fe2 C43 40.87(16) . . ? C51 Fe2 C43 123.9(2) . . ? C52 Fe2 C43 109.66(19) . . ? C47 Fe2 C43 40.40(16) . . ? C7 N1 C1 117.2(3) . . ? C7 N1 C13 118.8(4) . . ? C1 N1 C13 118.2(4) . . ? C27 N2 C33 117.4(3) . . ? C27 N2 C39 119.0(3) . . ? C33 N2 C39 119.3(3) . . ? C6 S1 C12 98.6(2) . . ? C32 S2 C38 99.22(19) . . ? C2 C1 C6 117.9(4) . . ? C2 C1 N1 123.3(4) . . ? C6 C1 N1 118.8(4) . . ? C3 C2 C1 121.4(4) . . ? C2 C3 C4 121.0(4) . . ? C3 C4 C5 117.6(4) . . ? C3 C4 C15 123.8(4) . . ? C5 C4 C15 118.5(4) . . ? C6 C5 C4 121.7(4) . . ? C5 C6 C1 120.2(4) . . ? C5 C6 S1 120.9(3) . . ? C1 C6 S1 118.8(3) . . ? C8 C7 C12 117.8(4) . . ? C8 C7 N1 122.8(4) . . ? C12 C7 N1 119.3(4) . . ? C9 C8 C7 120.5(5) . . ? C10 C9 C8 121.0(5) . . ? C9 C10 C11 119.7(5) . . ? C10 C11 C12 119.4(5) . . ? C11 C12 C7 121.4(4) . . ? C11 C12 S1 120.1(4) . . ? C7 C12 S1 118.5(3) . . ? N1 C13 C14 112.0(4) . . ? C16 C15 C4 128.8(4) . . ? C15 C16 C17 124.6(4) . . ? C21 C17 C18 106.7(4) . . ? C21 C17 C16 126.6(4) . . ? C18 C17 C16 126.5(4) . . ? C21 C17 Fe1 68.4(2) . . ? C18 C17 Fe1 68.5(2) . . ? C16 C17 Fe1 124.4(3) . . ? C19 C18 C17 108.9(4) . . ? C19 C18 Fe1 69.9(3) . . ? C17 C18 Fe1 70.9(3) . . ? C20 C19 C18 107.8(4) . . ? C20 C19 Fe1 69.8(3) . . ? C18 C19 Fe1 69.3(3) . . ? C19 C20 C21 108.0(4) . . ? C19 C20 Fe1 69.8(3) . . ? C21 C20 Fe1 69.1(3) . . ? C17 C21 C20 108.6(4) . . ? C17 C21 Fe1 71.0(3) . . ? C20 C21 Fe1 69.9(3) . . ? C23 C22 C26 106.5(5) . . ? C23 C22 Fe1 70.3(3) . . ? C26 C22 Fe1 68.5(3) . . ? C24 C23 C22 108.9(6) . . ? C24 C23 Fe1 70.4(3) . . ? C22 C23 Fe1 69.5(3) . . ? C23 C24 C25 109.1(6) . . ? C23 C24 Fe1 70.2(3) . . ? C25 C24 Fe1 69.2(3) . . ? C24 C25 C26 108.6(5) . . ? C24 C25 Fe1 71.1(3) . . ? C26 C25 Fe1 69.5(3) . . ? C25 C26 C22 106.8(5) . . ? C25 C26 Fe1 69.9(3) . . ? C22 C26 Fe1 69.8(3) . . ? C28 C27 C32 117.4(4) . . ? C28 C27 N2 122.3(4) . . ? C32 C27 N2 120.3(4) . . ? C29 C28 C27 120.7(4) . . ? C28 C29 C30 122.6(4) . . ? C29 C30 C31 116.6(4) . . ? C29 C30 C41 120.4(4) . . ? C31 C30 C41 123.0(4) . . ? C32 C31 C30 121.1(4) . . ? C31 C32 C27 121.3(4) . . ? C31 C32 S2 120.2(3) . . ? C27 C32 S2 118.5(3) . . ? C34 C33 C38 118.2(4) . . ? C34 C33 N2 122.4(4) . . ? C38 C33 N2 119.4(4) . . ? C33 C34 C35 119.9(4) . . ? C36 C35 C34 121.4(4) . . ? C35 C36 C37 119.2(4) . . ? C38 C37 C36 120.4(4) . . ? C37 C38 C33 120.9(4) . . ? C37 C38 S2 120.2(3) . . ? C33 C38 S2 118.9(3) . . ? N2 C39 C40 113.1(4) . . ? C42 C41 C30 127.7(4) . . ? C41 C42 C43 125.7(4) . . ? C47 C43 C44 107.4(4) . . ? C47 C43 C42 127.6(4) . . ? C44 C43 C42 125.0(4) . . ? C47 C43 Fe2 69.0(3) . . ? C44 C43 Fe2 68.5(3) . . ? C42 C43 Fe2 126.8(3) . . ? C45 C44 C43 107.8(5) . . ? C45 C44 Fe2 69.2(3) . . ? C43 C44 Fe2 70.7(3) . . ? C46 C45 C44 108.8(5) . . ? C46 C45 Fe2 70.0(3) . . ? C44 C45 Fe2 70.2(3) . . ? C45 C46 C47 108.4(5) . . ? C45 C46 Fe2 69.7(3) . . ? C47 C46 Fe2 70.2(3) . . ? C43 C47 C46 107.6(5) . . ? C43 C47 Fe2 70.6(3) . . ? C46 C47 Fe2 68.9(3) . . ? C49 C48 C52 107.9(7) . . ? C49 C48 Fe2 69.2(4) . . ? C52 C48 Fe2 70.5(3) . . ? C50 C49 C48 109.5(8) . . ? C50 C49 Fe2 71.2(5) . . ? C48 C49 Fe2 71.1(4) . . ? C49 C50 C51 109.3(8) . . ? C49 C50 Fe2 70.6(5) . . ? C51 C50 Fe2 70.0(4) . . ? C52 C51 C50 104.4(6) . . ? C52 C51 Fe2 70.2(3) . . ? C50 C51 Fe2 68.3(4) . . ? C48 C52 C51 108.9(6) . . ? C48 C52 Fe2 69.9(3) . . ? C51 C52 Fe2 70.0(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.584 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.066 #==========================================================end data_ccdc299717 _database_code_depnum_ccdc_archive 'CCDC 299717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H25 Cl2 Fe I3 N' _chemical_formula_weight 870.93 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' I I -0.4742 1.8119 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.060(2) _cell_length_b 9.176(2) _cell_length_c 18.634(4) _cell_angle_alpha 86.787(4) _cell_angle_beta 78.170(3) _cell_angle_gamma 77.194(4) _cell_volume 1478.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1779 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 21.804 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 1.902 _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 3.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2711 _exptl_absorpt_correction_T_max 0.6352 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 7814 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5143 _reflns_number_gt 2662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5143 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.24643(12) 1.20286(12) 0.64061(6) 0.0542(3) Uani 1 1 d . . . Cl1 Cl 0.4735(4) 0.6158(3) 0.63699(18) 0.1415(12) Uani 1 1 d . . . Cl2 Cl 0.6062(3) 0.3726(4) 0.72312(18) 0.1298(11) Uani 1 1 d . . . I1 I 0.08092(6) 0.19035(6) 0.36142(3) 0.06524(19) Uani 1 1 d . . . I2 I -0.14409(7) 0.30926(7) 0.48880(4) 0.0890(2) Uani 1 1 d . . . I3 I 0.31243(6) 0.07005(7) 0.23045(4) 0.0857(2) Uani 1 1 d . . . N1 N 0.1981(8) 0.3662(8) 0.9488(4) 0.069(2) Uani 1 1 d . . . C1 C 0.2199(11) 0.4985(10) 0.9167(4) 0.067(2) Uani 1 1 d . . . C2 C 0.3355(11) 0.5767(11) 0.9171(5) 0.084(3) Uani 1 1 d . . . H2 H 0.4168 0.5367 0.9407 0.101 Uiso 1 1 calc R . . C3 C 0.3278(13) 0.7119(12) 0.8829(5) 0.093(3) Uani 1 1 d . . . H3 H 0.4038 0.7645 0.8845 0.112 Uiso 1 1 calc R . . C4 C 0.2119(15) 0.7737(11) 0.8459(5) 0.091(4) Uani 1 1 d . . . C5 C 0.0952(10) 0.6972(10) 0.8455(4) 0.068(2) Uani 1 1 d . . . H5 H 0.0152 0.7384 0.8213 0.082 Uiso 1 1 calc R . . C6 C 0.0980(9) 0.5606(10) 0.8808(4) 0.061(2) Uani 1 1 d . . . C7 C 0.0019(10) 0.4518(10) 0.8914(4) 0.063(2) Uani 1 1 d . . . C8 C -0.1295(12) 0.4469(12) 0.8672(5) 0.082(3) Uani 1 1 d . . . H8 H -0.1751 0.5255 0.8397 0.099 Uiso 1 1 calc R . . C9 C -0.1936(12) 0.3218(16) 0.8843(6) 0.101(4) Uani 1 1 d . . . H9 H -0.2816 0.3155 0.8674 0.121 Uiso 1 1 calc R . . C10 C -0.1272(14) 0.2072(13) 0.9264(6) 0.100(3) Uani 1 1 d . . . H10 H -0.1738 0.1259 0.9378 0.120 Uiso 1 1 calc R . . C11 C 0.0053(12) 0.2074(11) 0.9523(5) 0.082(3) Uani 1 1 d . . . H11 H 0.0495 0.1289 0.9802 0.098 Uiso 1 1 calc R . . C12 C 0.0676(10) 0.3324(10) 0.9339(4) 0.063(2) Uani 1 1 d . . . C13 C 0.3027(11) 0.2745(10) 0.9935(6) 0.095(3) Uani 1 1 d . . . H13A H 0.3520 0.3381 1.0163 0.114 Uiso 1 1 calc R . . H13B H 0.2445 0.2222 1.0320 0.114 Uiso 1 1 calc R . . C14 C 0.4189(14) 0.1677(12) 0.9457(6) 0.138(4) Uani 1 1 d . . . H14A H 0.4891 0.1087 0.9738 0.207 Uiso 1 1 calc R . . H14B H 0.4748 0.2204 0.9074 0.207 Uiso 1 1 calc R . . H14C H 0.3693 0.1034 0.9245 0.207 Uiso 1 1 calc R . . C15 C 0.2181(12) 0.9313(15) 0.8109(6) 0.107(4) Uani 1 1 d . . . H15 H 0.2973 0.9768 0.8161 0.128 Uiso 1 1 calc R . . C16 C 0.1242(12) 0.9931(13) 0.7782(5) 0.100(4) Uani 1 1 d . . . H16 H 0.0461 0.9475 0.7716 0.120 Uiso 1 1 calc R . . C17 C 0.1313(11) 1.1521(9) 0.7460(5) 0.068(3) Uani 1 1 d . . . C18 C 0.2253(10) 1.2531(10) 0.7497(4) 0.069(2) Uani 1 1 d . . . H18 H 0.3068 1.2384 0.7744 0.083 Uiso 1 1 calc R . . C19 C 0.1728(11) 1.3809(9) 0.7090(5) 0.075(3) Uani 1 1 d . . . H19 H 0.2140 1.4661 0.7026 0.090 Uiso 1 1 calc R . . C20 C 0.0509(10) 1.3601(9) 0.6801(5) 0.074(3) Uani 1 1 d . . . H20 H -0.0039 1.4287 0.6513 0.089 Uiso 1 1 calc R . . C21 C 0.0230(10) 1.2168(10) 0.7017(5) 0.073(3) Uani 1 1 d . . . H21 H -0.0518 1.1735 0.6892 0.088 Uiso 1 1 calc R . . C22 C 0.4730(13) 1.110(2) 0.5944(6) 0.118(5) Uani 1 1 d . . . H22 H 0.5540 1.0916 0.6197 0.141 Uiso 1 1 calc R . . C23 C 0.379(2) 1.0120(12) 0.5862(7) 0.126(6) Uani 1 1 d . . . H23 H 0.3872 0.9149 0.6046 0.152 Uiso 1 1 calc R . . C24 C 0.2734(14) 1.0869(15) 0.5456(6) 0.102(4) Uani 1 1 d . . . H24 H 0.1966 1.0482 0.5321 0.123 Uiso 1 1 calc R . . C25 C 0.2996(11) 1.2250(13) 0.5287(5) 0.081(3) Uani 1 1 d . . . H25 H 0.2432 1.2967 0.5018 0.097 Uiso 1 1 calc R . . C26 C 0.4208(12) 1.2434(13) 0.5570(6) 0.087(3) Uani 1 1 d . . . H26 H 0.4620 1.3285 0.5525 0.105 Uiso 1 1 calc R . . C27 C 0.5807(14) 0.5598(13) 0.7033(6) 0.142(5) Uani 1 1 d . . . H27A H 0.6812 0.5844 0.6872 0.170 Uiso 1 1 calc R . . H27B H 0.5302 0.6151 0.7477 0.170 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 0.0590(7) 0.0499(7) 0.0487(7) -0.0033(5) -0.0006(5) -0.0101(5) Cl1 0.195(3) 0.097(2) 0.142(3) 0.038(2) -0.044(3) -0.052(2) Cl2 0.114(2) 0.126(3) 0.157(3) 0.017(2) -0.059(2) -0.0187(19) I1 0.0648(4) 0.0616(4) 0.0783(4) 0.0041(3) -0.0265(3) -0.0222(3) I2 0.0773(4) 0.0943(5) 0.0978(5) -0.0129(4) -0.0113(4) -0.0257(4) I3 0.0631(4) 0.0950(5) 0.0982(5) -0.0066(4) -0.0114(3) -0.0178(3) N1 0.071(5) 0.059(5) 0.071(5) 0.019(4) -0.015(4) -0.007(4) C1 0.088(7) 0.056(6) 0.049(5) 0.006(5) -0.006(5) -0.006(5) C2 0.100(8) 0.076(7) 0.078(7) 0.015(6) -0.027(6) -0.019(6) C3 0.117(9) 0.094(8) 0.072(7) 0.006(6) -0.010(6) -0.040(7) C4 0.147(11) 0.060(7) 0.054(6) 0.016(5) 0.016(7) -0.034(7) C5 0.084(7) 0.071(6) 0.036(5) 0.001(5) -0.001(4) 0.003(5) C6 0.063(6) 0.067(6) 0.043(5) 0.007(4) -0.001(4) -0.003(5) C7 0.064(6) 0.079(7) 0.037(5) -0.001(4) -0.002(4) -0.001(5) C8 0.088(8) 0.095(8) 0.055(6) -0.013(5) -0.008(6) -0.003(6) C9 0.075(7) 0.158(12) 0.075(8) -0.018(8) -0.012(6) -0.033(8) C10 0.107(9) 0.109(9) 0.082(8) -0.014(7) 0.015(7) -0.048(8) C11 0.084(7) 0.085(7) 0.071(7) -0.001(5) -0.001(6) -0.016(6) C12 0.069(6) 0.065(6) 0.048(5) -0.004(5) 0.000(5) -0.011(5) C13 0.103(8) 0.071(7) 0.109(8) 0.007(6) -0.027(7) -0.007(6) C14 0.148(11) 0.105(9) 0.157(12) 0.016(9) -0.049(9) -0.007(8) C15 0.077(8) 0.164(13) 0.073(8) -0.049(8) -0.003(6) -0.012(8) C16 0.081(8) 0.138(11) 0.074(8) -0.034(7) -0.006(6) -0.008(7) C17 0.080(7) 0.046(5) 0.059(6) 0.005(5) 0.021(5) -0.007(5) C18 0.079(6) 0.074(7) 0.052(5) -0.018(5) 0.000(5) -0.022(5) C19 0.089(7) 0.048(6) 0.075(6) -0.027(5) 0.030(6) -0.025(5) C20 0.062(6) 0.048(6) 0.094(7) 0.002(5) 0.007(5) 0.004(5) C21 0.062(6) 0.062(6) 0.088(7) -0.004(5) 0.006(5) -0.014(5) C22 0.073(8) 0.185(15) 0.060(7) -0.026(10) -0.004(6) 0.041(9) C23 0.185(15) 0.056(8) 0.075(9) -0.011(6) 0.047(10) 0.041(9) C24 0.137(11) 0.087(9) 0.077(8) -0.033(7) 0.009(7) -0.033(8) C25 0.087(8) 0.093(8) 0.057(6) 0.007(5) -0.005(5) -0.018(6) C26 0.062(7) 0.114(9) 0.087(8) -0.035(7) 0.029(6) -0.052(7) C27 0.185(13) 0.136(11) 0.143(11) 0.003(9) -0.075(10) -0.075(10) _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 C19 2.035(8) . ? Fe1 C25 2.050(8) . ? Fe1 C20 2.052(7) . ? Fe1 C26 2.061(8) . ? Fe1 C24 2.061(10) . ? Fe1 C22 2.064(10) . ? Fe1 C18 2.071(8) . ? Fe1 C23 2.076(10) . ? Fe1 C21 2.090(8) . ? Fe1 C17 2.106(8) . ? Cl1 C27 1.713(11) . ? Cl2 C27 1.711(11) . ? I1 I2 2.8810(9) . ? I1 I3 2.9581(9) . ? N1 C1 1.358(9) . ? N1 C12 1.371(10) . ? N1 C13 1.481(10) . ? C1 C2 1.396(12) . ? C1 C6 1.404(11) . ? C2 C3 1.357(12) . ? C2 H2 0.9300 . ? C3 C4 1.374(13) . ? C3 H3 0.9300 . ? C4 C5 1.394(12) . ? C4 C15 1.560(14) . ? C5 C6 1.381(10) . ? C5 H5 0.9300 . ? C6 C7 1.445(11) . ? C7 C8 1.367(12) . ? C7 C12 1.410(10) . ? C8 C9 1.391(13) . ? C8 H8 0.9300 . ? C9 C10 1.379(13) . ? C9 H9 0.9300 . ? C10 C11 1.383(13) . ? C10 H10 0.9300 . ? C11 C12 1.384(11) . ? C11 H11 0.9300 . ? C13 C14 1.455(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.174(11) . ? C15 H15 0.9300 . ? C16 C17 1.555(13) . ? C16 H16 0.9300 . ? C17 C18 1.404(11) . ? C17 C21 1.421(11) . ? C18 C19 1.406(11) . ? C18 H18 0.9300 . ? C19 C20 1.376(11) . ? C19 H19 0.9300 . ? C20 C21 1.414(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.403(16) . ? C22 C26 1.407(14) . ? C22 H22 0.9300 . ? C23 C24 1.384(16) . ? C23 H23 0.9300 . ? C24 C25 1.349(12) . ? C24 H24 0.9300 . ? C25 C26 1.357(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? 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 C19 Fe1 C25 122.9(4) . . ? C19 Fe1 C20 39.4(3) . . ? C25 Fe1 C20 108.7(4) . . ? C19 Fe1 C26 109.6(4) . . ? C25 Fe1 C26 38.6(3) . . ? C20 Fe1 C26 123.8(4) . . ? C19 Fe1 C24 156.5(5) . . ? C25 Fe1 C24 38.3(4) . . ? C20 Fe1 C24 122.7(5) . . ? C26 Fe1 C24 64.9(4) . . ? C19 Fe1 C22 126.0(6) . . ? C25 Fe1 C22 65.7(4) . . ? C20 Fe1 C22 160.2(6) . . ? C26 Fe1 C22 39.9(4) . . ? C24 Fe1 C22 65.8(5) . . ? C19 Fe1 C18 40.1(3) . . ? C25 Fe1 C18 158.3(4) . . ? C20 Fe1 C18 66.8(4) . . ? C26 Fe1 C18 124.7(4) . . ? C24 Fe1 C18 162.2(5) . . ? C22 Fe1 C18 110.8(4) . . ? C19 Fe1 C23 162.4(7) . . ? C25 Fe1 C23 65.2(4) . . ? C20 Fe1 C23 157.6(7) . . ? C26 Fe1 C23 66.1(4) . . ? C24 Fe1 C23 39.1(4) . . ? C22 Fe1 C23 39.6(4) . . ? C18 Fe1 C23 127.0(5) . . ? C19 Fe1 C21 66.6(3) . . ? C25 Fe1 C21 124.4(4) . . ? C20 Fe1 C21 39.9(3) . . ? C26 Fe1 C21 158.9(5) . . ? C24 Fe1 C21 109.7(4) . . ? C22 Fe1 C21 159.1(6) . . ? C18 Fe1 C21 66.8(3) . . ? C23 Fe1 C21 123.8(5) . . ? C19 Fe1 C17 66.1(3) . . ? C25 Fe1 C17 160.6(4) . . ? C20 Fe1 C17 66.3(3) . . ? C26 Fe1 C17 160.0(5) . . ? C24 Fe1 C17 127.0(4) . . ? C22 Fe1 C17 125.3(5) . . ? C18 Fe1 C17 39.3(3) . . ? C23 Fe1 C17 111.7(4) . . ? C21 Fe1 C17 39.6(3) . . ? I2 I1 I3 179.65(3) . . ? C1 N1 C12 110.5(7) . . ? C1 N1 C13 123.5(8) . . ? C12 N1 C13 126.0(7) . . ? N1 C1 C2 130.6(9) . . ? N1 C1 C6 109.7(9) . . ? C2 C1 C6 119.6(8) . . ? C3 C2 C1 119.3(9) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 122.4(10) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 118.9(9) . . ? C3 C4 C15 115.9(11) . . ? C5 C4 C15 125.1(11) . . ? C6 C5 C4 120.3(9) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 119.6(9) . . ? C5 C6 C7 135.7(9) . . ? C1 C6 C7 104.7(8) . . ? C8 C7 C12 119.7(9) . . ? C8 C7 C6 132.0(9) . . ? C12 C7 C6 108.2(8) . . ? C7 C8 C9 118.6(10) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 120.3(11) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 123.1(11) . . ? C9 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 115.4(10) . . ? C10 C11 H11 122.3 . . ? C12 C11 H11 122.3 . . ? N1 C12 C11 130.4(9) . . ? N1 C12 C7 106.8(8) . . ? C11 C12 C7 122.8(9) . . ? C14 C13 N1 108.4(9) . . ? C14 C13 H13A 110.0 . . ? N1 C13 H13A 110.0 . . ? C14 C13 H13B 110.0 . . ? N1 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C4 121.0(13) . . ? C16 C15 H15 119.5 . . ? C4 C15 H15 119.5 . . ? C15 C16 C17 119.5(13) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C21 108.4(8) . . ? C18 C17 C16 134.3(10) . . ? C21 C17 C16 117.3(9) . . ? C18 C17 Fe1 69.0(4) . . ? C21 C17 Fe1 69.6(5) . . ? C16 C17 Fe1 126.3(6) . . ? C17 C18 C19 107.1(8) . . ? C17 C18 Fe1 71.7(5) . . ? C19 C18 Fe1 68.6(5) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? Fe1 C18 H18 124.8 . . ? C20 C19 C18 109.3(8) . . ? C20 C19 Fe1 71.0(5) . . ? C18 C19 Fe1 71.4(4) . . ? C20 C19 H19 125.4 . . ? C18 C19 H19 125.4 . . ? Fe1 C19 H19 123.8 . . ? C19 C20 C21 108.6(8) . . ? C19 C20 Fe1 69.6(5) . . ? C21 C20 Fe1 71.5(4) . . ? C19 C20 H20 125.7 . . ? C21 C20 H20 125.7 . . ? Fe1 C20 H20 124.8 . . ? C20 C21 C17 106.6(8) . . ? C20 C21 Fe1 68.6(4) . . ? C17 C21 Fe1 70.8(5) . . ? C20 C21 H21 126.7 . . ? C17 C21 H21 126.7 . . ? Fe1 C21 H21 125.4 . . ? C23 C22 C26 106.7(12) . . ? C23 C22 Fe1 70.6(7) . . ? C26 C22 Fe1 69.9(5) . . ? C23 C22 H22 126.6 . . ? C26 C22 H22 126.6 . . ? Fe1 C22 H22 124.4 . . ? C24 C23 C22 107.0(12) . . ? C24 C23 Fe1 69.9(6) . . ? C22 C23 Fe1 69.7(6) . . ? C24 C23 H23 126.5 . . ? C22 C23 H23 126.5 . . ? Fe1 C23 H23 125.5 . . ? C25 C24 C23 108.9(12) . . ? C25 C24 Fe1 70.4(6) . . ? C23 C24 Fe1 71.0(6) . . ? C25 C24 H24 125.5 . . ? C23 C24 H24 125.5 . . ? Fe1 C24 H24 124.6 . . ? C24 C25 C26 109.7(10) . . ? C24 C25 Fe1 71.3(5) . . ? C26 C25 Fe1 71.1(5) . . ? C24 C25 H25 125.2 . . ? C26 C25 H25 125.2 . . ? Fe1 C25 H25 124.0 . . ? C25 C26 C22 107.7(10) . . ? C25 C26 Fe1 70.3(5) . . ? C22 C26 Fe1 70.2(6) . . ? C25 C26 H26 126.2 . . ? C22 C26 H26 126.2 . . ? Fe1 C26 H26 125.0 . . ? Cl2 C27 Cl1 113.5(6) . . ? Cl2 C27 H27A 108.9 . . ? Cl1 C27 H27A 108.9 . . ? Cl2 C27 H27B 108.9 . . ? Cl1 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.630 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.114 #==========================================================end data_ccdc716278 _database_code_depnum_ccdc_archive 'CCDC 716278' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H23 Fe N' _chemical_formula_weight 405.30 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 6.0614(16) _cell_length_b 11.568(3) _cell_length_c 28.688(7) _cell_angle_alpha 81.177(4) _cell_angle_beta 88.213(4) _cell_angle_gamma 87.043(4) _cell_volume 1984.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2029 _cell_measurement_theta_min 3.145 _cell_measurement_theta_max 22.084 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 1.305 _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6722 _exptl_absorpt_correction_T_max 0.9065 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 10545 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6918 _reflns_number_gt 3702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6918 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.66177(10) 0.79644(5) 0.457755(19) 0.0459(2) Uani 1 1 d . . . Fe2 Fe 0.02648(10) 0.65660(5) 0.66126(2) 0.0486(2) Uani 1 1 d . . . N1 N -0.1037(6) 0.7352(3) 0.18732(12) 0.0538(10) Uani 1 1 d . . . N2 N 0.6930(7) 0.8242(4) 0.93284(14) 0.0718(12) Uani 1 1 d . . . C1 C 0.0026(7) 0.7833(4) 0.22119(14) 0.0487(11) Uani 1 1 d . . . C2 C -0.0674(8) 0.8773(4) 0.24361(15) 0.0597(12) Uani 1 1 d . . . H2 H -0.1994 0.9193 0.2357 0.072 Uiso 1 1 calc R . . C3 C 0.0630(8) 0.9064(4) 0.27757(16) 0.0617(13) Uani 1 1 d . . . H3 H 0.0183 0.9697 0.2926 0.074 Uiso 1 1 calc R . . C4 C 0.2614(8) 0.8444(4) 0.29050(14) 0.0523(12) Uani 1 1 d . . . C5 C 0.3296(7) 0.7515(4) 0.26746(15) 0.0518(12) Uani 1 1 d . . . H5 H 0.4624 0.7101 0.2752 0.062 Uiso 1 1 calc R . . C6 C 0.1995(7) 0.7200(3) 0.23274(14) 0.0462(11) Uani 1 1 d . . . C7 C 0.2161(8) 0.6288(4) 0.20375(14) 0.0507(11) Uani 1 1 d . . . C8 C 0.3696(8) 0.5385(4) 0.19939(17) 0.0698(14) Uani 1 1 d . . . H8 H 0.4966 0.5295 0.2172 0.084 Uiso 1 1 calc R . . C9 C 0.3334(11) 0.4623(4) 0.1685(2) 0.0869(17) Uani 1 1 d . . . H9 H 0.4338 0.3997 0.1664 0.104 Uiso 1 1 calc R . . C10 C 0.1507(11) 0.4775(5) 0.14094(19) 0.0836(17) Uani 1 1 d . . . H10 H 0.1329 0.4267 0.1193 0.100 Uiso 1 1 calc R . . C11 C -0.0055(9) 0.5650(4) 0.14431(16) 0.0681(14) Uani 1 1 d . . . H11 H -0.1309 0.5730 0.1260 0.082 Uiso 1 1 calc R . . C12 C 0.0282(8) 0.6423(4) 0.17607(15) 0.0506(11) Uani 1 1 d . . . C13 C -0.2948(8) 0.7878(4) 0.16149(17) 0.0721(14) Uani 1 1 d . . . H13A H -0.3962 0.8227 0.1828 0.087 Uiso 1 1 calc R . . H13B H -0.3707 0.7275 0.1492 0.087 Uiso 1 1 calc R . . C14 C -0.2300(10) 0.8796(5) 0.12150(18) 0.104(2) Uani 1 1 d . . . H14A H -0.3596 0.9122 0.1050 0.156 Uiso 1 1 calc R . . H14B H -0.1305 0.8451 0.1002 0.156 Uiso 1 1 calc R . . H14C H -0.1583 0.9405 0.1336 0.156 Uiso 1 1 calc R . . C15 C 0.3805(9) 0.8840(4) 0.32976(17) 0.0737(15) Uani 1 1 d . . . H15 H 0.3183 0.9497 0.3411 0.088 Uiso 1 1 calc R . . C16 C 0.5518(9) 0.8399(4) 0.34904(18) 0.0755(15) Uani 1 1 d . . . H16 H 0.6211 0.7760 0.3376 0.091 Uiso 1 1 calc R . . C17 C 0.6555(9) 0.8837(4) 0.39018(16) 0.0602(13) Uani 1 1 d . . . C18 C 0.5606(7) 0.9545(4) 0.42166(16) 0.0561(12) Uani 1 1 d . . . H18 H 0.4166 0.9866 0.4211 0.067 Uiso 1 1 calc R . . C19 C 0.7228(8) 0.9686(4) 0.45450(15) 0.0571(13) Uani 1 1 d . . . H19 H 0.7051 1.0116 0.4793 0.069 Uiso 1 1 calc R . . C20 C 0.9130(8) 0.9064(4) 0.44283(16) 0.0599(13) Uani 1 1 d . . . H20 H 1.0456 0.9009 0.4586 0.072 Uiso 1 1 calc R . . C21 C 0.8734(8) 0.8534(4) 0.40362(17) 0.0648(13) Uani 1 1 d . . . H21 H 0.9740 0.8063 0.3890 0.078 Uiso 1 1 calc R . . C22 C 0.5526(14) 0.6347(5) 0.4594(2) 0.0849(17) Uani 1 1 d . . . H22 H 0.5265 0.6009 0.4329 0.102 Uiso 1 1 calc R . . C23 C 0.4051(10) 0.7003(6) 0.4814(3) 0.106(3) Uani 1 1 d . . . H23 H 0.2594 0.7188 0.4728 0.128 Uiso 1 1 calc R . . C24 C 0.508(2) 0.7358(5) 0.5195(3) 0.133(4) Uani 1 1 d . . . H24 H 0.4474 0.7825 0.5407 0.160 Uiso 1 1 calc R . . C25 C 0.7190(16) 0.6868(6) 0.5187(2) 0.107(3) Uani 1 1 d . . . H25 H 0.8278 0.6945 0.5400 0.129 Uiso 1 1 calc R . . C26 C 0.7440(10) 0.6263(5) 0.4825(3) 0.0846(18) Uani 1 1 d . . . H26 H 0.8724 0.5854 0.4746 0.101 Uiso 1 1 calc R . . C27 C 0.6071(8) 0.8368(4) 0.88836(17) 0.0585(12) Uani 1 1 d . . . C28 C 0.6860(8) 0.8968(4) 0.84647(18) 0.0674(14) Uani 1 1 d . . . H28 H 0.8132 0.9388 0.8455 0.081 Uiso 1 1 calc R . . C29 C 0.5724(8) 0.8928(4) 0.80636(17) 0.0638(13) Uani 1 1 d . . . H29 H 0.6255 0.9329 0.7780 0.077 Uiso 1 1 calc R . . C30 C 0.3826(8) 0.8319(4) 0.80604(15) 0.0538(12) Uani 1 1 d . . . C31 C 0.3011(7) 0.7742(4) 0.84890(16) 0.0539(12) Uani 1 1 d . . . H31 H 0.1705 0.7350 0.8498 0.065 Uiso 1 1 calc R . . C32 C 0.4143(8) 0.7749(4) 0.89045(15) 0.0514(11) Uani 1 1 d . . . C33 C 0.3834(8) 0.7223(4) 0.93870(16) 0.0586(12) Uani 1 1 d . . . C34 C 0.2283(10) 0.6506(4) 0.96249(19) 0.0873(17) Uani 1 1 d . . . H34 H 0.1128 0.6263 0.9463 0.105 Uiso 1 1 calc R . . C35 C 0.2456(11) 0.6152(5) 1.0104(2) 0.107(2) Uani 1 1 d . . . H35 H 0.1415 0.5665 1.0264 0.128 Uiso 1 1 calc R . . C36 C 0.4146(12) 0.6507(6) 1.0348(2) 0.105(2) Uani 1 1 d . . . H36 H 0.4212 0.6270 1.0673 0.127 Uiso 1 1 calc R . . C37 C 0.5745(10) 0.7207(5) 1.0122(2) 0.0884(18) Uani 1 1 d . . . H37 H 0.6912 0.7432 1.0286 0.106 Uiso 1 1 calc R . . C38 C 0.5541(9) 0.7562(4) 0.96411(18) 0.0680(14) Uani 1 1 d . . . C39 C 0.8654(9) 0.8946(5) 0.94654(18) 0.0873(17) Uani 1 1 d . . . H39A H 0.9770 0.9054 0.9215 0.105 Uiso 1 1 calc R . . H39B H 0.9355 0.8531 0.9746 0.105 Uiso 1 1 calc R . . C40 C 0.7755(9) 1.0126(5) 0.9563(2) 0.114(2) Uani 1 1 d . . . H40A H 0.8939 1.0562 0.9652 0.171 Uiso 1 1 calc R . . H40B H 0.6671 1.0023 0.9815 0.171 Uiso 1 1 calc R . . H40C H 0.7084 1.0546 0.9284 0.171 Uiso 1 1 calc R . . C41 C 0.2759(8) 0.8298(4) 0.76065(16) 0.0577(12) Uani 1 1 d . . . H41 H 0.3406 0.8748 0.7346 0.069 Uiso 1 1 calc R . . C42 C 0.1065(8) 0.7749(4) 0.75179(16) 0.0602(13) Uani 1 1 d . . . H42 H 0.0403 0.7275 0.7769 0.072 Uiso 1 1 calc R . . C43 C 0.0093(8) 0.7810(4) 0.70523(15) 0.0542(12) Uani 1 1 d . . . C44 C 0.1005(8) 0.8270(3) 0.66017(16) 0.0538(12) Uani 1 1 d . . . H44 H 0.2395 0.8574 0.6545 0.065 Uiso 1 1 calc R . . C45 C -0.0563(8) 0.8185(4) 0.62545(16) 0.0601(13) Uani 1 1 d . . . H45 H -0.0386 0.8421 0.5931 0.072 Uiso 1 1 calc R . . C46 C -0.2432(8) 0.7681(4) 0.64863(17) 0.0630(13) Uani 1 1 d . . . H46 H -0.3715 0.7526 0.6342 0.076 Uiso 1 1 calc R . . C47 C -0.2047(8) 0.7450(4) 0.69691(16) 0.0642(13) Uani 1 1 d . . . H47 H -0.3032 0.7114 0.7199 0.077 Uiso 1 1 calc R . . C48 C 0.1295(10) 0.4994(4) 0.69748(18) 0.0729(15) Uani 1 1 d . . . H48 H 0.1302 0.4806 0.7302 0.087 Uiso 1 1 calc R . . C49 C 0.2980(9) 0.5477(4) 0.6698(3) 0.0841(17) Uani 1 1 d . . . H49 H 0.4330 0.5668 0.6804 0.101 Uiso 1 1 calc R . . C50 C 0.2334(15) 0.5636(5) 0.6228(3) 0.108(3) Uani 1 1 d . . . H50 H 0.3154 0.5946 0.5963 0.130 Uiso 1 1 calc R . . C51 C 0.0173(14) 0.5227(5) 0.6240(2) 0.099(2) Uani 1 1 d . . . H51 H -0.0713 0.5225 0.5981 0.118 Uiso 1 1 calc R . . C52 C -0.0378(10) 0.4835(4) 0.6699(2) 0.0823(17) Uani 1 1 d . . . H52 H -0.1706 0.4507 0.6805 0.099 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 0.0507(4) 0.0438(4) 0.0422(4) -0.0035(3) 0.0008(3) -0.0029(3) Fe2 0.0550(5) 0.0436(4) 0.0465(4) -0.0051(3) 0.0025(3) -0.0039(3) N1 0.052(3) 0.059(3) 0.051(2) -0.0096(19) -0.005(2) -0.001(2) N2 0.058(3) 0.095(3) 0.067(3) -0.024(2) -0.011(2) -0.012(2) C1 0.053(3) 0.049(3) 0.043(3) -0.004(2) 0.007(2) -0.003(2) C2 0.059(3) 0.063(3) 0.058(3) -0.013(2) 0.000(3) 0.008(3) C3 0.071(4) 0.049(3) 0.063(3) -0.008(2) 0.009(3) 0.004(3) C4 0.069(4) 0.056(3) 0.032(2) -0.001(2) 0.001(2) -0.021(3) C5 0.048(3) 0.051(3) 0.052(3) 0.002(2) 0.003(2) 0.000(2) C6 0.056(3) 0.038(3) 0.043(3) 0.001(2) -0.002(2) -0.001(2) C7 0.064(3) 0.037(3) 0.050(3) -0.003(2) 0.004(2) 0.000(2) C8 0.074(4) 0.055(3) 0.077(4) -0.005(3) 0.001(3) 0.013(3) C9 0.119(5) 0.046(3) 0.095(4) -0.018(3) 0.006(4) 0.018(3) C10 0.121(6) 0.063(4) 0.072(4) -0.025(3) 0.010(4) -0.007(4) C11 0.080(4) 0.066(4) 0.059(3) -0.011(3) 0.006(3) -0.019(3) C12 0.057(3) 0.049(3) 0.045(3) -0.004(2) 0.004(2) -0.007(2) C13 0.045(3) 0.087(4) 0.086(4) -0.020(3) -0.005(3) 0.001(3) C14 0.121(5) 0.097(5) 0.087(4) 0.012(3) -0.032(4) 0.002(4) C15 0.069(4) 0.066(4) 0.076(4) 0.020(3) 0.008(3) -0.010(3) C16 0.070(4) 0.069(4) 0.079(4) 0.011(3) 0.014(3) 0.002(3) C17 0.069(4) 0.067(3) 0.043(3) 0.001(2) -0.003(3) -0.017(3) C18 0.042(3) 0.050(3) 0.069(3) 0.014(2) 0.005(3) 0.000(2) C19 0.073(4) 0.043(3) 0.057(3) -0.010(2) 0.001(3) -0.008(3) C20 0.053(3) 0.064(3) 0.063(3) -0.003(3) -0.008(3) -0.014(3) C21 0.060(4) 0.068(3) 0.065(3) -0.007(3) 0.020(3) -0.005(3) C22 0.118(6) 0.055(4) 0.083(4) -0.010(3) -0.005(4) -0.015(4) C23 0.049(4) 0.077(5) 0.168(8) 0.056(5) 0.015(5) -0.003(4) C24 0.244(11) 0.043(4) 0.098(6) 0.007(4) 0.108(7) 0.017(6) C25 0.201(9) 0.069(5) 0.051(4) 0.009(3) -0.037(5) -0.033(5) C26 0.071(4) 0.055(4) 0.112(5) 0.027(4) 0.003(4) 0.014(3) C27 0.052(3) 0.065(3) 0.062(3) -0.023(3) -0.003(3) 0.005(3) C28 0.055(3) 0.082(4) 0.070(4) -0.023(3) -0.002(3) -0.015(3) C29 0.066(4) 0.066(3) 0.061(3) -0.015(3) 0.009(3) -0.005(3) C30 0.058(3) 0.049(3) 0.055(3) -0.013(2) -0.006(3) 0.005(2) C31 0.050(3) 0.047(3) 0.068(3) -0.019(2) -0.005(3) -0.003(2) C32 0.055(3) 0.047(3) 0.055(3) -0.019(2) -0.003(2) 0.005(2) C33 0.063(3) 0.056(3) 0.057(3) -0.012(2) -0.001(3) -0.002(3) C34 0.101(5) 0.085(4) 0.075(4) 0.001(3) -0.010(3) -0.024(4) C35 0.130(6) 0.111(5) 0.077(4) 0.012(4) -0.014(4) -0.043(4) C36 0.130(6) 0.114(5) 0.070(4) -0.002(4) -0.011(4) -0.009(5) C37 0.094(5) 0.103(5) 0.070(4) -0.016(3) -0.022(3) -0.004(4) C38 0.067(4) 0.073(4) 0.065(4) -0.016(3) -0.005(3) 0.006(3) C39 0.063(4) 0.118(5) 0.086(4) -0.033(4) -0.016(3) -0.003(4) C40 0.072(4) 0.134(6) 0.156(6) -0.080(5) -0.005(4) -0.011(4) C41 0.058(3) 0.045(3) 0.070(3) -0.013(2) 0.003(3) 0.002(2) C42 0.058(3) 0.057(3) 0.066(3) -0.015(2) 0.006(3) 0.003(3) C43 0.064(3) 0.047(3) 0.053(3) -0.012(2) -0.004(3) 0.001(2) C44 0.052(3) 0.037(3) 0.072(3) -0.006(2) 0.003(3) -0.005(2) C45 0.068(4) 0.049(3) 0.058(3) 0.003(2) -0.001(3) 0.007(3) C46 0.055(3) 0.068(3) 0.068(3) -0.014(3) -0.010(3) 0.001(3) C47 0.061(4) 0.074(4) 0.059(3) -0.016(3) 0.009(3) -0.001(3) C48 0.073(4) 0.066(4) 0.071(4) 0.010(3) 0.004(3) 0.009(3) C49 0.060(4) 0.052(3) 0.143(6) -0.027(4) 0.007(4) -0.001(3) C50 0.175(8) 0.044(4) 0.095(5) 0.000(3) 0.085(5) 0.014(4) C51 0.175(8) 0.049(4) 0.076(5) -0.023(3) -0.036(5) 0.011(4) C52 0.080(4) 0.054(3) 0.110(5) 0.006(3) -0.013(4) -0.015(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 C23 2.000(5) . ? Fe1 C22 2.010(5) . ? Fe1 C24 2.018(6) . ? Fe1 C25 2.024(5) . ? Fe1 C20 2.028(4) . ? Fe1 C26 2.029(5) . ? Fe1 C19 2.032(4) . ? Fe1 C18 2.034(4) . ? Fe1 C21 2.035(4) . ? Fe1 C17 2.044(4) . ? Fe2 C51 2.017(5) . ? Fe2 C49 2.018(5) . ? Fe2 C50 2.022(5) . ? Fe2 C48 2.029(5) . ? Fe2 C47 2.034(5) . ? Fe2 C46 2.035(5) . ? Fe2 C52 2.036(5) . ? Fe2 C44 2.039(4) . ? Fe2 C45 2.039(4) . ? Fe2 C43 2.050(4) . ? N1 C12 1.378(5) . ? N1 C1 1.382(5) . ? N1 C13 1.451(5) . ? N2 C27 1.377(5) . ? N2 C38 1.392(6) . ? N2 C39 1.456(6) . ? C1 C2 1.388(6) . ? C1 C6 1.389(6) . ? C2 C3 1.365(6) . ? C3 C4 1.398(6) . ? C4 C5 1.385(6) . ? C4 C15 1.497(6) . ? C5 C6 1.391(5) . ? C6 C7 1.439(6) . ? C7 C8 1.380(6) . ? C7 C12 1.397(6) . ? C8 C9 1.371(6) . ? C9 C10 1.370(7) . ? C10 C11 1.363(7) . ? C11 C12 1.397(6) . ? C13 C14 1.497(6) . ? C15 C16 1.240(6) . ? C16 C17 1.519(7) . ? C17 C21 1.399(6) . ? C17 C18 1.402(6) . ? C18 C19 1.415(6) . ? C19 C20 1.387(6) . ? C20 C21 1.393(6) . ? C22 C26 1.345(7) . ? C22 C23 1.348(8) . ? C23 C24 1.399(9) . ? C24 C25 1.371(9) . ? C25 C26 1.340(8) . ? C27 C28 1.377(6) . ? C27 C32 1.397(6) . ? C28 C29 1.367(6) . ? C29 C30 1.381(6) . ? C30 C31 1.395(5) . ? C30 C41 1.476(6) . ? C31 C32 1.395(5) . ? C32 C33 1.435(6) . ? C33 C34 1.380(6) . ? C33 C38 1.390(6) . ? C34 C35 1.378(6) . ? C35 C36 1.373(7) . ? C36 C37 1.377(7) . ? C37 C38 1.386(6) . ? C39 C40 1.507(7) . ? C41 C42 1.287(5) . ? C42 C43 1.467(6) . ? C43 C47 1.421(6) . ? C43 C44 1.426(5) . ? C44 C45 1.415(6) . ? C45 C46 1.403(6) . ? C46 C47 1.394(6) . ? C48 C52 1.342(6) . ? C48 C49 1.363(6) . ? C49 C50 1.399(8) . ? C50 C51 1.413(8) . ? C51 C52 1.362(7) . ? 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 C23 Fe1 C22 39.3(2) . . ? C23 Fe1 C24 40.7(3) . . ? C22 Fe1 C24 67.1(3) . . ? C23 Fe1 C25 66.2(3) . . ? C22 Fe1 C25 65.4(2) . . ? C24 Fe1 C25 39.6(3) . . ? C23 Fe1 C20 171.0(4) . . ? C22 Fe1 C20 148.0(3) . . ? C24 Fe1 C20 131.2(4) . . ? C25 Fe1 C20 110.0(2) . . ? C23 Fe1 C26 65.6(2) . . ? C22 Fe1 C26 38.9(2) . . ? C24 Fe1 C26 66.3(2) . . ? C25 Fe1 C26 38.6(2) . . ? C20 Fe1 C26 117.1(2) . . ? C23 Fe1 C19 133.5(3) . . ? C22 Fe1 C19 171.2(3) . . ? C24 Fe1 C19 110.6(2) . . ? C25 Fe1 C19 118.7(2) . . ? C20 Fe1 C19 39.95(17) . . ? C26 Fe1 C19 149.0(3) . . ? C23 Fe1 C18 111.5(2) . . ? C22 Fe1 C18 132.1(3) . . ? C24 Fe1 C18 119.3(3) . . ? C25 Fe1 C18 151.6(3) . . ? C20 Fe1 C18 67.53(18) . . ? C26 Fe1 C18 168.8(3) . . ? C19 Fe1 C18 40.73(16) . . ? C23 Fe1 C21 148.6(3) . . ? C22 Fe1 C21 116.4(2) . . ? C24 Fe1 C21 168.2(4) . . ? C25 Fe1 C21 130.0(3) . . ? C20 Fe1 C21 40.12(16) . . ? C26 Fe1 C21 108.7(2) . . ? C19 Fe1 C21 67.67(19) . . ? C18 Fe1 C21 67.63(18) . . ? C23 Fe1 C17 118.2(3) . . ? C22 Fe1 C17 109.7(2) . . ? C24 Fe1 C17 151.2(4) . . ? C25 Fe1 C17 167.3(3) . . ? C20 Fe1 C17 67.35(18) . . ? C26 Fe1 C17 130.4(3) . . ? C19 Fe1 C17 67.89(18) . . ? C18 Fe1 C17 40.21(17) . . ? C21 Fe1 C17 40.13(17) . . ? C51 Fe2 C49 67.4(2) . . ? C51 Fe2 C50 41.0(2) . . ? C49 Fe2 C50 40.5(2) . . ? C51 Fe2 C48 66.1(2) . . ? C49 Fe2 C48 39.36(19) . . ? C50 Fe2 C48 67.1(2) . . ? C51 Fe2 C47 134.1(3) . . ? C49 Fe2 C47 143.1(2) . . ? C50 Fe2 C47 174.8(3) . . ? C48 Fe2 C47 113.6(2) . . ? C51 Fe2 C46 110.9(2) . . ? C49 Fe2 C46 176.7(3) . . ? C50 Fe2 C46 136.4(3) . . ? C48 Fe2 C46 143.0(2) . . ? C47 Fe2 C46 40.07(16) . . ? C51 Fe2 C52 39.3(2) . . ? C49 Fe2 C52 65.8(2) . . ? C50 Fe2 C52 67.0(2) . . ? C48 Fe2 C52 38.56(18) . . ? C47 Fe2 C52 110.1(2) . . ? C46 Fe2 C52 114.8(2) . . ? C51 Fe2 C44 146.2(3) . . ? C49 Fe2 C44 111.9(2) . . ? C50 Fe2 C44 115.4(2) . . ? C48 Fe2 C44 136.0(2) . . ? C47 Fe2 C44 67.98(18) . . ? C46 Fe2 C44 67.86(18) . . ? C52 Fe2 C44 173.7(2) . . ? C51 Fe2 C45 115.7(2) . . ? C49 Fe2 C45 137.5(2) . . ? C50 Fe2 C45 111.8(2) . . ? C48 Fe2 C45 176.1(2) . . ? C47 Fe2 C45 67.81(18) . . ? C46 Fe2 C45 40.28(16) . . ? C52 Fe2 C45 145.0(2) . . ? C44 Fe2 C45 40.60(16) . . ? C51 Fe2 C43 172.7(3) . . ? C49 Fe2 C43 113.8(2) . . ? C50 Fe2 C43 144.4(3) . . ? C48 Fe2 C43 109.9(2) . . ? C47 Fe2 C43 40.71(17) . . ? C46 Fe2 C43 68.25(18) . . ? C52 Fe2 C43 133.9(2) . . ? C44 Fe2 C43 40.82(15) . . ? C45 Fe2 C43 68.65(18) . . ? C12 N1 C1 107.7(4) . . ? C12 N1 C13 125.7(4) . . ? C1 N1 C13 125.4(4) . . ? C27 N2 C38 108.7(4) . . ? C27 N2 C39 124.6(5) . . ? C38 N2 C39 125.0(4) . . ? N1 C1 C2 128.6(4) . . ? N1 C1 C6 110.0(4) . . ? C2 C1 C6 121.3(4) . . ? C3 C2 C1 118.1(5) . . ? C2 C3 C4 122.3(4) . . ? C5 C4 C3 118.8(4) . . ? C5 C4 C15 125.4(5) . . ? C3 C4 C15 115.8(5) . . ? C4 C5 C6 120.0(4) . . ? C1 C6 C5 119.4(4) . . ? C1 C6 C7 106.2(4) . . ? C5 C6 C7 134.4(4) . . ? C8 C7 C12 119.5(4) . . ? C8 C7 C6 133.7(5) . . ? C12 C7 C6 106.7(4) . . ? C9 C8 C7 119.5(5) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 121.8(5) . . ? C10 C11 C12 118.0(5) . . ? N1 C12 C7 109.4(4) . . ? N1 C12 C11 130.1(5) . . ? C7 C12 C11 120.5(5) . . ? N1 C13 C14 111.5(4) . . ? C16 C15 C4 128.1(6) . . ? C15 C16 C17 124.2(6) . . ? C21 C17 C18 107.9(4) . . ? C21 C17 C16 122.9(5) . . ? C18 C17 C16 129.2(5) . . ? C21 C17 Fe1 69.6(2) . . ? C18 C17 Fe1 69.5(2) . . ? C16 C17 Fe1 124.9(3) . . ? C17 C18 C19 107.8(4) . . ? C17 C18 Fe1 70.3(3) . . ? C19 C18 Fe1 69.6(2) . . ? C20 C19 C18 107.4(4) . . ? C20 C19 Fe1 69.9(3) . . ? C18 C19 Fe1 69.7(2) . . ? C19 C20 C21 109.1(4) . . ? C19 C20 Fe1 70.2(3) . . ? C21 C20 Fe1 70.2(2) . . ? C20 C21 C17 107.9(5) . . ? C20 C21 Fe1 69.7(3) . . ? C17 C21 Fe1 70.3(3) . . ? C26 C22 C23 108.4(6) . . ? C26 C22 Fe1 71.3(3) . . ? C23 C22 Fe1 70.0(3) . . ? C22 C23 C24 108.4(7) . . ? C22 C23 Fe1 70.8(3) . . ? C24 C23 Fe1 70.3(4) . . ? C25 C24 C23 105.1(6) . . ? C25 C24 Fe1 70.4(4) . . ? C23 C24 Fe1 68.9(3) . . ? C26 C25 C24 109.5(7) . . ? C26 C25 Fe1 70.9(3) . . ? C24 C25 Fe1 70.0(4) . . ? C25 C26 C22 108.6(6) . . ? C25 C26 Fe1 70.5(3) . . ? C22 C26 Fe1 69.8(3) . . ? N2 C27 C28 129.6(5) . . ? N2 C27 C32 109.0(4) . . ? C28 C27 C32 121.4(4) . . ? C29 C28 C27 118.2(4) . . ? C28 C29 C30 123.0(4) . . ? C29 C30 C31 118.2(4) . . ? C29 C30 C41 118.9(4) . . ? C31 C30 C41 122.9(4) . . ? C30 C31 C32 120.4(4) . . ? C31 C32 C27 118.7(4) . . ? C31 C32 C33 134.7(4) . . ? C27 C32 C33 106.6(4) . . ? C34 C33 C38 118.5(5) . . ? C34 C33 C32 134.1(5) . . ? C38 C33 C32 107.4(4) . . ? C35 C34 C33 119.6(5) . . ? C36 C35 C34 120.9(5) . . ? C35 C36 C37 121.2(5) . . ? C36 C37 C38 117.2(5) . . ? C37 C38 C33 122.6(5) . . ? C37 C38 N2 129.0(5) . . ? C33 C38 N2 108.3(4) . . ? N2 C39 C40 112.0(5) . . ? C42 C41 C30 129.5(5) . . ? C41 C42 C43 125.3(5) . . ? C47 C43 C44 106.2(4) . . ? C47 C43 C42 125.2(4) . . ? C44 C43 C42 128.5(4) . . ? C47 C43 Fe2 69.0(3) . . ? C44 C43 Fe2 69.2(2) . . ? C42 C43 Fe2 128.3(3) . . ? C45 C44 C43 108.5(4) . . ? C45 C44 Fe2 69.7(2) . . ? C43 C44 Fe2 70.0(2) . . ? C46 C45 C44 107.6(4) . . ? C46 C45 Fe2 69.7(2) . . ? C44 C45 Fe2 69.7(2) . . ? C47 C46 C45 108.6(4) . . ? C47 C46 Fe2 69.9(3) . . ? C45 C46 Fe2 70.0(3) . . ? C46 C47 C43 109.0(4) . . ? C46 C47 Fe2 70.0(3) . . ? C43 C47 Fe2 70.3(3) . . ? C52 C48 C49 109.0(5) . . ? C52 C48 Fe2 71.0(3) . . ? C49 C48 Fe2 69.9(3) . . ? C48 C49 C50 108.3(6) . . ? C48 C49 Fe2 70.8(3) . . ? C50 C49 Fe2 69.9(3) . . ? C49 C50 C51 105.6(5) . . ? C49 C50 Fe2 69.6(3) . . ? C51 C50 Fe2 69.3(3) . . ? C52 C51 C50 107.7(6) . . ? C52 C51 Fe2 71.1(3) . . ? C50 C51 Fe2 69.7(3) . . ? C48 C52 C51 109.4(5) . . ? C48 C52 Fe2 70.4(3) . . ? C51 C52 Fe2 69.6(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.535 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.061 #==========================================================end data_ccdc716279 _database_code_depnum_ccdc_archive 'CCDC 716279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H33 Fe2 N' _chemical_formula_weight 615.35 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 23.522(17) _cell_length_b 11.106(8) _cell_length_c 11.329(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.047(14) _cell_angle_gamma 90.00 _cell_volume 2905(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 2.545 _cell_measurement_theta_max 17.667 _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5549 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 13824 _diffrn_reflns_av_R_equivalents 0.1226 _diffrn_reflns_av_sigmaI/netI 0.1995 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4815 _reflns_number_gt 2123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4815 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1784 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _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 0.06351(4) 0.67007(8) 0.15981(9) 0.0403(3) Uani 1 1 d . . . Fe2 Fe 0.43267(5) 1.10731(9) 1.27883(10) 0.0544(4) Uani 1 1 d . . . N1 N 0.2156(2) 0.4318(5) 0.9480(6) 0.0504(16) Uani 1 1 d . . . C1 C 0.1178(3) 0.5423(7) 0.2471(7) 0.051(2) Uani 1 1 d . . . C2 C 0.1491(3) 0.6284(6) 0.1910(6) 0.047(2) Uani 1 1 d . . . H2 H 0.1793 0.6766 0.2298 0.057 Uiso 1 1 calc R . . C3 C 0.1263(3) 0.6276(6) 0.0665(7) 0.053(2) Uani 1 1 d . . . H3 H 0.1382 0.6761 0.0088 0.064 Uiso 1 1 calc R . . C4 C 0.0833(3) 0.5422(6) 0.0457(7) 0.056(2) Uani 1 1 d . . . H4 H 0.0617 0.5224 -0.0295 0.067 Uiso 1 1 calc R . . C5 C 0.0767(3) 0.4897(6) 0.1534(7) 0.052(2) Uani 1 1 d . . . H5 H 0.0500 0.4303 0.1626 0.063 Uiso 1 1 calc R . . C6 C 0.0288(4) 0.7522(7) 0.2872(7) 0.061(2) Uani 1 1 d . . . H6 H 0.0380 0.7355 0.3691 0.073 Uiso 1 1 calc R . . C7 C 0.0565(3) 0.8382(6) 0.2270(7) 0.053(2) Uani 1 1 d . . . H7 H 0.0870 0.8880 0.2614 0.064 Uiso 1 1 calc R . . C8 C 0.0301(4) 0.8347(7) 0.1074(7) 0.069(3) Uani 1 1 d . . . H8 H 0.0396 0.8829 0.0469 0.083 Uiso 1 1 calc R . . C9 C -0.0138(4) 0.7461(8) 0.0917(8) 0.068(3) Uani 1 1 d . . . H9 H -0.0376 0.7247 0.0195 0.082 Uiso 1 1 calc R . . C10 C -0.0146(3) 0.6961(7) 0.2054(8) 0.059(2) Uani 1 1 d . . . H10 H -0.0396 0.6365 0.2225 0.071 Uiso 1 1 calc R . . C11 C 0.4415(3) 0.9405(7) 1.2056(7) 0.055(2) Uani 1 1 d . . . C12 C 0.4568(4) 1.0338(7) 1.1307(8) 0.069(2) Uani 1 1 d . . . H12 H 0.4394 1.0475 1.0509 0.083 Uiso 1 1 calc R . . C13 C 0.5019(3) 1.1006(7) 1.1969(9) 0.068(2) Uani 1 1 d . . . H13 H 0.5194 1.1666 1.1683 0.082 Uiso 1 1 calc R . . C14 C 0.5167(3) 1.0536(7) 1.3121(9) 0.071(3) Uani 1 1 d . . . H14 H 0.5458 1.0820 1.3732 0.085 Uiso 1 1 calc R . . C15 C 0.4796(3) 0.9545(7) 1.3205(7) 0.065(2) Uani 1 1 d . . . H15 H 0.4799 0.9070 1.3882 0.078 Uiso 1 1 calc R . . C16 C 0.3720(5) 1.2352(10) 1.2272(9) 0.089(3) Uani 1 1 d . . . H16 H 0.3609 1.2660 1.1499 0.106 Uiso 1 1 calc R . . C17 C 0.4162(5) 1.2799(8) 1.3158(13) 0.091(3) Uani 1 1 d . . . H17 H 0.4403 1.3449 1.3093 0.110 Uiso 1 1 calc R . . C18 C 0.4169(5) 1.2084(12) 1.4147(10) 0.092(3) Uani 1 1 d . . . H18 H 0.4420 1.2184 1.4881 0.111 Uiso 1 1 calc R . . C19 C 0.3759(5) 1.1210(9) 1.3912(10) 0.084(3) Uani 1 1 d . . . H19 H 0.3685 1.0616 1.4440 0.101 Uiso 1 1 calc R . . C20 C 0.3474(4) 1.1372(9) 1.2734(12) 0.088(3) Uani 1 1 d . . . H20 H 0.3171 1.0905 1.2327 0.106 Uiso 1 1 calc R . . C21 C 0.1957(3) 0.4528(6) 0.8258(6) 0.0430(18) Uani 1 1 d . . . C22 C 0.1574(3) 0.3880(6) 0.7456(7) 0.049(2) Uani 1 1 d . . . H22 H 0.1392 0.3207 0.7700 0.059 Uiso 1 1 calc R . . C23 C 0.1464(3) 0.4235(6) 0.6293(7) 0.049(2) Uani 1 1 d . . . H23 H 0.1202 0.3802 0.5733 0.059 Uiso 1 1 calc R . . C24 C 0.1744(3) 0.5266(6) 0.5911(7) 0.0446(19) Uani 1 1 d . . . C25 C 0.2130(3) 0.5918(6) 0.6736(6) 0.0423(18) Uani 1 1 d . . . H25 H 0.2323 0.6576 0.6491 0.051 Uiso 1 1 calc R . . C26 C 0.2226(3) 0.5582(6) 0.7933(6) 0.0384(17) Uani 1 1 d . . . C27 C 0.2607(3) 0.6006(6) 0.9013(6) 0.0431(18) Uani 1 1 d . . . C28 C 0.2974(3) 0.6972(6) 0.9273(7) 0.050(2) Uani 1 1 d . . . H28 H 0.3002 0.7530 0.8675 0.060 Uiso 1 1 calc R . . C29 C 0.3305(3) 0.7128(6) 1.0430(7) 0.052(2) Uani 1 1 d . . . C30 C 0.3231(3) 0.6256(7) 1.1297(7) 0.053(2) Uani 1 1 d . . . H30 H 0.3447 0.6346 1.2070 0.064 Uiso 1 1 calc R . . C31 C 0.2877(3) 0.5322(7) 1.1092(6) 0.053(2) Uani 1 1 d . . . H31 H 0.2847 0.4773 1.1697 0.063 Uiso 1 1 calc R . . C32 C 0.2543(3) 0.5189(6) 0.9903(6) 0.0434(18) Uani 1 1 d . . . C33 C 0.1651(3) 0.5592(5) 0.4626(7) 0.0425(18) Uani 1 1 d . . . H33 H 0.1895 0.6182 0.4418 0.051 Uiso 1 1 calc R . . C34 C 0.1267(3) 0.5150(6) 0.3743(7) 0.052(2) Uani 1 1 d . . . H34 H 0.1015 0.4583 0.3963 0.063 Uiso 1 1 calc R . . C35 C 0.3709(3) 0.8130(6) 1.0712(7) 0.056(2) Uani 1 1 d . . . H35 H 0.3778 0.8580 1.0062 0.067 Uiso 1 1 calc R . . C36 C 0.3991(3) 0.8474(6) 1.1794(7) 0.057(2) Uani 1 1 d . . . H36 H 0.3901 0.8063 1.2450 0.068 Uiso 1 1 calc R . . C37 C 0.2077(4) 0.3183(8) 1.0048(8) 0.075(3) Uani 1 1 d . . . H37A H 0.1673 0.2949 0.9837 0.090 Uiso 1 1 calc R . . H37B H 0.2173 0.3283 1.0914 0.090 Uiso 1 1 calc R . . C38 C 0.2444(4) 0.2200(7) 0.9687(9) 0.096(4) Uani 1 1 d . . . H38A H 0.2380 0.1469 1.0094 0.145 Uiso 1 1 calc R . . H38B H 0.2845 0.2423 0.9901 0.145 Uiso 1 1 calc R . . H38C H 0.2343 0.2079 0.8833 0.145 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 0.0399(6) 0.0418(6) 0.0391(6) -0.0025(5) 0.0077(5) -0.0005(5) Fe2 0.0499(7) 0.0457(7) 0.0659(9) -0.0038(6) 0.0069(6) -0.0037(5) N1 0.047(4) 0.048(4) 0.053(5) -0.007(3) 0.001(3) -0.006(3) C1 0.045(5) 0.062(5) 0.041(5) 0.009(4) 0.000(4) -0.003(4) C2 0.045(5) 0.051(5) 0.040(5) 0.000(4) -0.007(4) 0.001(4) C3 0.052(5) 0.047(5) 0.066(6) -0.002(4) 0.025(4) 0.000(4) C4 0.084(6) 0.045(5) 0.040(5) -0.005(4) 0.014(4) 0.001(4) C5 0.049(5) 0.064(5) 0.045(5) -0.011(4) 0.009(4) -0.003(4) C6 0.065(6) 0.079(6) 0.045(5) 0.022(5) 0.026(5) 0.011(5) C7 0.057(5) 0.041(5) 0.063(6) -0.009(4) 0.016(4) 0.000(4) C8 0.132(8) 0.029(4) 0.048(6) -0.001(4) 0.019(5) 0.027(5) C9 0.063(6) 0.071(6) 0.057(7) -0.005(5) -0.019(5) 0.017(5) C10 0.042(5) 0.056(5) 0.084(7) -0.012(5) 0.026(5) 0.003(4) C11 0.060(5) 0.048(5) 0.053(5) -0.003(4) 0.003(4) -0.001(4) C12 0.062(6) 0.073(6) 0.073(6) -0.003(5) 0.017(5) -0.008(5) C13 0.051(5) 0.064(6) 0.092(7) -0.014(5) 0.021(5) -0.021(4) C14 0.038(5) 0.074(6) 0.094(8) -0.017(6) -0.003(5) -0.014(4) C15 0.065(5) 0.060(5) 0.061(6) -0.010(4) -0.011(5) -0.002(5) C16 0.082(8) 0.090(8) 0.087(8) 0.008(7) 0.000(6) 0.016(6) C17 0.083(8) 0.043(6) 0.163(12) -0.016(7) 0.063(8) -0.008(5) C18 0.071(7) 0.121(10) 0.080(9) -0.043(7) 0.001(6) 0.007(7) C19 0.093(8) 0.081(7) 0.088(9) 0.025(6) 0.044(7) 0.010(6) C20 0.047(6) 0.069(7) 0.150(11) -0.018(7) 0.022(7) 0.001(5) C21 0.032(4) 0.049(5) 0.048(5) 0.007(4) 0.005(4) -0.002(4) C22 0.034(4) 0.046(5) 0.063(6) 0.003(4) -0.001(4) -0.005(4) C23 0.038(4) 0.054(5) 0.050(5) 0.000(4) -0.001(4) -0.003(4) C24 0.031(4) 0.050(5) 0.052(5) 0.004(4) 0.003(4) 0.012(3) C25 0.041(4) 0.036(4) 0.049(5) 0.004(4) 0.005(4) -0.006(3) C26 0.035(4) 0.034(4) 0.046(5) -0.009(4) 0.007(4) 0.000(3) C27 0.042(4) 0.042(5) 0.046(5) -0.001(4) 0.009(4) -0.002(4) C28 0.061(5) 0.036(5) 0.054(6) 0.001(4) 0.016(4) 0.007(4) C29 0.042(5) 0.041(5) 0.071(6) -0.010(4) 0.010(4) 0.009(4) C30 0.056(5) 0.057(5) 0.051(5) -0.001(4) 0.020(4) -0.018(4) C31 0.061(5) 0.052(5) 0.045(5) 0.012(4) 0.013(4) 0.005(4) C32 0.044(4) 0.054(5) 0.033(5) 0.002(4) 0.008(4) 0.009(4) C33 0.035(4) 0.029(4) 0.064(6) -0.005(4) 0.010(4) -0.007(3) C34 0.050(5) 0.051(5) 0.057(6) 0.002(4) 0.010(4) 0.003(4) C35 0.062(5) 0.050(5) 0.049(5) 0.003(4) -0.003(4) -0.007(4) C36 0.061(5) 0.050(5) 0.052(5) -0.004(4) -0.006(4) 0.015(4) C37 0.086(7) 0.062(6) 0.076(7) -0.008(5) 0.018(5) -0.031(5) C38 0.081(7) 0.054(6) 0.145(10) 0.041(6) -0.001(7) -0.015(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 C6 2.009(8) . ? Fe1 C9 2.018(7) . ? Fe1 C10 2.023(8) . ? Fe1 C3 2.030(7) . ? Fe1 C2 2.030(7) . ? Fe1 C5 2.031(7) . ? Fe1 C8 2.033(7) . ? Fe1 C4 2.034(7) . ? Fe1 C1 2.034(7) . ? Fe1 C7 2.035(7) . ? Fe2 C18 1.997(9) . ? Fe2 C17 2.015(9) . ? Fe2 C19 2.018(9) . ? Fe2 C16 2.018(9) . ? Fe2 C20 2.021(9) . ? Fe2 C13 2.024(8) . ? Fe2 C14 2.029(8) . ? Fe2 C15 2.030(8) . ? Fe2 C12 2.042(8) . ? Fe2 C11 2.056(8) . ? N1 C32 1.352(8) . ? N1 C21 1.394(8) . ? N1 C37 1.443(9) . ? C1 C5 1.418(9) . ? C1 C2 1.428(9) . ? C1 C34 1.448(9) . ? C2 C3 1.410(9) . ? C2 H2 0.9300 . ? C3 C4 1.373(9) . ? C3 H3 0.9300 . ? C4 C5 1.388(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.389(10) . ? C6 C7 1.405(9) . ? C6 H6 0.9300 . ? C7 C8 1.379(9) . ? C7 H7 0.9300 . ? C8 C9 1.412(11) . ? C8 H8 0.9300 . ? C9 C10 1.406(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C36 1.428(10) . ? C11 C12 1.428(10) . ? C11 C15 1.441(10) . ? C12 C13 1.391(10) . ? C12 H12 0.9300 . ? C13 C14 1.387(10) . ? C13 H13 0.9300 . ? C14 C15 1.418(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.381(12) . ? C16 C17 1.391(12) . ? C16 H16 0.9300 . ? C17 C18 1.371(12) . ? C17 H17 0.9300 . ? C18 C19 1.357(12) . ? C18 H18 0.9300 . ? C19 C20 1.385(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.357(9) . ? C21 C26 1.413(9) . ? C22 C23 1.351(9) . ? C22 H22 0.9300 . ? C23 C24 1.430(9) . ? C23 H23 0.9300 . ? C24 C25 1.377(9) . ? C24 C33 1.475(9) . ? C25 C26 1.383(8) . ? C25 H25 0.9300 . ? C26 C27 1.451(9) . ? C27 C28 1.372(9) . ? C27 C32 1.386(9) . ? C28 C29 1.402(9) . ? C28 H28 0.9300 . ? C29 C30 1.414(9) . ? C29 C35 1.458(9) . ? C30 C31 1.322(9) . ? C30 H30 0.9300 . ? C31 C32 1.431(9) . ? C31 H31 0.9300 . ? C33 C34 1.308(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.333(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.496(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? 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 C6 Fe1 C9 67.9(3) . . ? C6 Fe1 C10 40.3(3) . . ? C9 Fe1 C10 40.7(3) . . ? C6 Fe1 C3 156.4(3) . . ? C9 Fe1 C3 126.1(3) . . ? C10 Fe1 C3 162.4(3) . . ? C6 Fe1 C2 120.3(3) . . ? C9 Fe1 C2 162.2(4) . . ? C10 Fe1 C2 155.2(3) . . ? C3 Fe1 C2 40.7(3) . . ? C6 Fe1 C5 124.0(3) . . ? C9 Fe1 C5 122.1(3) . . ? C10 Fe1 C5 107.6(3) . . ? C3 Fe1 C5 67.7(3) . . ? C2 Fe1 C5 68.1(3) . . ? C6 Fe1 C8 67.3(3) . . ? C9 Fe1 C8 40.8(3) . . ? C10 Fe1 C8 68.1(3) . . ? C3 Fe1 C8 109.6(3) . . ? C2 Fe1 C8 124.8(4) . . ? C5 Fe1 C8 158.4(3) . . ? C6 Fe1 C4 161.5(3) . . ? C9 Fe1 C4 110.4(3) . . ? C10 Fe1 C4 126.3(3) . . ? C3 Fe1 C4 39.5(3) . . ? C2 Fe1 C4 67.1(3) . . ? C5 Fe1 C4 39.9(3) . . ? C8 Fe1 C4 124.4(3) . . ? C6 Fe1 C1 105.7(3) . . ? C9 Fe1 C1 155.9(4) . . ? C10 Fe1 C1 119.5(3) . . ? C3 Fe1 C1 68.9(3) . . ? C2 Fe1 C1 41.1(3) . . ? C5 Fe1 C1 40.8(3) . . ? C8 Fe1 C1 160.1(3) . . ? C4 Fe1 C1 67.9(3) . . ? C6 Fe1 C7 40.7(3) . . ? C9 Fe1 C7 68.2(3) . . ? C10 Fe1 C7 68.4(3) . . ? C3 Fe1 C7 121.8(3) . . ? C2 Fe1 C7 107.0(3) . . ? C5 Fe1 C7 160.5(3) . . ? C8 Fe1 C7 39.6(3) . . ? C4 Fe1 C7 157.4(3) . . ? C1 Fe1 C7 123.1(3) . . ? C18 Fe2 C17 40.0(4) . . ? C18 Fe2 C19 39.5(4) . . ? C17 Fe2 C19 67.7(4) . . ? C18 Fe2 C16 66.6(4) . . ? C17 Fe2 C16 40.3(4) . . ? C19 Fe2 C16 67.3(4) . . ? C18 Fe2 C20 66.5(4) . . ? C17 Fe2 C20 67.7(4) . . ? C19 Fe2 C20 40.1(3) . . ? C16 Fe2 C20 40.0(4) . . ? C18 Fe2 C13 131.2(4) . . ? C17 Fe2 C13 109.5(4) . . ? C19 Fe2 C13 168.2(5) . . ? C16 Fe2 C13 118.6(4) . . ? C20 Fe2 C13 150.7(5) . . ? C18 Fe2 C14 109.9(4) . . ? C17 Fe2 C14 117.4(4) . . ? C19 Fe2 C14 130.0(4) . . ? C16 Fe2 C14 150.4(4) . . ? C20 Fe2 C14 168.2(5) . . ? C13 Fe2 C14 40.0(3) . . ? C18 Fe2 C15 117.6(4) . . ? C17 Fe2 C15 149.8(5) . . ? C19 Fe2 C15 108.2(4) . . ? C16 Fe2 C15 168.0(4) . . ? C20 Fe2 C15 129.5(4) . . ? C13 Fe2 C15 68.1(4) . . ? C14 Fe2 C15 40.9(3) . . ? C18 Fe2 C12 168.7(5) . . ? C17 Fe2 C12 130.2(4) . . ? C19 Fe2 C12 150.4(4) . . ? C16 Fe2 C12 109.6(4) . . ? C20 Fe2 C12 118.1(4) . . ? C13 Fe2 C12 40.0(3) . . ? C14 Fe2 C12 67.8(3) . . ? C15 Fe2 C12 68.5(3) . . ? C18 Fe2 C11 149.9(5) . . ? C17 Fe2 C11 168.2(5) . . ? C19 Fe2 C11 116.9(4) . . ? C16 Fe2 C11 129.6(4) . . ? C20 Fe2 C11 108.2(4) . . ? C13 Fe2 C11 68.3(3) . . ? C14 Fe2 C11 68.9(3) . . ? C15 Fe2 C11 41.3(3) . . ? C12 Fe2 C11 40.8(3) . . ? C32 N1 C21 107.9(6) . . ? C32 N1 C37 127.0(6) . . ? C21 N1 C37 122.8(6) . . ? C5 C1 C2 106.2(6) . . ? C5 C1 C34 127.3(7) . . ? C2 C1 C34 126.5(6) . . ? C5 C1 Fe1 69.5(4) . . ? C2 C1 Fe1 69.3(4) . . ? C34 C1 Fe1 125.9(5) . . ? C3 C2 C1 108.1(6) . . ? C3 C2 Fe1 69.7(4) . . ? C1 C2 Fe1 69.6(4) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.4 . . ? C4 C3 C2 107.6(7) . . ? C4 C3 Fe1 70.4(5) . . ? C2 C3 Fe1 69.7(4) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe1 C3 H3 125.3 . . ? C3 C4 C5 110.0(7) . . ? C3 C4 Fe1 70.1(4) . . ? C5 C4 Fe1 69.9(4) . . ? C3 C4 H4 125.0 . . ? C5 C4 H4 125.0 . . ? Fe1 C4 H4 126.6 . . ? C4 C5 C1 108.1(7) . . ? C4 C5 Fe1 70.2(4) . . ? C1 C5 Fe1 69.7(4) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe1 C5 H5 125.7 . . ? C10 C6 C7 109.3(7) . . ? C10 C6 Fe1 70.4(5) . . ? C7 C6 Fe1 70.7(4) . . ? C10 C6 H6 125.3 . . ? C7 C6 H6 125.3 . . ? Fe1 C6 H6 125.2 . . ? C8 C7 C6 107.1(7) . . ? C8 C7 Fe1 70.1(4) . . ? C6 C7 Fe1 68.7(4) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? Fe1 C7 H7 126.3 . . ? C7 C8 C9 108.9(8) . . ? C7 C8 Fe1 70.2(4) . . ? C9 C8 Fe1 69.0(4) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? Fe1 C8 H8 126.8 . . ? C10 C9 C8 107.4(7) . . ? C10 C9 Fe1 69.8(4) . . ? C8 C9 Fe1 70.2(4) . . ? C10 C9 H9 126.3 . . ? C8 C9 H9 126.3 . . ? Fe1 C9 H9 125.3 . . ? C6 C10 C9 107.2(7) . . ? C6 C10 Fe1 69.3(5) . . ? C9 C10 Fe1 69.5(5) . . ? C6 C10 H10 126.4 . . ? C9 C10 H10 126.4 . . ? Fe1 C10 H10 126.4 . . ? C36 C11 C12 130.3(7) . . ? C36 C11 C15 123.7(7) . . ? C12 C11 C15 105.9(7) . . ? C36 C11 Fe2 128.0(6) . . ? C12 C11 Fe2 69.1(5) . . ? C15 C11 Fe2 68.4(4) . . ? C13 C12 C11 108.6(8) . . ? C13 C12 Fe2 69.3(5) . . ? C11 C12 Fe2 70.1(5) . . ? C13 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? Fe2 C12 H12 126.4 . . ? C14 C13 C12 109.6(7) . . ? C14 C13 Fe2 70.2(5) . . ? C12 C13 Fe2 70.7(5) . . ? C14 C13 H13 125.2 . . ? C12 C13 H13 125.2 . . ? Fe2 C13 H13 125.5 . . ? C13 C14 C15 108.0(7) . . ? C13 C14 Fe2 69.8(5) . . ? C15 C14 Fe2 69.6(4) . . ? C13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Fe2 C14 H14 126.2 . . ? C14 C15 C11 107.9(8) . . ? C14 C15 Fe2 69.5(4) . . ? C11 C15 Fe2 70.3(4) . . ? C14 C15 H15 126.0 . . ? C11 C15 H15 126.0 . . ? Fe2 C15 H15 125.7 . . ? C20 C16 C17 108.4(9) . . ? C20 C16 Fe2 70.1(5) . . ? C17 C16 Fe2 69.7(5) . . ? C20 C16 H16 125.8 . . ? C17 C16 H16 125.8 . . ? Fe2 C16 H16 126.0 . . ? C18 C17 C16 105.9(9) . . ? C18 C17 Fe2 69.3(6) . . ? C16 C17 Fe2 70.0(5) . . ? C18 C17 H17 127.1 . . ? C16 C17 H17 127.1 . . ? Fe2 C17 H17 125.3 . . ? C19 C18 C17 110.9(9) . . ? C19 C18 Fe2 71.1(6) . . ? C17 C18 Fe2 70.7(6) . . ? C19 C18 H18 124.6 . . ? C17 C18 H18 124.6 . . ? Fe2 C18 H18 125.2 . . ? C18 C19 C20 106.9(9) . . ? C18 C19 Fe2 69.4(6) . . ? C20 C19 Fe2 70.1(6) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.6 . . ? Fe2 C19 H19 125.6 . . ? C16 C20 C19 107.9(9) . . ? C16 C20 Fe2 69.9(5) . . ? C19 C20 Fe2 69.8(5) . . ? C16 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? Fe2 C20 H20 125.8 . . ? C22 C21 N1 129.1(7) . . ? C22 C21 C26 122.5(7) . . ? N1 C21 C26 108.4(6) . . ? C23 C22 C21 118.5(7) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 121.0(6) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 119.8(6) . . ? C25 C24 C33 119.7(7) . . ? C23 C24 C33 120.4(6) . . ? C24 C25 C26 119.1(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C21 118.9(6) . . ? C25 C26 C27 134.3(6) . . ? C21 C26 C27 106.5(6) . . ? C28 C27 C32 120.5(7) . . ? C28 C27 C26 134.1(7) . . ? C32 C27 C26 105.4(6) . . ? C27 C28 C29 120.8(7) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 116.3(7) . . ? C28 C29 C35 121.4(7) . . ? C30 C29 C35 122.2(7) . . ? C31 C30 C29 125.0(7) . . ? C31 C30 H30 117.5 . . ? C29 C30 H30 117.5 . . ? C30 C31 C32 117.4(7) . . ? C30 C31 H31 121.3 . . ? C32 C31 H31 121.3 . . ? N1 C32 C27 111.7(6) . . ? N1 C32 C31 128.2(7) . . ? C27 C32 C31 120.0(7) . . ? C34 C33 C24 127.8(7) . . ? C34 C33 H33 116.1 . . ? C24 C33 H33 116.1 . . ? C33 C34 C1 128.9(7) . . ? C33 C34 H34 115.5 . . ? C1 C34 H34 115.5 . . ? C36 C35 C29 127.5(8) . . ? C36 C35 H35 116.3 . . ? C29 C35 H35 116.3 . . ? C35 C36 C11 127.1(8) . . ? C35 C36 H36 116.4 . . ? C11 C36 H36 116.4 . . ? N1 C37 C38 112.6(7) . . ? N1 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? N1 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Fe1 C1 C5 124.3(5) . . . . ? C9 Fe1 C1 C5 53.3(9) . . . . ? C10 Fe1 C1 C5 83.0(5) . . . . ? C3 Fe1 C1 C5 -79.9(5) . . . . ? C2 Fe1 C1 C5 -117.4(6) . . . . ? C8 Fe1 C1 C5 -169.3(9) . . . . ? C4 Fe1 C1 C5 -37.3(4) . . . . ? C7 Fe1 C1 C5 165.1(4) . . . . ? C6 Fe1 C1 C2 -118.3(5) . . . . ? C9 Fe1 C1 C2 170.7(7) . . . . ? C10 Fe1 C1 C2 -159.7(4) . . . . ? C3 Fe1 C1 C2 37.5(4) . . . . ? C5 Fe1 C1 C2 117.4(6) . . . . ? C8 Fe1 C1 C2 -51.9(12) . . . . ? C4 Fe1 C1 C2 80.1(5) . . . . ? C7 Fe1 C1 C2 -77.5(5) . . . . ? C6 Fe1 C1 C34 2.5(7) . . . . ? C9 Fe1 C1 C34 -68.5(10) . . . . ? C10 Fe1 C1 C34 -38.9(7) . . . . ? C3 Fe1 C1 C34 158.3(7) . . . . ? C2 Fe1 C1 C34 120.8(8) . . . . ? C5 Fe1 C1 C34 -121.8(8) . . . . ? C8 Fe1 C1 C34 68.9(13) . . . . ? C4 Fe1 C1 C34 -159.1(7) . . . . ? C7 Fe1 C1 C34 43.2(7) . . . . ? C5 C1 C2 C3 0.8(8) . . . . ? C34 C1 C2 C3 -179.2(7) . . . . ? Fe1 C1 C2 C3 -59.2(5) . . . . ? C5 C1 C2 Fe1 60.0(5) . . . . ? C34 C1 C2 Fe1 -120.0(8) . . . . ? C6 Fe1 C2 C3 -161.6(4) . . . . ? C9 Fe1 C2 C3 -48.1(11) . . . . ? C10 Fe1 C2 C3 165.6(6) . . . . ? C5 Fe1 C2 C3 80.7(4) . . . . ? C8 Fe1 C2 C3 -79.5(5) . . . . ? C4 Fe1 C2 C3 37.4(4) . . . . ? C1 Fe1 C2 C3 119.5(6) . . . . ? C7 Fe1 C2 C3 -119.3(4) . . . . ? C6 Fe1 C2 C1 78.9(5) . . . . ? C9 Fe1 C2 C1 -167.5(9) . . . . ? C10 Fe1 C2 C1 46.1(9) . . . . ? C3 Fe1 C2 C1 -119.5(6) . . . . ? C5 Fe1 C2 C1 -38.7(4) . . . . ? C8 Fe1 C2 C1 161.0(5) . . . . ? C4 Fe1 C2 C1 -82.0(5) . . . . ? C7 Fe1 C2 C1 121.2(5) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? Fe1 C2 C3 C4 -60.5(5) . . . . ? C1 C2 C3 Fe1 59.1(5) . . . . ? C6 Fe1 C3 C4 161.3(7) . . . . ? C9 Fe1 C3 C4 -78.0(6) . . . . ? C10 Fe1 C3 C4 -41.4(12) . . . . ? C2 Fe1 C3 C4 118.3(6) . . . . ? C5 Fe1 C3 C4 36.4(4) . . . . ? C8 Fe1 C3 C4 -120.7(5) . . . . ? C1 Fe1 C3 C4 80.5(5) . . . . ? C7 Fe1 C3 C4 -162.9(4) . . . . ? C6 Fe1 C3 C2 43.0(9) . . . . ? C9 Fe1 C3 C2 163.7(5) . . . . ? C10 Fe1 C3 C2 -159.7(9) . . . . ? C5 Fe1 C3 C2 -82.0(4) . . . . ? C8 Fe1 C3 C2 121.0(5) . . . . ? C4 Fe1 C3 C2 -118.3(6) . . . . ? C1 Fe1 C3 C2 -37.9(4) . . . . ? C7 Fe1 C3 C2 78.8(5) . . . . ? C2 C3 C4 C5 1.4(9) . . . . ? Fe1 C3 C4 C5 -58.7(6) . . . . ? C2 C3 C4 Fe1 60.0(5) . . . . ? C6 Fe1 C4 C3 -156.2(9) . . . . ? C9 Fe1 C4 C3 122.6(5) . . . . ? C10 Fe1 C4 C3 165.7(5) . . . . ? C2 Fe1 C4 C3 -38.5(4) . . . . ? C5 Fe1 C4 C3 -121.3(7) . . . . ? C8 Fe1 C4 C3 79.0(6) . . . . ? C1 Fe1 C4 C3 -83.2(5) . . . . ? C7 Fe1 C4 C3 40.7(10) . . . . ? C6 Fe1 C4 C5 -34.9(12) . . . . ? C9 Fe1 C4 C5 -116.1(5) . . . . ? C10 Fe1 C4 C5 -73.1(6) . . . . ? C3 Fe1 C4 C5 121.3(7) . . . . ? C2 Fe1 C4 C5 82.8(5) . . . . ? C8 Fe1 C4 C5 -159.7(5) . . . . ? C1 Fe1 C4 C5 38.1(4) . . . . ? C7 Fe1 C4 C5 162.0(7) . . . . ? C3 C4 C5 C1 -0.9(9) . . . . ? Fe1 C4 C5 C1 -59.6(5) . . . . ? C3 C4 C5 Fe1 58.8(5) . . . . ? C2 C1 C5 C4 0.0(9) . . . . ? C34 C1 C5 C4 -179.9(7) . . . . ? Fe1 C1 C5 C4 59.9(5) . . . . ? C2 C1 C5 Fe1 -59.9(5) . . . . ? C34 C1 C5 Fe1 120.2(8) . . . . ? C6 Fe1 C5 C4 167.3(5) . . . . ? C9 Fe1 C5 C4 83.7(6) . . . . ? C10 Fe1 C5 C4 126.0(5) . . . . ? C3 Fe1 C5 C4 -36.0(4) . . . . ? C2 Fe1 C5 C4 -80.0(5) . . . . ? C8 Fe1 C5 C4 51.1(11) . . . . ? C1 Fe1 C5 C4 -119.0(6) . . . . ? C7 Fe1 C5 C4 -159.2(8) . . . . ? C6 Fe1 C5 C1 -73.7(6) . . . . ? C9 Fe1 C5 C1 -157.3(5) . . . . ? C10 Fe1 C5 C1 -115.0(5) . . . . ? C3 Fe1 C5 C1 83.0(5) . . . . ? C2 Fe1 C5 C1 39.0(4) . . . . ? C8 Fe1 C5 C1 170.1(9) . . . . ? C4 Fe1 C5 C1 119.0(6) . . . . ? C7 Fe1 C5 C1 -40.1(11) . . . . ? C9 Fe1 C6 C10 38.1(4) . . . . ? C3 Fe1 C6 C10 169.6(7) . . . . ? C2 Fe1 C6 C10 -159.4(5) . . . . ? C5 Fe1 C6 C10 -76.6(5) . . . . ? C8 Fe1 C6 C10 82.4(5) . . . . ? C4 Fe1 C6 C10 -50.3(11) . . . . ? C1 Fe1 C6 C10 -117.3(5) . . . . ? C7 Fe1 C6 C10 119.8(6) . . . . ? C9 Fe1 C6 C7 -81.7(5) . . . . ? C10 Fe1 C6 C7 -119.8(6) . . . . ? C3 Fe1 C6 C7 49.8(9) . . . . ? C2 Fe1 C6 C7 80.7(5) . . . . ? C5 Fe1 C6 C7 163.5(4) . . . . ? C8 Fe1 C6 C7 -37.4(5) . . . . ? C4 Fe1 C6 C7 -170.1(9) . . . . ? C1 Fe1 C6 C7 122.9(5) . . . . ? C10 C6 C7 C8 -0.1(9) . . . . ? Fe1 C6 C7 C8 59.9(5) . . . . ? C10 C6 C7 Fe1 -60.0(5) . . . . ? C6 Fe1 C7 C8 -118.5(7) . . . . ? C9 Fe1 C7 C8 -37.4(6) . . . . ? C10 Fe1 C7 C8 -81.4(6) . . . . ? C3 Fe1 C7 C8 82.6(6) . . . . ? C2 Fe1 C7 C8 124.5(6) . . . . ? C5 Fe1 C7 C8 -163.1(8) . . . . ? C4 Fe1 C7 C8 53.3(10) . . . . ? C1 Fe1 C7 C8 166.7(6) . . . . ? C9 Fe1 C7 C6 81.1(5) . . . . ? C10 Fe1 C7 C6 37.1(4) . . . . ? C3 Fe1 C7 C6 -158.9(5) . . . . ? C2 Fe1 C7 C6 -117.0(5) . . . . ? C5 Fe1 C7 C6 -44.6(11) . . . . ? C8 Fe1 C7 C6 118.5(7) . . . . ? C4 Fe1 C7 C6 171.8(7) . . . . ? C1 Fe1 C7 C6 -74.8(6) . . . . ? C6 C7 C8 C9 -0.6(9) . . . . ? Fe1 C7 C8 C9 58.3(5) . . . . ? C6 C7 C8 Fe1 -58.9(5) . . . . ? C6 Fe1 C8 C7 38.4(5) . . . . ? C9 Fe1 C8 C7 120.4(8) . . . . ? C10 Fe1 C8 C7 82.1(5) . . . . ? C3 Fe1 C8 C7 -116.6(5) . . . . ? C2 Fe1 C8 C7 -73.7(6) . . . . ? C5 Fe1 C8 C7 164.7(8) . . . . ? C4 Fe1 C8 C7 -158.1(5) . . . . ? C1 Fe1 C8 C7 -34.6(13) . . . . ? C6 Fe1 C8 C9 -82.0(5) . . . . ? C10 Fe1 C8 C9 -38.3(5) . . . . ? C3 Fe1 C8 C9 123.0(5) . . . . ? C2 Fe1 C8 C9 165.9(5) . . . . ? C5 Fe1 C8 C9 44.3(12) . . . . ? C4 Fe1 C8 C9 81.5(6) . . . . ? C1 Fe1 C8 C9 -155.0(9) . . . . ? C7 Fe1 C8 C9 -120.4(8) . . . . ? C7 C8 C9 C10 1.1(9) . . . . ? Fe1 C8 C9 C10 60.2(5) . . . . ? C7 C8 C9 Fe1 -59.1(6) . . . . ? C6 Fe1 C9 C10 -37.8(4) . . . . ? C3 Fe1 C9 C10 164.0(4) . . . . ? C2 Fe1 C9 C10 -159.1(9) . . . . ? C5 Fe1 C9 C10 79.6(6) . . . . ? C8 Fe1 C9 C10 -118.1(7) . . . . ? C4 Fe1 C9 C10 122.4(5) . . . . ? C1 Fe1 C9 C10 41.3(10) . . . . ? C7 Fe1 C9 C10 -81.8(5) . . . . ? C6 Fe1 C9 C8 80.3(5) . . . . ? C10 Fe1 C9 C8 118.1(7) . . . . ? C3 Fe1 C9 C8 -77.9(6) . . . . ? C2 Fe1 C9 C8 -41.0(12) . . . . ? C5 Fe1 C9 C8 -162.4(5) . . . . ? C4 Fe1 C9 C8 -119.5(5) . . . . ? C1 Fe1 C9 C8 159.4(7) . . . . ? C7 Fe1 C9 C8 36.3(5) . . . . ? C7 C6 C10 C9 0.8(9) . . . . ? Fe1 C6 C10 C9 -59.3(5) . . . . ? C7 C6 C10 Fe1 60.2(5) . . . . ? C8 C9 C10 C6 -1.2(9) . . . . ? Fe1 C9 C10 C6 59.2(5) . . . . ? C8 C9 C10 Fe1 -60.4(6) . . . . ? C9 Fe1 C10 C6 -118.7(7) . . . . ? C3 Fe1 C10 C6 -166.2(9) . . . . ? C2 Fe1 C10 C6 46.3(9) . . . . ? C5 Fe1 C10 C6 122.2(5) . . . . ? C8 Fe1 C10 C6 -80.3(5) . . . . ? C4 Fe1 C10 C6 162.3(4) . . . . ? C1 Fe1 C10 C6 79.3(5) . . . . ? C7 Fe1 C10 C6 -37.4(4) . . . . ? C6 Fe1 C10 C9 118.7(7) . . . . ? C3 Fe1 C10 C9 -47.5(12) . . . . ? C2 Fe1 C10 C9 165.0(6) . . . . ? C5 Fe1 C10 C9 -119.1(5) . . . . ? C8 Fe1 C10 C9 38.4(4) . . . . ? C4 Fe1 C10 C9 -79.0(6) . . . . ? C1 Fe1 C10 C9 -162.0(5) . . . . ? C7 Fe1 C10 C9 81.2(5) . . . . ? C18 Fe2 C11 C36 61.0(10) . . . . ? C17 Fe2 C11 C36 -81(2) . . . . ? C19 Fe2 C11 C36 29.3(9) . . . . ? C16 Fe2 C11 C36 -52.4(9) . . . . ? C20 Fe2 C11 C36 -13.3(8) . . . . ? C13 Fe2 C11 C36 -162.3(8) . . . . ? C14 Fe2 C11 C36 154.6(8) . . . . ? C15 Fe2 C11 C36 116.7(9) . . . . ? C12 Fe2 C11 C36 -125.4(9) . . . . ? C18 Fe2 C11 C12 -173.6(7) . . . . ? C17 Fe2 C11 C12 44.6(19) . . . . ? C19 Fe2 C11 C12 154.8(6) . . . . ? C16 Fe2 C11 C12 73.0(7) . . . . ? C20 Fe2 C11 C12 112.2(6) . . . . ? C13 Fe2 C11 C12 -36.8(5) . . . . ? C14 Fe2 C11 C12 -80.0(5) . . . . ? C15 Fe2 C11 C12 -117.9(7) . . . . ? C18 Fe2 C11 C15 -55.7(9) . . . . ? C17 Fe2 C11 C15 162.5(16) . . . . ? C19 Fe2 C11 C15 -87.3(6) . . . . ? C16 Fe2 C11 C15 -169.1(6) . . . . ? C20 Fe2 C11 C15 -129.9(6) . . . . ? C13 Fe2 C11 C15 81.1(5) . . . . ? C14 Fe2 C11 C15 37.9(5) . . . . ? C12 Fe2 C11 C15 117.9(7) . . . . ? C36 C11 C12 C13 -178.5(8) . . . . ? C15 C11 C12 C13 0.1(10) . . . . ? Fe2 C11 C12 C13 58.8(6) . . . . ? C36 C11 C12 Fe2 122.7(9) . . . . ? C15 C11 C12 Fe2 -58.7(5) . . . . ? C18 Fe2 C12 C13 43(2) . . . . ? C17 Fe2 C12 C13 70.9(7) . . . . ? C19 Fe2 C12 C13 -170.2(7) . . . . ? C16 Fe2 C12 C13 111.5(6) . . . . ? C20 Fe2 C12 C13 154.5(6) . . . . ? C14 Fe2 C12 C13 -36.9(5) . . . . ? C15 Fe2 C12 C13 -81.1(5) . . . . ? C11 Fe2 C12 C13 -120.0(7) . . . . ? C18 Fe2 C12 C11 163.4(17) . . . . ? C17 Fe2 C12 C11 -169.2(6) . . . . ? C19 Fe2 C12 C11 -50.3(9) . . . . ? C16 Fe2 C12 C11 -128.5(6) . . . . ? C20 Fe2 C12 C11 -85.6(6) . . . . ? C13 Fe2 C12 C11 120.0(7) . . . . ? C14 Fe2 C12 C11 83.1(5) . . . . ? C15 Fe2 C12 C11 38.8(5) . . . . ? C11 C12 C13 C14 0.3(10) . . . . ? Fe2 C12 C13 C14 59.6(6) . . . . ? C11 C12 C13 Fe2 -59.3(6) . . . . ? C18 Fe2 C13 C14 70.1(7) . . . . ? C17 Fe2 C13 C14 109.7(6) . . . . ? C19 Fe2 C13 C14 35(2) . . . . ? C16 Fe2 C13 C14 153.0(5) . . . . ? C20 Fe2 C13 C14 -171.3(7) . . . . ? C15 Fe2 C13 C14 -38.0(4) . . . . ? C12 Fe2 C13 C14 -120.2(7) . . . . ? C11 Fe2 C13 C14 -82.7(5) . . . . ? C18 Fe2 C13 C12 -169.7(6) . . . . ? C17 Fe2 C13 C12 -130.1(6) . . . . ? C19 Fe2 C13 C12 155.7(17) . . . . ? C16 Fe2 C13 C12 -86.8(6) . . . . ? C20 Fe2 C13 C12 -51.0(9) . . . . ? C14 Fe2 C13 C12 120.2(7) . . . . ? C15 Fe2 C13 C12 82.2(5) . . . . ? C11 Fe2 C13 C12 37.5(5) . . . . ? C12 C13 C14 C15 -0.6(10) . . . . ? Fe2 C13 C14 C15 59.3(6) . . . . ? C12 C13 C14 Fe2 -59.9(6) . . . . ? C18 Fe2 C14 C13 -131.2(6) . . . . ? C17 Fe2 C14 C13 -88.2(7) . . . . ? C19 Fe2 C14 C13 -171.1(6) . . . . ? C16 Fe2 C14 C13 -53.9(10) . . . . ? C20 Fe2 C14 C13 158.7(17) . . . . ? C15 Fe2 C14 C13 119.2(7) . . . . ? C12 Fe2 C14 C13 36.9(5) . . . . ? C11 Fe2 C14 C13 80.9(5) . . . . ? C18 Fe2 C14 C15 109.6(7) . . . . ? C17 Fe2 C14 C15 152.7(6) . . . . ? C19 Fe2 C14 C15 69.7(7) . . . . ? C16 Fe2 C14 C15 -173.0(7) . . . . ? C20 Fe2 C14 C15 40(2) . . . . ? C13 Fe2 C14 C15 -119.2(7) . . . . ? C12 Fe2 C14 C15 -82.3(5) . . . . ? C11 Fe2 C14 C15 -38.3(5) . . . . ? C13 C14 C15 C11 0.6(10) . . . . ? Fe2 C14 C15 C11 60.1(6) . . . . ? C13 C14 C15 Fe2 -59.5(6) . . . . ? C36 C11 C15 C14 178.2(7) . . . . ? C12 C11 C15 C14 -0.4(9) . . . . ? Fe2 C11 C15 C14 -59.6(6) . . . . ? C36 C11 C15 Fe2 -122.2(8) . . . . ? C12 C11 C15 Fe2 59.2(6) . . . . ? C18 Fe2 C15 C14 -89.0(7) . . . . ? C17 Fe2 C15 C14 -54.1(10) . . . . ? C19 Fe2 C15 C14 -130.9(6) . . . . ? C16 Fe2 C15 C14 163.3(18) . . . . ? C20 Fe2 C15 C14 -170.3(6) . . . . ? C13 Fe2 C15 C14 37.3(5) . . . . ? C12 Fe2 C15 C14 80.5(5) . . . . ? C11 Fe2 C15 C14 118.8(8) . . . . ? C18 Fe2 C15 C11 152.2(6) . . . . ? C17 Fe2 C15 C11 -173.0(7) . . . . ? C19 Fe2 C15 C11 110.3(6) . . . . ? C16 Fe2 C15 C11 44(2) . . . . ? C20 Fe2 C15 C11 70.9(7) . . . . ? C13 Fe2 C15 C11 -81.6(5) . . . . ? C14 Fe2 C15 C11 -118.8(8) . . . . ? C12 Fe2 C15 C11 -38.4(5) . . . . ? C18 Fe2 C16 C20 -80.8(7) . . . . ? C17 Fe2 C16 C20 -119.5(9) . . . . ? C19 Fe2 C16 C20 -37.7(6) . . . . ? C13 Fe2 C16 C20 153.6(6) . . . . ? C14 Fe2 C16 C20 -170.1(8) . . . . ? C15 Fe2 C16 C20 32(2) . . . . ? C12 Fe2 C16 C20 110.7(7) . . . . ? C11 Fe2 C16 C20 69.1(8) . . . . ? C18 Fe2 C16 C17 38.7(6) . . . . ? C19 Fe2 C16 C17 81.8(7) . . . . ? C20 Fe2 C16 C17 119.5(9) . . . . ? C13 Fe2 C16 C17 -86.9(7) . . . . ? C14 Fe2 C16 C17 -50.6(11) . . . . ? C15 Fe2 C16 C17 151.8(17) . . . . ? C12 Fe2 C16 C17 -129.8(7) . . . . ? C11 Fe2 C16 C17 -171.4(6) . . . . ? C20 C16 C17 C18 -0.7(11) . . . . ? Fe2 C16 C17 C18 -60.3(7) . . . . ? C20 C16 C17 Fe2 59.6(7) . . . . ? C19 Fe2 C17 C18 36.0(6) . . . . ? C16 Fe2 C17 C18 116.7(9) . . . . ? C20 Fe2 C17 C18 79.5(7) . . . . ? C13 Fe2 C17 C18 -131.8(7) . . . . ? C14 Fe2 C17 C18 -88.8(7) . . . . ? C15 Fe2 C17 C18 -52.1(10) . . . . ? C12 Fe2 C17 C18 -171.9(6) . . . . ? C11 Fe2 C17 C18 151.2(17) . . . . ? C18 Fe2 C17 C16 -116.7(9) . . . . ? C19 Fe2 C17 C16 -80.7(7) . . . . ? C20 Fe2 C17 C16 -37.2(6) . . . . ? C13 Fe2 C17 C16 111.6(7) . . . . ? C14 Fe2 C17 C16 154.6(7) . . . . ? C15 Fe2 C17 C16 -168.7(7) . . . . ? C12 Fe2 C17 C16 71.4(8) . . . . ? C11 Fe2 C17 C16 34(2) . . . . ? C16 C17 C18 C19 0.8(12) . . . . ? Fe2 C17 C18 C19 -60.0(8) . . . . ? C16 C17 C18 Fe2 60.8(7) . . . . ? C17 Fe2 C18 C19 121.3(9) . . . . ? C16 Fe2 C18 C19 82.2(7) . . . . ? C20 Fe2 C18 C19 38.4(6) . . . . ? C13 Fe2 C18 C19 -169.5(6) . . . . ? C14 Fe2 C18 C19 -129.5(7) . . . . ? C15 Fe2 C18 C19 -85.3(7) . . . . ? C12 Fe2 C18 C19 154.5(17) . . . . ? C11 Fe2 C18 C19 -47.4(10) . . . . ? C19 Fe2 C18 C17 -121.3(9) . . . . ? C16 Fe2 C18 C17 -39.1(6) . . . . ? C20 Fe2 C18 C17 -82.8(6) . . . . ? C13 Fe2 C18 C17 69.2(8) . . . . ? C14 Fe2 C18 C17 109.3(7) . . . . ? C15 Fe2 C18 C17 153.4(6) . . . . ? C12 Fe2 C18 C17 33(2) . . . . ? C11 Fe2 C18 C17 -168.7(7) . . . . ? C17 C18 C19 C20 -0.6(12) . . . . ? Fe2 C18 C19 C20 -60.3(7) . . . . ? C17 C18 C19 Fe2 59.7(8) . . . . ? C17 Fe2 C19 C18 -36.4(6) . . . . ? C16 Fe2 C19 C18 -80.2(7) . . . . ? C20 Fe2 C19 C18 -117.8(9) . . . . ? C13 Fe2 C19 C18 42(2) . . . . ? C14 Fe2 C19 C18 71.4(8) . . . . ? C15 Fe2 C19 C18 111.6(7) . . . . ? C12 Fe2 C19 C18 -170.1(7) . . . . ? C11 Fe2 C19 C18 155.6(6) . . . . ? C18 Fe2 C19 C20 117.8(9) . . . . ? C17 Fe2 C19 C20 81.4(6) . . . . ? C16 Fe2 C19 C20 37.6(5) . . . . ? C13 Fe2 C19 C20 160.0(16) . . . . ? C14 Fe2 C19 C20 -170.8(5) . . . . ? C15 Fe2 C19 C20 -130.5(6) . . . . ? C12 Fe2 C19 C20 -52.3(10) . . . . ? C11 Fe2 C19 C20 -86.6(6) . . . . ? C17 C16 C20 C19 0.3(12) . . . . ? Fe2 C16 C20 C19 59.7(7) . . . . ? C17 C16 C20 Fe2 -59.4(7) . . . . ? C18 C19 C20 C16 0.2(12) . . . . ? Fe2 C19 C20 C16 -59.8(7) . . . . ? C18 C19 C20 Fe2 59.9(7) . . . . ? C18 Fe2 C20 C16 81.0(7) . . . . ? C17 Fe2 C20 C16 37.5(6) . . . . ? C19 Fe2 C20 C16 118.9(9) . . . . ? C13 Fe2 C20 C16 -52.9(10) . . . . ? C14 Fe2 C20 C16 155.6(16) . . . . ? C15 Fe2 C20 C16 -171.7(6) . . . . ? C12 Fe2 C20 C16 -87.4(7) . . . . ? C11 Fe2 C20 C16 -130.7(6) . . . . ? C18 Fe2 C20 C19 -37.8(6) . . . . ? C17 Fe2 C20 C19 -81.4(6) . . . . ? C16 Fe2 C20 C19 -118.9(9) . . . . ? C13 Fe2 C20 C19 -171.8(7) . . . . ? C14 Fe2 C20 C19 37(2) . . . . ? C15 Fe2 C20 C19 69.4(7) . . . . ? C12 Fe2 C20 C19 153.7(6) . . . . ? C11 Fe2 C20 C19 110.4(6) . . . . ? C32 N1 C21 C22 178.7(7) . . . . ? C37 N1 C21 C22 14.8(12) . . . . ? C32 N1 C21 C26 -1.2(8) . . . . ? C37 N1 C21 C26 -165.2(7) . . . . ? N1 C21 C22 C23 -177.4(7) . . . . ? C26 C21 C22 C23 2.6(11) . . . . ? C21 C22 C23 C24 0.2(11) . . . . ? C22 C23 C24 C25 -0.5(11) . . . . ? C22 C23 C24 C33 175.6(6) . . . . ? C23 C24 C25 C26 -2.0(10) . . . . ? C33 C24 C25 C26 -178.1(6) . . . . ? C24 C25 C26 C21 4.6(10) . . . . ? C24 C25 C26 C27 176.8(7) . . . . ? C22 C21 C26 C25 -5.0(10) . . . . ? N1 C21 C26 C25 174.9(6) . . . . ? C22 C21 C26 C27 -179.2(6) . . . . ? N1 C21 C26 C27 0.8(8) . . . . ? C25 C26 C27 C28 7.8(14) . . . . ? C21 C26 C27 C28 -179.3(8) . . . . ? C25 C26 C27 C32 -172.9(7) . . . . ? C21 C26 C27 C32 0.0(8) . . . . ? C32 C27 C28 C29 2.4(11) . . . . ? C26 C27 C28 C29 -178.4(7) . . . . ? C27 C28 C29 C30 -1.1(10) . . . . ? C27 C28 C29 C35 178.1(7) . . . . ? C28 C29 C30 C31 0.1(12) . . . . ? C35 C29 C30 C31 -179.2(7) . . . . ? C29 C30 C31 C32 -0.3(12) . . . . ? C21 N1 C32 C27 1.3(8) . . . . ? C37 N1 C32 C27 164.4(7) . . . . ? C21 N1 C32 C31 -177.4(7) . . . . ? C37 N1 C32 C31 -14.3(12) . . . . ? C28 C27 C32 N1 178.7(6) . . . . ? C26 C27 C32 N1 -0.8(8) . . . . ? C28 C27 C32 C31 -2.5(11) . . . . ? C26 C27 C32 C31 178.0(6) . . . . ? C30 C31 C32 N1 -179.9(7) . . . . ? C30 C31 C32 C27 1.5(11) . . . . ? C25 C24 C33 C34 -173.1(7) . . . . ? C23 C24 C33 C34 10.8(11) . . . . ? C24 C33 C34 C1 -177.7(7) . . . . ? C5 C1 C34 C33 177.8(7) . . . . ? C2 C1 C34 C33 -2.1(13) . . . . ? Fe1 C1 C34 C33 -91.7(9) . . . . ? C28 C29 C35 C36 170.4(7) . . . . ? C30 C29 C35 C36 -10.4(12) . . . . ? C29 C35 C36 C11 175.5(7) . . . . ? C12 C11 C36 C35 13.4(14) . . . . ? C15 C11 C36 C35 -164.9(8) . . . . ? Fe2 C11 C36 C35 107.3(9) . . . . ? C32 N1 C37 C38 -90.2(9) . . . . ? C21 N1 C37 C38 70.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.456 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.069