# 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 _publ_contact_author_name 'Francois Varret' _publ_contact_author_email 'VARRET FRANCOIS@YAHOO.FR' _publ_section_title ; Spin-transition in [FeII(L5)2][ClO4]2 [L5 = 2-[3-(2'-pyridyl)pyrazol-1-ylmethyl](1-methylimidazole)]: a further example of coexistence of features typical for disorder and cooperativity ; loop_ _publ_author_name 'Francois Varret' 'Cherif Balde' 'Epiphane Codjovi' 'Cedric Desplanches' 'Cristian Enachescu' ; J.-F.Letard ; 'Jorge Linares' 'Vibha Mishra' 'Haritosh Mishra' 'R Mukherjee' #===END data_5maram _database_code_depnum_ccdc_archive 'CCDC 711283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H29 Cl2 Fe N11 O8' _chemical_formula_sum 'C28 H29 Cl2 Fe N11 O8' _chemical_formula_weight 774.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.805(5) _cell_length_b 9.328(5) _cell_length_c 19.936(5) _cell_angle_alpha 91.853(5) _cell_angle_beta 93.625(5) _cell_angle_gamma 94.966(5) _cell_volume 1626.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.46 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8733 _exptl_absorpt_correction_T_max 0.9337 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _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 10944 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.46 _reflns_number_total 7807 _reflns_number_gt 4192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1291P)^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 7807 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1568 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.2527 _refine_ls_wR_factor_gt 0.2069 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.71133(8) 0.38205(7) 0.27205(4) 0.0302(2) Uani 1 1 d . . . Cl1 Cl 0.1222(2) 0.7586(2) 0.07754(10) 0.0785(6) Uani 1 1 d . . . Cl2 Cl 0.24425(18) 0.12689(17) 0.44395(8) 0.0564(4) Uani 1 1 d . . . O1 O 0.0845(10) 0.8490(8) 0.0260(3) 0.151(3) Uani 1 1 d . . . O2 O 0.2539(13) 0.8333(9) 0.1121(6) 0.226(6) Uani 1 1 d . . . O3 O 0.1594(10) 0.6223(8) 0.0562(4) 0.141(3) Uani 1 1 d . . . O4 O 0.0332(17) 0.7553(18) 0.1258(6) 0.316(9) Uani 1 1 d . . . O5 O 0.3556(8) 0.2040(9) 0.4872(4) 0.140(3) Uani 1 1 d . . . O6 O 0.2903(7) 0.1188(6) 0.3771(3) 0.0906(17) Uani 1 1 d . . . O7 O 0.1079(6) 0.1977(6) 0.4431(3) 0.0903(17) Uani 1 1 d . . . O8 O 0.2152(9) -0.0089(6) 0.4669(3) 0.124(2) Uani 1 1 d . . . N1 N 0.8094(4) 0.5824(4) 0.2930(2) 0.0326(9) Uani 1 1 d . . . N2 N 0.7595(5) 0.3716(4) 0.3659(2) 0.0360(10) Uani 1 1 d . . . N3 N 0.7255(5) 0.2705(4) 0.4110(2) 0.0387(10) Uani 1 1 d . . . N4 N 0.5383(5) -0.0319(5) 0.3035(2) 0.0449(11) Uani 1 1 d . . . N5 N 0.6184(5) 0.1797(4) 0.2704(2) 0.0366(10) Uani 1 1 d . . . N6 N 0.5065(4) 0.4522(4) 0.2836(2) 0.0330(9) Uani 1 1 d . . . N7 N 0.6549(5) 0.4221(5) 0.1812(2) 0.0389(10) Uani 1 1 d . . . N8 N 0.7301(5) 0.4253(5) 0.1246(2) 0.0481(12) Uani 1 1 d . . . N9 N 1.0698(5) 0.2337(5) 0.1760(3) 0.0504(12) Uani 1 1 d . . . N10 N 0.9004(4) 0.3115(4) 0.2416(2) 0.0342(10) Uani 1 1 d . . . C1 C 0.8402(6) 0.6900(6) 0.2501(3) 0.0433(13) Uani 1 1 d . . . H1 H 0.8140 0.6717 0.2045 0.052 Uiso 1 1 calc R . . C2 C 0.9056(7) 0.8203(6) 0.2696(3) 0.0537(16) Uani 1 1 d . . . H2 H 0.9234 0.8900 0.2380 0.064 Uiso 1 1 calc R . . C3 C 0.9470(7) 0.8513(6) 0.3370(4) 0.0542(16) Uani 1 1 d . . . H3 H 0.9926 0.9414 0.3516 0.065 Uiso 1 1 calc R . . C4 C 0.9182(7) 0.7441(6) 0.3815(3) 0.0492(14) Uani 1 1 d . . . H4 H 0.9459 0.7605 0.4271 0.059 Uiso 1 1 calc R . . C5 C 0.8489(6) 0.6135(6) 0.3585(3) 0.0390(12) Uani 1 1 d . . . C6 C 0.8110(6) 0.4925(5) 0.4007(3) 0.0370(12) Uani 1 1 d . . . C7 C 0.8099(8) 0.4699(6) 0.4689(3) 0.0560(17) Uani 1 1 d . . . H7 H 0.8398 0.5366 0.5039 0.067 Uiso 1 1 calc R . . C8 C 0.7563(8) 0.3313(7) 0.4741(3) 0.0575(17) Uani 1 1 d . . . H8 H 0.7425 0.2848 0.5141 0.069 Uiso 1 1 calc R . . C9 C 0.6814(7) 0.1199(6) 0.3912(3) 0.0485(14) Uani 1 1 d . . . H9A H 0.6087 0.0806 0.4219 0.058 Uiso 1 1 calc R . . H9B H 0.7711 0.0666 0.3959 0.058 Uiso 1 1 calc R . . C10 C 0.6134(6) 0.0969(5) 0.3220(3) 0.0337(11) Uani 1 1 d . . . C11 C 0.5065(8) -0.1543(6) 0.3463(3) 0.0583(17) Uani 1 1 d . . . H11A H 0.4511 -0.2321 0.3200 0.087 Uiso 1 1 calc R . . H11B H 0.4464 -0.1258 0.3822 0.087 Uiso 1 1 calc R . . H11C H 0.6010 -0.1853 0.3648 0.087 Uiso 1 1 calc R . . C12 C 0.4921(7) -0.0280(6) 0.2363(3) 0.0510(15) Uani 1 1 d . . . H12 H 0.4386 -0.1014 0.2095 0.061 Uiso 1 1 calc R . . C13 C 0.5418(6) 0.1066(6) 0.2175(3) 0.0476(14) Uani 1 1 d . . . H13 H 0.5254 0.1422 0.1748 0.057 Uiso 1 1 calc R . . C14 C 0.4302(6) 0.4545(5) 0.3394(3) 0.0395(12) Uani 1 1 d . . . H14 H 0.4741 0.4200 0.3787 0.047 Uiso 1 1 calc R . . C15 C 0.2881(7) 0.5064(6) 0.3404(3) 0.0505(15) Uani 1 1 d . . . H15 H 0.2376 0.5057 0.3800 0.061 Uiso 1 1 calc R . . C16 C 0.2217(7) 0.5587(7) 0.2840(3) 0.0535(16) Uani 1 1 d . . . H16 H 0.1264 0.5946 0.2846 0.064 Uiso 1 1 calc R . . C17 C 0.2984(6) 0.5573(7) 0.2260(3) 0.0520(15) Uani 1 1 d . . . H17 H 0.2561 0.5929 0.1867 0.062 Uiso 1 1 calc R . . C18 C 0.4384(6) 0.5026(6) 0.2269(3) 0.0406(13) Uani 1 1 d . . . C19 C 0.5297(6) 0.4917(6) 0.1684(3) 0.0424(13) Uani 1 1 d . . . C20 C 0.5268(8) 0.5410(8) 0.1043(3) 0.070(2) Uani 1 1 d . . . H20 H 0.4528 0.5928 0.0835 0.083 Uiso 1 1 calc R . . C21 C 0.6541(8) 0.4986(8) 0.0775(3) 0.070(2) Uani 1 1 d . . . H21 H 0.6840 0.5166 0.0344 0.083 Uiso 1 1 calc R . . C22 C 0.8663(8) 0.3527(8) 0.1174(3) 0.069(2) Uani 1 1 d . . . H22A H 0.9395 0.4170 0.0961 0.083 Uiso 1 1 calc R . . H22B H 0.8406 0.2695 0.0871 0.083 Uiso 1 1 calc R . . C23 C 0.9415(6) 0.3040(6) 0.1792(3) 0.0427(13) Uani 1 1 d . . . C24 C 1.1556(9) 0.2140(8) 0.1170(4) 0.078(2) Uani 1 1 d . . . H24A H 1.2423 0.1620 0.1287 0.116 Uiso 1 1 calc R . . H24B H 1.1898 0.3063 0.1009 0.116 Uiso 1 1 calc R . . H24C H 1.0913 0.1606 0.0825 0.116 Uiso 1 1 calc R . . C25 C 1.1118(6) 0.1950(6) 0.2391(3) 0.0503(15) Uani 1 1 d . . . H25 H 1.1947 0.1447 0.2522 0.060 Uiso 1 1 calc R . . C26 C 1.0089(6) 0.2446(6) 0.2786(3) 0.0414(13) Uani 1 1 d . . . H26 H 1.0106 0.2351 0.3250 0.050 Uiso 1 1 calc R . . C2S C 0.4000(14) 0.1399(13) -0.0043(7) 0.130(4) Uiso 1 1 d . . . N1S N 0.4810(14) 0.2002(13) 0.0432(6) 0.171(4) Uiso 1 1 d . . . C1S C 0.3082(14) 0.0843(13) -0.0626(6) 0.140(4) Uiso 1 1 d . . . H1S1 H 0.3303 0.1431 -0.1001 0.210 Uiso 1 1 calc R . . H1S2 H 0.2021 0.0850 -0.0542 0.210 Uiso 1 1 calc R . . H1S3 H 0.3306 -0.0127 -0.0728 0.210 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 0.0315(4) 0.0326(4) 0.0270(4) 0.0023(3) 0.0027(3) 0.0047(3) Cl1 0.0870(13) 0.1038(16) 0.0504(11) 0.0166(11) 0.0073(10) 0.0337(12) Cl2 0.0622(10) 0.0596(10) 0.0476(9) 0.0071(7) 0.0005(8) 0.0065(8) O1 0.216(8) 0.166(7) 0.082(5) 0.051(5) -0.005(5) 0.073(6) O2 0.242(11) 0.116(6) 0.290(13) 0.002(7) -0.178(11) -0.013(7) O3 0.187(8) 0.128(6) 0.112(6) -0.024(5) -0.012(5) 0.067(6) O4 0.319(16) 0.52(2) 0.175(10) 0.174(13) 0.195(11) 0.241(16) O5 0.108(5) 0.173(7) 0.128(6) -0.048(5) -0.037(5) 0.007(5) O6 0.111(4) 0.109(4) 0.061(3) 0.015(3) 0.030(3) 0.038(3) O7 0.090(4) 0.128(5) 0.060(3) -0.004(3) 0.009(3) 0.047(3) O8 0.183(7) 0.072(4) 0.115(5) 0.046(4) -0.006(5) -0.003(4) N1 0.032(2) 0.035(2) 0.031(2) 0.0015(18) 0.0036(18) 0.0055(17) N2 0.038(2) 0.038(2) 0.032(2) 0.0042(19) 0.0038(19) 0.0011(18) N3 0.053(3) 0.030(2) 0.034(3) 0.0071(19) 0.005(2) 0.006(2) N4 0.049(3) 0.038(3) 0.047(3) 0.002(2) 0.002(2) 0.001(2) N5 0.041(2) 0.036(2) 0.031(2) -0.005(2) 0.001(2) 0.0036(19) N6 0.033(2) 0.031(2) 0.034(2) 0.0001(18) 0.0048(18) -0.0016(17) N7 0.038(2) 0.050(3) 0.029(2) 0.002(2) 0.0075(19) 0.004(2) N8 0.049(3) 0.068(3) 0.029(3) 0.004(2) 0.004(2) 0.014(2) N9 0.048(3) 0.063(3) 0.042(3) -0.006(2) 0.011(2) 0.010(2) N10 0.034(2) 0.038(2) 0.031(2) 0.0027(19) 0.0048(19) 0.0041(18) C1 0.043(3) 0.048(3) 0.039(3) 0.016(3) 0.001(3) 0.001(3) C2 0.062(4) 0.040(3) 0.059(4) 0.007(3) 0.004(3) 0.003(3) C3 0.052(3) 0.036(3) 0.073(5) -0.007(3) 0.008(3) -0.006(3) C4 0.057(3) 0.038(3) 0.051(4) -0.003(3) 0.003(3) 0.001(3) C5 0.037(3) 0.040(3) 0.042(3) 0.001(2) 0.007(2) 0.007(2) C6 0.045(3) 0.034(3) 0.031(3) -0.001(2) -0.002(2) 0.004(2) C7 0.093(5) 0.045(3) 0.026(3) -0.006(3) 0.000(3) -0.006(3) C8 0.092(5) 0.056(4) 0.024(3) 0.005(3) 0.006(3) 0.005(4) C9 0.066(4) 0.035(3) 0.044(3) 0.005(3) -0.002(3) -0.002(3) C10 0.038(3) 0.025(2) 0.039(3) 0.000(2) 0.003(2) 0.002(2) C11 0.068(4) 0.033(3) 0.074(5) 0.002(3) 0.010(4) -0.003(3) C12 0.058(4) 0.042(3) 0.050(4) -0.013(3) -0.002(3) 0.001(3) C13 0.049(3) 0.048(3) 0.045(4) -0.003(3) 0.000(3) 0.003(3) C14 0.040(3) 0.040(3) 0.039(3) 0.002(2) 0.011(2) 0.003(2) C15 0.050(3) 0.050(4) 0.052(4) 0.003(3) 0.016(3) -0.001(3) C16 0.043(3) 0.054(4) 0.064(4) 0.003(3) 0.014(3) 0.000(3) C17 0.043(3) 0.056(4) 0.057(4) 0.009(3) -0.005(3) 0.010(3) C18 0.035(3) 0.038(3) 0.049(3) 0.001(3) 0.002(2) 0.006(2) C19 0.039(3) 0.051(3) 0.037(3) 0.010(3) -0.007(2) 0.002(2) C20 0.068(4) 0.091(5) 0.054(4) 0.018(4) 0.000(4) 0.027(4) C21 0.077(5) 0.102(6) 0.035(4) 0.020(4) 0.000(3) 0.032(4) C22 0.074(5) 0.089(5) 0.049(4) 0.006(4) 0.007(4) 0.038(4) C23 0.037(3) 0.043(3) 0.049(4) -0.001(3) 0.008(3) 0.006(2) C24 0.082(5) 0.085(5) 0.071(5) -0.016(4) 0.021(4) 0.028(4) C25 0.042(3) 0.050(4) 0.061(4) 0.004(3) -0.002(3) 0.011(3) C26 0.040(3) 0.041(3) 0.044(3) 0.005(3) 0.000(3) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.901(4) . ? Fe1 N7 1.905(4) . ? Fe1 N10 1.966(4) . ? Fe1 N5 1.990(4) . ? Fe1 N6 1.995(4) . ? Fe1 N1 2.009(4) . ? Cl1 O4 1.279(8) . ? Cl1 O1 1.392(6) . ? Cl1 O3 1.400(7) . ? Cl1 O2 1.425(8) . ? Cl2 O8 1.369(5) . ? Cl2 O5 1.397(7) . ? Cl2 O7 1.419(5) . ? Cl2 O6 1.419(5) . ? N1 C5 1.347(7) . ? N1 C1 1.360(6) . ? N2 C6 1.334(6) . ? N2 N3 1.351(6) . ? N3 C8 1.363(7) . ? N3 C9 1.460(7) . ? N4 C10 1.349(6) . ? N4 C12 1.379(7) . ? N4 C11 1.466(7) . ? N5 C10 1.307(6) . ? N5 C13 1.348(7) . ? N6 C14 1.336(6) . ? N6 C18 1.362(7) . ? N7 C19 1.342(7) . ? N7 N8 1.344(6) . ? N8 C21 1.356(7) . ? N8 C22 1.440(7) . ? N9 C25 1.358(7) . ? N9 C23 1.359(7) . ? N9 C24 1.453(8) . ? N10 C23 1.319(7) . ? N10 C26 1.374(6) . ? C1 C2 1.334(8) . ? C2 C3 1.384(9) . ? C3 C4 1.376(8) . ? C4 C5 1.366(7) . ? C5 C6 1.458(7) . ? C6 C7 1.382(7) . ? C7 C8 1.347(8) . ? C9 C10 1.470(7) . ? C12 C13 1.365(8) . ? C14 C15 1.382(7) . ? C15 C16 1.359(8) . ? C16 C17 1.376(8) . ? C17 C18 1.373(7) . ? C18 C19 1.463(8) . ? C19 C20 1.371(8) . ? C20 C21 1.355(9) . ? C22 C23 1.465(8) . ? C25 C26 1.339(7) . ? C2S N1S 1.238(14) . ? C2S C1S 1.430(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N7 171.05(18) . . ? N2 Fe1 N10 97.21(18) . . ? N7 Fe1 N10 88.73(18) . . ? N2 Fe1 N5 89.24(18) . . ? N7 Fe1 N5 97.57(18) . . ? N10 Fe1 N5 89.12(17) . . ? N2 Fe1 N6 94.09(17) . . ? N7 Fe1 N6 80.18(18) . . ? N10 Fe1 N6 168.64(17) . . ? N5 Fe1 N6 89.90(17) . . ? N2 Fe1 N1 79.77(17) . . ? N7 Fe1 N1 93.25(18) . . ? N10 Fe1 N1 93.35(17) . . ? N5 Fe1 N1 168.95(17) . . ? N6 Fe1 N1 89.76(16) . . ? O4 Cl1 O1 115.2(6) . . ? O4 Cl1 O3 113.5(8) . . ? O1 Cl1 O3 115.0(5) . . ? O4 Cl1 O2 98.7(9) . . ? O1 Cl1 O2 103.8(6) . . ? O3 Cl1 O2 108.6(6) . . ? O8 Cl2 O5 109.4(5) . . ? O8 Cl2 O7 108.9(4) . . ? O5 Cl2 O7 109.1(4) . . ? O8 Cl2 O6 109.9(4) . . ? O5 Cl2 O6 111.6(4) . . ? O7 Cl2 O6 107.9(3) . . ? C5 N1 C1 116.1(5) . . ? C5 N1 Fe1 115.1(3) . . ? C1 N1 Fe1 128.8(4) . . ? C6 N2 N3 107.2(4) . . ? C6 N2 Fe1 118.3(3) . . ? N3 N2 Fe1 133.0(3) . . ? N2 N3 C8 108.4(4) . . ? N2 N3 C9 122.5(4) . . ? C8 N3 C9 128.7(5) . . ? C10 N4 C12 107.6(4) . . ? C10 N4 C11 127.3(5) . . ? C12 N4 C11 125.1(5) . . ? C10 N5 C13 107.9(4) . . ? C10 N5 Fe1 125.6(4) . . ? C13 N5 Fe1 126.5(4) . . ? C14 N6 C18 117.4(4) . . ? C14 N6 Fe1 127.8(4) . . ? C18 N6 Fe1 114.7(3) . . ? C19 N7 N8 106.1(4) . . ? C19 N7 Fe1 118.6(4) . . ? N8 N7 Fe1 133.5(3) . . ? N7 N8 C21 109.8(5) . . ? N7 N8 C22 122.4(5) . . ? C21 N8 C22 127.7(5) . . ? C25 N9 C23 107.9(5) . . ? C25 N9 C24 125.4(5) . . ? C23 N9 C24 126.4(6) . . ? C23 N10 C26 105.0(4) . . ? C23 N10 Fe1 126.7(4) . . ? C26 N10 Fe1 127.9(4) . . ? C2 C1 N1 123.9(6) . . ? C1 C2 C3 119.7(6) . . ? C4 C3 C2 117.7(6) . . ? C5 C4 C3 119.8(6) . . ? N1 C5 C4 122.8(5) . . ? N1 C5 C6 112.4(5) . . ? C4 C5 C6 124.9(5) . . ? N2 C6 C7 109.8(5) . . ? N2 C6 C5 113.6(5) . . ? C7 C6 C5 136.5(5) . . ? C8 C7 C6 105.7(5) . . ? C7 C8 N3 108.8(5) . . ? N3 C9 C10 114.3(4) . . ? N5 C10 N4 109.9(5) . . ? N5 C10 C9 131.0(5) . . ? N4 C10 C9 118.9(4) . . ? C13 C12 N4 105.2(5) . . ? N5 C13 C12 109.3(5) . . ? N6 C14 C15 121.9(5) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C17 118.5(6) . . ? C18 C17 C16 119.2(6) . . ? N6 C18 C17 122.5(5) . . ? N6 C18 C19 113.0(4) . . ? C17 C18 C19 124.5(5) . . ? N7 C19 C20 110.3(5) . . ? N7 C19 C18 112.6(5) . . ? C20 C19 C18 137.0(5) . . ? C21 C20 C19 105.9(6) . . ? C20 C21 N8 107.8(6) . . ? N8 C22 C23 116.7(5) . . ? N10 C23 N9 110.4(5) . . ? N10 C23 C22 129.7(5) . . ? N9 C23 C22 119.8(5) . . ? C26 C25 N9 105.6(5) . . ? C25 C26 N10 111.0(5) . . ? N1S C2S C1S 174.0(14) . . ? 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 N2 Fe1 N1 C5 -4.2(3) . . . . ? N7 Fe1 N1 C5 170.2(3) . . . . ? N10 Fe1 N1 C5 -100.9(3) . . . . ? N5 Fe1 N1 C5 1.8(10) . . . . ? N6 Fe1 N1 C5 90.0(3) . . . . ? N2 Fe1 N1 C1 176.2(4) . . . . ? N7 Fe1 N1 C1 -9.4(4) . . . . ? N10 Fe1 N1 C1 79.5(4) . . . . ? N5 Fe1 N1 C1 -177.8(7) . . . . ? N6 Fe1 N1 C1 -89.6(4) . . . . ? N7 Fe1 N2 C6 -31.1(13) . . . . ? N10 Fe1 N2 C6 100.2(4) . . . . ? N5 Fe1 N2 C6 -170.7(4) . . . . ? N6 Fe1 N2 C6 -80.9(4) . . . . ? N1 Fe1 N2 C6 8.1(4) . . . . ? N7 Fe1 N2 N3 133.2(10) . . . . ? N10 Fe1 N2 N3 -95.5(4) . . . . ? N5 Fe1 N2 N3 -6.5(4) . . . . ? N6 Fe1 N2 N3 83.4(4) . . . . ? N1 Fe1 N2 N3 172.4(5) . . . . ? C6 N2 N3 C8 0.2(6) . . . . ? Fe1 N2 N3 C8 -165.3(4) . . . . ? C6 N2 N3 C9 -173.2(5) . . . . ? Fe1 N2 N3 C9 21.3(7) . . . . ? N2 Fe1 N5 C10 -1.5(4) . . . . ? N7 Fe1 N5 C10 -175.7(4) . . . . ? N10 Fe1 N5 C10 95.7(4) . . . . ? N6 Fe1 N5 C10 -95.6(4) . . . . ? N1 Fe1 N5 C10 -7.4(11) . . . . ? N2 Fe1 N5 C13 174.2(4) . . . . ? N7 Fe1 N5 C13 0.0(4) . . . . ? N10 Fe1 N5 C13 -88.6(4) . . . . ? N6 Fe1 N5 C13 80.1(4) . . . . ? N1 Fe1 N5 C13 168.3(7) . . . . ? N2 Fe1 N6 C14 -12.6(4) . . . . ? N7 Fe1 N6 C14 174.3(4) . . . . ? N10 Fe1 N6 C14 161.6(7) . . . . ? N5 Fe1 N6 C14 76.6(4) . . . . ? N1 Fe1 N6 C14 -92.4(4) . . . . ? N2 Fe1 N6 C18 167.8(4) . . . . ? N7 Fe1 N6 C18 -5.3(3) . . . . ? N10 Fe1 N6 C18 -18.0(10) . . . . ? N5 Fe1 N6 C18 -103.0(4) . . . . ? N1 Fe1 N6 C18 88.1(4) . . . . ? N2 Fe1 N7 C19 -41.6(13) . . . . ? N10 Fe1 N7 C19 -173.4(4) . . . . ? N5 Fe1 N7 C19 97.7(4) . . . . ? N6 Fe1 N7 C19 9.1(4) . . . . ? N1 Fe1 N7 C19 -80.1(4) . . . . ? N2 Fe1 N7 N8 120.8(11) . . . . ? N10 Fe1 N7 N8 -11.0(5) . . . . ? N5 Fe1 N7 N8 -100.0(5) . . . . ? N6 Fe1 N7 N8 171.5(5) . . . . ? N1 Fe1 N7 N8 82.3(5) . . . . ? C19 N7 N8 C21 1.3(7) . . . . ? Fe1 N7 N8 C21 -162.7(5) . . . . ? C19 N7 N8 C22 -175.8(6) . . . . ? Fe1 N7 N8 C22 20.2(8) . . . . ? N2 Fe1 N10 C23 -174.5(4) . . . . ? N7 Fe1 N10 C23 -1.2(4) . . . . ? N5 Fe1 N10 C23 96.4(4) . . . . ? N6 Fe1 N10 C23 11.3(11) . . . . ? N1 Fe1 N10 C23 -94.4(4) . . . . ? N2 Fe1 N10 C26 13.7(4) . . . . ? N7 Fe1 N10 C26 -173.1(4) . . . . ? N5 Fe1 N10 C26 -75.5(4) . . . . ? N6 Fe1 N10 C26 -160.6(7) . . . . ? N1 Fe1 N10 C26 93.8(4) . . . . ? C5 N1 C1 C2 0.1(8) . . . . ? Fe1 N1 C1 C2 179.7(4) . . . . ? N1 C1 C2 C3 0.4(9) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C2 C3 C4 C5 -1.0(9) . . . . ? C1 N1 C5 C4 -1.1(7) . . . . ? Fe1 N1 C5 C4 179.3(4) . . . . ? C1 N1 C5 C6 179.7(4) . . . . ? Fe1 N1 C5 C6 0.0(5) . . . . ? C3 C4 C5 N1 1.6(8) . . . . ? C3 C4 C5 C6 -179.3(5) . . . . ? N3 N2 C6 C7 -0.2(6) . . . . ? Fe1 N2 C6 C7 167.8(4) . . . . ? N3 N2 C6 C5 -178.4(4) . . . . ? Fe1 N2 C6 C5 -10.4(6) . . . . ? N1 C5 C6 N2 6.3(6) . . . . ? C4 C5 C6 N2 -172.9(5) . . . . ? N1 C5 C6 C7 -171.2(6) . . . . ? C4 C5 C6 C7 9.6(10) . . . . ? N2 C6 C7 C8 0.1(7) . . . . ? C5 C6 C7 C8 177.7(6) . . . . ? C6 C7 C8 N3 0.0(7) . . . . ? N2 N3 C8 C7 -0.2(7) . . . . ? C9 N3 C8 C7 172.7(6) . . . . ? N2 N3 C9 C10 -25.2(7) . . . . ? C8 N3 C9 C10 162.8(6) . . . . ? C13 N5 C10 N4 1.8(6) . . . . ? Fe1 N5 C10 N4 178.2(3) . . . . ? C13 N5 C10 C9 177.8(5) . . . . ? Fe1 N5 C10 C9 -5.9(8) . . . . ? C12 N4 C10 N5 -0.8(6) . . . . ? C11 N4 C10 N5 -179.4(5) . . . . ? C12 N4 C10 C9 -177.3(5) . . . . ? C11 N4 C10 C9 4.1(8) . . . . ? N3 C9 C10 N5 19.0(9) . . . . ? N3 C9 C10 N4 -165.4(5) . . . . ? C10 N4 C12 C13 -0.5(6) . . . . ? C11 N4 C12 C13 178.1(5) . . . . ? C10 N5 C13 C12 -2.2(6) . . . . ? Fe1 N5 C13 C12 -178.5(4) . . . . ? N4 C12 C13 N5 1.6(6) . . . . ? C18 N6 C14 C15 -0.5(7) . . . . ? Fe1 N6 C14 C15 180.0(4) . . . . ? N6 C14 C15 C16 -0.6(9) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C15 C16 C17 C18 0.4(9) . . . . ? C14 N6 C18 C17 1.5(7) . . . . ? Fe1 N6 C18 C17 -178.8(4) . . . . ? C14 N6 C18 C19 -178.4(4) . . . . ? Fe1 N6 C18 C19 1.2(5) . . . . ? C16 C17 C18 N6 -1.5(9) . . . . ? C16 C17 C18 C19 178.4(5) . . . . ? N8 N7 C19 C20 -1.1(7) . . . . ? Fe1 N7 C19 C20 165.7(5) . . . . ? N8 N7 C19 C18 -177.6(4) . . . . ? Fe1 N7 C19 C18 -10.8(6) . . . . ? N6 C18 C19 N7 5.8(7) . . . . ? C17 C18 C19 N7 -174.2(5) . . . . ? N6 C18 C19 C20 -169.4(7) . . . . ? C17 C18 C19 C20 10.7(11) . . . . ? N7 C19 C20 C21 0.5(8) . . . . ? C18 C19 C20 C21 175.7(7) . . . . ? C19 C20 C21 N8 0.3(8) . . . . ? N7 N8 C21 C20 -1.0(8) . . . . ? C22 N8 C21 C20 175.9(7) . . . . ? N7 N8 C22 C23 -14.3(9) . . . . ? C21 N8 C22 C23 169.1(6) . . . . ? C26 N10 C23 N9 0.8(6) . . . . ? Fe1 N10 C23 N9 -172.6(3) . . . . ? C26 N10 C23 C22 177.6(6) . . . . ? Fe1 N10 C23 C22 4.3(9) . . . . ? C25 N9 C23 N10 0.0(6) . . . . ? C24 N9 C23 N10 -175.0(5) . . . . ? C25 N9 C23 C22 -177.2(6) . . . . ? C24 N9 C23 C22 7.8(9) . . . . ? N8 C22 C23 N10 2.9(10) . . . . ? N8 C22 C23 N9 179.4(5) . . . . ? C23 N9 C25 C26 -0.7(6) . . . . ? C24 N9 C25 C26 174.3(6) . . . . ? N9 C25 C26 N10 1.2(6) . . . . ? C23 N10 C26 C25 -1.3(6) . . . . ? Fe1 N10 C26 C25 172.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.815 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.111 #===END # Attachment 'CIF_revised.txt' data_2decam _database_code_depnum_ccdc_archive 'CCDC 712624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H29 Cl2 Fe N11 O8' _chemical_formula_sum 'C28 H29 Cl2 Fe N11 O8' _chemical_formula_weight 774.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.638(5) _cell_length_b 9.241(5) _cell_length_c 19.902(5) _cell_angle_alpha 91.673(5) _cell_angle_beta 93.681(5) _cell_angle_gamma 95.246(5) _cell_volume 1577.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9317 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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 10643 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7530 _reflns_number_gt 6226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0844P)^2^+0.9960P] 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 7530 _refine_ls_number_parameters 456 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.049 _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 Fe Fe 0.20775(4) 0.38550(4) 0.271934(17) 0.01222(11) Uani 1 1 d . . . Cl1 Cl 0.62933(9) 0.76167(9) 0.07542(3) 0.02870(18) Uani 1 1 d . . . Cl2 Cl -0.25954(8) 0.12483(7) 0.44408(3) 0.02104(15) Uani 1 1 d . . . O1 O 0.5773(3) 0.8476(3) 0.02113(12) 0.0430(6) Uani 1 1 d . . . O2 O 0.7747(3) 0.8300(3) 0.10566(14) 0.0517(7) Uani 1 1 d . . . O3 O 0.5167(4) 0.7470(4) 0.12405(15) 0.0654(10) Uani 1 1 d . . . O4 O 0.6569(3) 0.6185(3) 0.05036(13) 0.0424(6) Uani 1 1 d . . . O5 O -0.2065(3) 0.1214(3) 0.37705(11) 0.0308(5) Uani 1 1 d . . . O6 O -0.3995(2) 0.1999(2) 0.44386(10) 0.0295(5) Uani 1 1 d . . . O7 O -0.2941(3) -0.0218(3) 0.46469(12) 0.0409(6) Uani 1 1 d . . . O8 O -0.1411(3) 0.1994(3) 0.48970(13) 0.0475(7) Uani 1 1 d . . . N1 N 0.3037(2) 0.5891(2) 0.29192(10) 0.0138(4) Uani 1 1 d . . . N2 N 0.2573(2) 0.3754(2) 0.36625(10) 0.0142(4) Uani 1 1 d . . . N3 N 0.2212(3) 0.2757(2) 0.41223(11) 0.0165(4) Uani 1 1 d . . . N4 N 0.0371(3) -0.0353(2) 0.30397(11) 0.0172(4) Uani 1 1 d . . . N5 N 0.1167(2) 0.1827(2) 0.27056(10) 0.0152(4) Uani 1 1 d . . . N6 N -0.0012(2) 0.4532(2) 0.28367(11) 0.0146(4) Uani 1 1 d . . . N7 N 0.1510(2) 0.4257(2) 0.18039(10) 0.0145(4) Uani 1 1 d . . . N8 N 0.2310(3) 0.4354(3) 0.12474(11) 0.0197(5) Uani 1 1 d . . . N9 N 0.5750(3) 0.2391(3) 0.17633(12) 0.0225(5) Uani 1 1 d . . . N10 N 0.4019(2) 0.3168(2) 0.24191(11) 0.0150(4) Uani 1 1 d . . . N1S N 1.0056(4) 0.8066(3) -0.04346(16) 0.0436(7) Uani 1 1 d . . . C1 C 0.3309(3) 0.6958(3) 0.24805(13) 0.0172(5) Uani 1 1 d . . . H1 H 0.3009 0.6762 0.2017 0.021 Uiso 1 1 calc R . . C2 C 0.4008(3) 0.8326(3) 0.26791(14) 0.0212(5) Uani 1 1 d . . . H2 H 0.4174 0.9052 0.2356 0.025 Uiso 1 1 calc R . . C3 C 0.4462(3) 0.8627(3) 0.33528(14) 0.0212(5) Uani 1 1 d . . . H3 H 0.4965 0.9552 0.3495 0.025 Uiso 1 1 calc R . . C4 C 0.4171(3) 0.7557(3) 0.38173(14) 0.0193(5) Uani 1 1 d . . . H4 H 0.4452 0.7742 0.4283 0.023 Uiso 1 1 calc R . . C5 C 0.3459(3) 0.6211(3) 0.35837(13) 0.0162(5) Uani 1 1 d . . . C6 C 0.3095(3) 0.4985(3) 0.40091(13) 0.0167(5) Uani 1 1 d . . . C7 C 0.3080(4) 0.4779(3) 0.47049(13) 0.0233(6) Uani 1 1 d D . . H7 H 0.3427 0.5571 0.51107 0.028 Uiso 1 1 calc RD . . C8 C 0.2523(4) 0.3341(3) 0.47558(13) 0.0237(6) Uani 1 1 d . . . H8 H 0.2383 0.2847 0.5162 0.028 Uiso 1 1 calc R . . C9 C 0.1789(3) 0.1237(3) 0.39372(13) 0.0187(5) Uani 1 1 d . . . H9A H 0.1022 0.0835 0.4247 0.022 Uiso 1 1 calc R . . H9B H 0.2728 0.0704 0.4000 0.022 Uiso 1 1 calc R . . C10 C 0.1115(3) 0.0965(3) 0.32286(12) 0.0151(5) Uani 1 1 d . . . C11 C 0.0029(3) -0.1564(3) 0.34803(14) 0.0228(6) Uani 1 1 d D . . H11A H -0.0574 -0.2472 0.31874 0.034 Uiso 1 1 calc RD . . H11B H -0.0699 -0.1229 0.38675 0.034 Uiso 1 1 calc R . . H11C H 0.1105 -0.1885 0.37118 0.034 Uiso 1 1 calc R . . C12 C -0.0087(3) -0.0324(3) 0.23675(13) 0.0201(5) Uani 1 1 d D . . H12 H -0.0719 -0.1197 0.20599 0.024 Uiso 1 1 calc RD . . C13 C 0.0410(3) 0.1019(3) 0.21660(13) 0.0187(5) Uani 1 1 d . . . H13 H 0.0260 0.1354 0.1722 0.022 Uiso 1 1 calc R . . C14 C -0.0796(3) 0.4542(3) 0.34020(13) 0.0181(5) Uani 1 1 d . . . H14 H -0.0350 0.4155 0.3799 0.022 Uiso 1 1 calc R . . C15 C -0.2226(3) 0.5098(3) 0.34223(14) 0.0214(5) Uani 1 1 d . . . H15 H -0.2749 0.5088 0.3828 0.026 Uiso 1 1 calc R . . C16 C -0.2891 0.5669 0.28489 0.0233 Uani 1 1 d D . . H16 H -0.4002 0.6123 0.28609 0.028 Uiso 1 1 calc RD . . C17 C -0.2124(3) 0.5652(3) 0.22618(14) 0.0211(5) Uani 1 1 d . . . H17 H -0.2563 0.6030 0.1861 0.025 Uiso 1 1 calc R . . C18 C -0.0695(3) 0.5070(3) 0.22691(13) 0.0166(5) Uani 1 1 d . . . C19 C 0.0247(3) 0.4974(3) 0.16836(13) 0.0180(5) Uani 1 1 d . . . C20 C 0.0219(3) 0.5532(3) 0.10393(14) 0.0243(6) Uani 1 1 d . . . H20 H -0.0542 0.6086 0.0832 0.029 Uiso 1 1 calc R . . C21 C 0.1535(3) 0.5105(3) 0.07720(14) 0.0240(6) Uani 1 1 d . . . H21 H 0.1852 0.5297 0.0333 0.029 Uiso 1 1 calc R . . C22 C 0.3667(4) 0.3591(4) 0.11543(14) 0.0267(6) Uani 1 1 d . . . H22A H 0.4435 0.4235 0.0927 0.032 Uiso 1 1 calc R . . H22B H 0.3360 0.2730 0.0851 0.032 Uiso 1 1 calc R . . C23 C 0.4436(3) 0.3099(3) 0.17907(13) 0.0185(5) Uani 1 1 d . . . C24 C 0.6599(4) 0.2118(4) 0.11657(15) 0.0316(7) Uani 1 1 d D . . H24A H 0.7594 0.1533 0.13052 0.047 Uiso 1 1 calc R . . H24B H 0.6994 0.3143 0.09559 0.047 Uiso 1 1 calc R . . H24C H 0.5838 0.1477 0.07945 0.047 Uiso 1 1 calc RD . . C25 C 0.6182(3) 0.1997(3) 0.24045(14) 0.0215(5) Uani 1 1 d . . . H25 H 0.7052 0.1490 0.2539 0.026 Uiso 1 1 calc R . . C26 C 0.5112(3) 0.2479(3) 0.28049(13) 0.0181(5) Uani 1 1 d D . . H26 H 0.5109 0.2348 0.33434 0.022 Uiso 1 1 calc RD . . C27 C 1.1966(3) 0.9093(3) 0.06111(15) 0.0448(9) Uani 1 1 d D . . H27A H 1.281 0.8353 0.0720 0.067 Uiso 1 1 calc R . . H27C H 1.1313 0.923 0.1037 0.067 Uiso 1 1 calc R . . H27B H 1.254 1.0107 0.0492 0.067 Uiso 1 1 calc RD . . C28 C 1.0841(3) 0.8480(3) -0.00064(15) 0.0359(8) Uani 1 1 d 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 Fe 0.01488(18) 0.01225(18) 0.00953(18) 0.00142(12) 0.00003(12) 0.00140(13) Cl1 0.0321(4) 0.0398(4) 0.0158(3) 0.0052(3) 0.0010(3) 0.0113(3) Cl2 0.0256(3) 0.0209(3) 0.0162(3) 0.0022(2) -0.0015(2) 0.0012(3) O1 0.0565(16) 0.0505(15) 0.0245(12) 0.0122(11) -0.0027(11) 0.0183(13) O2 0.0531(17) 0.0484(16) 0.0503(17) 0.0010(13) -0.0195(13) 0.0039(13) O3 0.0629(19) 0.099(3) 0.0446(16) 0.0257(17) 0.0317(14) 0.0378(18) O4 0.0466(15) 0.0417(14) 0.0399(14) -0.0008(11) -0.0015(11) 0.0132(12) O5 0.0344(12) 0.0376(12) 0.0223(11) 0.0068(9) 0.0071(9) 0.0084(10) O6 0.0320(11) 0.0362(12) 0.0216(10) -0.0016(9) 0.0012(8) 0.0117(10) O7 0.0568(16) 0.0285(12) 0.0372(14) 0.0176(10) -0.0023(11) 0.0018(11) O8 0.0381(14) 0.0595(17) 0.0404(14) -0.0159(13) -0.0140(11) -0.0030(13) N1 0.0148(10) 0.0135(10) 0.0131(10) 0.0012(8) 0.0009(7) 0.0017(8) N2 0.0172(10) 0.0150(10) 0.0102(9) 0.0024(8) 0.0001(7) 0.0007(8) N3 0.0238(11) 0.0136(10) 0.0122(10) 0.0047(8) 0.0009(8) 0.0006(9) N4 0.0227(11) 0.0120(10) 0.0163(10) -0.0003(8) 0.0002(8) -0.0004(9) N5 0.0161(10) 0.0157(10) 0.0133(10) 0.0004(8) -0.0015(8) 0.0014(8) N6 0.0178(10) 0.0110(9) 0.0147(10) 0.0007(8) 0.0015(8) -0.0002(8) N7 0.0174(10) 0.0172(10) 0.0091(9) 0.0011(8) 0.0004(7) 0.0018(8) N8 0.0229(11) 0.0233(11) 0.0131(10) 0.0017(9) 0.0020(8) 0.0033(9) N9 0.0212(11) 0.0277(12) 0.0188(11) -0.0007(9) 0.0000(9) 0.0053(10) N10 0.0164(10) 0.0142(10) 0.0143(10) 0.0007(8) -0.0004(8) 0.0013(8) N1S 0.060(2) 0.0395(17) 0.0319(16) 0.0014(13) 0.0064(15) 0.0046(15) C1 0.0197(12) 0.0171(12) 0.0152(12) 0.0040(9) 0.0017(9) 0.0022(10) C2 0.0236(13) 0.0176(12) 0.0224(13) 0.0064(10) 0.0027(10) -0.0008(11) C3 0.0241(13) 0.0161(12) 0.0231(14) 0.0010(10) 0.0037(10) -0.0014(10) C4 0.0223(13) 0.0172(12) 0.0178(12) -0.0005(10) 0.0001(10) -0.0002(10) C5 0.0176(12) 0.0165(12) 0.0148(12) 0.0003(9) 0.0029(9) 0.0027(10) C6 0.0197(12) 0.0144(11) 0.0162(12) 0.0016(9) 0.0004(9) 0.0025(10) C7 0.0374(16) 0.0188(13) 0.0125(12) 0.0009(10) -0.0006(11) -0.0028(12) C8 0.0376(16) 0.0198(13) 0.0128(12) 0.0032(10) -0.0007(11) -0.0008(12) C9 0.0256(13) 0.0133(12) 0.0164(12) 0.0021(9) -0.0024(10) -0.0002(10) C10 0.0171(12) 0.0128(11) 0.0157(12) 0.0018(9) 0.0010(9) 0.0017(9) C11 0.0306(15) 0.0132(12) 0.0240(14) 0.0025(10) 0.0005(11) -0.0007(11) C12 0.0229(13) 0.0188(12) 0.0179(13) -0.0013(10) -0.0027(10) 0.0017(11) C13 0.0212(12) 0.0191(12) 0.0154(12) -0.0018(10) -0.0017(9) 0.0031(10) C14 0.0205(12) 0.0148(11) 0.0193(13) 0.0018(9) 0.0040(10) 0.0006(10) C15 0.0226(13) 0.0218(13) 0.0198(13) 0.0011(10) 0.0051(10) 0.0004(11) C16 0.0199(13) 0.0220(13) 0.0282(15) 0.0017(11) 0.0039(11) 0.0013(11) C17 0.0195(13) 0.0226(13) 0.0213(13) 0.0053(10) -0.0013(10) 0.0031(11) C18 0.0183(12) 0.0147(11) 0.0164(12) 0.0012(9) -0.0004(9) 0.0002(10) C19 0.0197(12) 0.0166(12) 0.0173(12) 0.0006(10) -0.0020(9) 0.0027(10) C20 0.0266(14) 0.0287(15) 0.0182(13) 0.0058(11) -0.0011(10) 0.0069(12) C21 0.0295(14) 0.0280(14) 0.0152(13) 0.0069(11) -0.0005(10) 0.0069(12) C22 0.0305(15) 0.0376(17) 0.0143(13) 0.0023(11) 0.0030(11) 0.0145(13) C23 0.0204(12) 0.0180(12) 0.0173(12) -0.0013(10) 0.0010(9) 0.0036(10) C24 0.0296(15) 0.0458(19) 0.0222(15) -0.0020(13) 0.0062(12) 0.0160(14) C25 0.0199(13) 0.0238(13) 0.0208(13) 0.0024(11) -0.0029(10) 0.0051(11) C26 0.0182(12) 0.0172(12) 0.0184(13) 0.0014(10) -0.0034(9) 0.0026(10) C27 0.049(2) 0.043(2) 0.044(2) 0.0063(17) 0.0021(17) 0.0105(17) C28 0.047(2) 0.0299(16) 0.0351(19) 0.0081(14) 0.0162(16) 0.0161(15) _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 Fe N2 1.905(2) . ? Fe N7 1.912(2) . ? Fe N5 1.964(2) . ? Fe N10 1.968(2) . ? Fe N6 1.989(2) . ? Fe N1 2.004(2) . ? Cl1 O3 1.416(3) . ? Cl1 O1 1.433(2) . ? Cl1 O2 1.440(3) . ? Cl1 O4 1.446(3) . ? Cl2 O8 1.436(2) . ? Cl2 O7 1.438(2) . ? Cl2 O5 1.438(2) . ? Cl2 O6 1.448(2) . ? N1 C1 1.350(3) . ? N1 C5 1.365(3) . ? N2 C6 1.339(3) . ? N2 N3 1.348(3) . ? N3 C8 1.358(3) . ? N3 C9 1.449(3) . ? N4 C10 1.355(3) . ? N4 C12 1.372(3) . ? N4 C11 1.462(3) . ? N5 C10 1.330(3) . ? N5 C13 1.383(3) . ? N6 C14 1.350(3) . ? N6 C18 1.368(3) . ? N7 C19 1.339(3) . ? N7 N8 1.344(3) . ? N8 C21 1.366(3) . ? N8 C22 1.441(4) . ? N9 C23 1.365(4) . ? N9 C25 1.375(3) . ? N9 C24 1.464(4) . ? N10 C23 1.325(3) . ? N10 C26 1.390(3) . ? N1S C28 1.092(4) . ? C1 C2 1.386(4) . ? C2 C3 1.385(4) . ? C3 C4 1.390(4) . ? C4 C5 1.390(4) . ? C5 C6 1.457(3) . ? C6 C7 1.404(4) . ? C7 C8 1.380(4) . ? C9 C10 1.496(3) . ? C12 C13 1.356(4) . ? C14 C15 1.383(4) . ? C15 C16 1.385(4) . ? C16 C17 1.380(4) . ? C17 C18 1.391(4) . ? C18 C19 1.468(4) . ? C19 C20 1.396(4) . ? C20 C21 1.370(4) . ? C22 C23 1.494(4) . ? C25 C26 1.355(4) . ? C27 C28 1.575(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe N7 171.15(9) . . ? N2 Fe N5 89.20(9) . . ? N7 Fe N5 97.80(9) . . ? N2 Fe N10 97.02(9) . . ? N7 Fe N10 88.55(9) . . ? N5 Fe N10 88.99(9) . . ? N2 Fe N6 93.85(9) . . ? N7 Fe N6 80.79(9) . . ? N5 Fe N6 90.04(9) . . ? N10 Fe N6 169.07(9) . . ? N2 Fe N1 80.25(9) . . ? N7 Fe N1 92.57(9) . . ? N5 Fe N1 169.36(9) . . ? N10 Fe N1 93.67(9) . . ? N6 Fe N1 89.27(9) . . ? O3 Cl1 O1 110.71(17) . . ? O3 Cl1 O2 110.3(2) . . ? O1 Cl1 O2 108.88(17) . . ? O3 Cl1 O4 108.8(2) . . ? O1 Cl1 O4 110.27(16) . . ? O2 Cl1 O4 107.77(17) . . ? O8 Cl2 O7 109.91(16) . . ? O8 Cl2 O5 109.85(16) . . ? O7 Cl2 O5 109.05(15) . . ? O8 Cl2 O6 109.67(15) . . ? O7 Cl2 O6 109.32(15) . . ? O5 Cl2 O6 109.03(13) . . ? C1 N1 C5 117.4(2) . . ? C1 N1 Fe 127.95(17) . . ? C5 N1 Fe 114.68(16) . . ? C6 N2 N3 106.5(2) . . ? C6 N2 Fe 118.24(17) . . ? N3 N2 Fe 133.54(17) . . ? N2 N3 C8 110.5(2) . . ? N2 N3 C9 122.2(2) . . ? C8 N3 C9 126.6(2) . . ? C10 N4 C12 107.9(2) . . ? C10 N4 C11 126.3(2) . . ? C12 N4 C11 125.8(2) . . ? C10 N5 C13 106.0(2) . . ? C10 N5 Fe 126.24(18) . . ? C13 N5 Fe 127.73(17) . . ? C14 N6 C18 117.7(2) . . ? C14 N6 Fe 127.94(18) . . ? C18 N6 Fe 114.35(17) . . ? C19 N7 N8 106.4(2) . . ? C19 N7 Fe 117.61(17) . . ? N8 N7 Fe 133.11(17) . . ? N7 N8 C21 110.0(2) . . ? N7 N8 C22 123.0(2) . . ? C21 N8 C22 126.4(2) . . ? C23 N9 C25 108.1(2) . . ? C23 N9 C24 126.9(2) . . ? C25 N9 C24 125.0(2) . . ? C23 N10 C26 106.3(2) . . ? C23 N10 Fe 126.40(18) . . ? C26 N10 Fe 126.79(18) . . ? N1 C1 C2 122.7(2) . . ? C3 C2 C1 119.4(2) . . ? C2 C3 C4 119.1(2) . . ? C5 C4 C3 118.4(2) . . ? N1 C5 C4 123.0(2) . . ? N1 C5 C6 112.5(2) . . ? C4 C5 C6 124.6(2) . . ? N2 C6 C7 110.6(2) . . ? N2 C6 C5 113.6(2) . . ? C7 C6 C5 135.7(2) . . ? C8 C7 C6 104.5(2) . . ? N3 C8 C7 108.0(2) . . ? N3 C9 C10 114.4(2) . . ? N5 C10 N4 110.3(2) . . ? N5 C10 C9 129.9(2) . . ? N4 C10 C9 119.8(2) . . ? C13 C12 N4 106.2(2) . . ? C12 C13 N5 109.6(2) . . ? N6 C14 C15 122.2(2) . . ? C14 C15 C16 119.7(3) . . ? C17 C16 C15 119.3(3) . . ? C16 C17 C18 118.6(2) . . ? N6 C18 C17 122.6(2) . . ? N6 C18 C19 112.8(2) . . ? C17 C18 C19 124.6(2) . . ? N7 C19 C20 110.9(2) . . ? N7 C19 C18 113.1(2) . . ? C20 C19 C18 135.8(2) . . ? C21 C20 C19 104.6(2) . . ? N8 C21 C20 108.1(2) . . ? N8 C22 C23 114.5(2) . . ? N10 C23 N9 109.9(2) . . ? N10 C23 C22 130.5(2) . . ? N9 C23 C22 119.5(2) . . ? C26 C25 N9 106.0(2) . . ? C25 C26 N10 109.7(2) . . ? N1S C28 C27 179.4(2) . . ? 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 N2 Fe N1 C1 176.6(2) . . . . ? N7 Fe N1 C1 -8.7(2) . . . . ? N5 Fe N1 C1 -175.7(4) . . . . ? N10 Fe N1 C1 80.1(2) . . . . ? N6 Fe N1 C1 -89.4(2) . . . . ? N2 Fe N1 C5 -3.36(17) . . . . ? N7 Fe N1 C5 171.43(18) . . . . ? N5 Fe N1 C5 4.4(6) . . . . ? N10 Fe N1 C5 -99.86(18) . . . . ? N6 Fe N1 C5 90.68(18) . . . . ? N7 Fe N2 C6 -28.7(7) . . . . ? N5 Fe N2 C6 -171.18(19) . . . . ? N10 Fe N2 C6 99.9(2) . . . . ? N6 Fe N2 C6 -81.2(2) . . . . ? N1 Fe N2 C6 7.40(19) . . . . ? N7 Fe N2 N3 133.8(5) . . . . ? N5 Fe N2 N3 -8.6(2) . . . . ? N10 Fe N2 N3 -97.5(2) . . . . ? N6 Fe N2 N3 81.4(2) . . . . ? N1 Fe N2 N3 170.0(2) . . . . ? C6 N2 N3 C8 -0.9(3) . . . . ? Fe N2 N3 C8 -165.0(2) . . . . ? C6 N2 N3 C9 -172.1(2) . . . . ? Fe N2 N3 C9 23.8(4) . . . . ? N2 Fe N5 C10 -1.4(2) . . . . ? N7 Fe N5 C10 -176.0(2) . . . . ? N10 Fe N5 C10 95.7(2) . . . . ? N6 Fe N5 C10 -95.2(2) . . . . ? N1 Fe N5 C10 -9.0(6) . . . . ? N2 Fe N5 C13 176.2(2) . . . . ? N7 Fe N5 C13 1.7(2) . . . . ? N10 Fe N5 C13 -86.7(2) . . . . ? N6 Fe N5 C13 82.4(2) . . . . ? N1 Fe N5 C13 168.6(4) . . . . ? N2 Fe N6 C14 -12.7(2) . . . . ? N7 Fe N6 C14 174.4(2) . . . . ? N5 Fe N6 C14 76.5(2) . . . . ? N10 Fe N6 C14 161.4(4) . . . . ? N1 Fe N6 C14 -92.8(2) . . . . ? N2 Fe N6 C18 166.09(18) . . . . ? N7 Fe N6 C18 -6.81(17) . . . . ? N5 Fe N6 C18 -104.71(18) . . . . ? N10 Fe N6 C18 -19.9(5) . . . . ? N1 Fe N6 C18 85.91(18) . . . . ? N2 Fe N7 C19 -42.6(7) . . . . ? N5 Fe N7 C19 99.4(2) . . . . ? N10 Fe N7 C19 -171.8(2) . . . . ? N6 Fe N7 C19 10.67(19) . . . . ? N1 Fe N7 C19 -78.2(2) . . . . ? N2 Fe N7 N8 115.0(6) . . . . ? N5 Fe N7 N8 -102.9(2) . . . . ? N10 Fe N7 N8 -14.2(2) . . . . ? N6 Fe N7 N8 168.3(2) . . . . ? N1 Fe N7 N8 79.5(2) . . . . ? C19 N7 N8 C21 -1.3(3) . . . . ? Fe N7 N8 C21 -160.7(2) . . . . ? C19 N7 N8 C22 -173.5(3) . . . . ? Fe N7 N8 C22 27.0(4) . . . . ? N2 Fe N10 C23 -174.6(2) . . . . ? N7 Fe N10 C23 -1.5(2) . . . . ? N5 Fe N10 C23 96.3(2) . . . . ? N6 Fe N10 C23 11.4(6) . . . . ? N1 Fe N10 C23 -94.0(2) . . . . ? N2 Fe N10 C26 15.0(2) . . . . ? N7 Fe N10 C26 -171.9(2) . . . . ? N5 Fe N10 C26 -74.1(2) . . . . ? N6 Fe N10 C26 -159.0(4) . . . . ? N1 Fe N10 C26 95.6(2) . . . . ? C5 N1 C1 C2 1.0(4) . . . . ? Fe N1 C1 C2 -178.9(2) . . . . ? N1 C1 C2 C3 0.4(4) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C1 N1 C5 C4 -1.3(4) . . . . ? Fe N1 C5 C4 178.6(2) . . . . ? C1 N1 C5 C6 179.4(2) . . . . ? Fe N1 C5 C6 -0.7(3) . . . . ? C3 C4 C5 N1 0.2(4) . . . . ? C3 C4 C5 C6 179.4(2) . . . . ? N3 N2 C6 C7 0.3(3) . . . . ? Fe N2 C6 C7 167.26(19) . . . . ? N3 N2 C6 C5 -176.7(2) . . . . ? Fe N2 C6 C5 -9.8(3) . . . . ? N1 C5 C6 N2 6.5(3) . . . . ? C4 C5 C6 N2 -172.9(2) . . . . ? N1 C5 C6 C7 -169.6(3) . . . . ? C4 C5 C6 C7 11.1(5) . . . . ? N2 C6 C7 C8 0.3(3) . . . . ? C5 C6 C7 C8 176.5(3) . . . . ? N2 N3 C8 C7 1.2(3) . . . . ? C9 N3 C8 C7 171.9(3) . . . . ? C6 C7 C8 N3 -0.9(3) . . . . ? N2 N3 C9 C10 -25.5(4) . . . . ? C8 N3 C9 C10 164.8(3) . . . . ? C13 N5 C10 N4 0.5(3) . . . . ? Fe N5 C10 N4 178.59(16) . . . . ? C13 N5 C10 C9 177.8(3) . . . . ? Fe N5 C10 C9 -4.2(4) . . . . ? C12 N4 C10 N5 -0.7(3) . . . . ? C11 N4 C10 N5 -177.2(2) . . . . ? C12 N4 C10 C9 -178.2(2) . . . . ? C11 N4 C10 C9 5.2(4) . . . . ? N3 C9 C10 N5 17.2(4) . . . . ? N3 C9 C10 N4 -165.8(2) . . . . ? C10 N4 C12 C13 0.5(3) . . . . ? C11 N4 C12 C13 177.1(2) . . . . ? N4 C12 C13 N5 -0.2(3) . . . . ? C10 N5 C13 C12 -0.2(3) . . . . ? Fe N5 C13 C12 -178.21(18) . . . . ? C18 N6 C14 C15 -1.3(4) . . . . ? Fe N6 C14 C15 177.45(19) . . . . ? N6 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C15 C16 C17 C18 -0.5(4) . . . . ? C14 N6 C18 C17 1.8(4) . . . . ? Fe N6 C18 C17 -177.1(2) . . . . ? C14 N6 C18 C19 -178.7(2) . . . . ? Fe N6 C18 C19 2.4(3) . . . . ? C16 C17 C18 N6 -0.9(4) . . . . ? C16 C17 C18 C19 179.7(3) . . . . ? N8 N7 C19 C20 0.5(3) . . . . ? Fe N7 C19 C20 163.70(19) . . . . ? N8 N7 C19 C18 -175.3(2) . . . . ? Fe N7 C19 C18 -12.2(3) . . . . ? N6 C18 C19 N7 6.0(3) . . . . ? C17 C18 C19 N7 -174.5(2) . . . . ? N6 C18 C19 C20 -168.5(3) . . . . ? C17 C18 C19 C20 11.0(5) . . . . ? N7 C19 C20 C21 0.4(3) . . . . ? C18 C19 C20 C21 175.0(3) . . . . ? N7 N8 C21 C20 1.6(3) . . . . ? C22 N8 C21 C20 173.5(3) . . . . ? C19 C20 C21 N8 -1.2(3) . . . . ? N7 N8 C22 C23 -19.7(4) . . . . ? C21 N8 C22 C23 169.3(3) . . . . ? C26 N10 C23 N9 0.1(3) . . . . ? Fe N10 C23 N9 -171.91(17) . . . . ? C26 N10 C23 C22 176.8(3) . . . . ? Fe N10 C23 C22 4.7(4) . . . . ? C25 N9 C23 N10 -0.1(3) . . . . ? C24 N9 C23 N10 -178.5(3) . . . . ? C25 N9 C23 C22 -177.2(3) . . . . ? C24 N9 C23 C22 4.4(4) . . . . ? N8 C22 C23 N10 4.9(5) . . . . ? N8 C22 C23 N9 -178.7(2) . . . . ? C23 N9 C25 C26 0.0(3) . . . . ? C24 N9 C25 C26 178.5(3) . . . . ? N9 C25 C26 N10 0.0(3) . . . . ? C23 N10 C26 C25 -0.1(3) . . . . ? Fe N10 C26 C25 171.89(18) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.924 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.107