# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data__Compound_{BnN(CH2CH2CH2-N-tert-butyl-imidazole-2-ylidene)2}FeCl2 _database_code_depnum_ccdc_archive 'CCDC 907140' #TrackingRef 'web_deposit_cif_file_0_NilayHazari_1360023780.XRay_SI.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H50 Cl2 Fe N5' _chemical_formula_weight 679.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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 9.5506(2) _cell_length_b 14.1282(3) _cell_length_c 14.2614(10) _cell_angle_alpha 85.624(6) _cell_angle_beta 87.635(6) _cell_angle_gamma 86.017(6) _cell_volume 1912.84(15) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 34723 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 65.8 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 4.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4556 _exptl_absorpt_correction_T_max 0.8002 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; 'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD' ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 55654 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 65.82 _reflns_number_total 6506 _reflns_number_gt 5633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. All disorders were refined with the help of similarity restraints on the 1,2- and 1,3- distances and displacement parameters as well as rigid bond restraints for anisotropic displacement parameters. All disordered benzene molecules were restrained to be flat. ; _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^)+(0.1773P)^2^+1.2766P] 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 6506 _refine_ls_number_parameters 595 _refine_ls_number_restraints 1051 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2486 _refine_ls_wR_factor_gt 0.2388 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.017 _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 Cl1 Cl 0.73636(11) -0.13956(7) 0.17303(7) 0.0494(3) Uani 1 1 d . . . Cl2 Cl 0.45193(10) 0.03129(7) 0.25108(7) 0.0468(3) Uani 1 1 d . . . Fe1 Fe 0.69682(6) 0.01116(4) 0.22604(4) 0.0405(2) Uani 1 1 d . . . C1 C 0.7398(4) 0.0522(3) 0.3641(3) 0.0419(9) Uani 1 1 d . . . N1 N 0.7564(4) 0.0035(3) 0.4501(2) 0.0443(8) Uani 1 1 d . . . C13 C 0.7648(5) -0.1028(3) 0.4680(3) 0.0494(10) Uani 1 1 d . . . C14 C 0.6231(5) -0.1378(4) 0.4493(4) 0.0625(13) Uani 1 1 d . . . H14A H 0.5519 -0.1108 0.4929 0.094 Uiso 1 1 calc R . . H14B H 0.6273 -0.2074 0.4584 0.094 Uiso 1 1 calc R . . H14C H 0.5982 -0.1178 0.3844 0.094 Uiso 1 1 calc R . . C15 C 0.8815(5) -0.1450(3) 0.4039(3) 0.0517(10) Uani 1 1 d . . . H15A H 0.8594 -0.1280 0.3380 0.078 Uiso 1 1 calc R . . H15B H 0.8889 -0.2144 0.4154 0.078 Uiso 1 1 calc R . . H15C H 0.9709 -0.1196 0.4172 0.078 Uiso 1 1 calc R . . C16 C 0.8038(6) -0.1298(4) 0.5688(3) 0.0665(14) Uani 1 1 d . . . H16A H 0.8929 -0.1032 0.5807 0.100 Uiso 1 1 calc R . . H16B H 0.8137 -0.1992 0.5793 0.100 Uiso 1 1 calc R . . H16C H 0.7300 -0.1044 0.6115 0.100 Uiso 1 1 calc R . . C2 C 0.7587(5) 0.0659(3) 0.5203(3) 0.0513(10) Uani 1 1 d . . . H2 H 0.7674 0.0495 0.5858 0.062 Uiso 1 1 calc R . . C3 C 0.7463(5) 0.1540(4) 0.4780(3) 0.0527(11) Uani 1 1 d . . . H3 H 0.7454 0.2120 0.5077 0.063 Uiso 1 1 calc R . . N2 N 0.7351(4) 0.1444(3) 0.3831(2) 0.0449(8) Uani 1 1 d . . . C4 C 0.7129(5) 0.2255(3) 0.3131(3) 0.0475(10) Uani 1 1 d . . . H4A H 0.7338 0.2038 0.2494 0.057 Uiso 1 1 calc R . . H4B H 0.7792 0.2742 0.3238 0.057 Uiso 1 1 calc R . . C5 C 0.5642(5) 0.2705(3) 0.3177(3) 0.0518(10) Uani 1 1 d . . . H5A H 0.4974 0.2221 0.3071 0.062 Uiso 1 1 calc R . . H5B H 0.5431 0.2932 0.3810 0.062 Uiso 1 1 calc R . . C6 C 0.5454(5) 0.3530(3) 0.2443(3) 0.0533(11) Uani 1 1 d . . . H6A H 0.4483 0.3817 0.2505 0.064 Uiso 1 1 calc R . . H6B H 0.6100 0.4020 0.2570 0.064 Uiso 1 1 calc R . . N3 N 0.5720(4) 0.3268(3) 0.1467(3) 0.0508(9) Uani 1 1 d . A . C21 C 0.5931(5) 0.4132(3) 0.0851(4) 0.0577(11) Uani 1 1 d DU . . H23A H 0.5130 0.4598 0.0961 0.069 Uiso 0.66(3) 1 calc PR A 1 H23B H 0.5908 0.3967 0.0190 0.069 Uiso 0.66(3) 1 calc PR A 1 H23C H 0.5099 0.4585 0.0910 0.069 Uiso 0.34(3) 1 calc PR A 2 H23D H 0.6030 0.3966 0.0189 0.069 Uiso 0.34(3) 1 calc PR A 2 C22 C 0.7257(12) 0.4603(9) 0.0968(19) 0.056(3) Uani 0.66(3) 1 d PDU A 1 C23 C 0.8552(11) 0.4095(9) 0.1011(13) 0.062(3) Uani 0.66(3) 1 d PDU A 1 H23 H 0.8600 0.3421 0.1003 0.075 Uiso 0.66(3) 1 calc PR A 1 C24 C 0.9763(11) 0.4551(8) 0.1064(14) 0.070(3) Uani 0.66(3) 1 d PDU A 1 H24 H 1.0639 0.4192 0.1114 0.084 Uiso 0.66(3) 1 calc PR A 1 C25 C 0.9711(11) 0.5529(7) 0.1046(13) 0.069(3) Uani 0.66(3) 1 d PDU A 1 H25 H 1.0555 0.5845 0.1065 0.083 Uiso 0.66(3) 1 calc PR A 1 C26 C 0.8436(12) 0.6052(7) 0.0999(11) 0.063(3) Uani 0.66(3) 1 d PDU A 1 H26 H 0.8400 0.6726 0.0991 0.076 Uiso 0.66(3) 1 calc PR A 1 C27 C 0.7218(13) 0.5592(8) 0.0965(13) 0.058(3) Uani 0.66(3) 1 d PDU A 1 H27 H 0.6341 0.5953 0.0938 0.070 Uiso 0.66(3) 1 calc PR A 1 C22A C 0.724(2) 0.4604(16) 0.111(4) 0.060(4) Uani 0.34(3) 1 d PDU A 2 C23A C 0.850(2) 0.4087(16) 0.132(2) 0.062(4) Uani 0.34(3) 1 d PDU A 2 H23E H 0.8523 0.3413 0.1339 0.074 Uiso 0.34(3) 1 calc PR A 2 C24A C 0.972(2) 0.4504(14) 0.150(2) 0.069(4) Uani 0.34(3) 1 d PDU A 2 H24A H 1.0551 0.4118 0.1627 0.083 Uiso 0.34(3) 1 calc PR A 2 C25A C 0.972(2) 0.5486(14) 0.149(2) 0.074(4) Uani 0.34(3) 1 d PDU A 2 H25A H 1.0562 0.5783 0.1585 0.089 Uiso 0.34(3) 1 calc PR A 2 C26A C 0.846(2) 0.6025(15) 0.135(2) 0.072(4) Uani 0.34(3) 1 d PDU A 2 H26A H 0.8429 0.6697 0.1370 0.086 Uiso 0.34(3) 1 calc PR A 2 C27A C 0.726(3) 0.5583(16) 0.118(3) 0.065(4) Uani 0.34(3) 1 d PDU A 2 H27A H 0.6406 0.5963 0.1118 0.078 Uiso 0.34(3) 1 calc PR A 2 C7 C 0.4522(5) 0.2795(3) 0.1159(3) 0.0535(11) Uani 1 1 d . . . H7A H 0.3719 0.3274 0.1086 0.064 Uiso 1 1 calc R A . H7B H 0.4254 0.2314 0.1663 0.064 Uiso 1 1 calc R . . C8 C 0.4751(5) 0.2306(3) 0.0241(3) 0.0513(10) Uani 1 1 d . A . H8A H 0.3819 0.2209 -0.0001 0.062 Uiso 1 1 calc R . . H8B H 0.5222 0.2746 -0.0224 0.062 Uiso 1 1 calc R . . C9 C 0.5601(4) 0.1360(3) 0.0285(3) 0.0475(10) Uani 1 1 d . . . H9A H 0.5220 0.0945 0.0813 0.057 Uiso 1 1 calc R A . H9B H 0.5482 0.1050 -0.0303 0.057 Uiso 1 1 calc R . . N4 N 0.7102(4) 0.1431(2) 0.0412(2) 0.0429(8) Uani 1 1 d . A . C10 C 0.7935(5) 0.1914(3) -0.0250(3) 0.0517(11) Uani 1 1 d . . . H10 H 0.7632 0.2267 -0.0807 0.062 Uiso 1 1 calc R A . C11 C 0.9245(5) 0.1789(3) 0.0044(3) 0.0508(10) Uani 1 1 d . A . H11 H 1.0053 0.2043 -0.0263 0.061 Uiso 1 1 calc R . . N5 N 0.9214(4) 0.1225(2) 0.0877(2) 0.0412(7) Uani 1 1 d . . . C17 C 1.0534(4) 0.0968(3) 0.1397(3) 0.0415(9) Uani 1 1 d . A . C18 C 1.1641(5) 0.0575(4) 0.0715(3) 0.0539(11) Uani 1 1 d . . . H18A H 1.1305 0.0016 0.0450 0.081 Uiso 1 1 calc R A . H18B H 1.2508 0.0392 0.1046 0.081 Uiso 1 1 calc R . . H18C H 1.1825 0.1062 0.0207 0.081 Uiso 1 1 calc R . . C19 C 1.0291(5) 0.0198(3) 0.2177(3) 0.0479(10) Uani 1 1 d . . . H19A H 0.9651 0.0455 0.2663 0.072 Uiso 1 1 calc R A . H19B H 1.1189 -0.0023 0.2453 0.072 Uiso 1 1 calc R . . H19C H 0.9877 -0.0337 0.1917 0.072 Uiso 1 1 calc R . . C20 C 1.0995(5) 0.1856(3) 0.1806(3) 0.0535(11) Uani 1 1 d . . . H20A H 1.1194 0.2336 0.1294 0.080 Uiso 1 1 calc R A . H20B H 1.1844 0.1694 0.2164 0.080 Uiso 1 1 calc R . . H20C H 1.0244 0.2110 0.2224 0.080 Uiso 1 1 calc R . . C12 C 0.7880(4) 0.0999(3) 0.1122(3) 0.0409(9) Uani 1 1 d . A . C1S C 0.3407(8) 0.7850(5) 0.2664(6) 0.0579(15) Uani 0.851(8) 1 d PDU B 1 H1S H 0.3704 0.8475 0.2692 0.070 Uiso 0.851(8) 1 calc PR B 1 C2S C 0.4378(6) 0.7110(4) 0.2508(4) 0.0584(14) Uani 0.851(8) 1 d PDU B 1 H2S H 0.5347 0.7222 0.2432 0.070 Uiso 0.851(8) 1 calc PR B 1 C3S C 0.3945(6) 0.6206(4) 0.2460(5) 0.0713(18) Uani 0.851(8) 1 d PDU B 1 H3S H 0.4613 0.5690 0.2359 0.086 Uiso 0.851(8) 1 calc PR B 1 C4S C 0.2548(6) 0.6058(4) 0.2559(7) 0.085(2) Uani 0.851(8) 1 d PDU B 1 H4S H 0.2246 0.5435 0.2527 0.102 Uiso 0.851(8) 1 calc PR B 1 C5S C 0.1571(7) 0.6801(5) 0.2704(7) 0.080(2) Uani 0.851(8) 1 d PDU B 1 H5S H 0.0599 0.6695 0.2750 0.096 Uiso 0.851(8) 1 calc PR B 1 C6S C 0.2009(8) 0.7690(5) 0.2781(8) 0.0650(16) Uani 0.851(8) 1 d PDU B 1 H6S H 0.1345 0.8198 0.2915 0.078 Uiso 0.851(8) 1 calc PR B 1 C1T C 0.366(4) 0.779(2) 0.263(4) 0.064(4) Uani 0.149(8) 1 d PDU B 2 H1T H 0.3907 0.8367 0.2311 0.077 Uiso 0.149(8) 1 calc PR B 2 C2T C 0.468(3) 0.711(2) 0.291(3) 0.070(4) Uani 0.149(8) 1 d PDU B 2 H2T H 0.5644 0.7226 0.2791 0.084 Uiso 0.149(8) 1 calc PR B 2 C3T C 0.432(3) 0.627(2) 0.337(3) 0.081(5) Uani 0.149(8) 1 d PDU B 2 H3T H 0.5024 0.5813 0.3588 0.097 Uiso 0.149(8) 1 calc PR B 2 C4T C 0.293(3) 0.609(2) 0.350(3) 0.089(5) Uani 0.149(8) 1 d PDU B 2 H4T H 0.2676 0.5487 0.3760 0.107 Uiso 0.149(8) 1 calc PR B 2 C5T C 0.191(3) 0.678(3) 0.326(3) 0.077(4) Uani 0.149(8) 1 d PDU B 2 H5T H 0.0946 0.6680 0.3412 0.093 Uiso 0.149(8) 1 calc PR B 2 C6T C 0.227(4) 0.763(3) 0.281(5) 0.069(4) Uani 0.149(8) 1 d PDU B 2 H6T H 0.1563 0.8103 0.2625 0.083 Uiso 0.149(8) 1 calc PR B 2 C1U C 0.789(2) 0.4286(9) 0.5041(9) 0.128(5) Uani 0.435(5) 1 d PDU C 1 H1U H 0.8008 0.3817 0.5550 0.154 Uiso 0.435(5) 1 calc PR C 1 C2U C 0.8800(16) 0.4270(9) 0.4287(9) 0.118(4) Uani 0.435(5) 1 d PDU C 1 H2U H 0.9534 0.3782 0.4269 0.142 Uiso 0.435(5) 1 calc PR C 1 C3U C 0.8677(16) 0.4943(9) 0.3555(8) 0.110(4) Uani 0.435(5) 1 d PDU C 1 H3U H 0.9283 0.4912 0.3012 0.132 Uiso 0.435(5) 1 calc PR C 1 C4U C 0.7651(17) 0.5667(9) 0.3624(9) 0.111(4) Uani 0.435(5) 1 d PDU C 1 H4U H 0.7582 0.6162 0.3135 0.134 Uiso 0.435(5) 1 calc PR C 1 C5U C 0.6741(18) 0.5694(8) 0.4368(10) 0.115(4) Uani 0.435(5) 1 d PDU C 1 H5U H 0.6056 0.6212 0.4402 0.138 Uiso 0.435(5) 1 calc PR C 1 C6U C 0.679(2) 0.4987(11) 0.5075(10) 0.137(5) Uani 0.435(5) 1 d PDU C 1 H6U H 0.6098 0.4971 0.5573 0.164 Uiso 0.435(5) 1 calc PR C 1 C1V C 1.097(8) 0.439(5) 0.504(6) 0.110(9) Uani 0.065(5) 1 d PDU C -2 H1V H 1.1779 0.4014 0.5229 0.132 Uiso 0.065(5) 1 calc PR C -2 C3V C 0.913(10) 0.475(6) 0.397(4) 0.113(7) Uani 0.065(5) 1 d PDU C -2 H3V H 0.8667 0.4612 0.3425 0.136 Uiso 0.065(5) 1 calc PR C -2 C2V C 1.029(10) 0.420(4) 0.425(5) 0.115(8) Uani 0.065(5) 1 d PDU C -2 H2V H 1.0641 0.3685 0.3898 0.138 Uiso 0.065(5) 1 calc PR C -2 C4V C 0.862(8) 0.548(5) 0.448(6) 0.113(7) Uani 0.065(5) 1 d PDU C -2 H4V H 0.7797 0.5856 0.4298 0.135 Uiso 0.065(5) 1 calc PR C -2 C5V C 0.930(10) 0.569(5) 0.527(5) 0.110(9) Uani 0.065(5) 1 d PDU C -2 H5V H 0.8957 0.6209 0.5611 0.132 Uiso 0.065(5) 1 calc PR C -2 C6V C 1.046(10) 0.514(6) 0.555(4) 0.109(10) Uani 0.065(5) 1 d PDU C -2 H6V H 1.0917 0.5273 0.6100 0.131 Uiso 0.065(5) 1 calc PR C -2 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 Cl1 0.0627(6) 0.0476(6) 0.0396(6) -0.0031(4) -0.0001(4) -0.0166(5) Cl2 0.0459(5) 0.0536(6) 0.0411(6) 0.0052(4) -0.0016(4) -0.0133(4) Fe1 0.0464(4) 0.0460(4) 0.0300(4) 0.0016(3) -0.0005(3) -0.0134(3) C1 0.043(2) 0.051(2) 0.032(2) 0.0020(16) -0.0022(15) -0.0112(17) N1 0.0493(19) 0.053(2) 0.0310(17) 0.0029(14) -0.0025(14) -0.0115(15) C13 0.058(2) 0.058(3) 0.032(2) 0.0044(18) 0.0017(18) -0.009(2) C14 0.053(3) 0.061(3) 0.072(3) 0.017(2) -0.005(2) -0.017(2) C15 0.058(3) 0.057(3) 0.040(2) -0.0036(19) 0.0022(19) -0.005(2) C16 0.085(4) 0.078(3) 0.033(2) 0.007(2) -0.002(2) 0.007(3) C2 0.059(3) 0.066(3) 0.031(2) -0.0044(19) -0.0063(18) -0.014(2) C3 0.062(3) 0.059(3) 0.040(2) -0.0066(19) -0.0045(19) -0.016(2) N2 0.054(2) 0.051(2) 0.0305(18) -0.0022(14) -0.0014(14) -0.0149(16) C4 0.056(2) 0.047(2) 0.040(2) 0.0012(17) -0.0019(18) -0.0141(19) C5 0.062(3) 0.050(2) 0.044(2) -0.0003(19) 0.005(2) -0.011(2) C6 0.064(3) 0.046(2) 0.051(3) -0.0009(19) -0.003(2) -0.009(2) N3 0.058(2) 0.049(2) 0.045(2) 0.0050(16) -0.0026(16) -0.0134(17) C21 0.066(2) 0.049(2) 0.057(3) 0.010(2) -0.005(2) -0.0118(19) C22 0.068(3) 0.046(3) 0.054(8) 0.008(4) -0.002(4) -0.013(3) C23 0.066(3) 0.047(3) 0.075(8) -0.001(4) 0.000(5) -0.014(2) C24 0.064(3) 0.055(3) 0.093(9) 0.000(5) 0.008(5) -0.016(3) C25 0.072(3) 0.054(3) 0.082(8) 0.008(5) 0.002(5) -0.028(3) C26 0.083(4) 0.045(3) 0.063(7) 0.009(4) -0.001(5) -0.019(2) C27 0.072(3) 0.047(3) 0.056(8) 0.005(4) -0.006(4) -0.010(3) C22A 0.066(4) 0.049(5) 0.063(10) 0.014(6) 0.009(6) -0.015(4) C23A 0.062(4) 0.051(5) 0.070(10) 0.013(7) 0.009(6) -0.017(4) C24A 0.068(5) 0.056(5) 0.083(10) 0.006(8) 0.003(7) -0.017(4) C25A 0.079(5) 0.058(5) 0.086(10) 0.007(8) 0.007(8) -0.025(5) C26A 0.087(6) 0.049(5) 0.078(11) 0.014(7) 0.007(8) -0.020(4) C27A 0.081(5) 0.050(4) 0.064(11) 0.008(6) 0.003(7) -0.013(4) C7 0.051(2) 0.055(3) 0.056(3) 0.000(2) -0.002(2) -0.014(2) C8 0.049(2) 0.056(3) 0.048(3) 0.007(2) -0.0028(19) -0.013(2) C9 0.046(2) 0.053(2) 0.044(2) 0.0072(18) -0.0039(17) -0.0151(19) N4 0.0484(19) 0.0481(19) 0.0319(18) 0.0061(14) 0.0005(14) -0.0123(15) C10 0.054(2) 0.062(3) 0.039(2) 0.0126(19) 0.0002(18) -0.016(2) C11 0.052(2) 0.062(3) 0.038(2) 0.0120(19) -0.0006(18) -0.015(2) N5 0.0460(18) 0.0481(19) 0.0295(17) 0.0045(13) -0.0011(13) -0.0126(14) C17 0.044(2) 0.047(2) 0.034(2) 0.0006(16) -0.0047(16) -0.0111(17) C18 0.046(2) 0.075(3) 0.040(2) -0.003(2) 0.0021(18) -0.005(2) C19 0.049(2) 0.055(2) 0.039(2) 0.0071(18) -0.0049(17) -0.0102(19) C20 0.059(3) 0.050(2) 0.053(3) -0.003(2) -0.008(2) -0.012(2) C12 0.045(2) 0.046(2) 0.032(2) 0.0030(16) -0.0021(15) -0.0117(17) C1S 0.081(4) 0.053(3) 0.041(3) -0.003(2) 0.004(3) -0.019(2) C2S 0.059(3) 0.061(3) 0.057(4) -0.001(3) -0.002(3) -0.021(2) C3S 0.062(3) 0.053(3) 0.101(5) -0.012(3) 0.006(3) -0.008(2) C4S 0.067(3) 0.051(3) 0.139(6) -0.009(4) 0.009(4) -0.021(2) C5S 0.057(3) 0.071(3) 0.113(6) -0.003(4) 0.008(4) -0.013(2) C6S 0.074(3) 0.058(3) 0.061(4) -0.004(3) 0.010(3) 0.003(3) C1T 0.075(7) 0.062(8) 0.057(9) -0.003(8) 0.004(8) -0.016(6) C2T 0.075(7) 0.062(8) 0.071(9) -0.002(8) 0.004(8) -0.014(6) C3T 0.082(7) 0.065(8) 0.093(10) 0.008(8) 0.015(9) -0.007(8) C4T 0.087(9) 0.066(9) 0.112(12) 0.006(10) 0.021(11) -0.016(7) C5T 0.075(7) 0.066(8) 0.093(9) -0.010(8) 0.016(8) -0.019(6) C6T 0.074(6) 0.065(7) 0.070(9) -0.009(8) 0.006(9) -0.013(7) C1U 0.262(15) 0.066(7) 0.063(7) 0.017(6) -0.042(8) -0.061(8) C2U 0.210(12) 0.086(7) 0.069(7) 0.008(6) -0.060(7) -0.068(7) C3U 0.183(12) 0.086(7) 0.072(7) 0.013(6) -0.041(7) -0.093(7) C4U 0.181(12) 0.084(7) 0.078(7) 0.032(6) -0.056(7) -0.090(7) C5U 0.210(13) 0.060(6) 0.083(8) 0.013(5) -0.047(7) -0.070(7) C6U 0.266(15) 0.069(7) 0.080(8) 0.016(6) -0.012(9) -0.063(8) C1V 0.18(2) 0.089(18) 0.064(18) 0.032(16) -0.035(14) -0.087(16) C3V 0.190(15) 0.086(12) 0.072(12) 0.027(11) -0.043(11) -0.087(11) C2V 0.194(16) 0.092(14) 0.067(14) 0.031(13) -0.041(13) -0.083(12) C4V 0.186(15) 0.084(12) 0.077(12) 0.026(11) -0.039(12) -0.092(11) C5V 0.18(2) 0.084(17) 0.070(17) 0.028(13) -0.034(15) -0.091(16) C6V 0.18(2) 0.085(19) 0.066(18) 0.034(15) -0.031(15) -0.091(18) _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 Cl1 Fe1 2.3149(12) . ? Cl2 Fe1 2.3521(11) . ? Fe1 C1 2.158(4) . ? Fe1 C12 2.166(4) . ? C1 N2 1.347(6) . ? C1 N1 1.368(5) . ? N1 C2 1.387(6) . ? N1 C13 1.501(6) . ? C13 C16 1.513(6) . ? C13 C14 1.513(7) . ? C13 C15 1.530(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C2 C3 1.341(7) . ? C2 H2 0.9500 . ? C3 N2 1.380(6) . ? C3 H3 0.9500 . ? N2 C4 1.471(5) . ? C4 C5 1.516(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.475(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N3 C7 1.463(6) . ? N3 C21 1.469(6) . ? C21 C22 1.491(10) . ? C21 C22A 1.528(14) . ? C21 H23A 0.9900 . ? C21 H23B 0.9900 . ? C21 H23C 0.9900 . ? C21 H23D 0.9900 . ? C22 C23 1.388(10) . ? C22 C27 1.396(9) . ? C23 C24 1.370(10) . ? C23 H23 0.9500 . ? C24 C25 1.378(10) . ? C24 H24 0.9500 . ? C25 C26 1.381(10) . ? C25 H25 0.9500 . ? C26 C27 1.375(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C22A C23A 1.394(13) . ? C22A C27A 1.397(13) . ? C23A C24A 1.379(14) . ? C23A H23E 0.9500 . ? C24A C25A 1.387(13) . ? C24A H24A 0.9500 . ? C25A C26A 1.391(14) . ? C25A H25A 0.9500 . ? C26A C27A 1.381(14) . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? C7 C8 1.527(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.513(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N4 1.464(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? N4 C12 1.363(5) . ? N4 C10 1.380(5) . ? C10 C11 1.332(6) . ? C10 H10 0.9500 . ? C11 N5 1.379(5) . ? C11 H11 0.9500 . ? N5 C12 1.360(5) . ? N5 C17 1.499(5) . ? C17 C18 1.513(6) . ? C17 C19 1.518(6) . ? C17 C20 1.523(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C1S C6S 1.371(9) . ? C1S C2S 1.374(8) . ? C1S H1S 0.9500 . ? C2S C3S 1.377(7) . ? C2S H2S 0.9500 . ? C3S C4S 1.365(8) . ? C3S H3S 0.9500 . ? C4S C5S 1.377(8) . ? C4S H4S 0.9500 . ? C5S C6S 1.364(9) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C1T C6T 1.37(2) . ? C1T C2T 1.369(13) . ? C1T H1T 0.9500 . ? C2T C3T 1.368(12) . ? C2T H2T 0.9500 . ? C3T C4T 1.369(12) . ? C3T H3T 0.9500 . ? C4T C5T 1.365(12) . ? C4T H4T 0.9500 . ? C5T C6T 1.372(14) . ? C5T H5T 0.9500 . ? C6T H6T 0.9500 . ? C1U C2U 1.352(12) . ? C1U C6U 1.397(19) . ? C1U H1U 0.9500 . ? C2U C3U 1.360(11) . ? C2U H2U 0.9500 . ? C3U C4U 1.373(11) . ? C3U H3U 0.9500 . ? C4U C5U 1.345(11) . ? C4U H4U 0.9500 . ? C5U C6U 1.364(11) . ? C5U H5U 0.9500 . ? C6U H6U 0.9500 . ? C1V C2V 1.368(14) . ? C1V C6V 1.38(2) . ? C1V H1V 0.9500 . ? C3V C2V 1.366(12) . ? C3V C4V 1.368(12) . ? C3V H3V 0.9500 . ? C2V H2V 0.9500 . ? C4V C5V 1.369(12) . ? C4V H4V 0.9500 . ? C5V C6V 1.366(14) . ? C5V H5V 0.9500 . ? C6V H6V 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C12 113.71(15) . . ? C1 Fe1 Cl1 126.20(12) . . ? C12 Fe1 Cl1 102.35(12) . . ? C1 Fe1 Cl2 93.44(11) . . ? C12 Fe1 Cl2 116.57(11) . . ? Cl1 Fe1 Cl2 104.91(4) . . ? N2 C1 N1 104.1(3) . . ? N2 C1 Fe1 121.3(3) . . ? N1 C1 Fe1 133.9(3) . . ? C1 N1 C2 110.7(4) . . ? C1 N1 C13 125.5(3) . . ? C2 N1 C13 123.8(3) . . ? N1 C13 C16 109.7(4) . . ? N1 C13 C14 108.2(4) . . ? C16 C13 C14 110.7(4) . . ? N1 C13 C15 108.6(4) . . ? C16 C13 C15 107.7(4) . . ? C14 C13 C15 112.0(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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C3 C2 N1 106.7(4) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 106.9(4) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C1 N2 C3 111.5(4) . . ? C1 N2 C4 124.9(3) . . ? C3 N2 C4 123.4(4) . . ? N2 C4 C5 112.6(4) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 111.0(4) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N3 C6 C5 114.0(4) . . ? N3 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? N3 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C7 N3 C21 109.7(4) . . ? C7 N3 C6 109.8(4) . . ? C21 N3 C6 109.2(4) . . ? N3 C21 C22 116.1(9) . . ? N3 C21 C22A 111.1(17) . . ? C22 C21 C22A 7(3) . . ? N3 C21 H23A 108.3 . . ? C22 C21 H23A 108.3 . . ? C22A C21 H23A 106.0 . . ? N3 C21 H23B 108.3 . . ? C22 C21 H23B 108.3 . . ? C22A C21 H23B 115.6 . . ? H23A C21 H23B 107.4 . . ? N3 C21 H23C 109.4 . . ? C22 C21 H23C 111.2 . . ? C22A C21 H23C 109.4 . . ? H23A C21 H23C 4.8 . . ? H23B C21 H23C 102.6 . . ? N3 C21 H23D 109.4 . . ? C22 C21 H23D 102.2 . . ? C22A C21 H23D 109.4 . . ? H23A C21 H23D 112.7 . . ? H23B C21 H23D 6.7 . . ? H23C C21 H23D 108.0 . . ? C23 C22 C27 118.4(8) . . ? C23 C22 C21 122.0(8) . . ? C27 C22 C21 119.4(9) . . ? C24 C23 C22 120.9(8) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.1(9) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.1(8) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.8(8) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C22 120.7(9) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C23A C22A C27A 114.5(14) . . ? C23A C22A C21 122.6(15) . . ? C27A C22A C21 122.8(15) . . ? C24A C23A C22A 123.5(15) . . ? C24A C23A H23E 118.3 . . ? C22A C23A H23E 118.3 . . ? C23A C24A C25A 120.1(15) . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C24A C25A C26A 118.3(15) . . ? C24A C25A H25A 120.8 . . ? C26A C25A H25A 120.8 . . ? C27A C26A C25A 120.0(15) . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C22A 123.3(16) . . ? C26A C27A H27A 118.4 . . ? C22A C27A H27A 118.4 . . ? N3 C7 C8 116.0(4) . . ? N3 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N3 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 116.9(4) . . ? C9 C8 H8A 108.1 . . ? C7 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C7 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? N4 C9 C8 114.1(4) . . ? N4 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? N4 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C12 N4 C10 111.2(4) . . ? C12 N4 C9 126.8(3) . . ? C10 N4 C9 121.8(3) . . ? C11 C10 N4 106.7(4) . . ? C11 C10 H10 126.6 . . ? N4 C10 H10 126.6 . . ? C10 C11 N5 107.5(4) . . ? C10 C11 H11 126.3 . . ? N5 C11 H11 126.3 . . ? C12 N5 C11 110.8(3) . . ? C12 N5 C17 128.7(3) . . ? C11 N5 C17 120.5(3) . . ? N5 C17 C18 108.3(3) . . ? N5 C17 C19 110.5(3) . . ? C18 C17 C19 107.8(4) . . ? N5 C17 C20 108.7(3) . . ? C18 C17 C20 111.2(4) . . ? C19 C17 C20 110.3(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C12 N4 103.8(3) . . ? N5 C12 Fe1 133.8(3) . . ? N4 C12 Fe1 122.3(3) . . ? C6S C1S C2S 120.2(5) . . ? C6S C1S H1S 119.9 . . ? C2S C1S H1S 119.9 . . ? C1S C2S C3S 119.9(5) . . ? C1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C4S C3S C2S 119.4(5) . . ? C4S C3S H3S 120.3 . . ? C2S C3S H3S 120.3 . . ? C3S C4S C5S 120.8(5) . . ? C3S C4S H4S 119.6 . . ? C5S C4S H4S 119.6 . . ? C6S C5S C4S 119.6(6) . . ? C6S C5S H5S 120.2 . . ? C4S C5S H5S 120.2 . . ? C5S C6S C1S 120.1(6) . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C6T C1T C2T 120.4(11) . . ? C6T C1T H1T 119.8 . . ? C2T C1T H1T 119.8 . . ? C3T C2T C1T 119.6(12) . . ? C3T C2T H2T 120.2 . . ? C1T C2T H2T 120.2 . . ? C2T C3T C4T 119.9(10) . . ? C2T C3T H3T 120.1 . . ? C4T C3T H3T 120.1 . . ? C5T C4T C3T 120.3(10) . . ? C5T C4T H4T 119.8 . . ? C3T C4T H4T 119.8 . . ? C4T C5T C6T 119.6(12) . . ? C4T C5T H5T 120.2 . . ? C6T C5T H5T 120.2 . . ? C1T C6T C5T 119.9(11) . . ? C1T C6T H6T 120.1 . . ? C5T C6T H6T 120.1 . . ? C2U C1U C6U 120.5(9) . . ? C2U C1U H1U 119.8 . . ? C6U C1U H1U 119.8 . . ? C1U C2U C3U 121.1(10) . . ? C1U C2U H2U 119.5 . . ? C3U C2U H2U 119.5 . . ? C2U C3U C4U 118.1(9) . . ? C2U C3U H3U 121.0 . . ? C4U C3U H3U 121.0 . . ? C5U C4U C3U 121.6(8) . . ? C5U C4U H4U 119.2 . . ? C3U C4U H4U 119.2 . . ? C4U C5U C6U 120.8(10) . . ? C4U C5U H5U 119.6 . . ? C6U C5U H5U 119.6 . . ? C5U C6U C1U 117.7(10) . . ? C5U C6U H6U 121.2 . . ? C1U C6U H6U 121.2 . . ? C2V C1V C6V 119.9(12) . . ? C2V C1V H1V 120.1 . . ? C6V C1V H1V 120.1 . . ? C2V C3V C4V 120.0(11) . . ? C2V C3V H3V 120.0 . . ? C4V C3V H3V 120.0 . . ? C3V C2V C1V 120.2(12) . . ? C3V C2V H2V 119.9 . . ? C1V C2V H2V 119.9 . . ? C3V C4V C5V 119.9(11) . . ? C3V C4V H4V 120.0 . . ? C5V C4V H4V 120.0 . . ? C6V C5V C4V 120.3(12) . . ? C6V C5V H5V 119.8 . . ? C4V C5V H5V 119.8 . . ? C5V C6V C1V 119.7(12) . . ? C5V C6V H6V 120.2 . . ? C1V C6V H6V 120.2 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 65.82 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.077 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.104 data__Compound_{BnN(CH2CH2-N-methylbenzimidazole-2-ylidene)2}FeCl2 _database_code_depnum_ccdc_archive 'CCDC 907141' #TrackingRef 'web_deposit_cif_file_0_NilayHazari_1360023780.XRay_SI.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H33 Cl2 Fe N5 O0.50' _chemical_formula_weight 586.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9406(3) _cell_length_b 9.3355(2) _cell_length_c 22.9686(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.132(6) _cell_angle_gamma 90.00 _cell_volume 2774.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 12905 _cell_measurement_theta_min 3.9 _cell_measurement_theta_max 65.1 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 6.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6644 _exptl_absorpt_correction_T_max 0.8321 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; 'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD' ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'micro focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 47039 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_unetI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 65.09 _reflns_number_total 4496 _reflns_number_gt 3791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. All disorders were refined with the help of similarity restraints on the 1,2- and 1,3- distances and displacement parameters as well as rigid bond restraints for anisotropic displacement parameters. ; _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^)+(0.0000P)^2^+14.0037P] 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 4496 _refine_ls_number_parameters 723 _refine_ls_number_restraints 1595 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1768 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 0.997 _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 Cl1 Cl 1.1484(9) 1.0752(9) 0.0883(5) 0.059(2) Uani 0.606(4) 1 d PDU A 1 Cl2 Cl 1.3040(3) 0.7567(5) 0.1240(2) 0.0624(10) Uani 0.606(4) 1 d PDU A 1 Fe1 Fe 1.1438(5) 0.8558(7) 0.1345(4) 0.0539(12) Uani 0.606(4) 1 d PDU A 1 C1 C 1.1070(14) 0.8840(18) 0.2229(5) 0.048(2) Uani 0.606(4) 1 d PDU A 1 N1 N 1.0425(15) 0.985(2) 0.2462(6) 0.057(3) Uani 0.606(4) 1 d PDU A 1 C8 C 0.9819(15) 1.0936(19) 0.2151(9) 0.091(5) Uani 0.606(4) 1 d PDU A 1 H8A H 0.9454 1.1532 0.2431 0.137 Uiso 0.606(4) 1 calc PR A 1 H8B H 0.9316 1.0467 0.1890 0.137 Uiso 0.606(4) 1 calc PR A 1 H8C H 1.0281 1.1538 0.1922 0.137 Uiso 0.606(4) 1 calc PR A 1 C2 C 1.036(2) 0.969(2) 0.3064(6) 0.060(3) Uani 0.606(4) 1 d PDU A 1 C3 C 0.9825(18) 1.046(2) 0.3464(6) 0.072(3) Uani 0.606(4) 1 d PDU A 1 H3 H 0.9397 1.1246 0.3353 0.086 Uiso 0.606(4) 1 calc PR A 1 C4 C 0.9936(16) 1.0040(19) 0.4040(6) 0.074(4) Uani 0.606(4) 1 d PDU A 1 H4 H 0.9555 1.0524 0.4330 0.089 Uiso 0.606(4) 1 calc PR A 1 C5 C 1.0593(17) 0.8922(18) 0.4206(6) 0.073(4) Uani 0.606(4) 1 d PDU A 1 H5 H 1.0680 0.8697 0.4607 0.087 Uiso 0.606(4) 1 calc PR A 1 C6 C 1.112(2) 0.814(2) 0.3801(7) 0.065(3) Uani 0.606(4) 1 d PDU A 1 H6 H 1.1548 0.7358 0.3912 0.078 Uiso 0.606(4) 1 calc PR A 1 C7 C 1.099(2) 0.855(3) 0.3216(6) 0.057(2) Uani 0.606(4) 1 d PDU A 1 N2 N 1.140(2) 0.805(2) 0.2694(6) 0.055(2) Uani 0.606(4) 1 d PDU A 1 C9 C 1.2005(14) 0.6740(17) 0.2638(9) 0.065(3) Uani 0.606(4) 1 d PDU A 1 H9A H 1.2578 0.6731 0.2930 0.078 Uiso 0.606(4) 1 calc PR A 1 H9B H 1.2304 0.6688 0.2245 0.078 Uiso 0.606(4) 1 calc PR A 1 C10 C 1.1278(7) 0.5435(11) 0.2736(4) 0.061(2) Uani 0.606(4) 1 d PDU A 1 H10A H 1.1703 0.4564 0.2795 0.073 Uiso 0.606(4) 1 calc PR A 1 H10B H 1.0882 0.5595 0.3095 0.073 Uiso 0.606(4) 1 calc PR A 1 N3 N 1.0553(6) 0.5198(8) 0.2247(3) 0.0518(17) Uani 0.606(4) 1 d PDU A 1 C21 C 0.9530(7) 0.4770(10) 0.2439(4) 0.057(2) Uani 0.606(4) 1 d PDU A 1 H21A H 0.9607 0.4004 0.2735 0.069 Uiso 0.606(4) 1 calc PR A 1 H21B H 0.9134 0.4371 0.2104 0.069 Uiso 0.606(4) 1 calc PR A 1 C22 C 0.8933(8) 0.5989(11) 0.2694(4) 0.050(2) Uani 0.606(4) 1 d PDU A 1 C23 C 0.8545(10) 0.7077(14) 0.2355(5) 0.055(2) Uani 0.606(4) 1 d PDU A 1 H23 H 0.8674 0.7070 0.1949 0.066 Uiso 0.606(4) 1 calc PR A 1 C24 C 0.7975(9) 0.8179(12) 0.2582(5) 0.071(2) Uani 0.606(4) 1 d PDU A 1 H24 H 0.7708 0.8905 0.2332 0.085 Uiso 0.606(4) 1 calc PR A 1 C25 C 0.7790(10) 0.8242(13) 0.3162(5) 0.081(3) Uani 0.606(4) 1 d PDU A 1 H25 H 0.7401 0.9010 0.3318 0.098 Uiso 0.606(4) 1 calc PR A 1 C26 C 0.8173(11) 0.7175(13) 0.3521(5) 0.085(3) Uani 0.606(4) 1 d PDU A 1 H26 H 0.8025 0.7194 0.3925 0.102 Uiso 0.606(4) 1 calc PR A 1 C27 C 0.8776(11) 0.6067(14) 0.3300(5) 0.074(3) Uani 0.606(4) 1 d PDU A 1 H27 H 0.9078 0.5374 0.3554 0.089 Uiso 0.606(4) 1 calc PR A 1 C11 C 1.0951(8) 0.4207(10) 0.1796(4) 0.058(2) Uani 0.606(4) 1 d PDU A 1 H11A H 1.0420 0.3473 0.1707 0.069 Uiso 0.606(4) 1 calc PR A 1 H11B H 1.1571 0.3709 0.1955 0.069 Uiso 0.606(4) 1 calc PR A 1 C12 C 1.1240(12) 0.4992(16) 0.1221(7) 0.047(3) Uani 0.606(4) 1 d PDU A 1 H12A H 1.1814 0.5669 0.1300 0.057 Uiso 0.606(4) 1 calc PR A 1 H12B H 1.1474 0.4283 0.0932 0.057 Uiso 0.606(4) 1 calc PR A 1 N4 N 1.0356(11) 0.5763(12) 0.0989(8) 0.037(2) Uani 0.606(4) 1 d PDU A 1 C13 C 0.9471(10) 0.5128(13) 0.0734(8) 0.035(2) Uani 0.606(4) 1 d PDU A 1 C14 C 0.9206(10) 0.3723(13) 0.0578(9) 0.040(3) Uani 0.606(4) 1 d PDU A 1 H14 H 0.9649 0.2943 0.0674 0.048 Uiso 0.606(4) 1 calc PR A 1 C15 C 0.8280(10) 0.3505(15) 0.0282(9) 0.042(3) Uani 0.606(4) 1 d PDU A 1 H15 H 0.8081 0.2566 0.0166 0.051 Uiso 0.606(4) 1 calc PR A 1 C16 C 0.7640(10) 0.4666(14) 0.0153(8) 0.044(3) Uani 0.606(4) 1 d PDU A 1 H16 H 0.7003 0.4497 -0.0049 0.052 Uiso 0.606(4) 1 calc PR A 1 C17 C 0.7892(11) 0.6049(14) 0.0307(8) 0.040(3) Uani 0.606(4) 1 d PDU A 1 H17 H 0.7442 0.6825 0.0217 0.048 Uiso 0.606(4) 1 calc PR A 1 C18 C 0.8813(9) 0.6265(13) 0.0593(8) 0.035(2) Uani 0.606(4) 1 d PDU A 1 N5 N 0.9313(8) 0.7505(13) 0.0771(8) 0.038(2) Uani 0.606(4) 1 d PDU A 1 C19 C 1.0250(9) 0.7221(11) 0.1014(8) 0.036(2) Uani 0.606(4) 1 d PDU A 1 C20 C 0.8839(10) 0.8925(15) 0.0716(7) 0.046(3) Uani 0.606(4) 1 d PDU A 1 H20A H 0.8147 0.8832 0.0539 0.068 Uiso 0.606(4) 1 calc PR A 1 H20B H 0.9266 0.9534 0.0470 0.068 Uiso 0.606(4) 1 calc PR A 1 H20C H 0.8786 0.9358 0.1103 0.068 Uiso 0.606(4) 1 calc PR A 1 Cl1A Cl 1.1204(13) 1.0774(13) 0.0934(9) 0.053(3) Uani 0.394(4) 1 d PDU A 2 Cl2A Cl 1.3132(5) 0.8116(8) 0.1373(4) 0.0698(18) Uani 0.394(4) 1 d PDU A 2 Fe1A Fe 1.1419(7) 0.8600(11) 0.1389(5) 0.0499(16) Uani 0.394(4) 1 d PDU A 2 C1A C 1.101(2) 0.863(3) 0.2276(7) 0.052(3) Uani 0.394(4) 1 d PDU A 2 N1A N 1.144(3) 0.785(3) 0.2723(9) 0.052(3) Uani 0.394(4) 1 d PDU A 2 C8A C 1.213(3) 0.660(3) 0.2705(15) 0.078(6) Uani 0.394(4) 1 d PDU A 2 H8A1 H 1.2237 0.6228 0.3100 0.116 Uiso 0.394(4) 1 calc PR A 2 H8A2 H 1.2794 0.6892 0.2546 0.116 Uiso 0.394(4) 1 calc PR A 2 H8A3 H 1.1817 0.5860 0.2458 0.116 Uiso 0.394(4) 1 calc PR A 2 C2A C 1.107(4) 0.830(4) 0.3253(9) 0.054(3) Uani 0.394(4) 1 d PDU A 2 C3A C 1.129(3) 0.783(4) 0.3799(9) 0.060(4) Uani 0.394(4) 1 d PDU A 2 H3A H 1.1795 0.7101 0.3873 0.072 Uiso 0.394(4) 1 calc PR A 2 C4A C 1.075(3) 0.846(3) 0.4240(9) 0.061(4) Uani 0.394(4) 1 d PDU A 2 H4A H 1.0832 0.8088 0.4623 0.074 Uiso 0.394(4) 1 calc PR A 2 C5A C 1.008(2) 0.961(3) 0.4149(8) 0.061(4) Uani 0.394(4) 1 d PDU A 2 H5A H 0.9748 1.0043 0.4471 0.073 Uiso 0.394(4) 1 calc PR A 2 C6A C 0.989(3) 1.014(3) 0.3595(9) 0.063(4) Uani 0.394(4) 1 d PDU A 2 H6A H 0.9443 1.0924 0.3524 0.076 Uiso 0.394(4) 1 calc PR A 2 C7A C 1.041(3) 0.944(4) 0.3139(8) 0.055(3) Uani 0.394(4) 1 d PDU A 2 N2A N 1.041(2) 0.962(3) 0.2532(8) 0.053(3) Uani 0.394(4) 1 d PDU A 2 C9A C 0.9761(16) 1.057(2) 0.2188(13) 0.063(4) Uani 0.394(4) 1 d PDU A 2 H9A1 H 1.0069 1.0703 0.1800 0.076 Uiso 0.394(4) 1 calc PR A 2 H9A2 H 0.9734 1.1519 0.2380 0.076 Uiso 0.394(4) 1 calc PR A 2 C10A C 0.8651(10) 0.9979(14) 0.2109(6) 0.054(3) Uani 0.394(4) 1 d PDU A 2 H10C H 0.8390 0.9724 0.2498 0.064 Uiso 0.394(4) 1 calc PR A 2 H10D H 0.8206 1.0756 0.1952 0.064 Uiso 0.394(4) 1 calc PR A 2 N3A N 0.8536(9) 0.8730(11) 0.1729(4) 0.051(2) Uani 0.394(4) 1 d PDU A 2 C21A C 0.7876(11) 0.7635(15) 0.1989(6) 0.060(3) Uani 0.394(4) 1 d PDU A 2 H21C H 0.7684 0.6922 0.1687 0.072 Uiso 0.394(4) 1 calc PR A 2 H21D H 0.7232 0.8094 0.2121 0.072 Uiso 0.394(4) 1 calc PR A 2 C22A C 0.8379(17) 0.687(2) 0.2494(7) 0.057(3) Uani 0.394(4) 1 d PDU A 2 C23A C 0.9170(12) 0.5916(17) 0.2429(6) 0.051(3) Uani 0.394(4) 1 d PDU A 2 H23A H 0.9421 0.5739 0.2049 0.061 Uiso 0.394(4) 1 calc PR A 2 C24A C 0.9614(12) 0.5200(16) 0.2894(6) 0.057(3) Uani 0.394(4) 1 d PDU A 2 H24A H 1.0158 0.4538 0.2829 0.068 Uiso 0.394(4) 1 calc PR A 2 C25A C 0.9284(14) 0.5428(19) 0.3450(6) 0.070(3) Uani 0.394(4) 1 d PDU A 2 H25A H 0.9612 0.4963 0.3772 0.084 Uiso 0.394(4) 1 calc PR A 2 C26A C 0.8462(17) 0.635(2) 0.3531(7) 0.082(4) Uani 0.394(4) 1 d PDU A 2 H26A H 0.8204 0.6484 0.3912 0.098 Uiso 0.394(4) 1 calc PR A 2 C27A C 0.8005(14) 0.709(2) 0.3065(6) 0.077(3) Uani 0.394(4) 1 d PDU A 2 H27A H 0.7449 0.7730 0.3129 0.093 Uiso 0.394(4) 1 calc PR A 2 C11A C 0.8218(10) 0.9033(14) 0.1114(5) 0.044(3) Uani 0.394(4) 1 d PDU A 2 H11C H 0.7999 1.0046 0.1079 0.053 Uiso 0.394(4) 1 calc PR A 2 H11D H 0.7620 0.8421 0.1004 0.053 Uiso 0.394(4) 1 calc PR A 2 C12A C 0.9121(16) 0.874(2) 0.0692(9) 0.041(3) Uani 0.394(4) 1 d PDU A 2 H12C H 0.8870 0.8885 0.0287 0.049 Uiso 0.394(4) 1 calc PR A 2 H12D H 0.9680 0.9443 0.0771 0.049 Uiso 0.394(4) 1 calc PR A 2 N4A N 0.9538(13) 0.7297(19) 0.0751(12) 0.033(2) Uani 0.394(4) 1 d PDU A 2 C13A C 0.9035(14) 0.604(2) 0.0554(13) 0.034(3) Uani 0.394(4) 1 d PDU A 2 C14A C 0.8095(16) 0.576(2) 0.0256(13) 0.038(3) Uani 0.394(4) 1 d PDU A 2 H14A H 0.7627 0.6503 0.0154 0.045 Uiso 0.394(4) 1 calc PR A 2 C15A C 0.7886(15) 0.434(2) 0.0119(12) 0.039(3) Uani 0.394(4) 1 d PDU A 2 H15A H 0.7264 0.4109 -0.0086 0.047 Uiso 0.394(4) 1 calc PR A 2 C16A C 0.8567(15) 0.325(2) 0.0275(13) 0.039(4) Uani 0.394(4) 1 d PDU A 2 H16A H 0.8392 0.2290 0.0177 0.046 Uiso 0.394(4) 1 calc PR A 2 C17A C 0.9493(16) 0.351(2) 0.0570(14) 0.038(3) Uani 0.394(4) 1 d PDU A 2 H17A H 0.9956 0.2766 0.0678 0.046 Uiso 0.394(4) 1 calc PR A 2 C18A C 0.9697(15) 0.4913(19) 0.0696(13) 0.033(3) Uani 0.394(4) 1 d PDU A 2 N5A N 1.0527(18) 0.5512(18) 0.0998(13) 0.038(3) Uani 0.394(4) 1 d PDU A 2 C19A C 1.0454(12) 0.6984(17) 0.1022(13) 0.034(3) Uani 0.394(4) 1 d PDU A 2 C20A C 1.133(2) 0.465(2) 0.1275(12) 0.048(4) Uani 0.394(4) 1 d PDU A 2 H20D H 1.1166 0.3631 0.1224 0.072 Uiso 0.394(4) 1 calc PR A 2 H20E H 1.1375 0.4876 0.1691 0.072 Uiso 0.394(4) 1 calc PR A 2 H20F H 1.1995 0.4856 0.1095 0.072 Uiso 0.394(4) 1 calc PR A 2 O1S O 0.8922(12) 0.3827(17) 0.4661(8) 0.083(4) Uani 0.347(10) 1 d PDU B -1 C1S C 0.9927(16) 0.367(2) 0.4501(11) 0.086(5) Uani 0.347(10) 1 d PDU B -1 H1S1 H 0.9992 0.3808 0.4076 0.103 Uiso 0.347(10) 1 calc PR B -1 H1S2 H 1.0186 0.2705 0.4606 0.103 Uiso 0.347(10) 1 calc PR B -1 C2S C 1.0545(16) 0.486(3) 0.4845(14) 0.084(5) Uani 0.347(10) 1 d PDU B -1 H2S1 H 1.1087 0.5292 0.4604 0.101 Uiso 0.347(10) 1 calc PR B -1 H2S2 H 1.0864 0.4470 0.5208 0.101 Uiso 0.347(10) 1 calc PR B -1 C3S C 0.9654(16) 0.596(2) 0.4979(12) 0.074(4) Uani 0.347(10) 1 d PDU B -1 H3S1 H 0.9798 0.6498 0.5342 0.089 Uiso 0.347(10) 1 calc PR B -1 H3S2 H 0.9542 0.6641 0.4653 0.089 Uiso 0.347(10) 1 calc PR B -1 C4S C 0.8715(16) 0.491(2) 0.5043(13) 0.081(5) Uani 0.347(10) 1 d PDU B -1 H4S1 H 0.8674 0.4548 0.5447 0.097 Uiso 0.347(10) 1 calc PR B -1 H4S2 H 0.8056 0.5397 0.4938 0.097 Uiso 0.347(10) 1 calc PR B -1 O1T O 1.015(3) 0.443(4) 0.4643(16) 0.085(5) Uani 0.153(10) 1 d PDU B -2 C1T C 1.100(3) 0.477(5) 0.499(3) 0.082(6) Uani 0.153(10) 1 d PDU B -2 H1T1 H 1.1640 0.4790 0.4760 0.098 Uiso 0.153(10) 1 calc PR B -2 H1T2 H 1.1086 0.4084 0.5314 0.098 Uiso 0.153(10) 1 calc PR B -2 C2T C 1.072(3) 0.631(5) 0.522(3) 0.074(6) Uani 0.153(10) 1 d PDU B -2 H2T1 H 1.0904 0.6417 0.5636 0.089 Uiso 0.153(10) 1 calc PR B -2 H2T2 H 1.1075 0.7064 0.4994 0.089 Uiso 0.153(10) 1 calc PR B -2 C3T C 0.951(3) 0.639(4) 0.512(2) 0.070(6) Uani 0.153(10) 1 d PDU B -2 H3T1 H 0.9326 0.7085 0.4806 0.084 Uiso 0.153(10) 1 calc PR B -2 H3T2 H 0.9156 0.6654 0.5478 0.084 Uiso 0.153(10) 1 calc PR B -2 C4T C 0.925(3) 0.481(5) 0.492(2) 0.081(5) Uani 0.153(10) 1 d PDU B -2 H4T1 H 0.9128 0.4181 0.5265 0.098 Uiso 0.153(10) 1 calc PR B -2 H4T2 H 0.8640 0.4770 0.4658 0.098 Uiso 0.153(10) 1 calc PR B -2 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 Cl1 0.077(6) 0.057(2) 0.043(3) 0.0014(17) 0.010(3) -0.025(2) Cl2 0.0509(18) 0.076(3) 0.061(2) -0.0076(18) 0.0028(13) -0.0213(16) Fe1 0.061(2) 0.063(2) 0.038(2) 0.0051(17) 0.0022(18) -0.019(2) C1 0.048(5) 0.056(6) 0.039(3) 0.008(3) -0.005(3) -0.018(4) N1 0.061(5) 0.072(7) 0.038(4) 0.003(4) -0.002(4) -0.010(4) C8 0.108(10) 0.098(11) 0.068(7) 0.022(8) 0.011(8) 0.028(7) C2 0.064(5) 0.077(8) 0.037(4) 0.000(4) -0.001(4) -0.021(5) C3 0.082(7) 0.094(9) 0.039(5) 0.001(5) 0.002(6) -0.010(6) C4 0.090(8) 0.095(10) 0.037(5) -0.003(6) -0.003(6) -0.015(6) C5 0.086(9) 0.093(11) 0.038(4) 0.000(5) -0.011(5) -0.022(7) C6 0.070(8) 0.085(9) 0.040(3) 0.003(4) -0.014(4) -0.024(5) C7 0.055(6) 0.077(7) 0.037(3) 0.005(4) -0.009(4) -0.028(5) N2 0.053(5) 0.072(5) 0.039(3) 0.010(4) -0.008(4) -0.016(4) C9 0.067(7) 0.083(6) 0.044(6) 0.019(5) -0.015(5) 0.000(3) C10 0.064(5) 0.072(5) 0.047(4) 0.021(4) -0.003(4) 0.010(4) N3 0.050(4) 0.061(4) 0.045(3) 0.011(3) 0.003(3) 0.016(3) C21 0.060(4) 0.056(5) 0.056(5) -0.002(4) 0.014(4) 0.005(4) C22 0.048(5) 0.049(4) 0.054(4) -0.005(4) 0.008(4) -0.003(3) C23 0.045(6) 0.058(5) 0.061(5) 0.002(4) 0.007(4) 0.001(4) C24 0.069(6) 0.064(5) 0.079(4) 0.006(4) 0.015(5) 0.015(4) C25 0.095(7) 0.071(6) 0.079(5) -0.009(5) 0.011(6) 0.028(5) C26 0.110(8) 0.082(7) 0.063(5) -0.010(4) 0.017(5) 0.035(6) C27 0.087(7) 0.078(6) 0.057(4) -0.001(4) 0.018(5) 0.029(5) C11 0.064(6) 0.062(5) 0.048(4) 0.018(3) 0.014(4) 0.027(4) C12 0.049(5) 0.048(6) 0.045(5) 0.014(5) 0.004(4) 0.024(4) N4 0.030(5) 0.042(4) 0.039(4) 0.004(4) 0.005(4) 0.012(3) C13 0.032(5) 0.038(4) 0.035(4) -0.008(4) 0.015(4) 0.014(3) C14 0.031(7) 0.037(4) 0.053(5) -0.004(4) 0.018(6) 0.012(4) C15 0.035(7) 0.039(5) 0.053(5) -0.016(5) 0.015(6) 0.010(5) C16 0.033(6) 0.046(6) 0.051(5) -0.015(5) 0.006(5) 0.010(4) C17 0.036(6) 0.039(5) 0.045(5) -0.014(4) 0.005(5) 0.015(4) C18 0.030(5) 0.038(4) 0.036(4) -0.003(4) 0.008(5) 0.012(3) N5 0.037(5) 0.036(4) 0.039(4) 0.004(4) -0.001(4) 0.011(3) C19 0.039(4) 0.037(4) 0.033(4) 0.006(4) 0.000(4) 0.011(3) C20 0.042(8) 0.038(4) 0.057(6) 0.002(5) -0.002(6) 0.018(5) Cl1A 0.069(7) 0.045(2) 0.047(4) 0.005(2) 0.017(4) -0.015(3) Cl2A 0.047(3) 0.084(5) 0.078(5) 0.023(3) 0.000(2) -0.015(3) Fe1A 0.048(3) 0.065(4) 0.037(3) 0.012(3) -0.009(3) -0.008(3) C1A 0.057(6) 0.061(7) 0.037(3) 0.005(3) -0.007(4) -0.016(5) N1A 0.055(6) 0.063(7) 0.036(3) 0.008(4) -0.004(5) -0.016(5) C8A 0.086(13) 0.084(11) 0.063(12) 0.017(8) 0.009(10) 0.012(8) C2A 0.057(6) 0.069(8) 0.037(3) 0.003(5) -0.008(5) -0.017(5) C3A 0.068(9) 0.075(10) 0.037(4) -0.003(5) -0.015(5) -0.010(6) C4A 0.073(9) 0.074(11) 0.037(5) 0.002(6) -0.014(6) -0.002(8) C5A 0.076(9) 0.073(11) 0.033(5) 0.010(6) -0.008(7) -0.002(7) C6A 0.081(7) 0.073(9) 0.035(6) 0.014(6) 0.002(7) -0.001(6) C7A 0.062(6) 0.068(8) 0.036(4) 0.004(5) -0.003(5) -0.016(5) N2A 0.057(5) 0.064(7) 0.038(4) 0.008(5) -0.002(4) -0.015(5) C9A 0.076(7) 0.065(8) 0.049(7) 0.009(6) -0.004(6) -0.005(5) C10A 0.059(6) 0.060(6) 0.042(6) -0.008(5) -0.001(5) 0.018(5) N3A 0.055(6) 0.052(5) 0.044(4) -0.005(3) -0.005(4) 0.022(4) C21A 0.055(7) 0.067(6) 0.059(5) -0.006(5) -0.002(5) 0.009(4) C22A 0.057(7) 0.058(6) 0.057(5) -0.003(4) 0.001(5) 0.002(5) C23A 0.050(6) 0.050(6) 0.053(5) 0.001(6) 0.001(5) -0.004(5) C24A 0.061(7) 0.053(6) 0.057(5) 0.004(5) 0.000(5) -0.002(5) C25A 0.085(9) 0.071(8) 0.054(5) 0.008(6) 0.002(6) 0.007(6) C26A 0.104(9) 0.085(9) 0.057(5) 0.001(7) 0.011(6) 0.021(7) C27A 0.090(7) 0.080(7) 0.062(5) -0.001(6) 0.010(5) 0.024(6) C11A 0.038(7) 0.046(6) 0.049(5) -0.011(4) -0.010(4) 0.024(5) C12A 0.040(8) 0.040(5) 0.042(5) -0.003(6) -0.009(5) 0.021(6) N4A 0.033(5) 0.036(4) 0.031(5) 0.000(4) 0.002(5) 0.015(4) C13A 0.026(6) 0.039(5) 0.037(6) -0.008(5) 0.010(5) 0.017(4) C14A 0.028(7) 0.041(6) 0.044(7) -0.012(6) 0.008(6) 0.017(5) C15A 0.028(7) 0.041(7) 0.048(6) -0.014(6) 0.014(6) 0.013(6) C16A 0.028(8) 0.039(6) 0.050(6) -0.004(6) 0.020(7) 0.013(5) C17A 0.030(8) 0.038(5) 0.047(6) -0.006(5) 0.019(7) 0.015(5) C18A 0.027(6) 0.037(4) 0.035(6) -0.003(5) 0.016(6) 0.018(4) N5A 0.036(6) 0.040(4) 0.039(5) 0.001(5) 0.002(5) 0.019(4) C19A 0.035(5) 0.037(4) 0.031(5) 0.004(5) 0.001(5) 0.016(4) C20A 0.052(8) 0.042(9) 0.051(9) 0.018(8) -0.005(7) 0.019(7) O1S 0.086(9) 0.081(7) 0.085(9) -0.021(6) 0.035(7) -0.018(7) C1S 0.083(9) 0.084(9) 0.092(10) -0.030(7) 0.028(9) -0.010(8) C2S 0.081(8) 0.089(9) 0.085(10) -0.033(8) 0.031(9) -0.010(7) C3S 0.078(9) 0.075(8) 0.070(10) -0.013(7) 0.031(8) -0.013(7) C4S 0.083(9) 0.078(9) 0.084(10) -0.017(7) 0.039(9) -0.017(8) O1T 0.082(10) 0.086(10) 0.088(11) -0.034(8) 0.031(9) -0.013(9) C1T 0.080(10) 0.086(12) 0.080(13) -0.036(11) 0.033(11) -0.007(10) C2T 0.074(11) 0.077(10) 0.072(12) -0.024(9) 0.036(11) -0.011(9) C3T 0.074(11) 0.077(10) 0.059(13) -0.014(10) 0.037(11) -0.013(9) C4T 0.080(9) 0.083(9) 0.081(10) -0.024(8) 0.032(9) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Fe1 2.308(7) . ? Cl2 Fe1 2.287(7) . ? Fe1 C19 2.110(8) . ? Fe1 C1 2.113(8) . ? C1 N2 1.360(12) . ? C1 N1 1.373(13) . ? N1 C2 1.394(13) . ? N1 C8 1.462(12) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C2 C3 1.369(14) . ? C2 C7 1.383(11) . ? C3 C4 1.386(13) . ? C3 H3 0.9500 . ? C4 C5 1.394(12) . ? C4 H4 0.9500 . ? C5 C6 1.373(14) . ? C5 H5 0.9500 . ? C6 C7 1.402(13) . ? C6 H6 0.9500 . ? C7 N2 1.400(13) . ? N2 C9 1.457(13) . ? C9 C10 1.559(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.466(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N3 C21 1.459(11) . ? N3 C11 1.489(9) . ? C21 C22 1.501(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.369(11) . ? C22 C27 1.412(14) . ? C23 C24 1.375(14) . ? C23 H23 0.9500 . ? C24 C25 1.358(13) . ? C24 H24 0.9500 . ? C25 C26 1.379(14) . ? C25 H25 0.9500 . ? C26 C27 1.399(13) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C11 C12 1.562(16) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N4 1.445(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N4 C19 1.369(11) . ? N4 C13 1.406(12) . ? C13 C18 1.395(9) . ? C13 C14 1.401(13) . ? C14 C15 1.381(12) . ? C14 H14 0.9500 . ? C15 C16 1.393(10) . ? C15 H15 0.9500 . ? C16 C17 1.376(12) . ? C16 H16 0.9500 . ? C17 C18 1.364(13) . ? C17 H17 0.9500 . ? C18 N5 1.385(12) . ? N5 C19 1.350(11) . ? N5 C20 1.465(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Cl1A Fe1A 2.297(10) . ? Cl2A Fe1A 2.263(9) . ? Fe1A C1A 2.112(11) . ? Fe1A C19A 2.123(11) . ? C1A N2A 1.354(15) . ? C1A N1A 1.369(15) . ? N1A C2A 1.383(17) . ? N1A C8A 1.466(15) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C2A C3A 1.356(16) . ? C2A C7A 1.382(12) . ? C3A C4A 1.377(16) . ? C3A H3A 0.9500 . ? C4A C5A 1.399(14) . ? C4A H4A 0.9500 . ? C5A C6A 1.379(15) . ? C5A H5A 0.9500 . ? C6A C7A 1.414(16) . ? C6A H6A 0.9500 . ? C7A N2A 1.406(15) . ? N2A C9A 1.443(15) . ? C9A C10A 1.546(19) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A N3A 1.463(11) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? N3A C21A 1.467(14) . ? N3A C11A 1.489(11) . ? C21A C22A 1.499(16) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.370(14) . ? C22A C27A 1.421(17) . ? C23A C24A 1.376(16) . ? C23A H23A 0.9500 . ? C24A C25A 1.370(16) . ? C24A H24A 0.9500 . ? C25A C26A 1.385(17) . ? C25A H25A 0.9500 . ? C26A C27A 1.394(16) . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? C11A C12A 1.557(17) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C12A N4A 1.458(13) . ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? N4A C19A 1.359(14) . ? N4A C13A 1.411(16) . ? C13A C18A 1.392(11) . ? C13A C14A 1.409(16) . ? C14A C15A 1.385(15) . ? C14A H14A 0.9500 . ? C15A C16A 1.389(13) . ? C15A H15A 0.9500 . ? C16A C17A 1.387(15) . ? C16A H16A 0.9500 . ? C17A C18A 1.362(16) . ? C17A H17A 0.9500 . ? C18A N5A 1.384(16) . ? N5A C19A 1.378(14) . ? N5A C20A 1.453(13) . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? O1S C1S 1.37(2) . ? O1S C4S 1.37(2) . ? C1S C2S 1.57(2) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.58(2) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.57(2) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? O1T C1T 1.38(2) . ? O1T C4T 1.39(2) . ? C1T C2T 1.58(2) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.57(2) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.58(2) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Fe1 C1 104.1(6) . . ? C19 Fe1 Cl2 112.2(4) . . ? C1 Fe1 Cl2 111.9(5) . . ? C19 Fe1 Cl1 112.6(5) . . ? C1 Fe1 Cl1 109.9(5) . . ? Cl2 Fe1 Cl1 106.2(3) . . ? N2 C1 N1 104.5(7) . . ? N2 C1 Fe1 127.8(9) . . ? N1 C1 Fe1 127.6(8) . . ? C1 N1 C2 111.2(9) . . ? C1 N1 C8 127.5(11) . . ? C2 N1 C8 121.2(11) . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C2 C7 122.9(11) . . ? C3 C2 N1 130.5(11) . . ? C7 C2 N1 106.6(11) . . ? C2 C3 C4 116.5(11) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? C3 C4 C5 121.6(12) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 121.4(11) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 117.1(11) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C2 C7 N2 105.8(10) . . ? C2 C7 C6 120.4(12) . . ? N2 C7 C6 133.8(11) . . ? C1 N2 C7 111.9(9) . . ? C1 N2 C9 123.2(11) . . ? C7 N2 C9 124.5(11) . . ? N2 C9 C10 108.6(15) . . ? N2 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N2 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N3 C10 C9 112.7(9) . . ? N3 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N3 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C21 N3 C10 112.3(7) . . ? C21 N3 C11 111.6(7) . . ? C10 N3 C11 113.7(7) . . ? N3 C21 C22 112.7(8) . . ? N3 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N3 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C27 117.7(10) . . ? C23 C22 C21 121.8(10) . . ? C27 C22 C21 120.5(9) . . ? C22 C23 C24 122.1(11) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C25 C24 C23 120.7(11) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.2(10) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C27 120.8(10) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 119.3(10) . . ? C26 C27 H27 120.4 . . ? C22 C27 H27 120.4 . . ? N3 C11 C12 112.9(9) . . ? N3 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N3 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N4 C12 C11 110.3(13) . . ? N4 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N4 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C19 N4 C13 110.8(7) . . ? C19 N4 C12 124.0(9) . . ? C13 N4 C12 125.1(9) . . ? C18 C13 C14 120.5(10) . . ? C18 C13 N4 105.3(9) . . ? C14 C13 N4 134.0(9) . . ? C15 C14 C13 118.0(9) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? C14 C15 C16 119.8(10) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 122.6(10) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C18 C17 C16 117.6(9) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C17 C18 N5 131.6(9) . . ? C17 C18 C13 121.6(10) . . ? N5 C18 C13 106.7(9) . . ? C19 N5 C18 111.6(7) . . ? C19 N5 C20 125.7(9) . . ? C18 N5 C20 122.6(9) . . ? N5 C19 N4 105.5(7) . . ? N5 C19 Fe1 132.4(7) . . ? N4 C19 Fe1 122.0(7) . . ? N5 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1A Fe1A C19A 103.7(9) . . ? C1A Fe1A Cl2A 106.3(8) . . ? C19A Fe1A Cl2A 114.8(7) . . ? C1A Fe1A Cl1A 113.3(7) . . ? C19A Fe1A Cl1A 112.4(7) . . ? Cl2A Fe1A Cl1A 106.2(5) . . ? N2A C1A N1A 105.5(10) . . ? N2A C1A Fe1A 125.8(12) . . ? N1A C1A Fe1A 127.7(13) . . ? C1A N1A C2A 110.9(12) . . ? C1A N1A C8A 129.7(16) . . ? C2A N1A C8A 119.2(16) . . ? N1A C8A H8A1 109.5 . . ? N1A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? N1A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C3A C2A C7A 123.1(15) . . ? C3A C2A N1A 129.9(15) . . ? C7A C2A N1A 106.9(13) . . ? C2A C3A C4A 115.9(14) . . ? C2A C3A H3A 122.1 . . ? C4A C3A H3A 122.1 . . ? C3A C4A C5A 123.1(15) . . ? C3A C4A H4A 118.4 . . ? C5A C4A H4A 118.4 . . ? C6A C5A C4A 120.4(14) . . ? C6A C5A H5A 119.8 . . ? C4A C5A H5A 119.8 . . ? C5A C6A C7A 116.4(13) . . ? C5A C6A H6A 121.8 . . ? C7A C6A H6A 121.8 . . ? C2A C7A N2A 105.8(13) . . ? C2A C7A C6A 120.9(14) . . ? N2A C7A C6A 133.3(14) . . ? C1A N2A C7A 110.9(11) . . ? C1A N2A C9A 121.0(15) . . ? C7A N2A C9A 127.5(15) . . ? N2A C9A C10A 111.8(18) . . ? N2A C9A H9A1 109.2 . . ? C10A C9A H9A1 109.2 . . ? N2A C9A H9A2 109.2 . . ? C10A C9A H9A2 109.2 . . ? H9A1 C9A H9A2 107.9 . . ? N3A C10A C9A 115.9(14) . . ? N3A C10A H10C 108.3 . . ? C9A C10A H10C 108.3 . . ? N3A C10A H10D 108.3 . . ? C9A C10A H10D 108.3 . . ? H10C C10A H10D 107.4 . . ? C10A N3A C21A 111.4(10) . . ? C10A N3A C11A 115.9(10) . . ? C21A N3A C11A 111.4(10) . . ? N3A C21A C22A 113.5(14) . . ? N3A C21A H21C 108.9 . . ? C22A C21A H21C 108.9 . . ? N3A C21A H21D 108.9 . . ? C22A C21A H21D 108.9 . . ? H21C C21A H21D 107.7 . . ? C23A C22A C27A 117.5(13) . . ? C23A C22A C21A 122.6(14) . . ? C27A C22A C21A 119.8(13) . . ? C22A C23A C24A 122.2(14) . . ? C22A C23A H23A 118.9 . . ? C24A C23A H23A 118.9 . . ? C25A C24A C23A 121.0(14) . . ? C25A C24A H24A 119.5 . . ? C23A C24A H24A 119.5 . . ? C24A C25A C26A 118.5(14) . . ? C24A C25A H25A 120.8 . . ? C26A C25A H25A 120.8 . . ? C25A C26A C27A 121.3(15) . . ? C25A C26A H26A 119.4 . . ? C27A C26A H26A 119.4 . . ? C26A C27A C22A 119.4(14) . . ? C26A C27A H27A 120.3 . . ? C22A C27A H27A 120.3 . . ? N3A C11A C12A 111.1(11) . . ? N3A C11A H11C 109.4 . . ? C12A C11A H11C 109.4 . . ? N3A C11A H11D 109.4 . . ? C12A C11A H11D 109.4 . . ? H11C C11A H11D 108.0 . . ? N4A C12A C11A 112.6(15) . . ? N4A C12A H12C 109.1 . . ? C11A C12A H12C 109.1 . . ? N4A C12A H12D 109.1 . . ? C11A C12A H12D 109.1 . . ? H12C C12A H12D 107.8 . . ? C19A N4A C13A 111.1(10) . . ? C19A N4A C12A 124.0(13) . . ? C13A N4A C12A 124.8(13) . . ? C18A C13A C14A 119.5(13) . . ? C18A C13A N4A 106.0(12) . . ? C14A C13A N4A 134.5(12) . . ? C15A C14A C13A 116.9(12) . . ? C15A C14A H14A 121.5 . . ? C13A C14A H14A 121.5 . . ? C14A C15A C16A 121.4(14) . . ? C14A C15A H15A 119.3 . . ? C16A C15A H15A 119.3 . . ? C17A C16A C15A 122.2(14) . . ? C17A C16A H16A 118.9 . . ? C15A C16A H16A 118.9 . . ? C18A C17A C16A 115.9(12) . . ? C18A C17A H17A 122.0 . . ? C16A C17A H17A 122.0 . . ? C17A C18A N5A 129.7(13) . . ? C17A C18A C13A 124.0(14) . . ? N5A C18A C13A 106.2(12) . . ? C19A N5A C18A 111.7(10) . . ? C19A N5A C20A 125.8(13) . . ? C18A N5A C20A 122.4(13) . . ? N4A C19A N5A 104.8(9) . . ? N4A C19A Fe1A 122.0(10) . . ? N5A C19A Fe1A 133.2(10) . . ? N5A C20A H20D 109.5 . . ? N5A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? N5A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C1S O1S C4S 116.8(15) . . ? O1S C1S C2S 105.5(13) . . ? O1S C1S H1S1 110.6 . . ? C2S C1S H1S1 110.6 . . ? O1S C1S H1S2 110.6 . . ? C2S C1S H1S2 110.6 . . ? H1S1 C1S H1S2 108.8 . . ? C1S C2S C3S 101.0(13) . . ? C1S C2S H2S1 111.6 . . ? C3S C2S H2S1 111.6 . . ? C1S C2S H2S2 111.6 . . ? C3S C2S H2S2 111.6 . . ? H2S1 C2S H2S2 109.4 . . ? C4S C3S C2S 100.5(14) . . ? C4S C3S H3S1 111.7 . . ? C2S C3S H3S1 111.7 . . ? C4S C3S H3S2 111.7 . . ? C2S C3S H3S2 111.7 . . ? H3S1 C3S H3S2 109.4 . . ? O1S C4S C3S 103.8(14) . . ? O1S C4S H4S1 111.0 . . ? C3S C4S H4S1 111.0 . . ? O1S C4S H4S2 111.0 . . ? C3S C4S H4S2 111.0 . . ? H4S1 C4S H4S2 109.0 . . ? C1T O1T C4T 110(3) . . ? O1T C1T C2T 102.4(19) . . ? O1T C1T H1T1 111.3 . . ? C2T C1T H1T1 111.3 . . ? O1T C1T H1T2 111.3 . . ? C2T C1T H1T2 111.3 . . ? H1T1 C1T H1T2 109.2 . . ? C3T C2T C1T 103.2(14) . . ? C3T C2T H2T1 111.1 . . ? C1T C2T H2T1 111.1 . . ? C3T C2T H2T2 111.1 . . ? C1T C2T H2T2 111.1 . . ? H2T1 C2T H2T2 109.1 . . ? C2T C3T C4T 101.9(15) . . ? C2T C3T H3T1 111.4 . . ? C4T C3T H3T1 111.4 . . ? C2T C3T H3T2 111.4 . . ? C4T C3T H3T2 111.4 . . ? H3T1 C3T H3T2 109.3 . . ? O1T C4T C3T 100.7(19) . . ? O1T C4T H4T1 111.6 . . ? C3T C4T H4T1 111.6 . . ? O1T C4T H4T2 111.6 . . ? C3T C4T H4T2 111.6 . . ? H4T1 C4T H4T2 109.4 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 65.09 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.387 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.070 data__Compound_{BnN(CH2CH2CH2-N-methylbenzimidazole-2-ylidene)2}FeCl2 _database_code_depnum_ccdc_archive 'CCDC 907142' #TrackingRef 'web_deposit_cif_file_0_NilayHazari_1360023780.XRay_SI.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Cl2 Fe N5' _chemical_formula_weight 617.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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 9.3137(2) _cell_length_b 29.3333(5) _cell_length_c 22.4626(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.700(7) _cell_angle_gamma 90.00 _cell_volume 6066.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 106166 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 68.3 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 5.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3882 _exptl_absorpt_correction_T_max 0.7591 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; 'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD' ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 74851 _diffrn_reflns_av_R_equivalents 0.1618 _diffrn_reflns_av_unetI/netI 0.0838 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 6.51 _diffrn_reflns_theta_max 55.99 _reflns_number_total 7859 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. All disorders were refined with the help of similarity restraints on the 1,2- and 1,3- distances and displacement parameters as well as rigid bond restraints for anisotropic displacement parameters. ; _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^)+(0.1043P)^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 7859 _refine_ls_number_parameters 741 _refine_ls_number_restraints 254 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.062 _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 Cl1 Cl 0.30328(12) 0.58244(4) 0.13820(5) 0.0465(3) Uani 1 1 d . . . Cl2 Cl 0.04507(11) 0.53782(4) 0.23390(5) 0.0414(3) Uani 1 1 d . . . Fe1 Fe 0.27856(7) 0.53461(2) 0.21596(3) 0.0365(2) Uani 1 1 d . . . C1 C 0.3414(5) 0.46730(17) 0.2005(2) 0.0442(12) Uani 1 1 d . . . N1 N 0.4105(4) 0.44962(14) 0.15590(18) 0.0480(10) Uani 1 1 d . . . C21 C 0.4369(7) 0.4736(2) 0.1019(2) 0.0652(15) Uani 1 1 d . . . H21A H 0.4023 0.5051 0.1032 0.098 Uiso 1 1 calc R . . H21B H 0.3850 0.4583 0.0663 0.098 Uiso 1 1 calc R . . H21C H 0.5413 0.4737 0.0999 0.098 Uiso 1 1 calc R . . C2 C 0.4500(5) 0.40446(18) 0.1675(2) 0.0508(13) Uani 1 1 d . . . C3 C 0.5222(5) 0.37327(19) 0.1360(3) 0.0568(14) Uani 1 1 d . . . H3 H 0.5560 0.3814 0.0995 0.068 Uiso 1 1 calc R . . C4 C 0.5423(6) 0.3306(2) 0.1596(3) 0.0594(15) Uani 1 1 d . . . H4 H 0.5900 0.3084 0.1389 0.071 Uiso 1 1 calc R . . C5 C 0.4946(5) 0.31875(18) 0.2138(3) 0.0584(15) Uani 1 1 d . . . H5 H 0.5105 0.2886 0.2289 0.070 Uiso 1 1 calc R . . C6 C 0.4241(5) 0.35020(17) 0.2460(3) 0.0508(13) Uani 1 1 d . . . H6 H 0.3924 0.3423 0.2829 0.061 Uiso 1 1 calc R . . C7 C 0.4029(5) 0.39339(16) 0.2215(2) 0.0422(12) Uani 1 1 d . . . N2 N 0.3377(4) 0.43238(12) 0.24020(17) 0.0389(9) Uani 1 1 d . . . C8 C 0.2718(5) 0.43571(16) 0.2954(2) 0.0416(11) Uani 1 1 d . . . H8A H 0.2032 0.4100 0.2963 0.050 Uiso 1 1 calc R . . H8B H 0.2150 0.4643 0.2940 0.050 Uiso 1 1 calc R . . C9 C 0.3791(5) 0.43504(17) 0.3526(2) 0.0436(12) Uani 1 1 d . . . H9A H 0.4484 0.4606 0.3523 0.052 Uiso 1 1 calc R . . H9B H 0.4349 0.4062 0.3551 0.052 Uiso 1 1 calc R . . C10 C 0.3006(5) 0.43929(16) 0.4071(2) 0.0438(12) Uani 1 1 d . . . H10A H 0.2250 0.4154 0.4052 0.053 Uiso 1 1 calc R . . H10B H 0.3707 0.4344 0.4443 0.053 Uiso 1 1 calc R . . N3 N 0.2324(4) 0.48448(12) 0.40975(16) 0.0390(9) Uani 1 1 d . . . C22 C 0.1059(5) 0.48147(17) 0.4418(2) 0.0440(12) Uani 1 1 d . . . H22A H 0.0691 0.5126 0.4472 0.053 Uiso 1 1 calc R . . H22B H 0.1378 0.4685 0.4824 0.053 Uiso 1 1 calc R . . C23 C -0.0153(5) 0.45305(16) 0.4102(2) 0.0410(12) Uani 1 1 d . . . C24 C -0.0700(5) 0.45970(16) 0.3493(2) 0.0442(12) Uani 1 1 d . . . H24 H -0.0295 0.4828 0.3273 0.053 Uiso 1 1 calc R . . C25 C -0.1822(5) 0.43302(18) 0.3207(2) 0.0513(13) Uani 1 1 d . . . H25 H -0.2171 0.4377 0.2792 0.062 Uiso 1 1 calc R . . C26 C -0.2448(5) 0.39927(18) 0.3524(3) 0.0507(13) Uani 1 1 d . . . H26 H -0.3222 0.3811 0.3328 0.061 Uiso 1 1 calc R . . C27 C -0.1926(5) 0.39282(16) 0.4123(2) 0.0470(12) Uani 1 1 d . . . H27 H -0.2357 0.3704 0.4344 0.056 Uiso 1 1 calc R . . C28 C -0.0781(5) 0.41855(15) 0.4407(2) 0.0398(11) Uani 1 1 d . . . H28 H -0.0412 0.4127 0.4817 0.048 Uiso 1 1 calc R . . C11 C 0.3381(5) 0.51721(17) 0.4399(2) 0.0449(12) Uani 1 1 d . . . H11A H 0.4327 0.5118 0.4262 0.054 Uiso 1 1 calc R . . H11B H 0.3511 0.5113 0.4838 0.054 Uiso 1 1 calc R . . C12 C 0.2974(5) 0.56679(16) 0.4292(2) 0.0407(11) Uani 1 1 d . . . H12A H 0.3662 0.5856 0.4569 0.049 Uiso 1 1 calc R . . H12B H 0.1994 0.5715 0.4401 0.049 Uiso 1 1 calc R . . C13 C 0.2969(5) 0.58416(15) 0.36546(19) 0.0382(11) Uani 1 1 d . . . H13A H 0.2159 0.5695 0.3386 0.046 Uiso 1 1 calc R . . H13B H 0.2785 0.6174 0.3647 0.046 Uiso 1 1 calc R . . N4 N 0.4333(4) 0.57536(11) 0.34176(16) 0.0345(9) Uani 1 1 d . . . C14 C 0.5708(4) 0.58841(15) 0.36978(19) 0.0337(10) Uani 1 1 d . . . C15 C 0.6189(5) 0.61434(15) 0.42039(19) 0.0380(11) Uani 1 1 d . . . H15 H 0.5531 0.6262 0.4449 0.046 Uiso 1 1 calc R . . C16 C 0.7658(5) 0.62218(16) 0.4337(2) 0.0418(12) Uani 1 1 d . . . H16 H 0.8021 0.6393 0.4687 0.050 Uiso 1 1 calc R . . C17 C 0.8636(5) 0.60569(15) 0.3972(2) 0.0408(12) Uani 1 1 d . . . H17 H 0.9642 0.6121 0.4076 0.049 Uiso 1 1 calc R . . C18 C 0.8163(5) 0.58029(15) 0.3464(2) 0.0388(11) Uani 1 1 d . . . H18 H 0.8821 0.5686 0.3218 0.047 Uiso 1 1 calc R . . C19 C 0.6680(5) 0.57248(14) 0.33302(19) 0.0349(11) Uani 1 1 d . . . N5 N 0.5842(4) 0.55101(12) 0.28488(16) 0.0363(9) Uani 1 1 d . . . C29 C 0.6432(5) 0.52996(17) 0.2343(2) 0.0475(13) Uani 1 1 d . . . H29A H 0.6354 0.4967 0.2368 0.071 Uiso 1 1 calc R . . H29B H 0.7455 0.5385 0.2361 0.071 Uiso 1 1 calc R . . H29C H 0.5881 0.5406 0.1962 0.071 Uiso 1 1 calc R . . C20 C 0.4403(5) 0.55304(14) 0.2890(2) 0.0357(11) Uani 1 1 d . . . Cl3 Cl 0.35880(11) 0.71609(4) 0.39171(5) 0.0457(3) Uani 1 1 d . . . Cl4 Cl 0.06852(12) 0.70430(4) 0.49308(5) 0.0496(3) Uani 1 1 d . . . Fe2 Fe 0.12767(7) 0.73278(2) 0.40557(3) 0.0362(2) Uani 1 1 d . . . C101 C 0.1153(5) 0.80505(16) 0.4088(2) 0.0383(11) Uani 1 1 d . . . N101 N 0.1833(4) 0.83114(13) 0.45524(16) 0.0411(9) Uani 1 1 d . . . C121 C 0.2710(6) 0.81219(18) 0.5089(2) 0.0549(13) Uani 1 1 d . . . H12C H 0.2173 0.7875 0.5250 0.082 Uiso 1 1 calc R . . H12D H 0.2924 0.8361 0.5394 0.082 Uiso 1 1 calc R . . H12E H 0.3621 0.8002 0.4983 0.082 Uiso 1 1 calc R . . C102 C 0.1576(5) 0.87724(16) 0.4442(2) 0.0434(12) Uani 1 1 d . . . C103 C 0.1990(6) 0.91570(18) 0.4782(2) 0.0550(14) Uani 1 1 d . . . H103 H 0.2573 0.9136 0.5166 0.066 Uiso 1 1 calc R . . C104 C 0.1512(7) 0.95757(19) 0.4536(2) 0.0635(15) Uani 1 1 d . . . H104 H 0.1783 0.9847 0.4755 0.076 Uiso 1 1 calc R . . C105 C 0.0640(7) 0.96026(19) 0.3973(3) 0.0677(16) Uani 1 1 d . . . H105 H 0.0321 0.9893 0.3819 0.081 Uiso 1 1 calc R . . C106 C 0.0232(6) 0.92176(17) 0.3635(2) 0.0592(14) Uani 1 1 d . . . H106 H -0.0344 0.9237 0.3249 0.071 Uiso 1 1 calc R . . C107 C 0.0698(5) 0.88034(16) 0.3883(2) 0.0445(12) Uani 1 1 d . . . N102 N 0.0475(4) 0.83564(13) 0.36831(16) 0.0389(9) Uani 1 1 d . . . C108 C -0.0306(5) 0.82334(16) 0.30844(19) 0.0401(11) Uani 1 1 d . . . H10C H -0.1255 0.8392 0.3017 0.048 Uiso 1 1 calc R . . H10D H -0.0494 0.7901 0.3071 0.048 Uiso 1 1 calc R . . C109 C 0.0550(5) 0.83603(17) 0.2589(2) 0.0501(13) Uani 1 1 d . . . H10E H 0.1542 0.8233 0.2685 0.060 Uiso 1 1 calc R . . H10F H 0.0635 0.8696 0.2573 0.060 Uiso 1 1 calc R . . C110 C -0.0154(5) 0.81847(17) 0.1972(2) 0.0493(13) Uani 1 1 d . . . H11C H -0.1131 0.8323 0.1873 0.059 Uiso 1 1 calc R . . H11D H 0.0432 0.8291 0.1666 0.059 Uiso 1 1 calc R . . N103 N -0.0301(4) 0.76868(12) 0.19252(16) 0.0404(9) Uani 1 1 d . A . C122 C -0.1041(2) 0.75864(7) 0.13106(9) 0.0463(11) Uani 1 1 d U . . H12F H -0.1009 0.7253 0.1242 0.056 Uiso 0.408(7) 1 calc PR A 1 H12G H -0.0503 0.7736 0.1017 0.056 Uiso 0.408(7) 1 calc PR A 1 H12H H -0.0944 0.7257 0.1232 0.056 Uiso 0.592(7) 1 calc PR A 2 H12I H -0.0540 0.7754 0.1019 0.056 Uiso 0.592(7) 1 calc PR A 2 C123 C -0.2631(2) 0.77446(7) 0.11921(9) 0.042(3) Uani 0.408(7) 1 d PRDU A 1 C124 C -0.3129(2) 0.80816(7) 0.07766(9) 0.050(3) Uani 0.408(7) 1 d PRDU A 1 H124 H -0.2459 0.8250 0.0584 0.060 Uiso 0.408(7) 1 calc PR A 1 C125 C -0.4608(2) 0.81720(7) 0.06427(9) 0.054(3) Uani 0.408(7) 1 d PRDU A 1 H125 H -0.4948 0.8402 0.0359 0.065 Uiso 0.408(7) 1 calc PR A 1 C126 C -0.5588(2) 0.79256(7) 0.09243(9) 0.053(3) Uani 0.408(7) 1 d PRDU A 1 H126 H -0.6599 0.7987 0.0833 0.064 Uiso 0.408(7) 1 calc PR A 1 C127 C -0.5091(2) 0.75886(7) 0.13399(9) 0.046(3) Uani 0.408(7) 1 d PRDU A 1 H127 H -0.5761 0.7420 0.1532 0.055 Uiso 0.408(7) 1 calc PR A 1 C128 C -0.3612(2) 0.74982(7) 0.14738(9) 0.042(2) Uani 0.408(7) 1 d PRDU A 1 H128 H -0.3272 0.7268 0.1758 0.050 Uiso 0.408(7) 1 calc PR A 1 C23A C -0.2641(2) 0.77108(7) 0.11973(9) 0.039(2) Uani 0.592(7) 1 d PRDU A 2 C24A C -0.3204(2) 0.79006(7) 0.06442(9) 0.050(2) Uani 0.592(7) 1 d PRDU A 2 H24A H -0.2574 0.7979 0.0365 0.059 Uiso 0.592(7) 1 calc PR A 2 C25A C -0.4689(2) 0.79758(7) 0.04997(9) 0.058(2) Uani 0.592(7) 1 d PRDU A 2 H25A H -0.5074 0.8106 0.0122 0.069 Uiso 0.592(7) 1 calc PR A 2 C26A C -0.5611(2) 0.78611(7) 0.09084(9) 0.050(2) Uani 0.592(7) 1 d PRDU A 2 H26A H -0.6627 0.7912 0.0810 0.060 Uiso 0.592(7) 1 calc PR A 2 C27A C -0.5048(2) 0.76713(7) 0.14616(9) 0.0463(19) Uani 0.592(7) 1 d PRDU A 2 H27A H -0.5678 0.7593 0.1741 0.056 Uiso 0.592(7) 1 calc PR A 2 C28A C -0.3563(2) 0.75962(7) 0.16061(9) 0.0382(18) Uani 0.592(7) 1 d PRDU A 2 H28A H -0.3178 0.7466 0.1984 0.046 Uiso 0.592(7) 1 calc PR A 2 C111 C 0.1136(2) 0.74698(7) 0.20089(9) 0.0512(13) Uani 1 1 d R . . H11E H 0.1689 0.7580 0.2393 0.061 Uiso 1 1 calc R . . H11F H 0.1660 0.7573 0.1681 0.061 Uiso 1 1 calc R . . C112 C 0.1139(5) 0.69521(18) 0.2017(2) 0.0489(13) Uani 1 1 d . A . H11G H 0.2044 0.6844 0.1882 0.059 Uiso 1 1 calc R . . H11H H 0.0315 0.6843 0.1721 0.059 Uiso 1 1 calc R . . C113 C 0.1031(5) 0.67327(17) 0.2626(2) 0.0436(12) Uani 1 1 d . . . H11I H 0.1093 0.6398 0.2584 0.052 Uiso 1 1 calc R A . H11J H 0.1874 0.6832 0.2920 0.052 Uiso 1 1 calc R . . N104 N -0.0308(4) 0.68440(12) 0.28672(16) 0.0367(9) Uani 1 1 d . A . C114 C -0.1694(5) 0.67222(15) 0.25932(19) 0.0360(11) Uani 1 1 d . . . C115 C -0.2175(5) 0.64610(16) 0.2086(2) 0.0426(12) Uani 1 1 d . A . H115 H -0.1521 0.6330 0.1848 0.051 Uiso 1 1 calc R . . C116 C -0.3654(5) 0.64041(16) 0.1947(2) 0.0441(12) Uani 1 1 d . . . H116 H -0.4031 0.6236 0.1596 0.053 Uiso 1 1 calc R A . C117 C -0.4621(5) 0.65837(15) 0.2303(2) 0.0411(12) Uani 1 1 d . A . H117 H -0.5633 0.6532 0.2193 0.049 Uiso 1 1 calc R . . C118 C -0.4130(5) 0.68355(15) 0.2813(2) 0.0383(11) Uani 1 1 d . . . H118 H -0.4781 0.6958 0.3058 0.046 Uiso 1 1 calc R A . C119 C -0.2651(4) 0.69007(14) 0.29475(19) 0.0334(10) Uani 1 1 d . A . N105 N -0.1799(4) 0.71290(12) 0.34179(15) 0.0338(9) Uani 1 1 d . . . C129 C -0.2398(5) 0.73861(16) 0.3882(2) 0.0409(11) Uani 1 1 d . A . H12J H -0.1625 0.7449 0.4219 0.061 Uiso 1 1 calc R . . H12K H -0.3164 0.7207 0.4026 0.061 Uiso 1 1 calc R . . H12L H -0.2805 0.7674 0.3712 0.061 Uiso 1 1 calc R . . C120 C -0.0353(5) 0.70936(15) 0.3383(2) 0.0399(11) Uani 1 1 d . A . C1S C 0.6435(7) 0.6184(3) 0.0296(3) 0.0771(18) Uani 1 1 d . . . H1S H 0.5416 0.6134 0.0213 0.092 Uiso 1 1 calc R . . C2S C 0.7337(8) 0.5859(2) 0.0603(3) 0.0738(17) Uani 1 1 d . . . H2S H 0.6939 0.5584 0.0732 0.089 Uiso 1 1 calc R . . C3S C 0.8799(7) 0.5932(2) 0.0722(3) 0.0679(16) Uani 1 1 d . . . H3S H 0.9423 0.5709 0.0930 0.082 Uiso 1 1 calc R . . C4S C 0.9364(7) 0.6334(2) 0.0538(3) 0.0669(16) Uani 1 1 d . . . H4S H 1.0380 0.6388 0.0627 0.080 Uiso 1 1 calc R . . C5S C 0.8491(8) 0.6654(2) 0.0232(3) 0.0740(17) Uani 1 1 d . . . H5S H 0.8900 0.6927 0.0103 0.089 Uiso 1 1 calc R . . C6S C 0.7040(7) 0.6585(2) 0.0110(3) 0.0754(17) Uani 1 1 d . . . H6S H 0.6431 0.6810 -0.0102 0.090 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 Cl1 0.0497(7) 0.0555(8) 0.0342(6) 0.0034(5) 0.0064(5) -0.0052(5) Cl2 0.0369(6) 0.0510(7) 0.0374(7) -0.0009(5) 0.0092(5) 0.0007(5) Fe1 0.0376(4) 0.0416(5) 0.0314(4) -0.0019(3) 0.0089(3) -0.0008(3) C1 0.038(3) 0.059(3) 0.037(3) -0.008(3) 0.010(2) 0.000(2) N1 0.049(2) 0.054(3) 0.042(3) -0.013(2) 0.012(2) 0.001(2) C21 0.087(4) 0.073(4) 0.042(3) -0.007(3) 0.028(3) 0.002(3) C2 0.043(3) 0.047(3) 0.061(4) -0.021(3) 0.005(3) 0.000(2) C3 0.049(3) 0.061(4) 0.062(4) -0.020(3) 0.012(3) 0.002(3) C4 0.051(3) 0.052(4) 0.076(4) -0.027(3) 0.010(3) 0.007(3) C5 0.039(3) 0.045(3) 0.087(4) -0.015(3) -0.003(3) -0.001(2) C6 0.040(3) 0.043(3) 0.069(4) -0.009(3) 0.007(3) 0.004(2) C7 0.039(3) 0.038(3) 0.049(3) -0.007(2) 0.007(2) 0.002(2) N2 0.042(2) 0.034(2) 0.043(2) 0.0000(19) 0.0148(19) 0.0030(17) C8 0.041(3) 0.041(3) 0.046(3) 0.004(2) 0.017(2) 0.000(2) C9 0.039(3) 0.047(3) 0.047(3) 0.005(2) 0.013(2) 0.006(2) C10 0.042(3) 0.045(3) 0.047(3) 0.009(2) 0.014(2) 0.006(2) N3 0.038(2) 0.043(2) 0.039(2) 0.0060(18) 0.0147(18) 0.0003(18) C22 0.043(3) 0.050(3) 0.042(3) 0.001(2) 0.016(2) 0.000(2) C23 0.038(3) 0.042(3) 0.045(3) -0.001(2) 0.012(2) 0.004(2) C24 0.043(3) 0.046(3) 0.045(3) 0.008(2) 0.013(2) 0.007(2) C25 0.048(3) 0.062(4) 0.042(3) -0.001(3) 0.002(3) 0.015(3) C26 0.034(3) 0.054(3) 0.065(4) -0.008(3) 0.009(3) 0.004(2) C27 0.046(3) 0.049(3) 0.050(3) 0.000(3) 0.021(3) -0.003(2) C28 0.037(3) 0.044(3) 0.041(3) -0.003(2) 0.015(2) 0.004(2) C11 0.033(3) 0.060(3) 0.043(3) 0.006(2) 0.010(2) -0.004(2) C12 0.035(3) 0.054(3) 0.034(3) -0.004(2) 0.009(2) -0.005(2) C13 0.038(3) 0.042(3) 0.036(3) -0.004(2) 0.009(2) 0.000(2) N4 0.031(2) 0.040(2) 0.033(2) -0.0002(17) 0.0071(17) -0.0001(16) C14 0.032(2) 0.038(3) 0.031(3) 0.005(2) 0.005(2) 0.000(2) C15 0.043(3) 0.042(3) 0.029(3) 0.003(2) 0.008(2) -0.001(2) C16 0.041(3) 0.048(3) 0.035(3) 0.001(2) 0.000(2) -0.005(2) C17 0.033(3) 0.046(3) 0.043(3) 0.005(2) 0.003(2) -0.001(2) C18 0.037(3) 0.045(3) 0.035(3) 0.004(2) 0.008(2) -0.001(2) C19 0.037(3) 0.038(3) 0.029(3) 0.003(2) 0.003(2) -0.002(2) N5 0.036(2) 0.045(2) 0.031(2) -0.0010(18) 0.0112(18) 0.0026(17) C29 0.041(3) 0.059(3) 0.045(3) -0.007(2) 0.013(2) 0.003(2) C20 0.043(3) 0.032(3) 0.033(3) 0.004(2) 0.012(2) 0.003(2) Cl3 0.0358(6) 0.0531(7) 0.0504(7) -0.0057(6) 0.0139(5) 0.0007(5) Cl4 0.0455(7) 0.0676(8) 0.0364(7) 0.0072(6) 0.0088(5) -0.0091(6) Fe2 0.0352(4) 0.0420(5) 0.0331(4) 0.0007(3) 0.0108(3) -0.0008(3) C101 0.036(3) 0.045(3) 0.035(3) 0.001(2) 0.012(2) 0.005(2) N101 0.050(2) 0.040(2) 0.032(2) -0.0011(19) 0.0038(19) -0.0015(18) C121 0.070(3) 0.057(3) 0.035(3) 0.003(2) -0.003(3) 0.002(3) C102 0.055(3) 0.040(3) 0.035(3) -0.001(2) 0.005(2) -0.002(2) C103 0.079(4) 0.052(4) 0.033(3) -0.002(3) 0.005(3) -0.005(3) C104 0.095(4) 0.049(4) 0.043(3) -0.002(3) -0.002(3) -0.007(3) C105 0.094(4) 0.045(3) 0.058(4) 0.002(3) -0.009(3) 0.002(3) C106 0.078(4) 0.048(4) 0.047(3) -0.001(3) -0.005(3) -0.001(3) C107 0.056(3) 0.037(3) 0.039(3) -0.001(2) 0.002(2) 0.000(2) N102 0.043(2) 0.040(2) 0.033(2) 0.0017(18) 0.0020(18) -0.0001(18) C108 0.042(3) 0.042(3) 0.034(3) 0.002(2) -0.002(2) -0.003(2) C109 0.058(3) 0.054(3) 0.038(3) 0.002(2) 0.005(2) -0.014(2) C110 0.052(3) 0.053(3) 0.041(3) 0.007(2) 0.003(2) -0.013(2) N103 0.036(2) 0.050(3) 0.035(2) 0.0034(18) 0.0018(18) -0.0028(17) C122 0.046(2) 0.057(3) 0.036(3) -0.005(2) 0.005(2) -0.003(2) C123 0.044(4) 0.052(6) 0.028(6) -0.002(5) 0.004(5) -0.007(5) C124 0.061(4) 0.056(6) 0.030(6) 0.002(4) 0.005(5) -0.006(4) C125 0.067(5) 0.057(7) 0.036(6) 0.006(5) -0.002(5) 0.003(5) C126 0.046(5) 0.054(6) 0.054(7) 0.000(5) -0.009(5) 0.001(5) C127 0.042(4) 0.053(6) 0.041(6) -0.002(4) 0.003(5) -0.003(5) C128 0.044(4) 0.050(6) 0.031(5) 0.001(4) 0.004(4) 0.001(4) C23A 0.045(3) 0.043(5) 0.028(4) -0.002(4) 0.002(3) -0.005(4) C24A 0.056(3) 0.053(5) 0.037(4) 0.010(4) 0.001(3) -0.019(4) C25A 0.063(4) 0.055(6) 0.048(4) 0.015(4) -0.016(3) -0.008(4) C26A 0.042(4) 0.046(5) 0.056(5) -0.008(4) -0.010(3) 0.000(4) C27A 0.044(3) 0.049(5) 0.045(4) -0.009(3) 0.004(4) -0.005(4) C28A 0.045(3) 0.037(4) 0.031(4) -0.003(3) 0.003(3) -0.001(3) C111 0.042(3) 0.071(4) 0.044(3) 0.011(3) 0.013(2) -0.005(3) C112 0.034(3) 0.074(4) 0.043(3) 0.002(3) 0.018(2) 0.008(2) C113 0.037(3) 0.054(3) 0.041(3) -0.001(2) 0.011(2) 0.012(2) N104 0.038(2) 0.040(2) 0.032(2) 0.0017(18) 0.0083(18) 0.0039(17) C114 0.036(3) 0.039(3) 0.032(3) 0.006(2) 0.001(2) 0.001(2) C115 0.043(3) 0.048(3) 0.037(3) 0.000(2) 0.007(2) 0.003(2) C116 0.047(3) 0.052(3) 0.033(3) -0.005(2) 0.006(2) -0.001(2) C117 0.036(3) 0.041(3) 0.044(3) 0.007(2) 0.001(2) -0.004(2) C118 0.040(3) 0.043(3) 0.033(3) 0.003(2) 0.009(2) -0.001(2) C119 0.033(3) 0.038(3) 0.029(2) 0.004(2) 0.007(2) -0.001(2) N105 0.032(2) 0.040(2) 0.032(2) 0.0017(17) 0.0101(17) 0.0009(16) C129 0.038(3) 0.050(3) 0.037(3) -0.005(2) 0.011(2) 0.001(2) C120 0.043(3) 0.039(3) 0.039(3) 0.004(2) 0.013(2) 0.002(2) C1S 0.067(4) 0.098(5) 0.065(4) -0.024(4) 0.007(3) -0.006(4) C2S 0.087(5) 0.071(4) 0.068(4) -0.016(3) 0.026(4) -0.009(4) C3S 0.081(5) 0.068(4) 0.058(4) -0.009(3) 0.021(3) 0.011(3) C4S 0.078(4) 0.075(4) 0.050(4) -0.004(3) 0.019(3) 0.008(4) C5S 0.091(5) 0.073(4) 0.060(4) -0.005(3) 0.019(4) -0.004(4) C6S 0.072(5) 0.084(5) 0.066(4) -0.007(4) -0.001(3) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Fe1 2.2790(13) . ? Cl2 Fe1 2.2727(12) . ? Fe1 C1 2.103(5) . ? Fe1 C20 2.123(5) . ? C1 N2 1.361(6) . ? C1 N1 1.372(6) . ? N1 C2 1.389(6) . ? N1 C21 1.456(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C2 C7 1.390(7) . ? C2 C3 1.391(7) . ? C3 C4 1.360(8) . ? C3 H3 0.9500 . ? C4 C5 1.401(8) . ? C4 H4 0.9500 . ? C5 C6 1.396(7) . ? C5 H5 0.9500 . ? C6 C7 1.384(7) . ? C6 H6 0.9500 . ? C7 N2 1.390(5) . ? N2 C8 1.467(6) . ? C8 C9 1.504(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.475(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N3 C11 1.466(6) . ? N3 C22 1.473(5) . ? C22 C23 1.494(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.398(6) . ? C23 C24 1.400(7) . ? C24 C25 1.384(7) . ? C24 H24 0.9500 . ? C25 C26 1.396(7) . ? C25 H25 0.9500 . ? C26 C27 1.373(7) . ? C26 H26 0.9500 . ? C27 C28 1.381(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C11 C12 1.513(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N4 1.473(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N4 C20 1.364(5) . ? N4 C14 1.393(5) . ? C14 C15 1.385(6) . ? C14 C19 1.394(6) . ? C15 C16 1.375(6) . ? C15 H15 0.9500 . ? C16 C17 1.400(6) . ? C16 H16 0.9500 . ? C17 C18 1.377(6) . ? C17 H17 0.9500 . ? C18 C19 1.387(6) . ? C18 H18 0.9500 . ? C19 N5 1.386(5) . ? N5 C20 1.359(5) . ? N5 C29 1.472(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? Cl3 Fe2 2.2745(12) . ? Cl4 Fe2 2.2786(13) . ? Fe2 C120 2.090(5) . ? Fe2 C101 2.125(5) . ? C101 N102 1.363(5) . ? C101 N101 1.369(5) . ? N101 C102 1.389(6) . ? N101 C121 1.459(6) . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C102 C103 1.385(7) . ? C102 C107 1.393(7) . ? C103 C104 1.392(7) . ? C103 H103 0.9500 . ? C104 C105 1.399(8) . ? C104 H104 0.9500 . ? C105 C106 1.382(7) . ? C105 H105 0.9500 . ? C106 C107 1.379(7) . ? C106 H106 0.9500 . ? C107 N102 1.391(6) . ? N102 C108 1.474(6) . ? C108 C109 1.510(6) . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.531(7) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 N103 1.469(6) . ? C110 H11C 0.9900 . ? C110 H11D 0.9900 . ? N103 C111 1.468(4) . ? N103 C122 1.476(4) . ? C122 C23A 1.5175 . ? C122 C123 1.5365 . ? C122 H12F 0.9900 . ? C122 H12G 0.9900 . ? C122 H12H 0.9900 . ? C122 H12I 0.9900 . ? C123 C124 1.3900 . ? C123 C128 1.3900 . ? C124 C125 1.3900 . ? C124 H124 0.9500 . ? C125 C126 1.3900 . ? C125 H125 0.9500 . ? C126 C127 1.3900 . ? C126 H126 0.9500 . ? C127 C128 1.3900 . ? C127 H127 0.9500 . ? C128 H128 0.9500 . ? C23A C24A 1.3900 . ? C23A C28A 1.3900 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? C111 C112 1.519(5) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 C113 1.528(6) . ? C112 H11G 0.9900 . ? C112 H11H 0.9900 . ? C113 N104 1.469(6) . ? C113 H11I 0.9900 . ? C113 H11J 0.9900 . ? N104 C120 1.376(6) . ? N104 C114 1.390(5) . ? C114 C119 1.384(6) . ? C114 C115 1.390(6) . ? C115 C116 1.376(6) . ? C115 H115 0.9500 . ? C116 C117 1.395(6) . ? C116 H116 0.9500 . ? C117 C118 1.381(6) . ? C117 H117 0.9500 . ? C118 C119 1.379(6) . ? C118 H118 0.9500 . ? C119 N105 1.393(5) . ? N105 C120 1.365(5) . ? N105 C129 1.464(5) . ? C129 H12J 0.9800 . ? C129 H12K 0.9800 . ? C129 H12L 0.9800 . ? C1S C2S 1.385(9) . ? C1S C6S 1.395(9) . ? C1S H1S 0.9500 . ? C2S C3S 1.365(8) . ? C2S H2S 0.9500 . ? C3S C4S 1.380(8) . ? C3S H3S 0.9500 . ? C4S C5S 1.358(8) . ? C4S H4S 0.9500 . ? C5S C6S 1.353(9) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C20 100.59(17) . . ? C1 Fe1 Cl2 111.46(13) . . ? C20 Fe1 Cl2 116.01(12) . . ? C1 Fe1 Cl1 112.87(14) . . ? C20 Fe1 Cl1 107.07(12) . . ? Cl2 Fe1 Cl1 108.71(5) . . ? N2 C1 N1 104.8(4) . . ? N2 C1 Fe1 124.3(3) . . ? N1 C1 Fe1 130.4(4) . . ? C1 N1 C2 111.4(4) . . ? C1 N1 C21 125.7(4) . . ? C2 N1 C21 122.9(4) . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C2 C7 106.0(4) . . ? N1 C2 C3 131.9(5) . . ? C7 C2 C3 122.1(5) . . ? C4 C3 C2 117.1(5) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 121.7(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 121.4(5) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C5 116.7(5) . . ? C7 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? C6 C7 N2 132.5(5) . . ? C6 C7 C2 121.1(4) . . ? N2 C7 C2 106.4(4) . . ? C1 N2 C7 111.4(4) . . ? C1 N2 C8 123.9(4) . . ? C7 N2 C8 124.6(4) . . ? N2 C8 C9 114.3(3) . . ? N2 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N2 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 110.4(4) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N3 C10 C9 111.6(4) . . ? N3 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C11 N3 C22 110.1(3) . . ? C11 N3 C10 110.1(3) . . ? C22 N3 C10 110.3(3) . . ? N3 C22 C23 113.8(4) . . ? N3 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N3 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 117.5(4) . . ? C28 C23 C22 120.9(4) . . ? C24 C23 C22 121.6(4) . . ? C25 C24 C23 120.8(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120.6(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 118.9(5) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 120.8(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C23 121.4(4) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? N3 C11 C12 115.0(4) . . ? N3 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? N3 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C11 C12 C13 115.9(4) . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? C11 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? N4 C13 C12 113.7(4) . . ? N4 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? N4 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C20 N4 C14 111.3(3) . . ? C20 N4 C13 123.7(4) . . ? C14 N4 C13 125.0(3) . . ? C15 C14 N4 133.1(4) . . ? C15 C14 C19 120.8(4) . . ? N4 C14 C19 106.0(4) . . ? C16 C15 C14 117.2(4) . . ? C16 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C15 C16 C17 121.9(4) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 116.9(4) . . ? C17 C18 H18 121.5 . . ? C19 C18 H18 121.5 . . ? N5 C19 C18 132.0(4) . . ? N5 C19 C14 106.0(4) . . ? C18 C19 C14 122.0(4) . . ? C20 N5 C19 111.8(3) . . ? C20 N5 C29 124.0(4) . . ? C19 N5 C29 124.1(3) . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C20 N4 104.9(4) . . ? N5 C20 Fe1 121.9(3) . . ? N4 C20 Fe1 132.3(3) . . ? C120 Fe2 C101 108.40(17) . . ? C120 Fe2 Cl3 115.40(13) . . ? C101 Fe2 Cl3 106.06(12) . . ? C120 Fe2 Cl4 105.05(13) . . ? C101 Fe2 Cl4 108.35(12) . . ? Cl3 Fe2 Cl4 113.36(5) . . ? N102 C101 N101 104.8(4) . . ? N102 C101 Fe2 131.0(3) . . ? N101 C101 Fe2 124.2(3) . . ? C101 N101 C102 111.1(4) . . ? C101 N101 C121 123.5(4) . . ? C102 N101 C121 125.3(4) . . ? N101 C121 H12C 109.5 . . ? N101 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? N101 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C103 C102 N101 131.9(4) . . ? C103 C102 C107 121.4(5) . . ? N101 C102 C107 106.7(4) . . ? C102 C103 C104 117.0(5) . . ? C102 C103 H103 121.5 . . ? C104 C103 H103 121.5 . . ? C103 C104 C105 121.1(5) . . ? C103 C104 H104 119.5 . . ? C105 C104 H104 119.5 . . ? C106 C105 C104 121.6(5) . . ? C106 C105 H105 119.2 . . ? C104 C105 H105 119.2 . . ? C107 C106 C105 117.0(5) . . ? C107 C106 H106 121.5 . . ? C105 C106 H106 121.5 . . ? C106 C107 N102 132.6(5) . . ? C106 C107 C102 121.8(5) . . ? N102 C107 C102 105.5(4) . . ? C101 N102 C107 111.9(4) . . ? C101 N102 C108 124.2(4) . . ? C107 N102 C108 123.7(4) . . ? N102 C108 C109 111.7(3) . . ? N102 C108 H10C 109.3 . . ? C109 C108 H10C 109.3 . . ? N102 C108 H10D 109.3 . . ? C109 C108 H10D 109.3 . . ? H10C C108 H10D 107.9 . . ? C108 C109 C110 112.5(4) . . ? C108 C109 H10E 109.1 . . ? C110 C109 H10E 109.1 . . ? C108 C109 H10F 109.1 . . ? C110 C109 H10F 109.1 . . ? H10E C109 H10F 107.8 . . ? N103 C110 C109 114.9(4) . . ? N103 C110 H11C 108.5 . . ? C109 C110 H11C 108.5 . . ? N103 C110 H11D 108.5 . . ? C109 C110 H11D 108.5 . . ? H11C C110 H11D 107.5 . . ? C111 N103 C110 110.4(3) . . ? C111 N103 C122 108.7(3) . . ? C110 N103 C122 106.9(3) . . ? N103 C122 C23A 114.61(16) . . ? N103 C122 C123 113.77(16) . . ? C23A C122 C123 3.7 . . ? N103 C122 H12F 108.8 . . ? C23A C122 H12F 105.3 . . ? C123 C122 H12F 108.8 . . ? N103 C122 H12G 108.8 . . ? C23A C122 H12G 111.4 . . ? C123 C122 H12G 108.8 . . ? H12F C122 H12G 107.7 . . ? N103 C122 H12H 108.6 . . ? C23A C122 H12H 108.6 . . ? C123 C122 H12H 112.1 . . ? H12F C122 H12H 3.9 . . ? H12G C122 H12H 104.3 . . ? N103 C122 H12I 108.6 . . ? C23A C122 H12I 108.6 . . ? C123 C122 H12I 105.9 . . ? H12F C122 H12I 110.9 . . ? H12G C122 H12I 3.6 . . ? H12H C122 H12I 107.6 . . ? C124 C123 C128 120.0 . . ? C124 C123 C122 123.1 . . ? C128 C123 C122 116.5 . . ? C125 C124 C123 120.0 . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C124 C125 C126 120.0 . . ? C124 C125 H125 120.0 . . ? C126 C125 H125 120.0 . . ? C127 C126 C125 120.0 . . ? C127 C126 H126 120.0 . . ? C125 C126 H126 120.0 . . ? C128 C127 C126 120.0 . . ? C128 C127 H127 120.0 . . ? C126 C127 H127 120.0 . . ? C127 C128 C123 120.0 . . ? C127 C128 H128 120.0 . . ? C123 C128 H128 120.0 . . ? C24A C23A C28A 120.0 . . ? C24A C23A C122 118.3 . . ? C28A C23A C122 121.3 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C27A C28A C23A 120.0 . . ? C27A C28A H28A 120.0 . . ? C23A C28A H28A 120.0 . . ? N103 C111 C112 115.8(3) . . ? N103 C111 H11E 108.3 . . ? C112 C111 H11E 108.3 . . ? N103 C111 H11F 108.3 . . ? C112 C111 H11F 108.3 . . ? H11E C111 H11F 107.4 . . ? C111 C112 C113 115.6(4) . . ? C111 C112 H11G 108.4 . . ? C113 C112 H11G 108.4 . . ? C111 C112 H11H 108.4 . . ? C113 C112 H11H 108.4 . . ? H11G C112 H11H 107.4 . . ? N104 C113 C112 114.3(4) . . ? N104 C113 H11I 108.7 . . ? C112 C113 H11I 108.7 . . ? N104 C113 H11J 108.7 . . ? C112 C113 H11J 108.7 . . ? H11I C113 H11J 107.6 . . ? C120 N104 C114 111.4(4) . . ? C120 N104 C113 124.3(4) . . ? C114 N104 C113 124.2(4) . . ? C119 C114 N104 106.5(4) . . ? C119 C114 C115 121.6(4) . . ? N104 C114 C115 131.9(4) . . ? C116 C115 C114 116.1(4) . . ? C116 C115 H115 121.9 . . ? C114 C115 H115 121.9 . . ? C115 C116 C117 122.4(4) . . ? C115 C116 H116 118.8 . . ? C117 C116 H116 118.8 . . ? C118 C117 C116 121.1(4) . . ? C118 C117 H117 119.5 . . ? C116 C117 H117 119.5 . . ? C119 C118 C117 116.8(4) . . ? C119 C118 H118 121.6 . . ? C117 C118 H118 121.6 . . ? C118 C119 C114 122.0(4) . . ? C118 C119 N105 132.0(4) . . ? C114 C119 N105 106.0(3) . . ? C120 N105 C119 111.9(3) . . ? C120 N105 C129 124.5(4) . . ? C119 N105 C129 123.6(3) . . ? N105 C129 H12J 109.5 . . ? N105 C129 H12K 109.5 . . ? H12J C129 H12K 109.5 . . ? N105 C129 H12L 109.5 . . ? H12J C129 H12L 109.5 . . ? H12K C129 H12L 109.5 . . ? N105 C120 N104 104.2(4) . . ? N105 C120 Fe2 123.2(3) . . ? N104 C120 Fe2 132.3(3) . . ? C2S C1S C6S 119.2(6) . . ? C2S C1S H1S 120.4 . . ? C6S C1S H1S 120.4 . . ? C3S C2S C1S 120.0(6) . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 119.4(6) . . ? C2S C3S H3S 120.3 . . ? C4S C3S H3S 120.3 . . ? C5S C4S C3S 121.0(6) . . ? C5S C4S H4S 119.5 . . ? C3S C4S H4S 119.5 . . ? C6S C5S C4S 120.1(6) . . ? C6S C5S H5S 119.9 . . ? C4S C5S H5S 119.9 . . ? C5S C6S C1S 120.2(6) . . ? C5S C6S H6S 119.9 . . ? C1S C6S H6S 119.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 55.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.769 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.078 data__Compound_{BnN(CH2CH2CH2-N-methylbenzimidazole-2-ylidene)2}FeBr2 _database_code_depnum_ccdc_archive 'CCDC 917785' #TrackingRef 'web_deposit_cif_file_0_NilayHazari_1360023780.XRay_SI.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H74 Br4 Fe2 N10' _chemical_formula_weight 1426.68 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' Br Br -0.2901 2.4595 '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 9.434(4) _cell_length_b 30.1020(7) _cell_length_c 23.0220(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.188(15) _cell_angle_gamma 90.00 _cell_volume 6414(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 82543 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.4 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 2.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5217 _exptl_absorpt_correction_T_max 0.7541 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; 'Rigaku R-AXIS RAPID, Rigaku R-AXIS RAPID imaging plate' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10 _diffrn_reflns_number 130163 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13093 _reflns_number_gt 9546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. All disorders were refined with the help of similarity restraints on the 1,2- and 1,3- distances and displacement parameters as well as rigid bond restraints for anisotropic displacement parameters. ; _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^)+(0.0385P)^2^+7.9132P] 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 13093 _refine_ls_number_parameters 798 _refine_ls_number_restraints 249 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.063 _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 0.74020(5) 0.029727(16) 0.22120(2) 0.03014(12) Uani 1 1 d . . . Br1 Br 0.49304(4) 0.032862(13) 0.232398(17) 0.04149(10) Uani 1 1 d . . . Br2 Br 0.75794(4) 0.078162(13) 0.138971(17) 0.04708(11) Uani 1 1 d . . . C1 C 0.9023(3) 0.05224(10) 0.29177(14) 0.0282(7) Uani 1 1 d . . . N1 N 1.0437(3) 0.05093(9) 0.28712(12) 0.0284(6) Uani 1 1 d . . . C21 C 1.0981(4) 0.02974(12) 0.23890(15) 0.0361(8) Uani 1 1 d . . . H21A H 1.0909 -0.0026 0.2423 0.054 Uiso 1 1 calc R . . H21B H 1.1994 0.0381 0.2410 0.054 Uiso 1 1 calc R . . H21C H 1.0407 0.0395 0.2009 0.054 Uiso 1 1 calc R . . C2 C 1.1295(3) 0.07362(10) 0.33325(14) 0.0295(7) Uani 1 1 d . . . C3 C 1.2782(4) 0.08179(11) 0.34569(16) 0.0351(8) Uani 1 1 d . . . H3 H 1.3409 0.0701 0.3218 0.042 Uiso 1 1 calc R . . C4 C 1.3285(4) 0.10779(12) 0.39447(16) 0.0393(9) Uani 1 1 d . . . H4 H 1.4291 0.1139 0.4048 0.047 Uiso 1 1 calc R . . C5 C 1.2367(4) 0.12537(12) 0.42912(16) 0.0401(9) Uani 1 1 d . . . H5 H 1.2758 0.1436 0.4621 0.048 Uiso 1 1 calc R . . C6 C 1.0891(4) 0.11691(11) 0.41664(15) 0.0361(8) Uani 1 1 d . . . H6 H 1.0264 0.1290 0.4402 0.043 Uiso 1 1 calc R . . C7 C 1.0373(3) 0.09011(10) 0.36843(14) 0.0280(7) Uani 1 1 d . . . N2 N 0.8989(3) 0.07546(9) 0.34206(11) 0.0275(6) Uani 1 1 d . . . C8 C 0.7668(3) 0.08393(11) 0.36536(15) 0.0302(7) Uani 1 1 d . . . H8A H 0.6855 0.0678 0.3405 0.036 Uiso 1 1 calc R . . H8B H 0.7444 0.1161 0.3618 0.036 Uiso 1 1 calc R . . C9 C 0.7765(4) 0.07003(11) 0.42965(15) 0.0328(8) Uani 1 1 d . . . H9A H 0.6794 0.0731 0.4396 0.039 Uiso 1 1 calc R . . H9B H 0.8416 0.0910 0.4551 0.039 Uiso 1 1 calc R . . C10 C 0.8303(4) 0.02292(11) 0.44524(16) 0.0344(8) Uani 1 1 d . . . H10A H 0.9239 0.0188 0.4325 0.041 Uiso 1 1 calc R . . H10B H 0.8478 0.0194 0.4888 0.041 Uiso 1 1 calc R . . N3 N 0.7306(3) -0.01189(9) 0.41815(13) 0.0318(6) Uani 1 1 d . . . C11 C 0.8093(4) -0.05438(11) 0.41769(16) 0.0362(8) Uani 1 1 d . . . H11A H 0.7418 -0.0794 0.4191 0.043 Uiso 1 1 calc R . . H11B H 0.8867 -0.0561 0.4534 0.043 Uiso 1 1 calc R . . C12 C 0.8753(4) -0.05883(12) 0.36297(15) 0.0345(8) Uani 1 1 d . . . H12A H 0.9381 -0.0854 0.3667 0.041 Uiso 1 1 calc R . . H12B H 0.9358 -0.0325 0.3593 0.041 Uiso 1 1 calc R . . C13 C 0.7572(4) -0.06293(12) 0.30796(15) 0.0340(8) Uani 1 1 d . . . H13A H 0.6955 -0.0888 0.3128 0.041 Uiso 1 1 calc R . . H13B H 0.6957 -0.0360 0.3046 0.041 Uiso 1 1 calc R . . N4 N 0.8111(3) -0.06832(9) 0.25325(12) 0.0328(6) Uani 1 1 d . . . C14 C 0.8728(3) -0.10739(11) 0.23749(16) 0.0349(8) Uani 1 1 d . . . C15 C 0.9007(4) -0.14830(12) 0.26532(18) 0.0431(9) Uani 1 1 d . . . H15 H 0.8767 -0.1542 0.3028 0.052 Uiso 1 1 calc R . . C16 C 0.9654(4) -0.18001(13) 0.2354(2) 0.0512(11) Uani 1 1 d . . . H16 H 0.9862 -0.2085 0.2529 0.061 Uiso 1 1 calc R . . C17 C 1.0004(4) -0.17139(14) 0.1809(2) 0.0561(12) Uani 1 1 d . . . H17 H 1.0455 -0.1940 0.1621 0.067 Uiso 1 1 calc R . . C18 C 0.9719(4) -0.13103(14) 0.15317(19) 0.0526(11) Uani 1 1 d . . . H18 H 0.9955 -0.1253 0.1156 0.063 Uiso 1 1 calc R . . C19 C 0.9069(4) -0.09908(12) 0.18274(17) 0.0406(9) Uani 1 1 d . . . N5 N 0.8619(3) -0.05589(10) 0.16752(13) 0.0403(7) Uani 1 1 d . . . C29 C 0.8715(6) -0.03558(15) 0.11079(18) 0.0613(12) Uani 1 1 d . . . H29A H 0.8279 -0.0059 0.1084 0.092 Uiso 1 1 calc R . . H29B H 0.8198 -0.0541 0.0785 0.092 Uiso 1 1 calc R . . H29C H 0.9732 -0.0331 0.1074 0.092 Uiso 1 1 calc R . . C20 C 0.8048(4) -0.03643(11) 0.21106(15) 0.0333(8) Uani 1 1 d . . . C22 C 0.6105(4) -0.01698(12) 0.44995(17) 0.0401(9) Uani 1 1 d . . . H22A H 0.5730 0.0128 0.4573 0.048 Uiso 1 1 calc R . . H22B H 0.6471 -0.0311 0.4888 0.048 Uiso 1 1 calc R . . C23 C 0.4884(4) -0.04475(11) 0.41609(17) 0.0366(8) Uani 1 1 d . . . C24 C 0.4302(4) -0.07999(12) 0.44182(17) 0.0412(9) Uani 1 1 d . . . H24 H 0.4690 -0.0878 0.4817 0.049 Uiso 1 1 calc R . . C25 C 0.3161(4) -0.10410(13) 0.4103(2) 0.0507(10) Uani 1 1 d . . . H25 H 0.2755 -0.1277 0.4291 0.061 Uiso 1 1 calc R . . C26 C 0.2607(4) -0.09430(14) 0.3521(2) 0.0520(11) Uani 1 1 d . . . H26 H 0.1825 -0.1110 0.3305 0.062 Uiso 1 1 calc R . . C27 C 0.3199(4) -0.06000(14) 0.3254(2) 0.0543(11) Uani 1 1 d . . . H27 H 0.2839 -0.0535 0.2849 0.065 Uiso 1 1 calc R . . C28 C 0.4312(4) -0.03490(13) 0.35699(19) 0.0482(10) Uani 1 1 d . . . H28 H 0.4690 -0.0107 0.3383 0.058 Uiso 1 1 calc R . . Fe2 Fe 0.37355(5) 0.729784(16) 0.10458(2) 0.03089(12) Uani 1 1 d . . . Br3 Br 0.12876(4) 0.721221(14) 0.11813(2) 0.04983(12) Uani 1 1 d . . . Br4 Br 0.41942(4) 0.692064(14) 0.017202(17) 0.04987(12) Uani 1 1 d . . . C101 C 0.3999(4) 0.79906(11) 0.09486(15) 0.0346(8) Uani 1 1 d . . . N101 N 0.3532(3) 0.82348(10) 0.04487(13) 0.0422(8) Uani 1 1 d . . . C121 C 0.2842(6) 0.80551(14) -0.01221(18) 0.0655(14) Uani 1 1 d . . . H12C H 0.3578 0.7989 -0.0357 0.098 Uiso 1 1 calc R . . H12D H 0.2157 0.8273 -0.0332 0.098 Uiso 1 1 calc R . . H12E H 0.2325 0.7782 -0.0062 0.098 Uiso 1 1 calc R . . C102 C 0.3789(4) 0.86857(12) 0.05534(17) 0.0456(10) Uani 1 1 d . . . C103 C 0.3533(5) 0.90553(14) 0.01870(19) 0.0605(12) Uani 1 1 d . . . H103 H 0.3103 0.9029 -0.0220 0.073 Uiso 1 1 calc R . . C104 C 0.3931(6) 0.94620(14) 0.0441(2) 0.0660(13) Uani 1 1 d . . . H104 H 0.3773 0.9722 0.0204 0.079 Uiso 1 1 calc R . . C105 C 0.4562(5) 0.94988(14) 0.1038(2) 0.0632(13) Uani 1 1 d . . . H105 H 0.4815 0.9785 0.1200 0.076 Uiso 1 1 calc R . . C106 C 0.4829(5) 0.91340(13) 0.14010(18) 0.0505(10) Uani 1 1 d . . . H106 H 0.5262 0.9162 0.1808 0.061 Uiso 1 1 calc R . . C107 C 0.4436(4) 0.87210(12) 0.11451(16) 0.0394(9) Uani 1 1 d . . . C108 C 0.5152(4) 0.81823(12) 0.19879(15) 0.0356(8) Uani 1 1 d . . . H10C H 0.6011 0.8370 0.2131 0.043 Uiso 1 1 calc R . . H10D H 0.5465 0.7868 0.2016 0.043 Uiso 1 1 calc R . . N102 N 0.4560(3) 0.82908(9) 0.13689(12) 0.0337(7) Uani 1 1 d . . . C109 C 0.4054(5) 0.82553(14) 0.23797(17) 0.0504(10) Uani 1 1 d . . . H10E H 0.3183 0.8075 0.2230 0.061 Uiso 1 1 calc R . . H10F H 0.3762 0.8572 0.2361 0.061 Uiso 1 1 calc R . . C110 C 0.4660(5) 0.81293(14) 0.30208(17) 0.0529(11) Uani 1 1 d . . . H11C H 0.5553 0.8303 0.3160 0.063 Uiso 1 1 calc R . . H11D H 0.3952 0.8216 0.3266 0.063 Uiso 1 1 calc R . . N103 N 0.4995(3) 0.76542(10) 0.31169(13) 0.0371(7) Uani 1 1 d . . . C111 C 0.3650(4) 0.73887(15) 0.30315(19) 0.0500(10) Uani 1 1 d . . . H11E H 0.3030 0.7477 0.2651 0.060 Uiso 1 1 calc R . . H11F H 0.3125 0.7464 0.3351 0.060 Uiso 1 1 calc R . . C112 C 0.3868(4) 0.68892(14) 0.30283(18) 0.0473(10) Uani 1 1 d . . . H11G H 0.4759 0.6817 0.3318 0.057 Uiso 1 1 calc R . . H11H H 0.3051 0.6747 0.3170 0.057 Uiso 1 1 calc R . . C113 C 0.3985(4) 0.66805(13) 0.24411(16) 0.0393(9) Uani 1 1 d . . . H11I H 0.3961 0.6353 0.2483 0.047 Uiso 1 1 calc R . . H11J H 0.3130 0.6768 0.2142 0.047 Uiso 1 1 calc R . . N104 N 0.5297(3) 0.68033(9) 0.22210(12) 0.0317(6) Uani 1 1 d . . . C114 C 0.6678(4) 0.66787(11) 0.25062(15) 0.0320(8) Uani 1 1 d . . . C115 C 0.7173(4) 0.64147(11) 0.29955(16) 0.0399(9) Uani 1 1 d . . . H115 H 0.6528 0.6280 0.3213 0.048 Uiso 1 1 calc R . . C116 C 0.8658(4) 0.63563(12) 0.31535(17) 0.0445(10) Uani 1 1 d . . . H116 H 0.9041 0.6180 0.3490 0.053 Uiso 1 1 calc R . . C117 C 0.9596(4) 0.65499(12) 0.28318(18) 0.0458(10) Uani 1 1 d . . . H117 H 1.0605 0.6502 0.2955 0.055 Uiso 1 1 calc R . . C118 C 0.9111(4) 0.68109(12) 0.23351(16) 0.0371(8) Uani 1 1 d . . . H118 H 0.9754 0.6940 0.2113 0.045 Uiso 1 1 calc R . . C119 C 0.7621(3) 0.68702(11) 0.21843(15) 0.0321(8) Uani 1 1 d . . . N105 N 0.6766(3) 0.70989(9) 0.17205(12) 0.0289(6) Uani 1 1 d . . . C129 C 0.7343(4) 0.73505(12) 0.12790(16) 0.0367(8) Uani 1 1 d . . . H12F H 0.6561 0.7421 0.0945 0.055 Uiso 1 1 calc R . . H12G H 0.8080 0.7173 0.1138 0.055 Uiso 1 1 calc R . . H12H H 0.7778 0.7627 0.1456 0.055 Uiso 1 1 calc R . . C120 C 0.5336(3) 0.70589(11) 0.17407(15) 0.0297(7) Uani 1 1 d . . . C122 C 0.5780(4) 0.76020(14) 0.37332(16) 0.0468(10) Uani 1 1 d . . . H12I H 0.5766 0.7284 0.3843 0.056 Uiso 1 1 calc R . . H12J H 0.5257 0.7769 0.3997 0.056 Uiso 1 1 calc R . . C123 C 0.7325(4) 0.77580(12) 0.38449(15) 0.0396(9) Uani 1 1 d . . . C124 C 0.8344(4) 0.75247(13) 0.36164(18) 0.0494(10) Uani 1 1 d . . . H124 H 0.8045 0.7284 0.3354 0.059 Uiso 1 1 calc R . . C125 C 0.9795(5) 0.76329(14) 0.3760(2) 0.0585(12) Uani 1 1 d . . . H125 H 1.0484 0.7466 0.3600 0.070 Uiso 1 1 calc R . . C126 C 1.0234(6) 0.79839(16) 0.4135(2) 0.0687(15) Uani 1 1 d . . . H126 H 1.1231 0.8055 0.4246 0.082 Uiso 1 1 calc R . . C127 C 0.9220(7) 0.82313(18) 0.4348(2) 0.0756(16) Uani 1 1 d . . . H127 H 0.9519 0.8480 0.4596 0.091 Uiso 1 1 calc R . . C128 C 0.7756(6) 0.81216(15) 0.42046(18) 0.0601(12) Uani 1 1 d . . . H128 H 0.7062 0.8295 0.4352 0.072 Uiso 1 1 calc R . . C7S C 0.1850(12) 0.1866(2) -0.0087(3) 0.108(3) Uani 0.892(11) 1 d PDU A 1 H7S1 H 0.0852 0.1968 -0.0218 0.162 Uiso 0.892(11) 1 calc PR A 1 H7S2 H 0.2345 0.1866 -0.0424 0.162 Uiso 0.892(11) 1 calc PR A 1 H7S3 H 0.2354 0.2066 0.0221 0.162 Uiso 0.892(11) 1 calc PR A 1 C1S C 0.1846(9) 0.1405(2) 0.0157(3) 0.0781(17) Uani 0.892(11) 1 d PDU A 1 C2S C 0.0620(8) 0.1171(3) 0.0127(3) 0.0753(17) Uani 0.892(11) 1 d PDU A 1 H2S H -0.0273 0.1304 -0.0049 0.090 Uiso 0.892(11) 1 calc PR A 1 C3S C 0.0621(8) 0.0730(3) 0.0350(3) 0.0814(18) Uani 0.892(11) 1 d PDU A 1 H3S H -0.0259 0.0569 0.0316 0.098 Uiso 0.892(11) 1 calc PR A 1 C4S C 0.1895(8) 0.0540(2) 0.0611(4) 0.0830(19) Uani 0.892(11) 1 d PDU A 1 H4S H 0.1911 0.0251 0.0778 0.100 Uiso 0.892(11) 1 calc PR A 1 C5S C 0.3164(8) 0.0773(3) 0.0631(3) 0.0856(19) Uani 0.892(11) 1 d PDU A 1 H5S H 0.4062 0.0638 0.0797 0.103 Uiso 0.892(11) 1 calc PR A 1 C6S C 0.3141(8) 0.1201(3) 0.0410(4) 0.0834(17) Uani 0.892(11) 1 d PDU A 1 H6S H 0.4023 0.1358 0.0432 0.100 Uiso 0.892(11) 1 calc PR A 1 C7T C 0.318(8) 0.1837(14) 0.004(2) 0.089(10) Uani 0.108(11) 1 d PDU A 2 H7T1 H 0.2745 0.1945 -0.0352 0.133 Uiso 0.108(11) 1 calc PR A 2 H7T2 H 0.4236 0.1826 0.0083 0.133 Uiso 0.108(11) 1 calc PR A 2 H7T3 H 0.2934 0.2038 0.0344 0.133 Uiso 0.108(11) 1 calc PR A 2 C1T C 0.263(5) 0.1383(15) 0.013(2) 0.084(5) Uani 0.108(11) 1 d PDU A 2 C2T C 0.117(5) 0.1310(18) 0.001(3) 0.082(5) Uani 0.108(11) 1 d PDU A 2 H2T H 0.0568 0.1479 -0.0292 0.098 Uiso 0.108(11) 1 calc PR A 2 C3T C 0.055(5) 0.099(2) 0.032(3) 0.084(5) Uani 0.108(11) 1 d PDU A 2 H3T H -0.0431 0.1013 0.0361 0.101 Uiso 0.108(11) 1 calc PR A 2 C4T C 0.139(6) 0.0637(19) 0.057(3) 0.084(5) Uani 0.108(11) 1 d PDU A 2 H4T H 0.1016 0.0348 0.0603 0.100 Uiso 0.108(11) 1 calc PR A 2 C5T C 0.283(6) 0.074(2) 0.077(3) 0.085(5) Uani 0.108(11) 1 d PDU A 2 H5T H 0.3393 0.0580 0.1089 0.102 Uiso 0.108(11) 1 calc PR A 2 C6T C 0.345(4) 0.109(2) 0.050(4) 0.083(5) Uani 0.108(11) 1 d PDU A 2 H6T H 0.4469 0.1120 0.0579 0.099 Uiso 0.108(11) 1 calc PR A 2 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 0.0324(3) 0.0323(3) 0.0255(3) -0.0018(2) 0.0052(2) -0.00346(19) Br1 0.0345(2) 0.0520(2) 0.0383(2) 0.00209(17) 0.00774(16) 0.00404(16) Br2 0.0566(2) 0.0526(2) 0.0306(2) 0.00697(17) 0.00481(17) -0.00859(18) C1 0.0353(18) 0.0253(17) 0.0246(17) 0.0015(13) 0.0073(14) -0.0019(13) N1 0.0265(14) 0.0333(15) 0.0264(15) -0.0011(12) 0.0075(11) -0.0017(11) C21 0.0342(19) 0.044(2) 0.032(2) -0.0071(16) 0.0102(15) -0.0011(15) C2 0.0314(18) 0.0299(17) 0.0264(18) 0.0038(14) 0.0035(14) -0.0031(13) C3 0.0305(18) 0.040(2) 0.036(2) 0.0043(16) 0.0093(15) -0.0009(14) C4 0.0314(19) 0.048(2) 0.037(2) 0.0048(17) 0.0026(16) -0.0114(16) C5 0.043(2) 0.045(2) 0.031(2) -0.0023(16) 0.0044(17) -0.0132(16) C6 0.044(2) 0.0369(19) 0.0293(19) -0.0016(15) 0.0112(16) -0.0074(15) C7 0.0326(17) 0.0290(17) 0.0233(17) 0.0034(13) 0.0076(14) -0.0041(13) N2 0.0285(14) 0.0324(15) 0.0224(14) 0.0008(11) 0.0068(11) -0.0050(11) C8 0.0280(17) 0.0315(18) 0.0322(19) 0.0005(14) 0.0086(14) -0.0001(13) C9 0.0346(18) 0.0361(19) 0.0293(19) -0.0026(15) 0.0103(15) -0.0046(14) C10 0.0317(18) 0.041(2) 0.0313(19) 0.0030(15) 0.0080(15) -0.0030(14) N3 0.0304(15) 0.0323(15) 0.0364(17) 0.0022(12) 0.0155(12) -0.0002(11) C11 0.042(2) 0.0346(19) 0.034(2) 0.0049(15) 0.0128(16) 0.0030(15) C12 0.0323(18) 0.0377(19) 0.033(2) 0.0003(15) 0.0066(15) 0.0066(14) C13 0.0355(19) 0.0356(19) 0.032(2) 0.0004(15) 0.0092(15) 0.0003(14) N4 0.0333(15) 0.0331(16) 0.0316(16) -0.0040(12) 0.0052(12) -0.0014(12) C14 0.0284(18) 0.0344(19) 0.040(2) -0.0110(16) 0.0019(15) 0.0000(14) C15 0.040(2) 0.040(2) 0.046(2) -0.0082(17) -0.0002(17) 0.0018(16) C16 0.049(2) 0.040(2) 0.057(3) -0.0103(19) -0.008(2) 0.0073(18) C17 0.052(3) 0.047(3) 0.065(3) -0.024(2) 0.000(2) 0.0107(19) C18 0.055(3) 0.057(3) 0.046(3) -0.024(2) 0.012(2) 0.000(2) C19 0.039(2) 0.041(2) 0.040(2) -0.0136(17) 0.0015(17) -0.0011(16) N5 0.0533(19) 0.0375(17) 0.0310(17) -0.0085(13) 0.0103(14) -0.0044(14) C29 0.096(4) 0.055(3) 0.040(3) -0.006(2) 0.029(2) 0.002(2) C20 0.0324(18) 0.0379(19) 0.0293(19) -0.0071(15) 0.0056(15) -0.0061(14) C22 0.047(2) 0.040(2) 0.040(2) -0.0026(17) 0.0240(18) -0.0070(16) C23 0.0375(19) 0.0334(19) 0.043(2) -0.0010(16) 0.0188(17) 0.0006(15) C24 0.052(2) 0.036(2) 0.038(2) 0.0004(16) 0.0174(18) -0.0037(17) C25 0.054(2) 0.038(2) 0.063(3) -0.001(2) 0.019(2) -0.0093(18) C26 0.034(2) 0.050(2) 0.070(3) -0.005(2) 0.007(2) 0.0062(17) C27 0.042(2) 0.059(3) 0.058(3) 0.010(2) 0.001(2) 0.010(2) C28 0.043(2) 0.048(2) 0.054(3) 0.0139(19) 0.0115(19) 0.0028(18) Fe2 0.0269(2) 0.0342(3) 0.0311(3) -0.0039(2) 0.0044(2) 0.00223(19) Br3 0.0303(2) 0.0530(2) 0.0680(3) -0.0010(2) 0.01398(18) 0.00122(16) Br4 0.0525(2) 0.0601(3) 0.0344(2) -0.01010(18) 0.00209(17) 0.02268(19) C101 0.0337(19) 0.0376(19) 0.0301(19) -0.0048(15) 0.0000(15) 0.0027(14) N101 0.058(2) 0.0366(17) 0.0270(17) -0.0018(13) -0.0048(14) 0.0041(14) C121 0.102(4) 0.049(3) 0.033(2) -0.0117(19) -0.017(2) 0.014(2) C102 0.061(3) 0.036(2) 0.036(2) -0.0006(17) -0.0001(18) 0.0029(18) C103 0.089(3) 0.050(3) 0.037(2) 0.005(2) -0.003(2) 0.008(2) C104 0.101(4) 0.038(2) 0.053(3) 0.007(2) 0.002(3) 0.008(2) C105 0.083(3) 0.036(2) 0.062(3) -0.002(2) -0.007(2) -0.007(2) C106 0.062(3) 0.039(2) 0.044(2) -0.0014(18) -0.008(2) -0.0020(19) C107 0.042(2) 0.038(2) 0.035(2) -0.0003(16) -0.0007(16) 0.0009(16) C108 0.0354(19) 0.0378(19) 0.0296(19) -0.0008(15) -0.0039(15) 0.0034(15) N102 0.0340(15) 0.0340(16) 0.0298(16) -0.0004(12) -0.0020(12) 0.0000(12) C109 0.057(3) 0.056(3) 0.039(2) -0.0004(19) 0.0106(19) 0.022(2) C110 0.070(3) 0.055(3) 0.034(2) -0.0067(19) 0.014(2) 0.017(2) N103 0.0407(17) 0.0430(18) 0.0272(16) -0.0030(13) 0.0060(13) 0.0024(13) C111 0.030(2) 0.079(3) 0.044(2) -0.011(2) 0.0164(18) 0.0050(18) C112 0.035(2) 0.068(3) 0.043(2) -0.001(2) 0.0167(17) -0.0152(18) C113 0.0331(19) 0.045(2) 0.040(2) -0.0019(17) 0.0076(16) -0.0136(15) N104 0.0310(15) 0.0320(15) 0.0314(16) -0.0013(12) 0.0045(12) -0.0027(11) C114 0.0340(18) 0.0283(17) 0.0318(19) -0.0049(14) 0.0013(15) -0.0014(14) C115 0.050(2) 0.0325(19) 0.037(2) 0.0001(16) 0.0070(17) -0.0065(16) C116 0.054(2) 0.035(2) 0.038(2) 0.0040(17) -0.0066(18) 0.0034(17) C117 0.039(2) 0.043(2) 0.048(2) -0.0045(18) -0.0084(18) 0.0073(17) C118 0.0312(19) 0.040(2) 0.040(2) -0.0021(16) 0.0063(16) 0.0040(15) C119 0.0313(18) 0.0307(18) 0.0320(19) -0.0052(14) 0.0006(15) 0.0014(14) N105 0.0258(14) 0.0325(15) 0.0291(15) 0.0010(12) 0.0068(12) 0.0015(11) C129 0.0279(18) 0.044(2) 0.040(2) 0.0067(16) 0.0101(15) 0.0000(15) C120 0.0296(18) 0.0302(17) 0.0294(19) -0.0020(14) 0.0064(14) -0.0027(13) C122 0.058(3) 0.054(2) 0.028(2) -0.0008(17) 0.0093(18) -0.0005(19) C123 0.054(2) 0.043(2) 0.0193(18) -0.0006(15) 0.0007(16) -0.0069(17) C124 0.054(3) 0.041(2) 0.049(3) -0.0073(18) -0.002(2) -0.0054(18) C125 0.050(3) 0.049(3) 0.072(3) 0.006(2) 0.001(2) -0.003(2) C126 0.067(3) 0.062(3) 0.062(3) 0.011(3) -0.024(3) -0.028(3) C127 0.105(4) 0.067(3) 0.045(3) -0.014(2) -0.008(3) -0.030(3) C128 0.088(3) 0.057(3) 0.034(2) -0.014(2) 0.009(2) -0.011(2) C7S 0.185(9) 0.074(4) 0.055(4) -0.009(3) 0.001(5) -0.005(4) C1S 0.115(5) 0.085(3) 0.035(3) -0.011(3) 0.015(3) 0.009(3) C2S 0.100(4) 0.095(4) 0.038(3) 0.006(3) 0.030(3) 0.024(3) C3S 0.094(4) 0.098(4) 0.061(4) 0.007(4) 0.036(3) 0.023(3) C4S 0.103(5) 0.090(4) 0.064(4) 0.009(3) 0.037(4) 0.032(3) C5S 0.099(4) 0.105(4) 0.061(4) 0.005(4) 0.034(3) 0.028(3) C6S 0.104(4) 0.100(4) 0.046(4) -0.006(3) 0.015(4) 0.008(3) C7T 0.13(2) 0.093(14) 0.05(2) -0.016(15) 0.02(2) 0.009(14) C1T 0.110(9) 0.098(9) 0.045(10) -0.005(8) 0.017(9) 0.012(8) C2T 0.107(8) 0.101(10) 0.041(10) 0.002(8) 0.021(10) 0.021(9) C3T 0.104(8) 0.099(10) 0.055(11) 0.006(10) 0.029(9) 0.028(8) C4T 0.099(8) 0.099(9) 0.059(9) 0.006(8) 0.031(9) 0.028(8) C5T 0.102(8) 0.099(9) 0.058(10) 0.000(8) 0.026(9) 0.026(8) C6T 0.101(9) 0.100(10) 0.050(10) -0.007(9) 0.022(9) 0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C20 2.109(3) . ? Fe1 C1 2.115(3) . ? Fe1 Br1 2.3969(12) . ? Fe1 Br2 2.4209(6) . ? C1 N2 1.358(4) . ? C1 N1 1.359(4) . ? N1 C2 1.384(4) . ? N1 C21 1.458(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C2 C7 1.390(5) . ? C2 C3 1.398(5) . ? C3 C4 1.376(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C7 1.382(5) . ? C6 H6 0.9500 . ? C7 N2 1.400(4) . ? N2 C8 1.472(4) . ? C8 C9 1.524(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.526(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.465(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N3 C22 1.471(4) . ? N3 C11 1.480(4) . ? C11 C12 1.516(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.521(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N4 1.456(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N4 C20 1.359(4) . ? N4 C14 1.391(4) . ? C14 C19 1.383(5) . ? C14 C15 1.390(5) . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 C17 1.384(6) . ? C16 H16 0.9500 . ? C17 C18 1.375(6) . ? C17 H17 0.9500 . ? C18 C19 1.388(5) . ? C18 H18 0.9500 . ? C19 N5 1.391(5) . ? N5 C20 1.359(4) . ? N5 C29 1.461(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C22 C23 1.511(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.380(5) . ? C23 C28 1.395(5) . ? C24 C25 1.382(5) . ? C24 H24 0.9500 . ? C25 C26 1.373(6) . ? C25 H25 0.9500 . ? C26 C27 1.373(6) . ? C26 H26 0.9500 . ? C27 C28 1.380(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? Fe2 C120 2.102(3) . ? Fe2 C101 2.117(4) . ? Fe2 Br3 2.4034(12) . ? Fe2 Br4 2.4210(6) . ? C101 N102 1.354(4) . ? C101 N101 1.365(4) . ? N101 C102 1.392(5) . ? N101 C121 1.453(5) . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C102 C107 1.384(5) . ? C102 C103 1.389(5) . ? C103 C104 1.377(6) . ? C103 H103 0.9500 . ? C104 C105 1.393(6) . ? C104 H104 0.9500 . ? C105 C106 1.373(6) . ? C105 H105 0.9500 . ? C106 C107 1.395(5) . ? C106 H106 0.9500 . ? C107 N102 1.390(4) . ? C108 N102 1.463(4) . ? C108 C109 1.515(5) . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.524(5) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 N103 1.472(5) . ? C110 H11C 0.9900 . ? C110 H11D 0.9900 . ? N103 C122 1.476(5) . ? N103 C111 1.480(5) . ? C111 C112 1.518(6) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 C113 1.514(5) . ? C112 H11G 0.9900 . ? C112 H11H 0.9900 . ? C113 N104 1.473(4) . ? C113 H11I 0.9900 . ? C113 H11J 0.9900 . ? N104 C120 1.354(4) . ? N104 C114 1.392(4) . ? C114 C115 1.384(5) . ? C114 C119 1.389(5) . ? C115 C116 1.389(5) . ? C115 H115 0.9500 . ? C116 C117 1.387(6) . ? C116 H116 0.9500 . ? C117 C118 1.389(5) . ? C117 H117 0.9500 . ? C118 C119 1.392(5) . ? C118 H118 0.9500 . ? C119 N105 1.390(4) . ? N105 C120 1.364(4) . ? N105 C129 1.455(4) . ? C129 H12F 0.9800 . ? C129 H12G 0.9800 . ? C129 H12H 0.9800 . ? C122 C123 1.505(5) . ? C122 H12I 0.9900 . ? C122 H12J 0.9900 . ? C123 C124 1.375(6) . ? C123 C128 1.385(5) . ? C124 C125 1.383(6) . ? C124 H124 0.9500 . ? C125 C126 1.377(6) . ? C125 H125 0.9500 . ? C126 C127 1.376(7) . ? C126 H126 0.9500 . ? C127 C128 1.396(7) . ? C127 H127 0.9500 . ? C128 H128 0.9500 . ? C7S C1S 1.499(9) . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C1S C2S 1.344(9) . ? C1S C6S 1.390(9) . ? C2S C3S 1.424(9) . ? C2S H2S 0.9500 . ? C3S C4S 1.362(8) . ? C3S H3S 0.9500 . ? C4S C5S 1.380(9) . ? C4S H4S 0.9500 . ? C5S C6S 1.383(9) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7T C1T 1.49(2) . ? C7T H7T1 0.9800 . ? C7T H7T2 0.9800 . ? C7T H7T3 0.9800 . ? C1T C6T 1.362(16) . ? C1T C2T 1.373(17) . ? C2T C3T 1.397(17) . ? C2T H2T 0.9500 . ? C3T C4T 1.383(17) . ? C3T H3T 0.9500 . ? C4T C5T 1.380(17) . ? C4T H4T 0.9500 . ? C5T C6T 1.399(17) . ? C5T H5T 0.9500 . ? C6T H6T 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Fe1 C1 101.90(13) . . ? C20 Fe1 Br1 110.93(9) . . ? C1 Fe1 Br1 118.58(9) . . ? C20 Fe1 Br2 114.63(10) . . ? C1 Fe1 Br2 104.96(9) . . ? Br1 Fe1 Br2 106.06(2) . . ? N2 C1 N1 105.5(3) . . ? N2 C1 Fe1 133.3(2) . . ? N1 C1 Fe1 120.3(2) . . ? C1 N1 C2 111.2(3) . . ? C1 N1 C21 124.7(3) . . ? C2 N1 C21 124.1(3) . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C2 C7 106.5(3) . . ? N1 C2 C3 131.2(3) . . ? C7 C2 C3 122.3(3) . . ? C4 C3 C2 116.2(3) . . ? C4 C3 H3 121.9 . . ? C2 C3 H3 121.9 . . ? C3 C4 C5 122.0(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.5(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C5 117.2(3) . . ? C7 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? C6 C7 C2 120.8(3) . . ? C6 C7 N2 133.4(3) . . ? C2 C7 N2 105.7(3) . . ? C1 N2 C7 110.9(3) . . ? C1 N2 C8 124.2(3) . . ? C7 N2 C8 124.9(3) . . ? N2 C8 C9 114.2(3) . . ? N2 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N2 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 116.0(3) . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N3 C10 C9 114.1(3) . . ? N3 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? N3 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 N3 C22 110.8(3) . . ? C10 N3 C11 109.8(3) . . ? C22 N3 C11 110.5(3) . . ? N3 C11 C12 111.7(3) . . ? N3 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N3 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 110.2(3) . . ? C11 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N4 C13 C12 114.0(3) . . ? N4 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? N4 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C20 N4 C14 111.9(3) . . ? C20 N4 C13 124.4(3) . . ? C14 N4 C13 123.6(3) . . ? C19 C14 C15 121.6(3) . . ? C19 C14 N4 105.5(3) . . ? C15 C14 N4 132.9(4) . . ? C16 C15 C14 116.3(4) . . ? C16 C15 H15 121.8 . . ? C14 C15 H15 121.8 . . ? C17 C16 C15 121.8(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C18 C17 C16 121.8(4) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 116.8(4) . . ? C17 C18 H18 121.6 . . ? C19 C18 H18 121.6 . . ? C14 C19 C18 121.7(4) . . ? C14 C19 N5 106.6(3) . . ? C18 C19 N5 131.8(4) . . ? C20 N5 C19 111.2(3) . . ? C20 N5 C29 125.5(3) . . ? C19 N5 C29 123.2(3) . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C20 N5 104.7(3) . . ? N4 C20 Fe1 124.2(2) . . ? N5 C20 Fe1 130.8(3) . . ? N3 C22 C23 112.6(3) . . ? N3 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N3 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C28 118.1(4) . . ? C24 C23 C22 122.1(3) . . ? C28 C23 C22 119.9(3) . . ? C23 C24 C25 120.8(4) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 120.7(4) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C23 120.6(4) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C120 Fe2 C101 109.61(13) . . ? C120 Fe2 Br3 115.53(10) . . ? C101 Fe2 Br3 104.77(10) . . ? C120 Fe2 Br4 104.72(9) . . ? C101 Fe2 Br4 109.30(10) . . ? Br3 Fe2 Br4 112.88(3) . . ? N102 C101 N101 105.1(3) . . ? N102 C101 Fe2 128.3(3) . . ? N101 C101 Fe2 126.5(2) . . ? C101 N101 C102 111.2(3) . . ? C101 N101 C121 125.2(3) . . ? C102 N101 C121 123.5(3) . . ? N101 C121 H12C 109.5 . . ? N101 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? N101 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C107 C102 C103 121.8(4) . . ? C107 C102 N101 105.9(3) . . ? C103 C102 N101 132.2(4) . . ? C104 C103 C102 117.0(4) . . ? C104 C103 H103 121.5 . . ? C102 C103 H103 121.5 . . ? C103 C104 C105 121.3(4) . . ? C103 C104 H104 119.4 . . ? C105 C104 H104 119.4 . . ? C106 C105 C104 122.0(4) . . ? C106 C105 H105 119.0 . . ? C104 C105 H105 119.0 . . ? C105 C106 C107 117.0(4) . . ? C105 C106 H106 121.5 . . ? C107 C106 H106 121.5 . . ? C102 C107 N102 106.4(3) . . ? C102 C107 C106 121.0(3) . . ? N102 C107 C106 132.6(3) . . ? N102 C108 C109 111.8(3) . . ? N102 C108 H10C 109.3 . . ? C109 C108 H10C 109.3 . . ? N102 C108 H10D 109.3 . . ? C109 C108 H10D 109.3 . . ? H10C C108 H10D 107.9 . . ? C101 N102 C107 111.3(3) . . ? C101 N102 C108 124.7(3) . . ? C107 N102 C108 123.9(3) . . ? C108 C109 C110 111.7(3) . . ? C108 C109 H10E 109.3 . . ? C110 C109 H10E 109.3 . . ? C108 C109 H10F 109.3 . . ? C110 C109 H10F 109.3 . . ? H10E C109 H10F 107.9 . . ? N103 C110 C109 114.6(3) . . ? N103 C110 H11C 108.6 . . ? C109 C110 H11C 108.6 . . ? N103 C110 H11D 108.6 . . ? C109 C110 H11D 108.6 . . ? H11C C110 H11D 107.6 . . ? C110 N103 C122 107.5(3) . . ? C110 N103 C111 110.6(3) . . ? C122 N103 C111 109.1(3) . . ? N103 C111 C112 115.0(3) . . ? N103 C111 H11E 108.5 . . ? C112 C111 H11E 108.5 . . ? N103 C111 H11F 108.5 . . ? C112 C111 H11F 108.5 . . ? H11E C111 H11F 107.5 . . ? C113 C112 C111 116.7(3) . . ? C113 C112 H11G 108.1 . . ? C111 C112 H11G 108.1 . . ? C113 C112 H11H 108.1 . . ? C111 C112 H11H 108.1 . . ? H11G C112 H11H 107.3 . . ? N104 C113 C112 114.5(3) . . ? N104 C113 H11I 108.6 . . ? C112 C113 H11I 108.6 . . ? N104 C113 H11J 108.6 . . ? C112 C113 H11J 108.6 . . ? H11I C113 H11J 107.6 . . ? C120 N104 C114 111.6(3) . . ? C120 N104 C113 125.6(3) . . ? C114 N104 C113 122.8(3) . . ? C115 C114 C119 121.5(3) . . ? C115 C114 N104 132.5(3) . . ? C119 C114 N104 105.9(3) . . ? C114 C115 C116 116.7(4) . . ? C114 C115 H115 121.6 . . ? C116 C115 H115 121.6 . . ? C117 C116 C115 121.5(4) . . ? C117 C116 H116 119.3 . . ? C115 C116 H116 119.3 . . ? C116 C117 C118 122.3(4) . . ? C116 C117 H117 118.8 . . ? C118 C117 H117 118.8 . . ? C117 C118 C119 115.6(4) . . ? C117 C118 H118 122.2 . . ? C119 C118 H118 122.2 . . ? C114 C119 N105 106.2(3) . . ? C114 C119 C118 122.3(3) . . ? N105 C119 C118 131.5(3) . . ? C120 N105 C119 111.2(3) . . ? C120 N105 C129 125.2(3) . . ? C119 N105 C129 123.6(3) . . ? N105 C129 H12F 109.5 . . ? N105 C129 H12G 109.5 . . ? H12F C129 H12G 109.5 . . ? N105 C129 H12H 109.5 . . ? H12F C129 H12H 109.5 . . ? H12G C129 H12H 109.5 . . ? N104 C120 N105 105.2(3) . . ? N104 C120 Fe2 133.4(2) . . ? N105 C120 Fe2 120.9(2) . . ? N103 C122 C123 114.8(3) . . ? N103 C122 H12I 108.6 . . ? C123 C122 H12I 108.6 . . ? N103 C122 H12J 108.6 . . ? C123 C122 H12J 108.6 . . ? H12I C122 H12J 107.5 . . ? C124 C123 C128 119.1(4) . . ? C124 C123 C122 120.1(3) . . ? C128 C123 C122 120.7(4) . . ? C123 C124 C125 121.4(4) . . ? C123 C124 H124 119.3 . . ? C125 C124 H124 119.3 . . ? C126 C125 C124 119.6(5) . . ? C126 C125 H125 120.2 . . ? C124 C125 H125 120.2 . . ? C127 C126 C125 119.6(5) . . ? C127 C126 H126 120.2 . . ? C125 C126 H126 120.2 . . ? C126 C127 C128 120.8(4) . . ? C126 C127 H127 119.6 . . ? C128 C127 H127 119.6 . . ? C123 C128 C127 119.4(5) . . ? C123 C128 H128 120.3 . . ? C127 C128 H128 120.3 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C2S C1S C6S 117.9(7) . . ? C2S C1S C7S 122.0(7) . . ? C6S C1S C7S 120.1(7) . . ? C1S C2S C3S 122.0(6) . . ? C1S C2S H2S 119.0 . . ? C3S C2S H2S 119.0 . . ? C4S C3S C2S 119.3(7) . . ? C4S C3S H3S 120.4 . . ? C2S C3S H3S 120.4 . . ? C3S C4S C5S 119.2(7) . . ? C3S C4S H4S 120.4 . . ? C5S C4S H4S 120.4 . . ? C4S C5S C6S 120.6(7) . . ? C4S C5S H5S 119.7 . . ? C6S C5S H5S 119.7 . . ? C5S C6S C1S 121.0(7) . . ? C5S C6S H6S 119.5 . . ? C1S C6S H6S 119.5 . . ? C1T C7T H7T1 109.5 . . ? C1T C7T H7T2 109.5 . . ? H7T1 C7T H7T2 109.5 . . ? C1T C7T H7T3 109.5 . . ? H7T1 C7T H7T3 109.5 . . ? H7T2 C7T H7T3 109.5 . . ? C6T C1T C2T 117(2) . . ? C6T C1T C7T 121(2) . . ? C2T C1T C7T 119(2) . . ? C1T C2T C3T 120(2) . . ? C1T C2T H2T 119.8 . . ? C3T C2T H2T 119.8 . . ? C4T C3T C2T 119(3) . . ? C4T C3T H3T 120.6 . . ? C2T C3T H3T 120.6 . . ? C5T C4T C3T 114(3) . . ? C5T C4T H4T 122.8 . . ? C3T C4T H4T 122.8 . . ? C4T C5T C6T 119(2) . . ? C4T C5T H5T 120.4 . . ? C6T C5T H5T 120.4 . . ? C1T C6T C5T 122(2) . . ? C1T C6T H6T 119.0 . . ? C5T C6T H6T 119.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.082 #============================================================================== # End of CIF #==============================================================================