# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wen Hua Sun' _publ_contact_author_email whsun@iccas.ac.cn _publ_section_title ; Access to highly active and thermally stable iron procatalysts using bulky 2-[1-(2,6-dibenzhydryl-4-methylphenylimino)ethyl]-6-[1-(arylimino)ethyl]pyridine ligands ; loop_ _publ_author_name 'Jiangang Yu' 'Wenjuan Zhang' 'Hao Liu' 'Xiang Hao' 'Wen Hua Sun' # Attachment 'CIF-for-chem.-commun.CIF' #TrackingRef 'CIF-for-chem.-commun.CIF' data_Fe1 _database_code_depnum_ccdc_archive 'CCDC 798843' #TrackingRef 'CIF-for-chem.-commun.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H45 Cl2 Fe N3' _chemical_formula_weight 814.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.851(2) _cell_length_b 11.505(2) _cell_length_c 20.416(4) _cell_angle_alpha 75.61(3) _cell_angle_beta 77.34(3) _cell_angle_gamma 72.54(3) _cell_volume 2111.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9073 _exptl_absorpt_correction_T_max 0.9615 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 26053 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9299 _reflns_number_gt 8408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+2.0869P] 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 9299 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0787 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1775 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.63303(4) 0.51564(4) 0.15473(2) 0.02180(13) Uani 1 1 d . . . N1 N 0.5040(3) 0.4398(2) 0.25411(13) 0.0209(5) Uani 1 1 d . . . Cl2 Cl 0.64636(10) 0.36301(8) 0.09491(4) 0.0339(2) Uani 1 1 d . . . N2 N 0.4152(3) 0.5989(2) 0.14720(13) 0.0219(5) Uani 1 1 d . . . Cl1 Cl 0.83650(9) 0.50969(10) 0.19133(5) 0.0390(2) Uani 1 1 d . . . N3 N 0.6247(3) 0.6781(2) 0.06732(13) 0.0225(5) Uani 1 1 d . . . C22 C 0.6672(3) 0.5845(3) 0.39175(16) 0.0252(6) Uani 1 1 d . . . C14 C 0.5903(3) 0.2302(3) 0.31821(16) 0.0249(6) Uani 1 1 d . . . C35 C 0.3667(3) 0.4696(3) 0.25573(16) 0.0221(6) Uani 1 1 d . . . C37 C 0.1737(3) 0.5812(3) 0.18006(17) 0.0262(7) Uani 1 1 d . . . H37A H 0.1031 0.5476 0.2124 0.031 Uiso 1 1 calc R . . C7 C 0.5612(4) 0.1765(3) 0.26253(16) 0.0260(7) Uani 1 1 d . . . H7A H 0.5708 0.2389 0.2191 0.031 Uiso 1 1 calc R . . C40 C 0.3809(3) 0.6779(3) 0.08937(16) 0.0230(6) Uani 1 1 d . . . C19 C 0.5638(3) 0.3578(3) 0.31254(15) 0.0222(6) Uani 1 1 d . . . C28 C 0.4286(3) 0.6256(3) 0.35283(17) 0.0265(7) Uani 1 1 d . . . C43 C 0.7431(3) 0.7307(3) 0.03343(16) 0.0247(6) Uani 1 1 d . . . C1 C 0.4082(4) 0.1631(3) 0.27422(18) 0.0318(7) Uani 1 1 d . . . C36 C 0.3136(3) 0.5526(3) 0.19256(15) 0.0215(6) Uani 1 1 d . . . C42 C 0.5014(3) 0.7269(3) 0.04678(16) 0.0230(6) Uani 1 1 d . . . C8 C 0.6794(4) 0.0592(3) 0.25150(17) 0.0290(7) Uani 1 1 d . . . C18 C 0.6003(3) 0.4078(3) 0.36086(16) 0.0228(6) Uani 1 1 d . . . C33 C 0.3285(4) 0.6015(3) 0.41040(19) 0.0312(7) Uani 1 1 d . . . H33A H 0.3549 0.5314 0.4456 0.037 Uiso 1 1 calc R . . C48 C 0.8383(4) 0.6817(3) -0.02053(17) 0.0271(7) Uani 1 1 d . . . C38 C 0.1391(3) 0.6600(3) 0.11947(18) 0.0307(7) Uani 1 1 d . . . H38A H 0.0442 0.6796 0.1092 0.037 Uiso 1 1 calc R . . C17 C 0.6552(4) 0.3258(3) 0.41704(16) 0.0274(7) Uani 1 1 d . . . H17A H 0.6767 0.3580 0.4510 0.033 Uiso 1 1 calc R . . C39 C 0.2422(3) 0.7103(3) 0.07382(17) 0.0280(7) Uani 1 1 d . . . H39A H 0.2188 0.7660 0.0325 0.034 Uiso 1 1 calc R . . C21 C 0.5841(3) 0.5484(3) 0.34789(16) 0.0226(6) Uani 1 1 d . . . H21A H 0.6294 0.5718 0.2993 0.027 Uiso 1 1 calc R . . C15 C 0.6490(4) 0.1514(3) 0.37494(17) 0.0303(7) Uani 1 1 d . . . H15A H 0.6683 0.0640 0.3793 0.036 Uiso 1 1 calc R . . C41 C 0.4711(4) 0.8302(3) -0.01326(18) 0.0319(7) Uani 1 1 d . . . H41A H 0.5606 0.8526 -0.0363 0.048 Uiso 1 1 calc R . . H41B H 0.4013 0.9026 0.0024 0.048 Uiso 1 1 calc R . . H41C H 0.4313 0.8034 -0.0453 0.048 Uiso 1 1 calc R . . C34 C 0.2556(3) 0.4369(3) 0.31436(16) 0.0282(7) Uani 1 1 d . . . H34A H 0.3031 0.3825 0.3526 0.042 Uiso 1 1 calc R . . H34B H 0.1982 0.3938 0.3002 0.042 Uiso 1 1 calc R . . H34C H 0.1926 0.5129 0.3289 0.042 Uiso 1 1 calc R . . C47 C 0.9520(4) 0.7350(3) -0.05184(18) 0.0324(7) Uani 1 1 d . . . H47A H 1.0192 0.7025 -0.0882 0.039 Uiso 1 1 calc R . . C6 C 0.3366(4) 0.1211(3) 0.3387(2) 0.0380(8) Uani 1 1 d . . . H6A H 0.3861 0.0949 0.3770 0.046 Uiso 1 1 calc R . . C44 C 0.7600(4) 0.8289(3) 0.05684(17) 0.0275(7) Uani 1 1 d . . . C16 C 0.6797(4) 0.1980(3) 0.42510(17) 0.0299(7) Uani 1 1 d . . . C46 C 0.9681(4) 0.8347(3) -0.03069(18) 0.0338(8) Uani 1 1 d . . . H46A H 1.0441 0.8720 -0.0536 0.041 Uiso 1 1 calc R . . C25 C 0.8261(4) 0.6540(4) 0.4665(2) 0.0410(9) Uani 1 1 d . . . H25A H 0.8801 0.6774 0.4919 0.049 Uiso 1 1 calc R . . C23 C 0.6023(4) 0.6724(3) 0.43231(18) 0.0307(7) Uani 1 1 d . . . H23A H 0.5018 0.7104 0.4346 0.037 Uiso 1 1 calc R . . C27 C 0.8164(4) 0.5323(3) 0.38808(18) 0.0305(7) Uani 1 1 d . . . H27A H 0.8644 0.4735 0.3596 0.037 Uiso 1 1 calc R . . C13 C 0.8118(4) 0.0735(3) 0.21390(19) 0.0354(8) Uani 1 1 d . . . H13A H 0.8227 0.1543 0.1929 0.043 Uiso 1 1 calc R . . C45 C 0.8740(4) 0.8804(3) 0.02381(18) 0.0343(8) Uani 1 1 d . . . H45A H 0.8875 0.9474 0.0388 0.041 Uiso 1 1 calc R . . C29 C 0.3874(4) 0.7277(3) 0.30161(19) 0.0366(8) Uani 1 1 d . . . H29A H 0.4548 0.7460 0.2620 0.044 Uiso 1 1 calc R . . C26 C 0.8937(4) 0.5663(4) 0.42568(19) 0.0356(8) Uani 1 1 d . . . H26A H 0.9943 0.5293 0.4236 0.043 Uiso 1 1 calc R . . C2 C 0.3333(5) 0.1990(4) 0.2192(2) 0.0431(9) Uani 1 1 d . . . H2A H 0.3805 0.2262 0.1747 0.052 Uiso 1 1 calc R . . C9 C 0.6651(4) -0.0594(3) 0.28045(18) 0.0368(8) Uani 1 1 d . . . H9A H 0.5750 -0.0709 0.3053 0.044 Uiso 1 1 calc R . . C10 C 0.7820(5) -0.1619(3) 0.2734(2) 0.0451(10) Uani 1 1 d . . . H10A H 0.7718 -0.2431 0.2941 0.054 Uiso 1 1 calc R . . C24 C 0.6810(4) 0.7065(4) 0.4698(2) 0.0370(8) Uani 1 1 d . . . H24A H 0.6339 0.7662 0.4978 0.044 Uiso 1 1 calc R . . C31 C 0.1493(4) 0.7791(4) 0.3658(2) 0.0502(11) Uani 1 1 d . . . H31A H 0.0540 0.8313 0.3703 0.060 Uiso 1 1 calc R . . C49 C 0.6586(4) 0.8758(3) 0.11713(19) 0.0369(8) Uani 1 1 d . . . H49A H 0.5854 0.8289 0.1333 0.055 Uiso 1 1 calc R . . H49B H 0.6116 0.9641 0.1032 0.055 Uiso 1 1 calc R . . H49C H 0.7129 0.8648 0.1541 0.055 Uiso 1 1 calc R . . C20 C 0.7421(5) 0.1102(3) 0.48606(19) 0.0433(9) Uani 1 1 d . . . H20A H 0.7572 0.1582 0.5161 0.065 Uiso 1 1 calc R . . H20B H 0.8345 0.0551 0.4702 0.065 Uiso 1 1 calc R . . H20C H 0.6752 0.0604 0.5114 0.065 Uiso 1 1 calc R . . C12 C 0.9270(5) -0.0285(4) 0.2069(2) 0.0444(9) Uani 1 1 d . . . H12A H 1.0169 -0.0176 0.1815 0.053 Uiso 1 1 calc R . . C50 C 0.8191(4) 0.5761(3) -0.0452(2) 0.0384(8) Uani 1 1 d . . . H50A H 0.8961 0.5551 -0.0831 0.058 Uiso 1 1 calc R . . H50B H 0.7255 0.6006 -0.0609 0.058 Uiso 1 1 calc R . . H50C H 0.8230 0.5037 -0.0076 0.058 Uiso 1 1 calc R . . C32 C 0.1908(4) 0.6788(4) 0.4167(2) 0.0408(9) Uani 1 1 d . . . H32A H 0.1238 0.6625 0.4569 0.049 Uiso 1 1 calc R . . C30 C 0.2465(5) 0.8034(4) 0.3084(2) 0.0508(11) Uani 1 1 d . . . H30A H 0.2180 0.8722 0.2728 0.061 Uiso 1 1 calc R . . C11 C 0.9120(5) -0.1464(4) 0.2367(2) 0.0467(10) Uani 1 1 d . . . H11A H 0.9914 -0.2167 0.2318 0.056 Uiso 1 1 calc R . . C5 C 0.1945(5) 0.1170(4) 0.3476(2) 0.0496(10) Uani 1 1 d . . . H5A H 0.1474 0.0875 0.3918 0.060 Uiso 1 1 calc R . . C4 C 0.1211(5) 0.1557(4) 0.2921(3) 0.0556(12) Uani 1 1 d . . . H4A H 0.0230 0.1546 0.2984 0.067 Uiso 1 1 calc R . . C3 C 0.1903(5) 0.1957(5) 0.2283(2) 0.0554(12) Uani 1 1 d . . . H3A H 0.1405 0.2212 0.1901 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0180(2) 0.0228(2) 0.0239(3) -0.00296(17) -0.00545(17) -0.00395(16) N1 0.0248(13) 0.0183(11) 0.0204(13) -0.0047(9) -0.0044(10) -0.0055(10) Cl2 0.0437(5) 0.0298(4) 0.0293(4) -0.0099(3) -0.0008(4) -0.0113(3) N2 0.0201(12) 0.0254(13) 0.0221(13) -0.0065(10) -0.0043(10) -0.0063(10) Cl1 0.0222(4) 0.0642(6) 0.0334(5) -0.0079(4) -0.0074(3) -0.0144(4) N3 0.0219(13) 0.0216(12) 0.0245(13) -0.0046(10) -0.0048(10) -0.0054(10) C22 0.0265(16) 0.0265(15) 0.0253(16) -0.0066(12) -0.0037(13) -0.0098(12) C14 0.0243(15) 0.0240(15) 0.0251(16) -0.0042(12) -0.0034(13) -0.0050(12) C35 0.0219(15) 0.0224(14) 0.0246(16) -0.0078(11) -0.0045(12) -0.0063(11) C37 0.0205(15) 0.0309(16) 0.0284(17) -0.0097(13) -0.0022(13) -0.0060(12) C7 0.0361(18) 0.0231(15) 0.0204(15) -0.0016(11) -0.0085(13) -0.0092(13) C40 0.0224(15) 0.0245(14) 0.0229(16) -0.0065(12) -0.0072(12) -0.0031(11) C19 0.0214(15) 0.0238(14) 0.0212(15) -0.0027(11) -0.0037(12) -0.0066(11) C28 0.0276(16) 0.0260(15) 0.0304(17) -0.0112(13) -0.0067(13) -0.0073(13) C43 0.0217(15) 0.0241(15) 0.0276(17) 0.0001(12) -0.0084(12) -0.0062(12) C1 0.0388(19) 0.0255(16) 0.0339(19) -0.0072(13) -0.0106(15) -0.0078(14) C36 0.0213(15) 0.0229(14) 0.0219(15) -0.0070(11) -0.0046(12) -0.0052(11) C42 0.0256(16) 0.0231(14) 0.0215(15) -0.0071(12) -0.0046(12) -0.0052(12) C8 0.0401(19) 0.0247(15) 0.0236(16) -0.0069(12) -0.0116(14) -0.0039(13) C18 0.0210(15) 0.0249(15) 0.0219(15) -0.0053(12) -0.0017(12) -0.0057(12) C33 0.0270(17) 0.0323(17) 0.039(2) -0.0123(14) -0.0103(14) -0.0060(13) C48 0.0285(17) 0.0267(15) 0.0255(17) -0.0035(12) -0.0040(13) -0.0079(13) C38 0.0185(15) 0.0356(18) 0.0375(19) -0.0098(14) -0.0088(14) -0.0010(13) C17 0.0305(17) 0.0310(16) 0.0219(16) -0.0073(12) -0.0060(13) -0.0064(13) C39 0.0257(16) 0.0301(16) 0.0268(17) -0.0030(13) -0.0095(13) -0.0036(13) C21 0.0234(15) 0.0247(15) 0.0212(15) -0.0073(12) -0.0032(12) -0.0064(12) C15 0.0375(19) 0.0241(15) 0.0289(18) -0.0039(13) -0.0088(14) -0.0058(13) C41 0.0327(18) 0.0303(17) 0.0321(18) 0.0044(13) -0.0116(14) -0.0110(14) C34 0.0254(16) 0.0337(17) 0.0256(17) -0.0046(13) -0.0021(13) -0.0099(13) C47 0.0265(17) 0.0359(18) 0.0305(18) 0.0006(14) -0.0029(14) -0.0089(14) C6 0.043(2) 0.0355(19) 0.038(2) 0.0026(15) -0.0169(17) -0.0143(16) C44 0.0293(17) 0.0251(15) 0.0295(17) -0.0022(12) -0.0113(14) -0.0068(13) C16 0.0324(18) 0.0289(16) 0.0271(17) -0.0050(13) -0.0085(14) -0.0039(13) C46 0.0277(17) 0.0383(19) 0.035(2) 0.0077(15) -0.0103(15) -0.0171(14) C25 0.039(2) 0.055(2) 0.041(2) -0.0191(18) -0.0048(17) -0.0226(18) C23 0.0274(17) 0.0352(18) 0.0333(19) -0.0137(14) -0.0037(14) -0.0087(14) C27 0.0270(17) 0.0334(17) 0.0313(18) -0.0070(14) -0.0034(14) -0.0085(14) C13 0.042(2) 0.0261(16) 0.035(2) -0.0041(14) -0.0081(16) -0.0051(14) C45 0.042(2) 0.0298(17) 0.037(2) 0.0046(14) -0.0190(16) -0.0174(15) C29 0.042(2) 0.0291(17) 0.037(2) -0.0025(14) -0.0133(16) -0.0050(15) C26 0.0243(17) 0.045(2) 0.039(2) -0.0094(16) -0.0073(15) -0.0093(15) C2 0.051(2) 0.048(2) 0.035(2) -0.0092(17) -0.0161(18) -0.0127(18) C9 0.053(2) 0.0265(17) 0.0302(19) -0.0047(14) -0.0073(16) -0.0093(16) C10 0.069(3) 0.0247(17) 0.040(2) -0.0058(15) -0.013(2) -0.0064(17) C24 0.0305(18) 0.045(2) 0.042(2) -0.0187(17) -0.0037(16) -0.0122(16) C31 0.031(2) 0.052(2) 0.068(3) -0.030(2) -0.019(2) 0.0104(18) C49 0.046(2) 0.0314(18) 0.038(2) -0.0123(15) -0.0064(17) -0.0132(16) C20 0.064(3) 0.0327(19) 0.034(2) -0.0031(15) -0.0238(19) -0.0061(18) C12 0.042(2) 0.045(2) 0.039(2) -0.0069(17) -0.0060(17) -0.0028(18) C50 0.041(2) 0.0372(19) 0.038(2) -0.0143(16) 0.0074(17) -0.0158(16) C32 0.0279(18) 0.051(2) 0.051(2) -0.0250(19) -0.0064(17) -0.0083(16) C30 0.053(3) 0.038(2) 0.059(3) -0.0123(19) -0.030(2) 0.0085(18) C11 0.057(3) 0.034(2) 0.043(2) -0.0141(17) -0.013(2) 0.0062(18) C5 0.047(2) 0.051(2) 0.053(3) 0.003(2) -0.011(2) -0.024(2) C4 0.044(2) 0.060(3) 0.071(3) -0.002(2) -0.023(2) -0.024(2) C3 0.053(3) 0.069(3) 0.052(3) -0.004(2) -0.030(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.094(3) . ? Fe1 N3 2.236(3) . ? Fe1 Cl1 2.2649(10) . ? Fe1 N1 2.269(3) . ? Fe1 Cl2 2.3344(11) . ? N1 C35 1.286(4) . ? N1 C19 1.441(4) . ? N2 C40 1.339(4) . ? N2 C36 1.345(4) . ? N3 C42 1.290(4) . ? N3 C43 1.437(4) . ? C22 C23 1.384(5) . ? C22 C27 1.404(5) . ? C22 C21 1.534(4) . ? C14 C19 1.391(4) . ? C14 C15 1.398(4) . ? C14 C7 1.534(4) . ? C35 C34 1.490(4) . ? C35 C36 1.494(4) . ? C37 C38 1.382(5) . ? C37 C36 1.384(4) . ? C37 H37A 0.9500 . ? C7 C1 1.522(5) . ? C7 C8 1.523(4) . ? C7 H7A 1.0000 . ? C40 C39 1.390(4) . ? C40 C42 1.479(4) . ? C19 C18 1.412(4) . ? C28 C33 1.387(5) . ? C28 C29 1.388(5) . ? C28 C21 1.519(4) . ? C43 C44 1.395(4) . ? C43 C48 1.397(5) . ? C1 C2 1.387(5) . ? C1 C6 1.394(5) . ? C42 C41 1.493(4) . ? C8 C9 1.381(5) . ? C8 C13 1.394(5) . ? C18 C17 1.388(4) . ? C18 C21 1.537(4) . ? C33 C32 1.380(5) . ? C33 H33A 0.9500 . ? C48 C47 1.393(5) . ? C48 C50 1.499(5) . ? C38 C39 1.380(5) . ? C38 H38A 0.9500 . ? C17 C16 1.390(5) . ? C17 H17A 0.9500 . ? C39 H39A 0.9500 . ? C21 H21A 1.0000 . ? C15 C16 1.391(5) . ? C15 H15A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C47 C46 1.383(5) . ? C47 H47A 0.9500 . ? C6 C5 1.386(6) . ? C6 H6A 0.9500 . ? C44 C45 1.391(5) . ? C44 C49 1.507(5) . ? C16 C20 1.512(5) . ? C46 C45 1.386(5) . ? C46 H46A 0.9500 . ? C25 C24 1.369(5) . ? C25 C26 1.388(5) . ? C25 H25A 0.9500 . ? C23 C24 1.390(5) . ? C23 H23A 0.9500 . ? C27 C26 1.380(5) . ? C27 H27A 0.9500 . ? C13 C12 1.378(5) . ? C13 H13A 0.9500 . ? C45 H45A 0.9500 . ? C29 C30 1.398(5) . ? C29 H29A 0.9500 . ? C26 H26A 0.9500 . ? C2 C3 1.391(6) . ? C2 H2A 0.9500 . ? C9 C10 1.391(5) . ? C9 H9A 0.9500 . ? C10 C11 1.373(6) . ? C10 H10A 0.9500 . ? C24 H24A 0.9500 . ? C31 C30 1.369(7) . ? C31 C32 1.374(6) . ? C31 H31A 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C12 C11 1.379(6) . ? C12 H12A 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C32 H32A 0.9500 . ? C30 H30A 0.9500 . ? C11 H11A 0.9500 . ? C5 C4 1.386(6) . ? C5 H5A 0.9500 . ? C4 C3 1.370(7) . ? C4 H4A 0.9500 . ? C3 H3A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N3 73.14(10) . . ? N2 Fe1 Cl1 149.85(8) . . ? N3 Fe1 Cl1 100.45(8) . . ? N2 Fe1 N1 73.08(10) . . ? N3 Fe1 N1 142.93(9) . . ? Cl1 Fe1 N1 101.05(7) . . ? N2 Fe1 Cl2 93.06(8) . . ? N3 Fe1 Cl2 98.99(7) . . ? Cl1 Fe1 Cl2 117.09(5) . . ? N1 Fe1 Cl2 97.59(7) . . ? C35 N1 C19 118.8(3) . . ? C35 N1 Fe1 115.7(2) . . ? C19 N1 Fe1 125.42(19) . . ? C40 N2 C36 120.1(3) . . ? C40 N2 Fe1 118.7(2) . . ? C36 N2 Fe1 119.6(2) . . ? C42 N3 C43 118.8(3) . . ? C42 N3 Fe1 115.5(2) . . ? C43 N3 Fe1 125.72(19) . . ? C23 C22 C27 118.0(3) . . ? C23 C22 C21 122.5(3) . . ? C27 C22 C21 119.4(3) . . ? C19 C14 C15 118.3(3) . . ? C19 C14 C7 121.1(3) . . ? C15 C14 C7 120.5(3) . . ? N1 C35 C34 127.5(3) . . ? N1 C35 C36 115.5(3) . . ? C34 C35 C36 116.9(3) . . ? C38 C37 C36 118.4(3) . . ? C38 C37 H37A 120.8 . . ? C36 C37 H37A 120.8 . . ? C1 C7 C8 115.0(3) . . ? C1 C7 C14 113.1(3) . . ? C8 C7 C14 109.9(3) . . ? C1 C7 H7A 106.0 . . ? C8 C7 H7A 106.0 . . ? C14 C7 H7A 106.0 . . ? N2 C40 C39 121.1(3) . . ? N2 C40 C42 113.8(3) . . ? C39 C40 C42 125.1(3) . . ? C14 C19 C18 121.5(3) . . ? C14 C19 N1 118.7(3) . . ? C18 C19 N1 119.7(3) . . ? C33 C28 C29 118.9(3) . . ? C33 C28 C21 121.0(3) . . ? C29 C28 C21 119.9(3) . . ? C44 C43 C48 122.1(3) . . ? C44 C43 N3 118.2(3) . . ? C48 C43 N3 119.7(3) . . ? C2 C1 C6 118.0(4) . . ? C2 C1 C7 119.1(3) . . ? C6 C1 C7 122.9(3) . . ? N2 C36 C37 121.6(3) . . ? N2 C36 C35 113.9(3) . . ? C37 C36 C35 124.5(3) . . ? N3 C42 C40 115.6(3) . . ? N3 C42 C41 125.5(3) . . ? C40 C42 C41 118.8(3) . . ? C9 C8 C13 118.7(3) . . ? C9 C8 C7 123.5(3) . . ? C13 C8 C7 117.7(3) . . ? C17 C18 C19 117.8(3) . . ? C17 C18 C21 122.8(3) . . ? C19 C18 C21 119.3(3) . . ? C32 C33 C28 120.3(3) . . ? C32 C33 H33A 119.9 . . ? C28 C33 H33A 119.9 . . ? C47 C48 C43 117.9(3) . . ? C47 C48 C50 120.5(3) . . ? C43 C48 C50 121.6(3) . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C18 C17 C16 122.0(3) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C38 C39 C40 118.8(3) . . ? C38 C39 H39A 120.6 . . ? C40 C39 H39A 120.6 . . ? C28 C21 C22 111.2(2) . . ? C28 C21 C18 113.6(3) . . ? C22 C21 C18 113.4(2) . . ? C28 C21 H21A 106.0 . . ? C22 C21 H21A 106.0 . . ? C18 C21 H21A 106.0 . . ? C16 C15 C14 121.5(3) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C46 C47 C48 120.8(3) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C5 C6 C1 121.0(4) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? C45 C44 C43 118.2(3) . . ? C45 C44 C49 121.2(3) . . ? C43 C44 C49 120.6(3) . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C20 121.1(3) . . ? C15 C16 C20 120.2(3) . . ? C47 C46 C45 120.3(3) . . ? C47 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C26 C27 C22 120.2(3) . . ? C26 C27 H27A 119.9 . . ? C22 C27 H27A 119.9 . . ? C12 C13 C8 120.7(3) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? C46 C45 C44 120.6(3) . . ? C46 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? C28 C29 C30 119.9(4) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C27 C26 C25 120.7(3) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C1 C2 C3 121.1(4) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C31 C32 C33 120.9(4) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C6 C5 C4 120.0(4) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C35 7.8(2) . . . . ? N3 Fe1 N1 C35 32.8(3) . . . . ? Cl1 Fe1 N1 C35 157.3(2) . . . . ? Cl2 Fe1 N1 C35 -83.1(2) . . . . ? N2 Fe1 N1 C19 -175.5(2) . . . . ? N3 Fe1 N1 C19 -150.4(2) . . . . ? Cl1 Fe1 N1 C19 -26.0(2) . . . . ? Cl2 Fe1 N1 C19 93.6(2) . . . . ? N3 Fe1 N2 C40 16.7(2) . . . . ? Cl1 Fe1 N2 C40 98.4(2) . . . . ? N1 Fe1 N2 C40 -178.8(2) . . . . ? Cl2 Fe1 N2 C40 -81.8(2) . . . . ? N3 Fe1 N2 C36 -178.1(2) . . . . ? Cl1 Fe1 N2 C36 -96.4(2) . . . . ? N1 Fe1 N2 C36 -13.6(2) . . . . ? Cl2 Fe1 N2 C36 83.4(2) . . . . ? N2 Fe1 N3 C42 -12.5(2) . . . . ? Cl1 Fe1 N3 C42 -162.1(2) . . . . ? N1 Fe1 N3 C42 -37.5(3) . . . . ? Cl2 Fe1 N3 C42 78.0(2) . . . . ? N2 Fe1 N3 C43 167.5(3) . . . . ? Cl1 Fe1 N3 C43 17.8(2) . . . . ? N1 Fe1 N3 C43 142.4(2) . . . . ? Cl2 Fe1 N3 C43 -102.1(2) . . . . ? C19 N1 C35 C34 5.1(5) . . . . ? Fe1 N1 C35 C34 -177.9(2) . . . . ? C19 N1 C35 C36 -178.7(2) . . . . ? Fe1 N1 C35 C36 -1.7(3) . . . . ? C19 C14 C7 C1 -88.9(4) . . . . ? C15 C14 C7 C1 93.4(4) . . . . ? C19 C14 C7 C8 141.1(3) . . . . ? C15 C14 C7 C8 -36.7(4) . . . . ? C36 N2 C40 C39 -2.3(4) . . . . ? Fe1 N2 C40 C39 162.9(2) . . . . ? C36 N2 C40 C42 176.3(3) . . . . ? Fe1 N2 C40 C42 -18.5(3) . . . . ? C15 C14 C19 C18 2.6(5) . . . . ? C7 C14 C19 C18 -175.2(3) . . . . ? C15 C14 C19 N1 179.7(3) . . . . ? C7 C14 C19 N1 1.9(4) . . . . ? C35 N1 C19 C14 83.7(4) . . . . ? Fe1 N1 C19 C14 -92.9(3) . . . . ? C35 N1 C19 C18 -99.1(3) . . . . ? Fe1 N1 C19 C18 84.2(3) . . . . ? C42 N3 C43 C44 87.4(4) . . . . ? Fe1 N3 C43 C44 -92.5(3) . . . . ? C42 N3 C43 C48 -93.7(4) . . . . ? Fe1 N3 C43 C48 86.4(3) . . . . ? C8 C7 C1 C2 -96.2(4) . . . . ? C14 C7 C1 C2 136.4(3) . . . . ? C8 C7 C1 C6 86.6(4) . . . . ? C14 C7 C1 C6 -40.9(4) . . . . ? C40 N2 C36 C37 2.3(4) . . . . ? Fe1 N2 C36 C37 -162.7(2) . . . . ? C40 N2 C36 C35 -177.8(3) . . . . ? Fe1 N2 C36 C35 17.2(3) . . . . ? C38 C37 C36 N2 -0.4(5) . . . . ? C38 C37 C36 C35 179.6(3) . . . . ? N1 C35 C36 N2 -9.4(4) . . . . ? C34 C35 C36 N2 167.2(3) . . . . ? N1 C35 C36 C37 170.5(3) . . . . ? C34 C35 C36 C37 -12.8(4) . . . . ? C43 N3 C42 C40 -172.8(3) . . . . ? Fe1 N3 C42 C40 7.2(3) . . . . ? C43 N3 C42 C41 4.3(5) . . . . ? Fe1 N3 C42 C41 -175.8(2) . . . . ? N2 C40 C42 N3 6.6(4) . . . . ? C39 C40 C42 N3 -174.8(3) . . . . ? N2 C40 C42 C41 -170.6(3) . . . . ? C39 C40 C42 C41 7.9(5) . . . . ? C1 C7 C8 C9 -30.4(4) . . . . ? C14 C7 C8 C9 98.6(4) . . . . ? C1 C7 C8 C13 154.0(3) . . . . ? C14 C7 C8 C13 -76.9(4) . . . . ? C14 C19 C18 C17 -4.1(5) . . . . ? N1 C19 C18 C17 178.9(3) . . . . ? C14 C19 C18 C21 173.3(3) . . . . ? N1 C19 C18 C21 -3.7(4) . . . . ? C29 C28 C33 C32 -0.7(5) . . . . ? C21 C28 C33 C32 174.4(3) . . . . ? C44 C43 C48 C47 -0.9(5) . . . . ? N3 C43 C48 C47 -179.7(3) . . . . ? C44 C43 C48 C50 179.9(3) . . . . ? N3 C43 C48 C50 1.0(5) . . . . ? C36 C37 C38 C39 -1.4(5) . . . . ? C19 C18 C17 C16 2.5(5) . . . . ? C21 C18 C17 C16 -174.8(3) . . . . ? C37 C38 C39 C40 1.4(5) . . . . ? N2 C40 C39 C38 0.4(5) . . . . ? C42 C40 C39 C38 -178.0(3) . . . . ? C33 C28 C21 C22 -76.0(4) . . . . ? C29 C28 C21 C22 99.1(3) . . . . ? C33 C28 C21 C18 53.3(4) . . . . ? C29 C28 C21 C18 -131.6(3) . . . . ? C23 C22 C21 C28 2.8(4) . . . . ? C27 C22 C21 C28 -173.4(3) . . . . ? C23 C22 C21 C18 -126.6(3) . . . . ? C27 C22 C21 C18 57.2(4) . . . . ? C17 C18 C21 C28 -114.0(3) . . . . ? C19 C18 C21 C28 68.8(4) . . . . ? C17 C18 C21 C22 14.2(4) . . . . ? C19 C18 C21 C22 -163.0(3) . . . . ? C19 C14 C15 C16 0.5(5) . . . . ? C7 C14 C15 C16 178.3(3) . . . . ? C43 C48 C47 C46 -1.0(5) . . . . ? C50 C48 C47 C46 178.2(3) . . . . ? C2 C1 C6 C5 -0.9(6) . . . . ? C7 C1 C6 C5 176.3(4) . . . . ? C48 C43 C44 C45 1.5(5) . . . . ? N3 C43 C44 C45 -179.6(3) . . . . ? C48 C43 C44 C49 -177.4(3) . . . . ? N3 C43 C44 C49 1.5(4) . . . . ? C18 C17 C16 C15 0.5(5) . . . . ? C18 C17 C16 C20 178.9(3) . . . . ? C14 C15 C16 C17 -2.0(5) . . . . ? C14 C15 C16 C20 179.5(3) . . . . ? C48 C47 C46 C45 2.3(5) . . . . ? C27 C22 C23 C24 -1.6(5) . . . . ? C21 C22 C23 C24 -177.8(3) . . . . ? C23 C22 C27 C26 1.8(5) . . . . ? C21 C22 C27 C26 178.2(3) . . . . ? C9 C8 C13 C12 -1.3(5) . . . . ? C7 C8 C13 C12 174.5(3) . . . . ? C47 C46 C45 C44 -1.7(5) . . . . ? C43 C44 C45 C46 -0.2(5) . . . . ? C49 C44 C45 C46 178.7(3) . . . . ? C33 C28 C29 C30 -0.6(5) . . . . ? C21 C28 C29 C30 -175.8(3) . . . . ? C22 C27 C26 C25 -1.3(6) . . . . ? C24 C25 C26 C27 0.5(6) . . . . ? C6 C1 C2 C3 1.4(6) . . . . ? C7 C1 C2 C3 -176.0(4) . . . . ? C13 C8 C9 C10 1.5(5) . . . . ? C7 C8 C9 C10 -174.0(3) . . . . ? C8 C9 C10 C11 -1.1(6) . . . . ? C26 C25 C24 C23 -0.3(6) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C8 C13 C12 C11 0.6(6) . . . . ? C30 C31 C32 C33 -0.8(6) . . . . ? C28 C33 C32 C31 1.5(5) . . . . ? C32 C31 C30 C29 -0.6(6) . . . . ? C28 C29 C30 C31 1.3(6) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C13 C12 C11 C10 -0.1(6) . . . . ? C1 C6 C5 C4 -0.5(7) . . . . ? C6 C5 C4 C3 1.4(7) . . . . ? C5 C4 C3 C2 -0.9(7) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.617 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.161 #==end data_Fe3 _database_code_depnum_ccdc_archive 'CCDC 798844' #TrackingRef 'CIF-for-chem.-commun.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H53 Cl2 Fe N3 O0' _chemical_formula_weight 870.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 16.461(3) _cell_length_b 14.946(3) _cell_length_c 18.995(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.10(3) _cell_angle_gamma 90.00 _cell_volume 4673.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12324 _cell_measurement_theta_min 1.3625 _cell_measurement_theta_max 25.3488 _exptl_crystal_description Prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8984 _exptl_absorpt_correction_T_max 0.9812 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 31868 _diffrn_reflns_av_R_equivalents 0.1228 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.31 _reflns_number_total 8450 _reflns_number_gt 7151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+21.4226P] 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 8450 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1802 _refine_ls_R_factor_gt 0.1568 _refine_ls_wR_factor_ref 0.3416 _refine_ls_wR_factor_gt 0.3231 _refine_ls_goodness_of_fit_ref 1.409 _refine_ls_restrained_S_all 1.409 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.35637(8) 0.68930(8) 0.19562(6) 0.0287(4) Uani 1 1 d . . . Cl1 Cl 0.41657(17) 0.55040(17) 0.18964(16) 0.0527(7) Uani 1 1 d . . . Cl2 Cl 0.28713(15) 0.71426(17) 0.09334(12) 0.0426(6) Uani 1 1 d . . . N3 N 0.4727(5) 0.7621(5) 0.1918(4) 0.0316(17) Uani 1 1 d . . . N1 N 0.2407(4) 0.6795(4) 0.2587(3) 0.0245(15) Uani 1 1 d . . . N2 N 0.3826(4) 0.7294(5) 0.2991(4) 0.0286(16) Uani 1 1 d . . . C35 C 0.2483(5) 0.6842(5) 0.3267(4) 0.0275(19) Uani 1 1 d . . . C8 C 0.1298(6) 0.8555(6) 0.3087(5) 0.032(2) Uani 1 1 d . . . C36 C 0.3282(5) 0.7178(5) 0.3514(4) 0.0270(19) Uani 1 1 d . . . C19 C 0.1638(5) 0.6649(6) 0.2269(4) 0.0271(19) Uani 1 1 d . . . C26 C 0.2795(7) 0.4357(7) 0.3975(5) 0.045(3) Uani 1 1 d . . . H26A H 0.3300 0.4346 0.4218 0.054 Uiso 1 1 calc R . . C13 C 0.1940(6) 0.8901(5) 0.3502(5) 0.036(2) Uani 1 1 d . . . H13A H 0.2448 0.9036 0.3291 0.043 Uiso 1 1 calc R . . C14 C 0.1133(6) 0.7394(6) 0.2124(4) 0.030(2) Uani 1 1 d . . . C37 C 0.3433(6) 0.7446(6) 0.4203(5) 0.035(2) Uani 1 1 d . . . H37A H 0.3047 0.7345 0.4566 0.042 Uiso 1 1 calc R . . C1 C 0.1135(6) 0.9072(6) 0.1814(5) 0.036(2) Uani 1 1 d . . . C38 C 0.4168(6) 0.7867(7) 0.4343(5) 0.043(2) Uani 1 1 d . . . H38A H 0.4288 0.8069 0.4806 0.052 Uiso 1 1 calc R . . C22 C 0.2028(6) 0.4676(5) 0.2907(4) 0.030(2) Uani 1 1 d . . . C9 C 0.0558(6) 0.8396(6) 0.3414(5) 0.040(2) Uani 1 1 d . . . H9A H 0.0118 0.8167 0.3145 0.049 Uiso 1 1 calc R . . C42 C 0.5059(5) 0.7820(5) 0.2502(4) 0.0275(19) Uani 1 1 d . . . C18 C 0.1413(5) 0.5786(6) 0.2056(4) 0.030(2) Uani 1 1 d . . . C34 C 0.1842(5) 0.6616(6) 0.3796(4) 0.0288(19) Uani 1 1 d . . . H34A H 0.1352 0.6409 0.3551 0.043 Uiso 1 1 calc R . . H34B H 0.1712 0.7149 0.4075 0.043 Uiso 1 1 calc R . . H34C H 0.2041 0.6142 0.4108 0.043 Uiso 1 1 calc R . . C39 C 0.4724(6) 0.7990(6) 0.3807(5) 0.040(2) Uani 1 1 d . . . H39A H 0.5226 0.8282 0.3896 0.048 Uiso 1 1 calc R . . C23 C 0.1325(6) 0.4394(6) 0.3249(4) 0.034(2) Uani 1 1 d . . . H23A H 0.0819 0.4396 0.3008 0.041 Uiso 1 1 calc R . . C3 C 0.0975(7) 0.9612(6) 0.0617(5) 0.044(3) Uani 1 1 d . . . H3A H 0.1017 0.9514 0.0125 0.053 Uiso 1 1 calc R . . C33 C 0.1791(6) 0.3381(6) 0.1767(5) 0.041(2) Uani 1 1 d . . . H33A H 0.1726 0.3201 0.2243 0.050 Uiso 1 1 calc R . . C21 C 0.2010(6) 0.5021(6) 0.2156(5) 0.032(2) Uani 1 1 d . . . H21A H 0.2559 0.5288 0.2075 0.039 Uiso 1 1 calc R . . C16 C 0.0128(6) 0.6389(6) 0.1598(5) 0.035(2) Uani 1 1 d . . . C5 C 0.0588(6) 1.0539(7) 0.1584(6) 0.047(3) Uani 1 1 d . . . H5A H 0.0372 1.1084 0.1761 0.057 Uiso 1 1 calc R . . C27 C 0.2755(6) 0.4651(6) 0.3283(5) 0.034(2) Uani 1 1 d . . . H27A H 0.3240 0.4841 0.3057 0.041 Uiso 1 1 calc R . . C17 C 0.0649(5) 0.5682(6) 0.1721(4) 0.033(2) Uani 1 1 d . . . H17A H 0.0489 0.5101 0.1574 0.039 Uiso 1 1 calc R . . C2 C 0.1217(6) 0.8957(6) 0.1081(5) 0.035(2) Uani 1 1 d . . . H2A H 0.1443 0.8418 0.0904 0.042 Uiso 1 1 calc R . . C44 C 0.5746(6) 0.7272(6) 0.0996(5) 0.037(2) Uani 1 1 d . . . C15 C 0.0391(5) 0.7246(6) 0.1800(4) 0.030(2) Uani 1 1 d . . . H15A H 0.0047 0.7744 0.1709 0.036 Uiso 1 1 calc R . . C43 C 0.5117(6) 0.7809(6) 0.1254(5) 0.036(2) Uani 1 1 d . . . C48 C 0.4785(6) 0.8541(6) 0.0875(5) 0.036(2) Uani 1 1 d . . . C45 C 0.6054(6) 0.7496(8) 0.0324(5) 0.047(3) Uani 1 1 d . . . H45A H 0.6477 0.7144 0.0127 0.057 Uiso 1 1 calc R . . C6 C 0.0826(6) 0.9863(6) 0.2055(5) 0.036(2) Uani 1 1 d . . . H6A H 0.0770 0.9957 0.2547 0.043 Uiso 1 1 calc R . . C31 C 0.1844(7) 0.3014(8) 0.0527(6) 0.050(3) Uani 1 1 d . . . H31A H 0.1812 0.2583 0.0160 0.060 Uiso 1 1 calc R . . C41 C 0.5906(6) 0.8178(7) 0.2607(5) 0.044(2) Uani 1 1 d . . . H41A H 0.6175 0.8237 0.2149 0.066 Uiso 1 1 calc R . . H41B H 0.6216 0.7766 0.2905 0.066 Uiso 1 1 calc R . . H41C H 0.5879 0.8766 0.2835 0.066 Uiso 1 1 calc R . . C12 C 0.1826(7) 0.9043(7) 0.4215(5) 0.048(3) Uani 1 1 d . . . H12A H 0.2264 0.9254 0.4497 0.058 Uiso 1 1 calc R . . C24 C 0.1365(7) 0.4111(6) 0.3945(5) 0.047(3) Uani 1 1 d . . . H24A H 0.0881 0.3933 0.4178 0.057 Uiso 1 1 calc R . . C25 C 0.2096(8) 0.4082(7) 0.4307(5) 0.052(3) Uani 1 1 d . . . H25A H 0.2114 0.3875 0.4779 0.062 Uiso 1 1 calc R . . C4 C 0.0667(6) 1.0418(7) 0.0870(5) 0.045(3) Uani 1 1 d . . . H4A H 0.0513 1.0879 0.0553 0.055 Uiso 1 1 calc R . . C28 C 0.1926(5) 0.4275(6) 0.1598(4) 0.0278(19) Uani 1 1 d . . . C52 C 0.4129(6) 0.9127(7) 0.1193(5) 0.043(2) Uani 1 1 d . . . H52A H 0.3818 0.8750 0.1535 0.051 Uiso 1 1 calc R . . C7 C 0.1445(5) 0.8337(6) 0.2316(5) 0.031(2) Uani 1 1 d . . . H7A H 0.2048 0.8318 0.2255 0.038 Uiso 1 1 calc R . . C20 C -0.0668(6) 0.6265(7) 0.1234(6) 0.048(3) Uani 1 1 d . . . H20A H -0.0948 0.6842 0.1200 0.073 Uiso 1 1 calc R . . H20B H -0.1003 0.5844 0.1503 0.073 Uiso 1 1 calc R . . H20C H -0.0575 0.6026 0.0760 0.073 Uiso 1 1 calc R . . C46 C 0.5757(6) 0.8208(7) -0.0050(5) 0.047(3) Uani 1 1 d . . . H46A H 0.5984 0.8352 -0.0495 0.056 Uiso 1 1 calc R . . C47 C 0.5127(7) 0.8721(8) 0.0218(5) 0.048(3) Uani 1 1 d . . . H47A H 0.4923 0.9207 -0.0052 0.057 Uiso 1 1 calc R . . C49 C 0.6092(7) 0.6452(7) 0.1368(6) 0.050(3) Uani 1 1 d . . . H49A H 0.5783 0.6372 0.1816 0.060 Uiso 1 1 calc R . . C29 C 0.2027(6) 0.4521(6) 0.0892(5) 0.038(2) Uani 1 1 d . . . H29A H 0.2129 0.5130 0.0778 0.046 Uiso 1 1 calc R . . C10 C 0.0448(6) 0.8563(7) 0.4124(5) 0.044(2) Uani 1 1 d . . . H10A H -0.0066 0.8456 0.4334 0.053 Uiso 1 1 calc R . . C54 C 0.4487(8) 0.9908(7) 0.1604(6) 0.060(3) Uani 1 1 d . . . H54A H 0.4865 0.9681 0.1961 0.090 Uiso 1 1 calc R . . H54B H 0.4049 1.0241 0.1835 0.090 Uiso 1 1 calc R . . H54C H 0.4778 1.0306 0.1281 0.090 Uiso 1 1 calc R . . C30 C 0.1982(6) 0.3897(7) 0.0364(5) 0.046(3) Uani 1 1 d . . . H30A H 0.2046 0.4075 -0.0113 0.055 Uiso 1 1 calc R . . C11 C 0.1073(7) 0.8880(7) 0.4523(5) 0.048(3) Uani 1 1 d . . . H11A H 0.0995 0.8990 0.5011 0.058 Uiso 1 1 calc R . . C53 C 0.3518(7) 0.9474(7) 0.0641(6) 0.057(3) Uani 1 1 d . . . H53A H 0.3280 0.8966 0.0388 0.086 Uiso 1 1 calc R . . H53B H 0.3800 0.9865 0.0307 0.086 Uiso 1 1 calc R . . H53C H 0.3087 0.9811 0.0877 0.086 Uiso 1 1 calc R . . C40 C 0.4539(6) 0.7684(6) 0.3142(5) 0.033(2) Uani 1 1 d . . . C51 C 0.6995(6) 0.6591(9) 0.1565(7) 0.061(3) Uani 1 1 d . . . H51A H 0.7049 0.7129 0.1857 0.092 Uiso 1 1 calc R . . H51B H 0.7317 0.6663 0.1135 0.092 Uiso 1 1 calc R . . H51C H 0.7191 0.6070 0.1828 0.092 Uiso 1 1 calc R . . C32 C 0.1753(7) 0.2745(8) 0.1218(6) 0.054(3) Uani 1 1 d . . . H32A H 0.1664 0.2132 0.1324 0.064 Uiso 1 1 calc R . . C50 C 0.5983(8) 0.5602(7) 0.0934(7) 0.066(4) Uani 1 1 d . . . H50A H 0.5405 0.5520 0.0824 0.099 Uiso 1 1 calc R . . H50B H 0.6180 0.5087 0.1203 0.099 Uiso 1 1 calc R . . H50C H 0.6291 0.5654 0.0495 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0369(7) 0.0281(7) 0.0209(6) 0.0017(5) -0.0025(5) -0.0006(6) Cl1 0.0516(16) 0.0343(14) 0.0723(19) 0.0067(13) 0.0083(14) 0.0015(12) Cl2 0.0516(15) 0.0509(15) 0.0254(11) 0.0043(10) -0.0036(10) -0.0061(12) N3 0.043(4) 0.030(4) 0.022(4) 0.002(3) 0.006(3) -0.005(3) N1 0.034(4) 0.021(4) 0.019(3) 0.001(3) 0.002(3) -0.001(3) N2 0.028(4) 0.024(4) 0.033(4) 0.000(3) 0.001(3) 0.002(3) C35 0.040(5) 0.020(4) 0.023(4) -0.005(3) -0.001(4) 0.001(4) C8 0.043(5) 0.027(5) 0.027(5) 0.008(4) 0.001(4) 0.003(4) C36 0.038(5) 0.025(4) 0.018(4) 0.002(3) -0.010(4) 0.003(4) C19 0.030(5) 0.033(5) 0.019(4) -0.002(3) -0.002(3) -0.006(4) C26 0.056(7) 0.045(6) 0.034(5) 0.004(5) -0.009(5) 0.010(5) C13 0.043(6) 0.015(4) 0.050(6) 0.001(4) -0.007(5) 0.009(4) C14 0.045(5) 0.024(4) 0.020(4) 0.002(3) 0.011(4) -0.002(4) C37 0.045(6) 0.037(5) 0.024(4) -0.005(4) 0.000(4) 0.003(4) C1 0.042(6) 0.025(5) 0.041(6) 0.004(4) 0.001(4) -0.008(4) C38 0.053(6) 0.046(6) 0.031(5) 0.003(4) -0.008(5) 0.002(5) C22 0.049(6) 0.016(4) 0.024(4) -0.001(3) -0.004(4) 0.001(4) C9 0.055(6) 0.038(5) 0.028(5) 0.003(4) -0.001(4) 0.001(5) C42 0.037(5) 0.022(4) 0.023(4) 0.003(3) 0.001(4) 0.002(4) C18 0.035(5) 0.038(5) 0.018(4) 0.010(4) 0.008(4) -0.001(4) C34 0.033(5) 0.032(5) 0.022(4) 0.003(4) -0.001(4) 0.004(4) C39 0.043(6) 0.036(5) 0.042(6) -0.007(4) -0.014(5) -0.015(4) C23 0.047(6) 0.032(5) 0.023(4) 0.000(4) 0.002(4) -0.004(4) C3 0.069(7) 0.034(5) 0.030(5) 0.006(4) 0.003(5) -0.006(5) C33 0.062(7) 0.030(5) 0.032(5) -0.002(4) 0.001(5) 0.001(5) C21 0.035(5) 0.034(5) 0.029(5) 0.000(4) -0.003(4) -0.001(4) C16 0.038(5) 0.037(5) 0.029(5) 0.004(4) -0.001(4) -0.003(4) C5 0.051(6) 0.041(6) 0.050(6) 0.016(5) -0.002(5) 0.000(5) C27 0.039(5) 0.032(5) 0.030(5) -0.001(4) -0.003(4) 0.009(4) C17 0.044(5) 0.035(5) 0.019(4) -0.001(4) -0.004(4) -0.011(4) C2 0.056(6) 0.021(4) 0.028(5) 0.000(4) 0.007(4) 0.005(4) C44 0.042(6) 0.036(5) 0.033(5) -0.003(4) 0.001(4) -0.019(4) C15 0.035(5) 0.025(4) 0.031(5) 0.011(4) -0.009(4) 0.009(4) C43 0.040(5) 0.041(5) 0.026(5) -0.008(4) 0.003(4) -0.001(4) C48 0.044(6) 0.035(5) 0.031(5) -0.006(4) -0.001(4) -0.003(4) C45 0.046(6) 0.063(7) 0.033(5) -0.008(5) 0.004(5) -0.010(5) C6 0.046(6) 0.030(5) 0.030(5) -0.006(4) -0.001(4) -0.002(4) C31 0.060(7) 0.053(7) 0.038(6) -0.010(5) -0.005(5) 0.004(6) C41 0.042(6) 0.048(6) 0.042(6) -0.011(5) -0.007(5) -0.017(5) C12 0.069(8) 0.044(6) 0.032(5) -0.019(5) -0.011(5) 0.007(5) C24 0.076(8) 0.029(5) 0.038(6) 0.006(4) 0.010(5) -0.002(5) C25 0.089(9) 0.040(6) 0.026(5) 0.002(4) 0.006(6) 0.019(6) C4 0.059(7) 0.035(6) 0.043(6) 0.011(5) -0.008(5) -0.003(5) C28 0.030(5) 0.034(5) 0.019(4) -0.006(4) -0.006(3) 0.006(4) C52 0.059(7) 0.044(6) 0.025(5) 0.013(4) -0.015(4) -0.005(5) C7 0.030(5) 0.029(5) 0.035(5) 0.010(4) 0.003(4) -0.001(4) C20 0.042(6) 0.036(6) 0.067(7) 0.008(5) -0.010(5) -0.001(5) C46 0.055(7) 0.055(7) 0.031(5) -0.002(5) 0.005(5) -0.021(6) C47 0.060(7) 0.053(7) 0.031(5) -0.006(5) -0.010(5) -0.020(6) C49 0.053(7) 0.043(6) 0.055(7) 0.004(5) 0.017(5) 0.013(5) C29 0.049(6) 0.033(5) 0.032(5) -0.002(4) 0.001(4) 0.010(4) C10 0.048(6) 0.049(6) 0.035(5) -0.013(5) 0.000(5) -0.001(5) C54 0.086(9) 0.043(6) 0.052(7) -0.006(5) -0.026(6) 0.006(6) C30 0.057(7) 0.050(7) 0.031(5) -0.008(5) -0.002(5) 0.005(5) C11 0.065(7) 0.043(6) 0.038(6) -0.008(5) 0.009(5) 0.017(5) C53 0.068(8) 0.045(7) 0.058(7) 0.011(6) -0.004(6) -0.006(6) C40 0.042(6) 0.024(5) 0.034(5) 0.001(4) -0.002(4) 0.008(4) C51 0.036(6) 0.068(8) 0.080(9) -0.004(7) 0.003(6) 0.004(6) C32 0.053(7) 0.042(6) 0.065(8) -0.008(6) -0.007(6) -0.008(5) C50 0.076(9) 0.038(6) 0.084(9) -0.008(6) 0.015(7) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.099(7) . ? Fe1 N3 2.204(7) . ? Fe1 N1 2.256(7) . ? Fe1 Cl2 2.282(3) . ? Fe1 Cl1 2.303(3) . ? N3 C42 1.272(11) . ? N3 C43 1.443(11) . ? N1 C35 1.299(10) . ? N1 C19 1.419(10) . ? N2 C40 1.342(11) . ? N2 C36 1.350(11) . ? C35 C36 1.484(12) . ? C35 C34 1.497(11) . ? C8 C9 1.389(13) . ? C8 C13 1.414(13) . ? C8 C7 1.521(12) . ? C36 C37 1.391(11) . ? C19 C18 1.402(12) . ? C19 C14 1.416(12) . ? C26 C25 1.375(15) . ? C26 C27 1.388(12) . ? C26 H26A 0.9500 . ? C13 C12 1.386(13) . ? C13 H13A 0.9500 . ? C14 C15 1.385(12) . ? C14 C7 1.544(12) . ? C37 C38 1.387(13) . ? C37 H37A 0.9500 . ? C1 C6 1.366(13) . ? C1 C2 1.410(12) . ? C1 C7 1.540(12) . ? C38 C39 1.384(13) . ? C38 H38A 0.9500 . ? C22 C27 1.392(12) . ? C22 C23 1.393(12) . ? C22 C21 1.518(12) . ? C9 C10 1.383(13) . ? C9 H9A 0.9500 . ? C42 C40 1.501(12) . ? C42 C41 1.506(12) . ? C18 C17 1.417(12) . ? C18 C21 1.520(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C39 C40 1.377(12) . ? C39 H39A 0.9500 . ? C23 C24 1.389(13) . ? C23 H23A 0.9500 . ? C3 C2 1.375(12) . ? C3 C4 1.393(14) . ? C3 H3A 0.9500 . ? C33 C28 1.392(13) . ? C33 C32 1.412(14) . ? C33 H33A 0.9500 . ? C21 C28 1.544(11) . ? C21 H21A 1.0000 . ? C16 C17 1.381(13) . ? C16 C15 1.405(12) . ? C16 C20 1.492(13) . ? C5 C4 1.375(14) . ? C5 C6 1.403(13) . ? C5 H5A 0.9500 . ? C27 H27A 0.9500 . ? C17 H17A 0.9500 . ? C2 H2A 0.9500 . ? C44 C43 1.398(13) . ? C44 C45 1.415(13) . ? C44 C49 1.525(14) . ? C15 H15A 0.9500 . ? C43 C48 1.418(13) . ? C48 C47 1.397(13) . ? C48 C52 1.517(14) . ? C45 C46 1.369(15) . ? C45 H45A 0.9500 . ? C6 H6A 0.9500 . ? C31 C30 1.375(15) . ? C31 C32 1.381(15) . ? C31 H31A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C12 C11 1.393(15) . ? C12 H12A 0.9500 . ? C24 C25 1.384(15) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C4 H4A 0.9500 . ? C28 C29 1.402(12) . ? C52 C54 1.523(14) . ? C52 C53 1.541(14) . ? C52 H52A 1.0000 . ? C7 H7A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C46 C47 1.387(15) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C49 C50 1.525(15) . ? C49 C51 1.546(15) . ? C49 H49A 1.0000 . ? C29 C30 1.371(13) . ? C29 H29A 0.9500 . ? C10 C11 1.363(14) . ? C10 H10A 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C30 H30A 0.9500 . ? C11 H11A 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C32 H32A 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N3 73.3(3) . . ? N2 Fe1 N1 72.2(3) . . ? N3 Fe1 N1 141.6(3) . . ? N2 Fe1 Cl2 148.5(2) . . ? N3 Fe1 Cl2 108.9(2) . . ? N1 Fe1 Cl2 92.42(19) . . ? N2 Fe1 Cl1 102.5(2) . . ? N3 Fe1 Cl1 94.0(2) . . ? N1 Fe1 Cl1 109.33(19) . . ? Cl2 Fe1 Cl1 108.64(11) . . ? C42 N3 C43 121.7(8) . . ? C42 N3 Fe1 117.3(6) . . ? C43 N3 Fe1 120.9(6) . . ? C35 N1 C19 121.0(7) . . ? C35 N1 Fe1 116.4(6) . . ? C19 N1 Fe1 122.5(5) . . ? C40 N2 C36 118.7(7) . . ? C40 N2 Fe1 120.2(6) . . ? C36 N2 Fe1 121.2(6) . . ? N1 C35 C36 114.6(7) . . ? N1 C35 C34 126.0(8) . . ? C36 C35 C34 119.3(7) . . ? C9 C8 C13 118.0(9) . . ? C9 C8 C7 122.3(8) . . ? C13 C8 C7 119.7(8) . . ? N2 C36 C37 122.5(8) . . ? N2 C36 C35 113.5(7) . . ? C37 C36 C35 123.6(8) . . ? C18 C19 C14 120.8(8) . . ? C18 C19 N1 119.9(8) . . ? C14 C19 N1 119.1(7) . . ? C25 C26 C27 119.3(10) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C12 C13 C8 119.9(9) . . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? C15 C14 C19 118.6(8) . . ? C15 C14 C7 122.9(8) . . ? C19 C14 C7 118.5(8) . . ? C38 C37 C36 117.7(9) . . ? C38 C37 H37A 121.1 . . ? C36 C37 H37A 121.1 . . ? C6 C1 C2 118.2(9) . . ? C6 C1 C7 122.3(9) . . ? C2 C1 C7 119.5(8) . . ? C39 C38 C37 119.8(9) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C27 C22 C23 117.8(8) . . ? C27 C22 C21 120.4(8) . . ? C23 C22 C21 121.8(8) . . ? C10 C9 C8 121.4(10) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? N3 C42 C40 115.5(8) . . ? N3 C42 C41 126.5(8) . . ? C40 C42 C41 118.0(8) . . ? C19 C18 C17 117.7(8) . . ? C19 C18 C21 119.1(8) . . ? C17 C18 C21 123.1(8) . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C39 C38 119.1(9) . . ? C40 C39 H39A 120.4 . . ? C38 C39 H39A 120.4 . . ? C24 C23 C22 119.8(9) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C2 C3 C4 120.0(9) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C28 C33 C32 118.8(9) . . ? C28 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C22 C21 C18 112.6(7) . . ? C22 C21 C28 113.6(7) . . ? C18 C21 C28 113.6(7) . . ? C22 C21 H21A 105.3 . . ? C18 C21 H21A 105.3 . . ? C28 C21 H21A 105.3 . . ? C17 C16 C15 117.4(8) . . ? C17 C16 C20 121.8(9) . . ? C15 C16 C20 120.7(8) . . ? C4 C5 C6 120.5(10) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C26 C27 C22 122.2(9) . . ? C26 C27 H27A 118.9 . . ? C22 C27 H27A 118.9 . . ? C16 C17 C18 122.8(9) . . ? C16 C17 H17A 118.6 . . ? C18 C17 H17A 118.6 . . ? C3 C2 C1 121.2(8) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C43 C44 C45 116.6(10) . . ? C43 C44 C49 125.1(8) . . ? C45 C44 C49 118.3(9) . . ? C14 C15 C16 122.5(8) . . ? C14 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C44 C43 C48 123.3(8) . . ? C44 C43 N3 121.7(9) . . ? C48 C43 N3 114.9(8) . . ? C47 C48 C43 116.5(9) . . ? C47 C48 C52 122.2(9) . . ? C43 C48 C52 121.2(8) . . ? C46 C45 C44 121.6(10) . . ? C46 C45 H45A 119.2 . . ? C44 C45 H45A 119.2 . . ? C1 C6 C5 120.9(9) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C30 C31 C32 120.7(10) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C13 C12 C11 120.4(10) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C25 C24 C23 121.4(10) . . ? C25 C24 H24A 119.3 . . ? C23 C24 H24A 119.3 . . ? C26 C25 C24 119.4(9) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C5 C4 C3 119.3(9) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C33 C28 C29 119.5(8) . . ? C33 C28 C21 123.4(8) . . ? C29 C28 C21 117.1(8) . . ? C48 C52 C54 111.8(9) . . ? C48 C52 C53 112.8(8) . . ? C54 C52 C53 110.0(9) . . ? C48 C52 H52A 107.3 . . ? C54 C52 H52A 107.3 . . ? C53 C52 H52A 107.3 . . ? C8 C7 C1 113.0(7) . . ? C8 C7 C14 111.6(7) . . ? C1 C7 C14 113.4(7) . . ? C8 C7 H7A 106.0 . . ? C1 C7 H7A 106.0 . . ? C14 C7 H7A 106.1 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C45 C46 C47 120.4(10) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? C46 C47 C48 121.6(10) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C44 C49 C50 112.0(10) . . ? C44 C49 C51 111.3(9) . . ? C50 C49 C51 110.8(9) . . ? C44 C49 H49A 107.5 . . ? C50 C49 H49A 107.5 . . ? C51 C49 H49A 107.5 . . ? C30 C29 C28 121.0(9) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C11 C10 C9 120.3(10) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C29 C30 C31 119.8(10) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C10 C11 C12 119.9(10) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C40 C39 122.1(9) . . ? N2 C40 C42 112.7(8) . . ? C39 C40 C42 125.0(9) . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C31 C32 C33 120.1(10) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N3 C42 9.3(6) . . . . ? N1 Fe1 N3 C42 36.0(9) . . . . ? Cl2 Fe1 N3 C42 156.3(6) . . . . ? Cl1 Fe1 N3 C42 -92.5(7) . . . . ? N2 Fe1 N3 C43 -174.6(7) . . . . ? N1 Fe1 N3 C43 -147.9(6) . . . . ? Cl2 Fe1 N3 C43 -27.6(7) . . . . ? Cl1 Fe1 N3 C43 83.6(7) . . . . ? N2 Fe1 N1 C35 -13.3(6) . . . . ? N3 Fe1 N1 C35 -40.2(8) . . . . ? Cl2 Fe1 N1 C35 -165.3(6) . . . . ? Cl1 Fe1 N1 C35 84.0(6) . . . . ? N2 Fe1 N1 C19 169.3(7) . . . . ? N3 Fe1 N1 C19 142.5(6) . . . . ? Cl2 Fe1 N1 C19 17.4(6) . . . . ? Cl1 Fe1 N1 C19 -93.4(6) . . . . ? N3 Fe1 N2 C40 -6.0(6) . . . . ? N1 Fe1 N2 C40 -169.0(7) . . . . ? Cl2 Fe1 N2 C40 -105.1(7) . . . . ? Cl1 Fe1 N2 C40 84.4(6) . . . . ? N3 Fe1 N2 C36 173.0(7) . . . . ? N1 Fe1 N2 C36 10.0(6) . . . . ? Cl2 Fe1 N2 C36 73.9(8) . . . . ? Cl1 Fe1 N2 C36 -96.6(6) . . . . ? C19 N1 C35 C36 -168.1(7) . . . . ? Fe1 N1 C35 C36 14.6(9) . . . . ? C19 N1 C35 C34 10.3(13) . . . . ? Fe1 N1 C35 C34 -167.1(6) . . . . ? C40 N2 C36 C37 -0.2(12) . . . . ? Fe1 N2 C36 C37 -179.2(7) . . . . ? C40 N2 C36 C35 173.0(7) . . . . ? Fe1 N2 C36 C35 -6.1(9) . . . . ? N1 C35 C36 N2 -6.2(10) . . . . ? C34 C35 C36 N2 175.3(7) . . . . ? N1 C35 C36 C37 166.8(8) . . . . ? C34 C35 C36 C37 -11.6(12) . . . . ? C35 N1 C19 C18 -98.2(9) . . . . ? Fe1 N1 C19 C18 79.0(9) . . . . ? C35 N1 C19 C14 86.5(10) . . . . ? Fe1 N1 C19 C14 -96.2(8) . . . . ? C9 C8 C13 C12 2.1(13) . . . . ? C7 C8 C13 C12 -175.7(8) . . . . ? C18 C19 C14 C15 3.3(12) . . . . ? N1 C19 C14 C15 178.5(7) . . . . ? C18 C19 C14 C7 -174.9(7) . . . . ? N1 C19 C14 C7 0.3(11) . . . . ? N2 C36 C37 C38 1.6(13) . . . . ? C35 C36 C37 C38 -170.9(8) . . . . ? C36 C37 C38 C39 -1.2(14) . . . . ? C13 C8 C9 C10 -0.5(14) . . . . ? C7 C8 C9 C10 177.2(9) . . . . ? C43 N3 C42 C40 173.0(8) . . . . ? Fe1 N3 C42 C40 -10.9(10) . . . . ? C43 N3 C42 C41 -6.6(14) . . . . ? Fe1 N3 C42 C41 169.5(7) . . . . ? C14 C19 C18 C17 -2.8(12) . . . . ? N1 C19 C18 C17 -178.0(7) . . . . ? C14 C19 C18 C21 173.9(7) . . . . ? N1 C19 C18 C21 -1.3(11) . . . . ? C37 C38 C39 C40 -0.5(15) . . . . ? C27 C22 C23 C24 0.7(13) . . . . ? C21 C22 C23 C24 -177.9(8) . . . . ? C27 C22 C21 C18 -123.9(9) . . . . ? C23 C22 C21 C18 54.6(11) . . . . ? C27 C22 C21 C28 105.1(9) . . . . ? C23 C22 C21 C28 -76.4(10) . . . . ? C19 C18 C21 C22 79.3(10) . . . . ? C17 C18 C21 C22 -104.3(9) . . . . ? C19 C18 C21 C28 -149.7(8) . . . . ? C17 C18 C21 C28 26.7(11) . . . . ? C25 C26 C27 C22 -0.2(15) . . . . ? C23 C22 C27 C26 0.1(13) . . . . ? C21 C22 C27 C26 178.7(8) . . . . ? C15 C16 C17 C18 2.0(13) . . . . ? C20 C16 C17 C18 179.0(9) . . . . ? C19 C18 C17 C16 0.1(12) . . . . ? C21 C18 C17 C16 -176.4(8) . . . . ? C4 C3 C2 C1 2.2(16) . . . . ? C6 C1 C2 C3 -1.5(14) . . . . ? C7 C1 C2 C3 -177.6(9) . . . . ? C19 C14 C15 C16 -1.1(13) . . . . ? C7 C14 C15 C16 177.0(8) . . . . ? C17 C16 C15 C14 -1.5(13) . . . . ? C20 C16 C15 C14 -178.6(9) . . . . ? C45 C44 C43 C48 0.6(14) . . . . ? C49 C44 C43 C48 -176.8(9) . . . . ? C45 C44 C43 N3 176.9(8) . . . . ? C49 C44 C43 N3 -0.4(14) . . . . ? C42 N3 C43 C44 77.9(12) . . . . ? Fe1 N3 C43 C44 -98.0(9) . . . . ? C42 N3 C43 C48 -105.4(10) . . . . ? Fe1 N3 C43 C48 78.6(9) . . . . ? C44 C43 C48 C47 -1.0(14) . . . . ? N3 C43 C48 C47 -177.6(8) . . . . ? C44 C43 C48 C52 -177.3(9) . . . . ? N3 C43 C48 C52 6.1(13) . . . . ? C43 C44 C45 C46 0.7(14) . . . . ? C49 C44 C45 C46 178.2(9) . . . . ? C2 C1 C6 C5 0.6(14) . . . . ? C7 C1 C6 C5 176.6(9) . . . . ? C4 C5 C6 C1 -0.3(15) . . . . ? C8 C13 C12 C11 -2.5(14) . . . . ? C22 C23 C24 C25 -1.4(15) . . . . ? C27 C26 C25 C24 -0.5(15) . . . . ? C23 C24 C25 C26 1.3(15) . . . . ? C6 C5 C4 C3 0.9(16) . . . . ? C2 C3 C4 C5 -1.8(16) . . . . ? C32 C33 C28 C29 -0.6(14) . . . . ? C32 C33 C28 C21 -177.7(9) . . . . ? C22 C21 C28 C33 6.5(12) . . . . ? C18 C21 C28 C33 -124.0(9) . . . . ? C22 C21 C28 C29 -170.6(8) . . . . ? C18 C21 C28 C29 58.9(11) . . . . ? C47 C48 C52 C54 -86.8(11) . . . . ? C43 C48 C52 C54 89.3(11) . . . . ? C47 C48 C52 C53 37.8(13) . . . . ? C43 C48 C52 C53 -146.1(9) . . . . ? C9 C8 C7 C1 82.6(10) . . . . ? C13 C8 C7 C1 -99.8(9) . . . . ? C9 C8 C7 C14 -46.6(11) . . . . ? C13 C8 C7 C14 131.1(8) . . . . ? C6 C1 C7 C8 5.1(12) . . . . ? C2 C1 C7 C8 -178.9(8) . . . . ? C6 C1 C7 C14 133.4(9) . . . . ? C2 C1 C7 C14 -50.7(11) . . . . ? C15 C14 C7 C8 99.0(10) . . . . ? C19 C14 C7 C8 -82.9(9) . . . . ? C15 C14 C7 C1 -30.0(11) . . . . ? C19 C14 C7 C1 148.2(8) . . . . ? C44 C45 C46 C47 -1.5(15) . . . . ? C45 C46 C47 C48 1.0(15) . . . . ? C43 C48 C47 C46 0.2(14) . . . . ? C52 C48 C47 C46 176.5(9) . . . . ? C43 C44 C49 C50 118.8(11) . . . . ? C45 C44 C49 C50 -58.5(12) . . . . ? C43 C44 C49 C51 -116.5(11) . . . . ? C45 C44 C49 C51 66.2(12) . . . . ? C33 C28 C29 C30 1.1(14) . . . . ? C21 C28 C29 C30 178.4(9) . . . . ? C8 C9 C10 C11 -0.8(16) . . . . ? C28 C29 C30 C31 -0.7(15) . . . . ? C32 C31 C30 C29 -0.2(17) . . . . ? C9 C10 C11 C12 0.4(16) . . . . ? C13 C12 C11 C10 1.2(16) . . . . ? C36 N2 C40 C39 -1.7(13) . . . . ? Fe1 N2 C40 C39 177.3(7) . . . . ? C36 N2 C40 C42 -176.4(7) . . . . ? Fe1 N2 C40 C42 2.7(9) . . . . ? C38 C39 C40 N2 2.1(14) . . . . ? C38 C39 C40 C42 176.0(9) . . . . ? N3 C42 C40 N2 5.6(11) . . . . ? C41 C42 C40 N2 -174.7(8) . . . . ? N3 C42 C40 C39 -168.8(9) . . . . ? C41 C42 C40 C39 10.8(13) . . . . ? C30 C31 C32 C33 0.7(17) . . . . ? C28 C33 C32 C31 -0.3(16) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.31 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.602 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.217 #==end data_Fe5 _database_code_depnum_ccdc_archive 'CCDC 798845' #TrackingRef 'CIF-for-chem.-commun.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H102 Cl4 Fe2 N6' _chemical_formula_weight 1713.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.245(3) _cell_length_b 16.820(3) _cell_length_c 24.704(5) _cell_angle_alpha 82.54(3) _cell_angle_beta 80.94(3) _cell_angle_gamma 88.01(3) _cell_volume 5388.5(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11776 _cell_measurement_theta_min 1.2211 _cell_measurement_theta_max 25.9594 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9523 _exptl_absorpt_correction_T_max 0.9837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 51617 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.1095 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 25.94 _reflns_number_total 20799 _reflns_number_gt 13635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+19.3648P] 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 20799 _refine_ls_number_parameters 1085 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.2625 _refine_ls_wR_factor_gt 0.2424 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.25945(6) 0.30808(4) 0.24891(3) 0.0283(2) Uani 1 1 d . . . Fe1 Fe 0.45922(6) 0.79951(4) 0.18851(3) 0.0296(2) Uani 1 1 d . . . Cl2A Cl 0.42814(11) 0.31224(8) 0.26759(6) 0.0371(3) Uani 1 1 d . . . Cl1A Cl 0.17360(12) 0.42671(8) 0.24576(7) 0.0395(4) Uani 1 1 d . . . Cl2 Cl 0.37589(12) 0.80767(9) 0.27841(7) 0.0431(4) Uani 1 1 d . . . Cl1 Cl 0.47232(13) 0.92077(8) 0.13582(7) 0.0419(4) Uani 1 1 d . . . N2A N 0.2767(3) 0.1870(3) 0.24412(19) 0.0290(10) Uani 1 1 d . . . N2 N 0.4856(3) 0.6765(3) 0.20544(18) 0.0269(10) Uani 1 1 d . . . N1 N 0.3392(4) 0.7413(3) 0.1577(2) 0.0317(10) Uani 1 1 d . . . N3 N 0.6240(3) 0.7812(2) 0.19602(18) 0.0266(10) Uani 1 1 d . . . C40 C 0.4065(4) 0.6269(3) 0.2057(2) 0.0289(12) Uani 1 1 d . . . N3A N 0.1744(3) 0.2482(3) 0.32640(18) 0.0285(10) Uani 1 1 d . . . N1A N 0.2907(4) 0.2953(3) 0.1611(2) 0.0314(10) Uani 1 1 d . . . C36A C 0.2522(4) 0.1335(3) 0.2893(2) 0.0297(12) Uani 1 1 d . . . C18 C 0.7508(4) 0.8601(3) 0.1300(2) 0.0327(13) Uani 1 1 d . . . C22A C 0.2862(5) 0.2580(4) 0.4410(2) 0.0353(13) Uani 1 1 d . . . C42 C 0.3245(4) 0.6656(3) 0.1754(2) 0.0327(13) Uani 1 1 d . . . C42A C 0.3272(4) 0.2272(3) 0.1488(2) 0.0308(12) Uani 1 1 d . . . C19A C 0.1062(4) 0.2915(3) 0.3638(2) 0.0320(12) Uani 1 1 d . . . C6 C 0.5577(5) 1.0154(4) 0.2793(3) 0.0440(16) Uani 1 1 d . . . H6A H 0.5271 1.0014 0.2496 0.053 Uiso 1 1 calc R . . C19 C 0.6982(4) 0.8456(3) 0.1826(2) 0.0248(11) Uani 1 1 d . . . C16 C 0.8382(4) 0.9702(3) 0.1587(2) 0.0328(13) Uani 1 1 d . . . C15 C 0.7810(4) 0.9554(3) 0.2111(3) 0.0324(13) Uani 1 1 d . . . H15A H 0.7915 0.9870 0.2388 0.039 Uiso 1 1 calc R . . C7A C -0.0315(5) 0.2545(3) 0.3109(3) 0.0350(13) Uani 1 1 d . . . H7AA H 0.0270 0.2584 0.2798 0.042 Uiso 1 1 calc R . . C34 C 0.7558(4) 0.6842(3) 0.2286(3) 0.0373(14) Uani 1 1 d . . . H34A H 0.8022 0.7297 0.2186 0.056 Uiso 1 1 calc R . . H34B H 0.7818 0.6405 0.2073 0.056 Uiso 1 1 calc R . . H34C H 0.7515 0.6656 0.2681 0.056 Uiso 1 1 calc R . . C34A C 0.1573(5) 0.1213(4) 0.3902(3) 0.0383(14) Uani 1 1 d . . . H34D H 0.1207 0.1549 0.4168 0.057 Uiso 1 1 calc R . . H34E H 0.2164 0.0955 0.4049 0.057 Uiso 1 1 calc R . . H34F H 0.1114 0.0802 0.3838 0.057 Uiso 1 1 calc R . . C43 C 0.2719(4) 0.7814(3) 0.1215(2) 0.0324(13) Uani 1 1 d . . . C41A C 0.3733(5) 0.2100(4) 0.0926(3) 0.0436(15) Uani 1 1 d . . . H41A H 0.4022 0.2592 0.0709 0.065 Uiso 1 1 calc R . . H41B H 0.3205 0.1902 0.0742 0.065 Uiso 1 1 calc R . . H41C H 0.4275 0.1692 0.0955 0.065 Uiso 1 1 calc R . . C8A C -0.1226(4) 0.2967(4) 0.2869(3) 0.0359(13) Uani 1 1 d . . . C17 C 0.8209(4) 0.9228(3) 0.1185(2) 0.0328(13) Uani 1 1 d . . . H17A H 0.8580 0.9335 0.0822 0.039 Uiso 1 1 calc R . . C1 C 0.6207(4) 0.9604(3) 0.3050(2) 0.0305(12) Uani 1 1 d . . . C40A C 0.3185(4) 0.1614(3) 0.1962(2) 0.0268(11) Uani 1 1 d . . . C39 C 0.4104(5) 0.5479(3) 0.2291(2) 0.0335(13) Uani 1 1 d . . . H39A H 0.3551 0.5132 0.2297 0.040 Uiso 1 1 calc R . . C37 C 0.5802(5) 0.5690(3) 0.2473(3) 0.0355(13) Uani 1 1 d . . . H37A H 0.6420 0.5492 0.2595 0.043 Uiso 1 1 calc R . . C38A C 0.3184(5) 0.0261(4) 0.2403(3) 0.0439(15) Uani 1 1 d . . . H38A H 0.3340 -0.0291 0.2387 0.053 Uiso 1 1 calc R . . C35 C 0.6518(4) 0.7098(3) 0.2159(2) 0.0289(12) Uani 1 1 d . . . C8 C 0.6876(5) 0.8134(3) 0.3189(2) 0.0337(13) Uani 1 1 d . . . C36 C 0.5701(4) 0.6494(3) 0.2241(2) 0.0327(13) Uani 1 1 d . . . C37A C 0.2723(4) 0.0515(3) 0.2893(3) 0.0330(13) Uani 1 1 d . . . H37B H 0.2548 0.0147 0.3217 0.040 Uiso 1 1 calc R . . C14A C 0.0036(4) 0.2966(4) 0.3563(2) 0.0337(13) Uani 1 1 d . . . C9 C 0.6232(5) 0.7532(3) 0.3488(3) 0.0407(15) Uani 1 1 d . . . H9A H 0.5523 0.7551 0.3463 0.049 Uiso 1 1 calc R . . C43A C 0.2762(5) 0.3606(3) 0.1185(2) 0.0368(14) Uani 1 1 d . . . C23A C 0.2250(5) 0.2290(4) 0.4909(3) 0.0412(15) Uani 1 1 d . . . H23A H 0.1625 0.2560 0.5021 0.049 Uiso 1 1 calc R . . C21 C 0.7324(4) 0.8087(3) 0.0856(2) 0.0313(12) Uani 1 1 d . . . H21A H 0.6584 0.7945 0.0938 0.038 Uiso 1 1 calc R . . C14 C 0.7088(4) 0.8950(3) 0.2237(2) 0.0289(12) Uani 1 1 d . . . C45 C 0.1191(5) 0.8498(4) 0.1040(3) 0.0403(15) Uani 1 1 d . . . H45A H 0.0526 0.8685 0.1176 0.048 Uiso 1 1 calc R . . C28 C 0.7486(5) 0.8571(3) 0.0271(2) 0.0358(13) Uani 1 1 d . . . C18A C 0.1417(4) 0.3338(4) 0.4011(2) 0.0364(13) Uani 1 1 d . . . C7 C 0.6435(5) 0.8811(3) 0.2816(2) 0.0321(12) Uani 1 1 d . . . H7A H 0.5761 0.8617 0.2756 0.039 Uiso 1 1 calc R . . C35A C 0.1927(4) 0.1722(3) 0.3371(2) 0.0297(12) Uani 1 1 d . . . C22 C 0.7914(5) 0.7305(4) 0.0890(3) 0.0376(14) Uani 1 1 d . . . C28A C 0.2964(4) 0.4087(4) 0.4183(3) 0.0356(13) Uani 1 1 d . . . C21A C 0.2574(4) 0.3312(4) 0.4040(3) 0.0376(14) Uani 1 1 d . . . H21B H 0.2928 0.3248 0.3659 0.045 Uiso 1 1 calc R . . C51A C 0.0944(5) 0.3097(5) 0.1295(3) 0.0552(19) Uani 1 1 d . . . H51A H 0.1227 0.2551 0.1258 0.066 Uiso 1 1 calc R . . H51B H 0.0778 0.3144 0.1694 0.066 Uiso 1 1 calc R . . C12 C 0.8308(6) 0.7452(4) 0.3554(3) 0.0476(17) Uani 1 1 d . . . H12A H 0.9017 0.7424 0.3580 0.057 Uiso 1 1 calc R . . C46 C 0.1536(5) 0.8628(4) 0.0479(3) 0.0427(15) Uani 1 1 d . . . C2 C 0.6650(5) 0.9817(4) 0.3482(3) 0.0384(14) Uani 1 1 d . . . H2A H 0.7098 0.9453 0.3657 0.046 Uiso 1 1 calc R . . C45A C 0.1612(5) 0.4362(4) 0.0654(3) 0.0450(16) Uani 1 1 d . . . H45B H 0.0960 0.4432 0.0538 0.054 Uiso 1 1 calc R . . C38 C 0.4971(5) 0.5199(4) 0.2517(3) 0.0434(15) Uani 1 1 d . . . H38B H 0.4989 0.4669 0.2703 0.052 Uiso 1 1 calc R . . C15A C -0.0638(5) 0.3413(4) 0.3902(3) 0.0415(15) Uani 1 1 d . . . H15B H -0.1341 0.3447 0.3863 0.050 Uiso 1 1 calc R . . C47A C 0.3328(5) 0.4811(4) 0.0591(3) 0.0427(15) Uani 1 1 d . . . H47A H 0.3849 0.5184 0.0436 0.051 Uiso 1 1 calc R . . C41 C 0.2415(5) 0.6153(4) 0.1657(3) 0.0406(14) Uani 1 1 d . . . H41D H 0.1936 0.6486 0.1458 0.061 Uiso 1 1 calc R . . H41E H 0.2053 0.5905 0.2012 0.061 Uiso 1 1 calc R . . H41F H 0.2706 0.5733 0.1436 0.061 Uiso 1 1 calc R . . C33 C 0.6817(6) 0.9204(4) 0.0151(3) 0.0449(16) Uani 1 1 d . . . H33A H 0.6255 0.9312 0.0423 0.054 Uiso 1 1 calc R . . C5 C 0.5385(5) 1.0910(4) 0.2962(3) 0.0455(16) Uani 1 1 d . . . H5A H 0.4948 1.1281 0.2782 0.055 Uiso 1 1 calc R . . C3 C 0.6435(5) 1.0564(4) 0.3655(3) 0.0465(16) Uani 1 1 d . . . H3A H 0.6711 1.0696 0.3963 0.056 Uiso 1 1 calc R . . C13 C 0.7911(5) 0.8099(3) 0.3221(2) 0.0369(14) Uani 1 1 d . . . H13A H 0.8352 0.8505 0.3020 0.044 Uiso 1 1 calc R . . C48A C 0.3546(5) 0.4152(4) 0.0976(2) 0.0370(13) Uani 1 1 d . . . C4 C 0.5830(5) 1.1119(4) 0.3389(3) 0.0415(15) Uani 1 1 d . . . H4A H 0.5722 1.1640 0.3500 0.050 Uiso 1 1 calc R . . C10A C -0.2935(5) 0.3014(4) 0.2648(3) 0.0516(18) Uani 1 1 d . . . H10A H -0.3583 0.2770 0.2689 0.062 Uiso 1 1 calc R . . C44A C 0.1773(5) 0.3700(3) 0.1038(3) 0.0398(14) Uani 1 1 d . . . C26 C 0.7943(7) 0.5870(4) 0.0914(3) 0.063(2) Uani 1 1 d . . . H26A H 0.7590 0.5394 0.0900 0.075 Uiso 1 1 calc R . . C49 C 0.4250(6) 0.7752(4) 0.0420(3) 0.0549(18) Uani 1 1 d . . . H49A H 0.4474 0.8111 0.0075 0.066 Uiso 1 1 calc R . . H49B H 0.4698 0.7844 0.0690 0.066 Uiso 1 1 calc R . . C48 C 0.3123(5) 0.7972(4) 0.0653(3) 0.0402(14) Uani 1 1 d . . . C27 C 0.7433(5) 0.6590(4) 0.0868(3) 0.0455(16) Uani 1 1 d . . . H27A H 0.6735 0.6603 0.0820 0.055 Uiso 1 1 calc R . . C11A C -0.2757(5) 0.3752(4) 0.2333(3) 0.0486(17) Uani 1 1 d . . . H11A H -0.3281 0.4008 0.2148 0.058 Uiso 1 1 calc R . . C27A C 0.3779(6) 0.2155(4) 0.4252(3) 0.0528(18) Uani 1 1 d . . . H27B H 0.4206 0.2329 0.3914 0.063 Uiso 1 1 calc R . . C29 C 0.8291(5) 0.8413(4) -0.0139(3) 0.0427(15) Uani 1 1 d . . . H29A H 0.8750 0.7979 -0.0070 0.051 Uiso 1 1 calc R . . C12A C -0.1839(6) 0.4116(4) 0.2285(3) 0.0534(18) Uani 1 1 d . . . H12B H -0.1725 0.4629 0.2076 0.064 Uiso 1 1 calc R . . C33A C 0.3320(5) 0.4141(4) 0.4675(3) 0.0453(16) Uani 1 1 d . . . H33B H 0.3310 0.3678 0.4941 0.054 Uiso 1 1 calc R . . C10 C 0.6630(6) 0.6906(4) 0.3822(3) 0.0510(18) Uani 1 1 d . . . H10B H 0.6189 0.6510 0.4035 0.061 Uiso 1 1 calc R . . C47 C 0.2502(5) 0.8361(4) 0.0291(3) 0.0447(16) Uani 1 1 d . . . H47B H 0.2754 0.8444 -0.0093 0.054 Uiso 1 1 calc R . . C9A C -0.2158(5) 0.2635(4) 0.2904(3) 0.0450(16) Uani 1 1 d . . . H9AA H -0.2282 0.2122 0.3112 0.054 Uiso 1 1 calc R . . C11 C 0.7662(7) 0.6862(4) 0.3842(3) 0.056(2) Uani 1 1 d . . . H11B H 0.7934 0.6420 0.4057 0.067 Uiso 1 1 calc R . . C17A C 0.0732(5) 0.3769(4) 0.4334(3) 0.0466(16) Uani 1 1 d . . . H17B H 0.0971 0.4053 0.4596 0.056 Uiso 1 1 calc R . . C39A C 0.3424(4) 0.0818(3) 0.1929(3) 0.0349(13) Uani 1 1 d . . . H39B H 0.3747 0.0648 0.1591 0.042 Uiso 1 1 calc R . . C44 C 0.1793(5) 0.8095(4) 0.1424(3) 0.0405(15) Uani 1 1 d . B . C26A C 0.4057(6) 0.1482(5) 0.4591(3) 0.059(2) Uani 1 1 d . . . H26B H 0.4683 0.1212 0.4481 0.070 Uiso 1 1 calc R . . C29A C 0.2993(6) 0.4775(4) 0.3793(3) 0.0561(19) Uani 1 1 d . . . H29B H 0.2754 0.4750 0.3452 0.067 Uiso 1 1 calc R . . C46A C 0.2359(6) 0.4919(4) 0.0435(3) 0.0464(17) Uani 1 1 d . . . C31 C 0.7824(7) 0.9521(5) -0.0769(3) 0.064(2) Uani 1 1 d . . . H31A H 0.7962 0.9854 -0.1113 0.077 Uiso 1 1 calc R . . C23 C 0.8922(5) 0.7275(4) 0.0952(3) 0.0445(15) Uani 1 1 d . . . H23B H 0.9251 0.7761 0.0972 0.053 Uiso 1 1 calc R . . C49A C 0.4580(5) 0.4018(4) 0.1159(3) 0.0420(15) Uani 1 1 d . . . H49C H 0.4908 0.3541 0.1004 0.050 Uiso 1 1 calc R . . H49D H 0.4479 0.3896 0.1566 0.050 Uiso 1 1 calc R . . C32 C 0.6953(6) 0.9675(4) -0.0353(3) 0.056(2) Uani 1 1 d . . . H32A H 0.6483 1.0099 -0.0430 0.067 Uiso 1 1 calc R . . C20 C 0.9154(5) 1.0358(4) 0.1446(3) 0.0459(16) Uani 1 1 d . . . H20A H 0.9219 1.0597 0.1780 0.069 Uiso 1 1 calc R . . H20B H 0.8930 1.0770 0.1170 0.069 Uiso 1 1 calc R . . H20C H 0.9817 1.0135 0.1296 0.069 Uiso 1 1 calc R . . C2A C -0.0142(6) 0.1111(4) 0.2915(4) 0.071(3) Uani 1 1 d . . . H2AA H 0.0159 0.1304 0.2549 0.086 Uiso 1 1 calc R . . C25A C 0.3459(7) 0.1196(5) 0.5076(3) 0.061(2) Uani 1 1 d . . . H25A H 0.3654 0.0729 0.5297 0.073 Uiso 1 1 calc R . . C13A C -0.1057(5) 0.3719(4) 0.2549(3) 0.0460(16) Uani 1 1 d . . . H13B H -0.0409 0.3963 0.2510 0.055 Uiso 1 1 calc R . . C24A C 0.2533(6) 0.1621(5) 0.5241(3) 0.0545(19) Uani 1 1 d . . . H24A H 0.2111 0.1443 0.5580 0.065 Uiso 1 1 calc R . . C1A C -0.0478(5) 0.1654(4) 0.3287(3) 0.0519(18) Uani 1 1 d . . . C16A C -0.0290(5) 0.3807(5) 0.4295(3) 0.0535(19) Uani 1 1 d . . . C30A C 0.3366(6) 0.5489(5) 0.3897(4) 0.065(2) Uani 1 1 d . . . H30A H 0.3372 0.5952 0.3632 0.078 Uiso 1 1 calc R . . C25 C 0.8946(6) 0.5820(4) 0.0980(4) 0.064(2) Uani 1 1 d . . . H25B H 0.9282 0.5312 0.1020 0.076 Uiso 1 1 calc R . . C53A C 0.2102(6) 0.5659(4) 0.0059(3) 0.0532(18) Uani 1 1 d . . . H53A H 0.1445 0.5586 -0.0062 0.080 Uiso 1 1 calc R . . H53B H 0.2638 0.5741 -0.0265 0.080 Uiso 1 1 calc R . . H53C H 0.2057 0.6128 0.0259 0.080 Uiso 1 1 calc R . . C6A C -0.0944(6) 0.1374(5) 0.3814(4) 0.066(2) Uani 1 1 d . . . H6AA H -0.1201 0.1735 0.4071 0.079 Uiso 1 1 calc R . . C30 C 0.8421(6) 0.8881(4) -0.0640(3) 0.0529(18) Uani 1 1 d . . . H30B H 0.8965 0.8747 -0.0914 0.064 Uiso 1 1 calc R . . C32A C 0.3693(6) 0.4859(5) 0.4792(3) 0.0532(18) Uani 1 1 d . . . H32B H 0.3915 0.4891 0.5136 0.064 Uiso 1 1 calc R . . C51 C 0.1372(6) 0.7944(5) 0.2043(3) 0.061(2) Uani 1 1 d D . . H51C H 0.1363 0.7356 0.2151 0.073 Uiso 1 1 calc R A 1 H51D H 0.1869 0.8163 0.2243 0.073 Uiso 1 1 calc R A 1 C53 C 0.0867(6) 0.9059(4) 0.0079(3) 0.0548(19) Uani 1 1 d . . . H53D H 0.1113 0.8929 -0.0295 0.082 Uiso 1 1 calc R . . H53E H 0.0899 0.9639 0.0083 0.082 Uiso 1 1 calc R . . H53F H 0.0158 0.8885 0.0193 0.082 Uiso 1 1 calc R . . C50A C 0.5306(6) 0.4716(4) 0.0990(3) 0.0570(19) Uani 1 1 d . . . H50A H 0.5952 0.4579 0.1128 0.085 Uiso 1 1 calc R . . H50B H 0.4998 0.5191 0.1146 0.085 Uiso 1 1 calc R . . H50C H 0.5436 0.4830 0.0586 0.085 Uiso 1 1 calc R . . C31A C 0.3731(6) 0.5526(5) 0.4389(4) 0.068(2) Uani 1 1 d . . . H31B H 0.4010 0.6012 0.4452 0.081 Uiso 1 1 calc R . . C24 C 0.9496(7) 0.6546(5) 0.0988(3) 0.064(2) Uani 1 1 d . . . H24B H 1.0203 0.6535 0.1016 0.076 Uiso 1 1 calc R . . C3A C -0.0242(8) 0.0276(5) 0.3074(6) 0.089(3) Uani 1 1 d . . . H3AA H -0.0005 -0.0096 0.2822 0.107 Uiso 1 1 calc R . . C5A C -0.1030(7) 0.0528(6) 0.3963(6) 0.094(4) Uani 1 1 d . . . H5AA H -0.1334 0.0329 0.4328 0.113 Uiso 1 1 calc R . . C50 C 0.4375(7) 0.6904(5) 0.0304(4) 0.076(3) Uani 1 1 d . . . H50D H 0.5102 0.6754 0.0259 0.114 Uiso 1 1 calc R . . H50E H 0.4104 0.6848 -0.0036 0.114 Uiso 1 1 calc R . . H50F H 0.4001 0.6553 0.0613 0.114 Uiso 1 1 calc R . . C20A C -0.1050(6) 0.4314(7) 0.4662(4) 0.092(4) Uani 1 1 d . . . H20D H -0.1728 0.4073 0.4727 0.138 Uiso 1 1 calc R . . H20E H -0.1090 0.4862 0.4474 0.138 Uiso 1 1 calc R . . H20F H -0.0810 0.4327 0.5016 0.138 Uiso 1 1 calc R . . C4A C -0.0704(8) 0.0014(6) 0.3615(6) 0.090(4) Uani 1 1 d . . . H4AA H -0.0782 -0.0545 0.3732 0.108 Uiso 1 1 calc R . . C52A C -0.0043(6) 0.3184(5) 0.1049(4) 0.070(2) Uani 1 1 d . . . H52A H -0.0544 0.2801 0.1261 0.105 Uiso 1 1 calc R . . H52B H 0.0094 0.3077 0.0664 0.105 Uiso 1 1 calc R . . H52C H -0.0317 0.3731 0.1065 0.105 Uiso 1 1 calc R . . C52 C 0.0355(12) 0.8263(14) 0.2248(7) 0.074(5) Uani 0.53(2) 1 d PDU B 1 H52D H 0.0228 0.8163 0.2653 0.111 Uiso 0.53(2) 1 calc PR B 1 H52E H -0.0168 0.7997 0.2099 0.111 Uiso 0.53(2) 1 calc PR B 1 H52F H 0.0326 0.8841 0.2130 0.111 Uiso 0.53(2) 1 calc PR B 1 C52' C 0.089(2) 0.8676(12) 0.2248(9) 0.081(6) Uani 0.47(2) 1 d PDU B 2 H52G H 0.0491 0.8535 0.2614 0.121 Uiso 0.47(2) 1 calc PR B 2 H52H H 0.0445 0.8926 0.1992 0.121 Uiso 0.47(2) 1 calc PR B 2 H52I H 0.1427 0.9053 0.2273 0.121 Uiso 0.47(2) 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 Fe1A 0.0287(4) 0.0226(4) 0.0333(4) -0.0049(3) -0.0029(3) -0.0009(3) Fe1 0.0319(4) 0.0215(4) 0.0366(5) -0.0037(3) -0.0089(4) 0.0002(3) Cl2A 0.0316(7) 0.0309(7) 0.0496(9) -0.0043(6) -0.0080(6) -0.0052(6) Cl1A 0.0395(8) 0.0254(7) 0.0513(9) -0.0036(6) -0.0013(7) 0.0041(6) Cl2 0.0438(9) 0.0432(8) 0.0421(9) -0.0085(7) -0.0040(7) -0.0012(7) Cl1 0.0521(9) 0.0231(7) 0.0486(9) 0.0012(6) -0.0077(7) 0.0032(6) N2A 0.030(2) 0.025(2) 0.033(3) 0.0013(19) -0.009(2) -0.0068(19) N2 0.026(2) 0.028(2) 0.027(2) -0.0014(18) -0.0087(19) 0.0039(18) N1 0.034(3) 0.027(2) 0.035(3) -0.008(2) -0.004(2) -0.002(2) N3 0.033(3) 0.021(2) 0.027(2) -0.0048(17) -0.0070(19) -0.0091(18) C40 0.029(3) 0.022(3) 0.037(3) -0.001(2) -0.010(2) -0.004(2) N3A 0.031(3) 0.029(2) 0.027(2) -0.0082(18) -0.0051(19) -0.0034(19) N1A 0.033(3) 0.025(2) 0.037(3) -0.0013(19) -0.007(2) -0.0080(19) C36A 0.029(3) 0.025(3) 0.036(3) -0.002(2) -0.010(2) -0.007(2) C18 0.029(3) 0.030(3) 0.041(3) -0.002(2) -0.011(3) -0.006(2) C22A 0.035(3) 0.043(3) 0.031(3) -0.008(3) -0.012(3) 0.003(3) C42 0.035(3) 0.031(3) 0.032(3) -0.008(2) 0.002(2) -0.005(2) C42A 0.029(3) 0.030(3) 0.035(3) -0.009(2) -0.004(2) -0.001(2) C19A 0.031(3) 0.031(3) 0.034(3) -0.004(2) -0.005(2) -0.003(2) C6 0.055(4) 0.035(3) 0.045(4) -0.012(3) -0.015(3) 0.013(3) C19 0.030(3) 0.023(2) 0.024(3) -0.003(2) -0.011(2) -0.005(2) C16 0.032(3) 0.029(3) 0.037(3) -0.002(2) -0.005(3) 0.001(2) C15 0.026(3) 0.029(3) 0.044(3) -0.007(2) -0.011(3) -0.001(2) C7A 0.032(3) 0.035(3) 0.041(3) -0.007(3) -0.010(3) -0.009(2) C34 0.031(3) 0.028(3) 0.055(4) -0.005(3) -0.013(3) 0.001(2) C34A 0.037(3) 0.036(3) 0.043(4) -0.003(3) -0.007(3) -0.004(3) C43 0.034(3) 0.023(3) 0.041(3) 0.000(2) -0.011(3) -0.003(2) C41A 0.045(4) 0.037(3) 0.046(4) -0.005(3) 0.001(3) -0.006(3) C8A 0.028(3) 0.037(3) 0.045(4) -0.008(3) -0.013(3) 0.002(2) C17 0.032(3) 0.030(3) 0.033(3) 0.003(2) -0.002(2) -0.007(2) C1 0.030(3) 0.035(3) 0.026(3) -0.005(2) 0.002(2) -0.008(2) C40A 0.027(3) 0.026(3) 0.028(3) -0.008(2) -0.004(2) -0.007(2) C39 0.039(3) 0.028(3) 0.033(3) -0.006(2) -0.001(3) -0.007(2) C37 0.037(3) 0.022(3) 0.048(4) 0.000(2) -0.014(3) -0.002(2) C38A 0.050(4) 0.030(3) 0.055(4) -0.011(3) -0.015(3) -0.004(3) C35 0.027(3) 0.023(3) 0.037(3) 0.001(2) -0.008(2) -0.005(2) C8 0.041(3) 0.027(3) 0.032(3) -0.004(2) -0.001(3) 0.005(2) C36 0.037(3) 0.022(3) 0.039(3) -0.007(2) -0.001(3) -0.005(2) C37A 0.030(3) 0.028(3) 0.042(3) 0.003(2) -0.012(3) -0.004(2) C14A 0.026(3) 0.040(3) 0.036(3) -0.002(2) -0.009(2) 0.000(2) C9 0.043(4) 0.031(3) 0.044(4) 0.005(3) -0.002(3) -0.003(3) C43A 0.047(4) 0.030(3) 0.032(3) -0.002(2) -0.008(3) 0.008(3) C23A 0.037(3) 0.048(4) 0.040(4) -0.009(3) -0.009(3) 0.005(3) C21 0.031(3) 0.023(3) 0.041(3) -0.003(2) -0.008(3) -0.002(2) C14 0.024(3) 0.029(3) 0.035(3) -0.003(2) -0.008(2) -0.003(2) C45 0.027(3) 0.044(3) 0.050(4) 0.002(3) -0.013(3) -0.005(3) C28 0.050(4) 0.029(3) 0.030(3) -0.005(2) -0.011(3) -0.003(3) C18A 0.030(3) 0.050(4) 0.030(3) -0.009(3) -0.004(2) 0.001(3) C7 0.039(3) 0.030(3) 0.029(3) -0.004(2) -0.012(2) 0.004(2) C35A 0.030(3) 0.028(3) 0.031(3) 0.001(2) -0.007(2) -0.003(2) C22 0.037(3) 0.040(3) 0.038(3) -0.017(3) -0.001(3) -0.004(3) C28A 0.031(3) 0.037(3) 0.038(3) -0.009(3) -0.002(3) 0.005(2) C21A 0.028(3) 0.045(3) 0.043(4) -0.015(3) -0.011(3) 0.005(3) C51A 0.043(4) 0.056(4) 0.068(5) -0.004(4) -0.016(4) -0.003(3) C12 0.062(5) 0.043(4) 0.043(4) -0.003(3) -0.027(3) 0.011(3) C46 0.043(4) 0.045(4) 0.045(4) 0.000(3) -0.021(3) -0.006(3) C2 0.042(4) 0.036(3) 0.039(3) -0.011(3) -0.010(3) 0.009(3) C45A 0.049(4) 0.046(4) 0.041(4) -0.009(3) -0.011(3) 0.012(3) C38 0.049(4) 0.030(3) 0.052(4) 0.002(3) -0.017(3) 0.004(3) C15A 0.028(3) 0.057(4) 0.040(4) -0.014(3) -0.003(3) 0.012(3) C47A 0.054(4) 0.039(3) 0.033(3) -0.008(3) -0.002(3) 0.006(3) C41 0.034(3) 0.034(3) 0.054(4) -0.004(3) -0.010(3) -0.004(3) C33 0.059(4) 0.042(4) 0.037(4) -0.005(3) -0.018(3) -0.006(3) C5 0.039(4) 0.038(3) 0.059(4) -0.005(3) -0.009(3) 0.010(3) C3 0.045(4) 0.040(3) 0.059(4) -0.021(3) -0.009(3) -0.006(3) C13 0.047(4) 0.030(3) 0.035(3) -0.005(2) -0.010(3) 0.006(3) C48A 0.042(3) 0.037(3) 0.030(3) -0.003(2) -0.001(3) -0.001(3) C4 0.042(4) 0.026(3) 0.056(4) -0.012(3) -0.003(3) 0.000(3) C10A 0.033(4) 0.053(4) 0.075(5) -0.022(4) -0.017(3) 0.003(3) C44A 0.051(4) 0.030(3) 0.039(3) -0.008(3) -0.007(3) -0.001(3) C26 0.075(6) 0.038(4) 0.073(6) -0.010(4) -0.004(4) 0.008(4) C49 0.068(5) 0.045(4) 0.048(4) -0.005(3) 0.002(4) 0.000(4) C48 0.042(4) 0.042(3) 0.040(4) -0.011(3) -0.012(3) 0.003(3) C27 0.045(4) 0.045(4) 0.044(4) -0.010(3) 0.006(3) -0.009(3) C11A 0.036(4) 0.056(4) 0.058(4) -0.011(3) -0.017(3) 0.020(3) C27A 0.054(4) 0.054(4) 0.049(4) 0.001(3) -0.015(3) 0.016(3) C29 0.044(4) 0.044(4) 0.043(4) -0.010(3) -0.011(3) -0.010(3) C12A 0.061(5) 0.048(4) 0.053(4) -0.002(3) -0.024(4) 0.015(3) C33A 0.043(4) 0.047(4) 0.047(4) -0.010(3) -0.009(3) -0.005(3) C10 0.052(4) 0.036(3) 0.059(5) 0.002(3) 0.003(3) -0.001(3) C47 0.052(4) 0.050(4) 0.030(3) -0.005(3) -0.003(3) 0.006(3) C9A 0.033(3) 0.044(4) 0.055(4) -0.001(3) -0.002(3) -0.002(3) C11 0.090(6) 0.034(3) 0.043(4) 0.004(3) -0.017(4) 0.015(4) C17A 0.033(3) 0.070(5) 0.041(4) -0.023(3) -0.006(3) 0.007(3) C39A 0.035(3) 0.028(3) 0.042(3) -0.006(2) -0.004(3) -0.005(2) C44 0.036(3) 0.035(3) 0.049(4) 0.003(3) -0.009(3) -0.002(3) C26A 0.062(5) 0.055(4) 0.050(4) 0.002(3) 0.005(4) 0.019(4) C29A 0.065(5) 0.046(4) 0.065(5) -0.019(3) -0.019(4) -0.002(3) C46A 0.072(5) 0.035(3) 0.028(3) -0.004(3) 0.004(3) 0.007(3) C31 0.102(7) 0.058(5) 0.034(4) 0.009(3) -0.015(4) -0.049(5) C23 0.046(4) 0.045(4) 0.046(4) -0.017(3) -0.008(3) 0.005(3) C49A 0.046(4) 0.037(3) 0.041(4) 0.004(3) -0.006(3) -0.006(3) C32 0.085(6) 0.030(3) 0.060(5) 0.005(3) -0.040(4) -0.011(3) C20 0.052(4) 0.040(3) 0.043(4) 0.004(3) -0.004(3) -0.025(3) C2A 0.068(5) 0.030(3) 0.135(8) -0.020(4) -0.070(6) 0.006(3) C25A 0.087(6) 0.051(4) 0.050(5) -0.012(3) -0.020(4) 0.014(4) C13A 0.041(4) 0.043(4) 0.053(4) -0.004(3) -0.005(3) -0.012(3) C24A 0.068(5) 0.064(5) 0.029(4) 0.003(3) -0.005(3) -0.008(4) C1A 0.044(4) 0.035(3) 0.081(5) -0.007(3) -0.021(4) -0.005(3) C16A 0.041(4) 0.074(5) 0.054(4) -0.031(4) -0.019(3) 0.018(4) C30A 0.065(5) 0.047(4) 0.087(6) -0.010(4) -0.022(5) 0.000(4) C25 0.062(5) 0.041(4) 0.084(6) -0.006(4) -0.003(4) 0.014(4) C53A 0.068(5) 0.048(4) 0.040(4) 0.003(3) -0.007(3) 0.009(3) C6A 0.044(4) 0.056(5) 0.095(7) 0.015(4) -0.020(4) -0.010(4) C30 0.055(4) 0.055(4) 0.048(4) -0.005(3) -0.001(3) -0.025(4) C32A 0.052(4) 0.063(5) 0.050(4) -0.020(4) -0.010(3) -0.006(4) C51 0.061(5) 0.075(5) 0.046(4) -0.007(4) -0.010(4) 0.017(4) C53 0.056(5) 0.056(4) 0.054(4) 0.007(3) -0.026(4) -0.002(4) C50A 0.061(5) 0.056(4) 0.050(4) 0.002(3) 0.002(4) -0.019(4) C31A 0.062(5) 0.056(5) 0.094(7) -0.044(5) -0.012(5) 0.005(4) C24 0.062(5) 0.057(5) 0.070(5) -0.012(4) -0.004(4) 0.020(4) C3A 0.092(7) 0.045(5) 0.146(11) -0.023(6) -0.058(7) 0.003(5) C5A 0.052(5) 0.057(6) 0.161(11) 0.043(7) -0.023(6) -0.015(4) C50 0.092(7) 0.051(5) 0.073(6) 0.000(4) 0.018(5) 0.004(4) C20A 0.048(5) 0.150(10) 0.094(7) -0.084(7) -0.013(5) 0.029(6) C4A 0.074(7) 0.046(5) 0.156(11) 0.010(6) -0.057(7) -0.007(5) C52A 0.057(5) 0.071(6) 0.079(6) 0.000(5) -0.012(4) 0.004(4) C52 0.065(8) 0.089(9) 0.065(8) -0.004(7) -0.006(6) 0.012(7) C52' 0.089(10) 0.081(9) 0.071(9) -0.013(7) -0.009(7) 0.016(7) _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 Fe1A N2A 2.058(4) . ? Fe1A N1A 2.182(5) . ? Fe1A N3A 2.202(5) . ? Fe1A Cl1A 2.2607(17) . ? Fe1A Cl2A 2.3567(17) . ? Fe1 N2 2.085(4) . ? Fe1 N1 2.179(5) . ? Fe1 N3 2.227(5) . ? Fe1 Cl1 2.2689(17) . ? Fe1 Cl2 2.3379(19) . ? N2A C40A 1.343(7) . ? N2A C36A 1.343(7) . ? N2 C36 1.322(7) . ? N2 C40 1.360(7) . ? N1 C42 1.303(7) . ? N1 C43 1.450(7) . ? N3 C35 1.301(7) . ? N3 C19 1.458(6) . ? C40 C39 1.381(7) . ? C40 C42 1.499(8) . ? N3A C35A 1.294(7) . ? N3A C19A 1.438(7) . ? N1A C42A 1.281(7) . ? N1A C43A 1.448(7) . ? C36A C37A 1.395(8) . ? C36A C35A 1.521(8) . ? C18 C19 1.370(8) . ? C18 C17 1.400(8) . ? C18 C21 1.535(8) . ? C22A C23A 1.404(9) . ? C22A C27A 1.414(9) . ? C22A C21A 1.512(8) . ? C42 C41 1.477(8) . ? C42A C41A 1.487(8) . ? C42A C40A 1.497(8) . ? C19A C18A 1.380(8) . ? C19A C14A 1.399(8) . ? C6 C1 1.385(8) . ? C6 C5 1.392(9) . ? C6 H6A 0.9500 . ? C19 C14 1.418(7) . ? C16 C15 1.390(8) . ? C16 C17 1.403(8) . ? C16 C20 1.499(8) . ? C15 C14 1.390(7) . ? C15 H15A 0.9500 . ? C7A C1A 1.519(8) . ? C7A C14A 1.536(8) . ? C7A C8A 1.540(8) . ? C7A H7AA 1.0000 . ? C34 C35 1.497(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34A C35A 1.487(8) . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C43 C44 1.348(8) . ? C43 C48 1.402(9) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C8A C9A 1.358(8) . ? C8A C13A 1.407(9) . ? C17 H17A 0.9500 . ? C1 C2 1.387(8) . ? C1 C7 1.522(8) . ? C40A C39A 1.374(8) . ? C39 C38 1.397(8) . ? C39 H39A 0.9500 . ? C37 C38 1.381(8) . ? C37 C36 1.410(7) . ? C37 H37A 0.9500 . ? C38A C37A 1.379(9) . ? C38A C39A 1.403(9) . ? C38A H38A 0.9500 . ? C35 C36 1.483(7) . ? C8 C13 1.385(8) . ? C8 C9 1.402(8) . ? C8 C7 1.531(7) . ? C37A H37B 0.9500 . ? C14A C15A 1.395(8) . ? C9 C10 1.392(9) . ? C9 H9A 0.9500 . ? C43A C48A 1.400(9) . ? C43A C44A 1.413(9) . ? C23A C24A 1.381(9) . ? C23A H23A 0.9500 . ? C21 C22 1.507(8) . ? C21 C28 1.551(8) . ? C21 H21A 1.0000 . ? C14 C7 1.545(8) . ? C45 C46 1.382(9) . ? C45 C44 1.424(8) . ? C45 H45A 0.9500 . ? C28 C33 1.394(9) . ? C28 C29 1.394(9) . ? C18A C17A 1.366(8) . ? C18A C21A 1.543(8) . ? C7 H7A 1.0000 . ? C22 C23 1.366(9) . ? C22 C27 1.390(9) . ? C28A C33A 1.386(9) . ? C28A C29A 1.404(10) . ? C28A C21A 1.521(8) . ? C21A H21B 1.0000 . ? C51A C52A 1.521(10) . ? C51A C44A 1.526(9) . ? C51A H51A 0.9900 . ? C51A H51B 0.9900 . ? C12 C11 1.382(10) . ? C12 C13 1.415(8) . ? C12 H12A 0.9500 . ? C46 C47 1.372(9) . ? C46 C53 1.527(8) . ? C2 C3 1.385(8) . ? C2 H2A 0.9500 . ? C45A C46A 1.384(10) . ? C45A C44A 1.399(9) . ? C45A H45B 0.9500 . ? C38 H38B 0.9500 . ? C15A C16A 1.387(9) . ? C15A H15B 0.9500 . ? C47A C46A 1.396(10) . ? C47A C48A 1.418(8) . ? C47A H47A 0.9500 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C33 C32 1.377(9) . ? C33 H33A 0.9500 . ? C5 C4 1.377(9) . ? C5 H5A 0.9500 . ? C3 C4 1.378(9) . ? C3 H3A 0.9500 . ? C13 H13A 0.9500 . ? C48A C49A 1.509(9) . ? C4 H4A 0.9500 . ? C10A C11A 1.384(10) . ? C10A C9A 1.385(9) . ? C10A H10A 0.9500 . ? C26 C25 1.362(11) . ? C26 C27 1.367(10) . ? C26 H26A 0.9500 . ? C49 C50 1.489(10) . ? C49 C48 1.563(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C48 C47 1.394(9) . ? C27 H27A 0.9500 . ? C11A C12A 1.362(10) . ? C11A H11A 0.9500 . ? C27A C26A 1.392(9) . ? C27A H27B 0.9500 . ? C29 C30 1.368(9) . ? C29 H29A 0.9500 . ? C12A C13A 1.413(9) . ? C12A H12B 0.9500 . ? C33A C32A 1.401(9) . ? C33A H33B 0.9500 . ? C10 C11 1.375(10) . ? C10 H10B 0.9500 . ? C47 H47B 0.9500 . ? C9A H9AA 0.9500 . ? C11 H11B 0.9500 . ? C17A C16A 1.370(9) . ? C17A H17B 0.9500 . ? C39A H39B 0.9500 . ? C44 C51 1.533(10) . ? C26A C25A 1.369(11) . ? C26A H26B 0.9500 . ? C29A C30A 1.384(10) . ? C29A H29B 0.9500 . ? C46A C53A 1.516(9) . ? C31 C30 1.349(11) . ? C31 C32 1.458(12) . ? C31 H31A 0.9500 . ? C23 C24 1.422(9) . ? C23 H23B 0.9500 . ? C49A C50A 1.517(9) . ? C49A H49C 0.9900 . ? C49A H49D 0.9900 . ? C32 H32A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C2A C1A 1.393(11) . ? C2A C3A 1.414(11) . ? C2A H2AA 0.9500 . ? C25A C24A 1.427(11) . ? C25A H25A 0.9500 . ? C13A H13B 0.9500 . ? C24A H24A 0.9500 . ? C1A C6A 1.381(11) . ? C16A C20A 1.555(10) . ? C30A C31A 1.385(12) . ? C30A H30A 0.9500 . ? C25 C24 1.447(11) . ? C25 H25B 0.9500 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C6A C5A 1.427(11) . ? C6A H6AA 0.9500 . ? C30 H30B 0.9500 . ? C32A C31A 1.398(12) . ? C32A H32B 0.9500 . ? C51 C52 1.472(13) . ? C51 C52' 1.477(14) . ? C51 H51C 0.9900 . ? C51 H51D 0.9900 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9800 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C31A H31B 0.9500 . ? C24 H24B 0.9500 . ? C3A C4A 1.401(15) . ? C3A H3AA 0.9500 . ? C5A C4A 1.313(15) . ? C5A H5AA 0.9500 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C4A H4AA 0.9500 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C52 H52D 0.9800 . ? C52 H52E 0.9800 . ? C52 H52F 0.9800 . ? C52' H52G 0.9800 . ? C52' H52H 0.9800 . ? C52' H52I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2A Fe1A N1A 73.83(18) . . ? N2A Fe1A N3A 74.13(17) . . ? N1A Fe1A N3A 139.81(16) . . ? N2A Fe1A Cl1A 154.78(14) . . ? N1A Fe1A Cl1A 100.17(13) . . ? N3A Fe1A Cl1A 98.54(13) . . ? N2A Fe1A Cl2A 89.92(13) . . ? N1A Fe1A Cl2A 99.79(13) . . ? N3A Fe1A Cl2A 103.78(13) . . ? Cl1A Fe1A Cl2A 115.30(7) . . ? N2 Fe1 N1 73.92(17) . . ? N2 Fe1 N3 72.42(16) . . ? N1 Fe1 N3 139.11(17) . . ? N2 Fe1 Cl1 155.08(14) . . ? N1 Fe1 Cl1 103.20(14) . . ? N3 Fe1 Cl1 97.72(12) . . ? N2 Fe1 Cl2 92.34(13) . . ? N1 Fe1 Cl2 98.60(14) . . ? N3 Fe1 Cl2 105.27(13) . . ? Cl1 Fe1 Cl2 112.48(7) . . ? C40A N2A C36A 119.5(5) . . ? C40A N2A Fe1A 119.7(3) . . ? C36A N2A Fe1A 120.6(4) . . ? C36 N2 C40 121.1(5) . . ? C36 N2 Fe1 120.3(4) . . ? C40 N2 Fe1 117.6(3) . . ? C42 N1 C43 118.0(5) . . ? C42 N1 Fe1 116.9(4) . . ? C43 N1 Fe1 125.0(3) . . ? C35 N3 C19 120.1(4) . . ? C35 N3 Fe1 116.7(3) . . ? C19 N3 Fe1 123.2(3) . . ? N2 C40 C39 120.3(5) . . ? N2 C40 C42 113.1(4) . . ? C39 C40 C42 126.4(5) . . ? C35A N3A C19A 122.2(5) . . ? C35A N3A Fe1A 115.7(4) . . ? C19A N3A Fe1A 122.0(3) . . ? C42A N1A C43A 121.3(5) . . ? C42A N1A Fe1A 116.1(4) . . ? C43A N1A Fe1A 122.5(4) . . ? N2A C36A C37A 122.6(5) . . ? N2A C36A C35A 111.9(5) . . ? C37A C36A C35A 125.3(5) . . ? C19 C18 C17 118.0(5) . . ? C19 C18 C21 120.4(5) . . ? C17 C18 C21 121.7(5) . . ? C23A C22A C27A 117.6(6) . . ? C23A C22A C21A 122.8(5) . . ? C27A C22A C21A 119.6(6) . . ? N1 C42 C41 127.3(6) . . ? N1 C42 C40 113.9(5) . . ? C41 C42 C40 118.7(5) . . ? N1A C42A C41A 125.3(5) . . ? N1A C42A C40A 114.9(5) . . ? C41A C42A C40A 119.8(5) . . ? C18A C19A C14A 121.2(5) . . ? C18A C19A N3A 121.7(5) . . ? C14A C19A N3A 116.6(5) . . ? C1 C6 C5 121.1(6) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C18 C19 C14 121.7(5) . . ? C18 C19 N3 119.5(5) . . ? C14 C19 N3 118.7(5) . . ? C15 C16 C17 118.1(5) . . ? C15 C16 C20 121.6(5) . . ? C17 C16 C20 120.3(5) . . ? C14 C15 C16 121.3(5) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C1A C7A C14A 112.2(5) . . ? C1A C7A C8A 113.0(5) . . ? C14A C7A C8A 113.6(5) . . ? C1A C7A H7AA 105.7 . . ? C14A C7A H7AA 105.7 . . ? C8A C7A H7AA 105.7 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35A C34A H34D 109.5 . . ? C35A C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C35A C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C44 C43 C48 122.2(6) . . ? C44 C43 N1 120.7(5) . . ? C48 C43 N1 116.7(5) . . ? C42A C41A H41A 109.5 . . ? C42A C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? C42A C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C9A C8A C13A 117.5(6) . . ? C9A C8A C7A 124.5(6) . . ? C13A C8A C7A 117.8(5) . . ? C18 C17 C16 122.2(5) . . ? C18 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C6 C1 C2 118.9(5) . . ? C6 C1 C7 117.9(5) . . ? C2 C1 C7 123.2(5) . . ? N2A C40A C39A 121.5(5) . . ? N2A C40A C42A 112.3(5) . . ? C39A C40A C42A 126.1(5) . . ? C40 C39 C38 118.8(5) . . ? C40 C39 H39A 120.6 . . ? C38 C39 H39A 120.6 . . ? C38 C37 C36 117.6(5) . . ? C38 C37 H37A 121.2 . . ? C36 C37 H37A 121.2 . . ? C37A C38A C39A 120.1(6) . . ? C37A C38A H38A 119.9 . . ? C39A C38A H38A 120.0 . . ? N3 C35 C36 114.0(5) . . ? N3 C35 C34 126.7(5) . . ? C36 C35 C34 119.2(5) . . ? C13 C8 C9 119.8(5) . . ? C13 C8 C7 120.4(5) . . ? C9 C8 C7 119.7(5) . . ? N2 C36 C37 121.5(5) . . ? N2 C36 C35 113.8(5) . . ? C37 C36 C35 124.6(5) . . ? C38A C37A C36A 117.3(5) . . ? C38A C37A H37B 121.3 . . ? C36A C37A H37B 121.3 . . ? C15A C14A C19A 118.1(5) . . ? C15A C14A C7A 122.0(5) . . ? C19A C14A C7A 119.9(5) . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C48A C43A C44A 122.8(5) . . ? C48A C43A N1A 120.5(5) . . ? C44A C43A N1A 116.4(5) . . ? C24A C23A C22A 121.7(6) . . ? C24A C23A H23A 119.2 . . ? C22A C23A H23A 119.2 . . ? C22 C21 C18 112.5(5) . . ? C22 C21 C28 113.5(5) . . ? C18 C21 C28 111.7(4) . . ? C22 C21 H21A 106.2 . . ? C18 C21 H21A 106.2 . . ? C28 C21 H21A 106.2 . . ? C15 C14 C19 118.5(5) . . ? C15 C14 C7 120.6(5) . . ? C19 C14 C7 120.9(5) . . ? C46 C45 C44 122.6(6) . . ? C46 C45 H45A 118.7 . . ? C44 C45 H45A 118.7 . . ? C33 C28 C29 118.2(6) . . ? C33 C28 C21 119.0(5) . . ? C29 C28 C21 122.8(5) . . ? C17A C18A C19A 118.6(6) . . ? C17A C18A C21A 122.8(6) . . ? C19A C18A C21A 118.6(5) . . ? C1 C7 C8 116.4(5) . . ? C1 C7 C14 110.5(4) . . ? C8 C7 C14 111.8(5) . . ? C1 C7 H7A 105.8 . . ? C8 C7 H7A 105.8 . . ? C14 C7 H7A 105.8 . . ? N3A C35A C34A 125.7(5) . . ? N3A C35A C36A 115.0(5) . . ? C34A C35A C36A 119.3(5) . . ? C23 C22 C27 118.5(6) . . ? C23 C22 C21 121.2(5) . . ? C27 C22 C21 120.3(6) . . ? C33A C28A C29A 118.3(6) . . ? C33A C28A C21A 123.1(6) . . ? C29A C28A C21A 118.6(6) . . ? C22A C21A C28A 112.9(5) . . ? C22A C21A C18A 111.3(5) . . ? C28A C21A C18A 113.3(5) . . ? C22A C21A H21B 106.3 . . ? C28A C21A H21B 106.3 . . ? C18A C21A H21B 106.3 . . ? C52A C51A C44A 115.8(6) . . ? C52A C51A H51A 108.3 . . ? C44A C51A H51A 108.3 . . ? C52A C51A H51B 108.3 . . ? C44A C51A H51B 108.3 . . ? H51A C51A H51B 107.4 . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C47 C46 C45 117.9(6) . . ? C47 C46 C53 120.9(6) . . ? C45 C46 C53 121.2(6) . . ? C3 C2 C1 119.5(6) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C46A C45A C44A 122.9(6) . . ? C46A C45A H45B 118.5 . . ? C44A C45A H45B 118.5 . . ? C37 C38 C39 120.3(5) . . ? C37 C38 H38B 119.8 . . ? C39 C38 H38B 119.8 . . ? C16A C15A C14A 120.6(6) . . ? C16A C15A H15B 119.7 . . ? C14A C15A H15B 119.7 . . ? C46A C47A C48A 121.0(6) . . ? C46A C47A H47A 119.5 . . ? C48A C47A H47A 119.5 . . ? C42 C41 H41D 109.5 . . ? C42 C41 H41E 109.5 . . ? H41D C41 H41E 109.5 . . ? C42 C41 H41F 109.5 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C32 C33 C28 121.3(7) . . ? C32 C33 H33A 119.3 . . ? C28 C33 H33A 119.3 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C4 C3 C2 121.5(6) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C8 C13 C12 119.5(6) . . ? C8 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C43A C48A C47A 117.6(6) . . ? C43A C48A C49A 119.8(5) . . ? C47A C48A C49A 122.6(6) . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C11A C10A C9A 119.4(6) . . ? C11A C10A H10A 120.3 . . ? C9A C10A H10A 120.3 . . ? C45A C44A C43A 116.6(6) . . ? C45A C44A C51A 123.3(6) . . ? C43A C44A C51A 120.1(6) . . ? C25 C26 C27 121.6(7) . . ? C25 C26 H26A 119.2 . . ? C27 C26 H26A 119.2 . . ? C50 C49 C48 112.8(7) . . ? C50 C49 H49A 109.0 . . ? C48 C49 H49A 109.0 . . ? C50 C49 H49B 109.0 . . ? C48 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? C47 C48 C43 118.5(6) . . ? C47 C48 C49 118.9(6) . . ? C43 C48 C49 122.5(6) . . ? C26 C27 C22 121.4(7) . . ? C26 C27 H27A 119.3 . . ? C22 C27 H27A 119.3 . . ? C12A C11A C10A 120.6(6) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C26A C27A C22A 120.2(7) . . ? C26A C27A H27B 119.9 . . ? C22A C27A H27B 119.9 . . ? C30 C29 C28 120.2(7) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C11A C12A C13A 119.1(7) . . ? C11A C12A H12B 120.5 . . ? C13A C12A H12B 120.5 . . ? C28A C33A C32A 122.0(7) . . ? C28A C33A H33B 119.0 . . ? C32A C33A H33B 119.0 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10B 120.0 . . ? C9 C10 H10B 120.0 . . ? C46 C47 C48 121.5(6) . . ? C46 C47 H47B 119.3 . . ? C48 C47 H47B 119.3 . . ? C8A C9A C10A 122.6(6) . . ? C8A C9A H9AA 118.7 . . ? C10A C9A H9AA 118.7 . . ? C10 C11 C12 120.7(6) . . ? C10 C11 H11B 119.6 . . ? C12 C11 H11B 119.6 . . ? C18A C17A C16A 122.3(6) . . ? C18A C17A H17B 118.8 . . ? C16A C17A H17B 118.8 . . ? C40A C39A C38A 118.8(6) . . ? C40A C39A H39B 120.6 . . ? C38A C39A H39B 120.6 . . ? C43 C44 C45 117.0(6) . . ? C43 C44 C51 121.9(6) . . ? C45 C44 C51 121.0(6) . . ? C25A C26A C27A 122.2(7) . . ? C25A C26A H26B 118.9 . . ? C27A C26A H26B 118.9 . . ? C30A C29A C28A 120.9(7) . . ? C30A C29A H29B 119.6 . . ? C28A C29A H29B 119.6 . . ? C45A C46A C47A 119.0(6) . . ? C45A C46A C53A 119.9(7) . . ? C47A C46A C53A 121.0(6) . . ? C30 C31 C32 116.5(6) . . ? C30 C31 H31A 121.8 . . ? C32 C31 H31A 121.8 . . ? C22 C23 C24 122.5(7) . . ? C22 C23 H23B 118.8 . . ? C24 C23 H23B 118.8 . . ? C48A C49A C50A 115.1(5) . . ? C48A C49A H49C 108.5 . . ? C50A C49A H49C 108.5 . . ? C48A C49A H49D 108.5 . . ? C50A C49A H49D 108.5 . . ? H49C C49A H49D 107.5 . . ? C33 C32 C31 119.6(7) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1A C2A C3A 121.0(10) . . ? C1A C2A H2AA 119.5 . . ? C3A C2A H2AA 119.5 . . ? C26A C25A C24A 118.1(7) . . ? C26A C25A H25A 120.9 . . ? C24A C25A H25A 120.9 . . ? C8A C13A C12A 120.8(6) . . ? C8A C13A H13B 119.6 . . ? C12A C13A H13B 119.6 . . ? C23A C24A C25A 120.1(7) . . ? C23A C24A H24A 119.9 . . ? C25A C24A H24A 119.9 . . ? C6A C1A C2A 119.5(7) . . ? C6A C1A C7A 121.0(7) . . ? C2A C1A C7A 119.5(7) . . ? C17A C16A C15A 119.0(6) . . ? C17A C16A C20A 121.2(6) . . ? C15A C16A C20A 119.8(6) . . ? C29A C30A C31A 119.8(8) . . ? C29A C30A H30A 120.1 . . ? C31A C30A H30A 120.1 . . ? C26 C25 C24 119.5(7) . . ? C26 C25 H25B 120.3 . . ? C24 C25 H25B 120.3 . . ? C46A C53A H53A 109.5 . . ? C46A C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C46A C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C1A C6A C5A 118.1(10) . . ? C1A C6A H6AA 120.9 . . ? C5A C6A H6AA 120.9 . . ? C31 C30 C29 123.9(7) . . ? C31 C30 H30B 118.0 . . ? C29 C30 H30B 118.0 . . ? C31A C32A C33A 118.1(7) . . ? C31A C32A H32B 121.0 . . ? C33A C32A H32B 121.0 . . ? C52 C51 C52' 40.2(10) . . ? C52 C51 C44 119.6(9) . . ? C52' C51 C44 111.4(11) . . ? C52 C51 H51C 107.4 . . ? C52' C51 H51C 138.9 . . ? C44 C51 H51C 107.4 . . ? C52 C51 H51D 107.4 . . ? C52' C51 H51D 73.6 . . ? C44 C51 H51D 107.4 . . ? H51C C51 H51D 107.0 . . ? C46 C53 H53D 109.5 . . ? C46 C53 H53E 109.5 . . ? H53D C53 H53E 109.5 . . ? C46 C53 H53F 109.5 . . ? H53D C53 H53F 109.5 . . ? H53E C53 H53F 109.5 . . ? C49A C50A H50A 109.5 . . ? C49A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? C49A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? C30A C31A C32A 120.9(7) . . ? C30A C31A H31B 119.5 . . ? C32A C31A H31B 119.5 . . ? C23 C24 C25 116.5(7) . . ? C23 C24 H24B 121.8 . . ? C25 C24 H24B 121.8 . . ? C4A C3A C2A 117.9(10) . . ? C4A C3A H3AA 121.1 . . ? C2A C3A H3AA 121.1 . . ? C4A C5A C6A 122.5(11) . . ? C4A C5A H5AA 118.8 . . ? C6A C5A H5AA 118.8 . . ? C49 C50 H50D 109.5 . . ? C49 C50 H50E 109.5 . . ? H50D C50 H50E 109.5 . . ? C49 C50 H50F 109.5 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C16A C20A H20D 109.5 . . ? C16A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C16A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C5A C4A C3A 121.0(9) . . ? C5A C4A H4AA 119.5 . . ? C3A C4A H4AA 119.5 . . ? C51A C52A H52A 109.5 . . ? C51A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C52 H52D 109.5 . . ? C51 C52 H52E 109.5 . . ? C51 C52 H52F 109.5 . . ? C51 C52' H52G 109.5 . . ? C51 C52' H52H 109.5 . . ? H52G C52' H52H 109.5 . . ? C51 C52' H52I 109.5 . . ? H52G C52' H52I 109.5 . . ? H52H C52' H52I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Fe1A N2A C40A 14.7(4) . . . . ? N3A Fe1A N2A C40A 170.1(4) . . . . ? Cl1A Fe1A N2A C40A 94.1(5) . . . . ? Cl2A Fe1A N2A C40A -85.5(4) . . . . ? N1A Fe1A N2A C36A -169.4(4) . . . . ? N3A Fe1A N2A C36A -14.0(4) . . . . ? Cl1A Fe1A N2A C36A -90.0(5) . . . . ? Cl2A Fe1A N2A C36A 90.4(4) . . . . ? N1 Fe1 N2 C36 171.7(5) . . . . ? N3 Fe1 N2 C36 15.3(4) . . . . ? Cl1 Fe1 N2 C36 84.9(5) . . . . ? Cl2 Fe1 N2 C36 -90.0(4) . . . . ? N1 Fe1 N2 C40 -19.2(4) . . . . ? N3 Fe1 N2 C40 -175.7(4) . . . . ? Cl1 Fe1 N2 C40 -106.0(4) . . . . ? Cl2 Fe1 N2 C40 79.0(4) . . . . ? N2 Fe1 N1 C42 16.5(4) . . . . ? N3 Fe1 N1 C42 52.1(5) . . . . ? Cl1 Fe1 N1 C42 170.9(4) . . . . ? Cl2 Fe1 N1 C42 -73.5(4) . . . . ? N2 Fe1 N1 C43 -166.9(5) . . . . ? N3 Fe1 N1 C43 -131.3(4) . . . . ? Cl1 Fe1 N1 C43 -12.5(5) . . . . ? Cl2 Fe1 N1 C43 103.2(4) . . . . ? N2 Fe1 N3 C35 -11.6(4) . . . . ? N1 Fe1 N3 C35 -47.5(5) . . . . ? Cl1 Fe1 N3 C35 -168.1(4) . . . . ? Cl2 Fe1 N3 C35 76.0(4) . . . . ? N2 Fe1 N3 C19 171.8(4) . . . . ? N1 Fe1 N3 C19 135.8(4) . . . . ? Cl1 Fe1 N3 C19 15.3(4) . . . . ? Cl2 Fe1 N3 C19 -100.6(4) . . . . ? C36 N2 C40 C39 4.4(8) . . . . ? Fe1 N2 C40 C39 -164.6(4) . . . . ? C36 N2 C40 C42 -171.4(5) . . . . ? Fe1 N2 C40 C42 19.7(6) . . . . ? N2A Fe1A N3A C35A 14.0(4) . . . . ? N1A Fe1A N3A C35A 52.3(5) . . . . ? Cl1A Fe1A N3A C35A 169.3(4) . . . . ? Cl2A Fe1A N3A C35A -71.9(4) . . . . ? N2A Fe1A N3A C19A -168.6(4) . . . . ? N1A Fe1A N3A C19A -130.3(4) . . . . ? Cl1A Fe1A N3A C19A -13.3(4) . . . . ? Cl2A Fe1A N3A C19A 105.5(4) . . . . ? N2A Fe1A N1A C42A -15.8(4) . . . . ? N3A Fe1A N1A C42A -54.1(5) . . . . ? Cl1A Fe1A N1A C42A -170.6(4) . . . . ? Cl2A Fe1A N1A C42A 71.3(4) . . . . ? N2A Fe1A N1A C43A 167.3(5) . . . . ? N3A Fe1A N1A C43A 128.9(4) . . . . ? Cl1A Fe1A N1A C43A 12.4(4) . . . . ? Cl2A Fe1A N1A C43A -105.7(4) . . . . ? C40A N2A C36A C37A 2.7(8) . . . . ? Fe1A N2A C36A C37A -173.3(4) . . . . ? C40A N2A C36A C35A -172.1(5) . . . . ? Fe1A N2A C36A C35A 12.0(6) . . . . ? C43 N1 C42 C41 -4.2(9) . . . . ? Fe1 N1 C42 C41 172.7(5) . . . . ? C43 N1 C42 C40 171.7(5) . . . . ? Fe1 N1 C42 C40 -11.4(6) . . . . ? N2 C40 C42 N1 -4.8(7) . . . . ? C39 C40 C42 N1 179.7(6) . . . . ? N2 C40 C42 C41 171.5(5) . . . . ? C39 C40 C42 C41 -4.0(9) . . . . ? C43A N1A C42A C41A 9.9(9) . . . . ? Fe1A N1A C42A C41A -167.1(5) . . . . ? C43A N1A C42A C40A -168.4(5) . . . . ? Fe1A N1A C42A C40A 14.5(6) . . . . ? C35A N3A C19A C18A 96.2(7) . . . . ? Fe1A N3A C19A C18A -81.0(6) . . . . ? C35A N3A C19A C14A -91.0(7) . . . . ? Fe1A N3A C19A C14A 91.7(5) . . . . ? C17 C18 C19 C14 3.8(8) . . . . ? C21 C18 C19 C14 -176.1(5) . . . . ? C17 C18 C19 N3 179.5(5) . . . . ? C21 C18 C19 N3 -0.4(8) . . . . ? C35 N3 C19 C18 92.7(6) . . . . ? Fe1 N3 C19 C18 -90.7(5) . . . . ? C35 N3 C19 C14 -91.4(6) . . . . ? Fe1 N3 C19 C14 85.2(5) . . . . ? C17 C16 C15 C14 0.2(8) . . . . ? C20 C16 C15 C14 179.3(5) . . . . ? C42 N1 C43 C44 82.4(7) . . . . ? Fe1 N1 C43 C44 -94.3(6) . . . . ? C42 N1 C43 C48 -104.8(6) . . . . ? Fe1 N1 C43 C48 78.6(6) . . . . ? C1A C7A C8A C9A 12.1(9) . . . . ? C14A C7A C8A C9A -117.3(7) . . . . ? C1A C7A C8A C13A -161.9(6) . . . . ? C14A C7A C8A C13A 68.8(7) . . . . ? C19 C18 C17 C16 -0.1(9) . . . . ? C21 C18 C17 C16 179.9(5) . . . . ? C15 C16 C17 C18 -2.0(9) . . . . ? C20 C16 C17 C18 179.0(6) . . . . ? C5 C6 C1 C2 -0.1(10) . . . . ? C5 C6 C1 C7 -176.0(6) . . . . ? C36A N2A C40A C39A -3.8(8) . . . . ? Fe1A N2A C40A C39A 172.2(4) . . . . ? C36A N2A C40A C42A 172.0(5) . . . . ? Fe1A N2A C40A C42A -12.0(6) . . . . ? N1A C42A C40A N2A -2.4(7) . . . . ? C41A C42A C40A N2A 179.1(5) . . . . ? N1A C42A C40A C39A 173.2(5) . . . . ? C41A C42A C40A C39A -5.3(9) . . . . ? N2 C40 C39 C38 -0.7(9) . . . . ? C42 C40 C39 C38 174.5(6) . . . . ? C19 N3 C35 C36 -176.2(5) . . . . ? Fe1 N3 C35 C36 7.0(6) . . . . ? C19 N3 C35 C34 1.3(9) . . . . ? Fe1 N3 C35 C34 -175.5(5) . . . . ? C40 N2 C36 C37 -2.9(9) . . . . ? Fe1 N2 C36 C37 165.7(4) . . . . ? C40 N2 C36 C35 174.6(5) . . . . ? Fe1 N2 C36 C35 -16.7(7) . . . . ? C38 C37 C36 N2 -2.2(9) . . . . ? C38 C37 C36 C35 -179.5(6) . . . . ? N3 C35 C36 N2 5.5(7) . . . . ? C34 C35 C36 N2 -172.3(5) . . . . ? N3 C35 C36 C37 -177.1(6) . . . . ? C34 C35 C36 C37 5.2(9) . . . . ? C39A C38A C37A C36A -0.6(9) . . . . ? N2A C36A C37A C38A -0.5(8) . . . . ? C35A C36A C37A C38A 173.6(5) . . . . ? C18A C19A C14A C15A -4.4(9) . . . . ? N3A C19A C14A C15A -177.1(5) . . . . ? C18A C19A C14A C7A 174.7(5) . . . . ? N3A C19A C14A C7A 2.0(8) . . . . ? C1A C7A C14A C15A -100.8(7) . . . . ? C8A C7A C14A C15A 29.0(8) . . . . ? C1A C7A C14A C19A 80.2(7) . . . . ? C8A C7A C14A C19A -150.1(5) . . . . ? C13 C8 C9 C10 0.9(9) . . . . ? C7 C8 C9 C10 178.9(6) . . . . ? C42A N1A C43A C48A -89.7(7) . . . . ? Fe1A N1A C43A C48A 87.2(6) . . . . ? C42A N1A C43A C44A 96.2(7) . . . . ? Fe1A N1A C43A C44A -86.9(6) . . . . ? C27A C22A C23A C24A 1.0(10) . . . . ? C21A C22A C23A C24A -179.8(6) . . . . ? C19 C18 C21 C22 -81.8(7) . . . . ? C17 C18 C21 C22 98.3(6) . . . . ? C19 C18 C21 C28 149.2(5) . . . . ? C17 C18 C21 C28 -30.7(7) . . . . ? C16 C15 C14 C19 3.3(8) . . . . ? C16 C15 C14 C7 -178.0(5) . . . . ? C18 C19 C14 C15 -5.5(8) . . . . ? N3 C19 C14 C15 178.8(5) . . . . ? C18 C19 C14 C7 175.9(5) . . . . ? N3 C19 C14 C7 0.1(7) . . . . ? C22 C21 C28 C33 165.2(5) . . . . ? C18 C21 C28 C33 -66.3(7) . . . . ? C22 C21 C28 C29 -16.3(8) . . . . ? C18 C21 C28 C29 112.2(6) . . . . ? C14A C19A C18A C17A 4.3(9) . . . . ? N3A C19A C18A C17A 176.7(6) . . . . ? C14A C19A C18A C21A -175.0(5) . . . . ? N3A C19A C18A C21A -2.6(9) . . . . ? C6 C1 C7 C8 -163.8(6) . . . . ? C2 C1 C7 C8 20.5(8) . . . . ? C6 C1 C7 C14 67.3(7) . . . . ? C2 C1 C7 C14 -108.4(6) . . . . ? C13 C8 C7 C1 -82.2(7) . . . . ? C9 C8 C7 C1 99.9(7) . . . . ? C13 C8 C7 C14 46.0(7) . . . . ? C9 C8 C7 C14 -131.9(6) . . . . ? C15 C14 C7 C1 33.9(7) . . . . ? C19 C14 C7 C1 -147.5(5) . . . . ? C15 C14 C7 C8 -97.5(6) . . . . ? C19 C14 C7 C8 81.2(6) . . . . ? C19A N3A C35A C34A -7.1(9) . . . . ? Fe1A N3A C35A C34A 170.3(4) . . . . ? C19A N3A C35A C36A 170.3(5) . . . . ? Fe1A N3A C35A C36A -12.3(6) . . . . ? N2A C36A C35A N3A 1.1(7) . . . . ? C37A C36A C35A N3A -173.5(5) . . . . ? N2A C36A C35A C34A 178.7(5) . . . . ? C37A C36A C35A C34A 4.1(8) . . . . ? C18 C21 C22 C23 -45.9(8) . . . . ? C28 C21 C22 C23 82.2(7) . . . . ? C18 C21 C22 C27 132.9(6) . . . . ? C28 C21 C22 C27 -99.0(7) . . . . ? C23A C22A C21A C28A 89.1(7) . . . . ? C27A C22A C21A C28A -91.7(7) . . . . ? C23A C22A C21A C18A -39.6(8) . . . . ? C27A C22A C21A C18A 139.6(6) . . . . ? C33A C28A C21A C22A -14.8(8) . . . . ? C29A C28A C21A C22A 163.3(6) . . . . ? C33A C28A C21A C18A 112.9(7) . . . . ? C29A C28A C21A C18A -69.1(8) . . . . ? C17A C18A C21A C22A 96.3(7) . . . . ? C19A C18A C21A C22A -84.4(7) . . . . ? C17A C18A C21A C28A -32.1(9) . . . . ? C19A C18A C21A C28A 147.1(6) . . . . ? C44 C45 C46 C47 -0.7(10) . . . . ? C44 C45 C46 C53 179.6(6) . . . . ? C6 C1 C2 C3 1.6(9) . . . . ? C7 C1 C2 C3 177.3(6) . . . . ? C36 C37 C38 C39 5.9(9) . . . . ? C40 C39 C38 C37 -4.5(9) . . . . ? C19A C14A C15A C16A 1.3(10) . . . . ? C7A C14A C15A C16A -177.8(6) . . . . ? C29 C28 C33 C32 -1.5(9) . . . . ? C21 C28 C33 C32 177.0(6) . . . . ? C1 C6 C5 C4 0.3(10) . . . . ? C1 C2 C3 C4 -3.4(10) . . . . ? C9 C8 C13 C12 0.1(9) . . . . ? C7 C8 C13 C12 -177.8(5) . . . . ? C11 C12 C13 C8 0.3(10) . . . . ? C44A C43A C48A C47A -1.7(9) . . . . ? N1A C43A C48A C47A -175.4(5) . . . . ? C44A C43A C48A C49A 179.1(6) . . . . ? N1A C43A C48A C49A 5.4(9) . . . . ? C46A C47A C48A C43A 1.4(9) . . . . ? C46A C47A C48A C49A -179.4(6) . . . . ? C6 C5 C4 C3 -2.0(10) . . . . ? C2 C3 C4 C5 3.6(10) . . . . ? C46A C45A C44A C43A -2.0(9) . . . . ? C46A C45A C44A C51A 178.1(6) . . . . ? C48A C43A C44A C45A 1.9(9) . . . . ? N1A C43A C44A C45A 175.9(5) . . . . ? C48A C43A C44A C51A -178.1(6) . . . . ? N1A C43A C44A C51A -4.1(9) . . . . ? C52A C51A C44A C45A 8.4(10) . . . . ? C52A C51A C44A C43A -171.6(6) . . . . ? C44 C43 C48 C47 -6.8(9) . . . . ? N1 C43 C48 C47 -179.6(5) . . . . ? C44 C43 C48 C49 171.4(6) . . . . ? N1 C43 C48 C49 -1.4(9) . . . . ? C50 C49 C48 C47 -97.7(8) . . . . ? C50 C49 C48 C43 84.1(9) . . . . ? C25 C26 C27 C22 -0.4(12) . . . . ? C23 C22 C27 C26 0.8(10) . . . . ? C21 C22 C27 C26 -178.1(6) . . . . ? C9A C10A C11A C12A -1.7(11) . . . . ? C23A C22A C27A C26A -1.1(10) . . . . ? C21A C22A C27A C26A 179.7(7) . . . . ? C33 C28 C29 C30 1.2(9) . . . . ? C21 C28 C29 C30 -177.3(6) . . . . ? C10A C11A C12A C13A 1.7(11) . . . . ? C29A C28A C33A C32A 0.6(10) . . . . ? C21A C28A C33A C32A 178.7(6) . . . . ? C8 C9 C10 C11 -2.5(11) . . . . ? C45 C46 C47 C48 -0.1(10) . . . . ? C53 C46 C47 C48 179.6(6) . . . . ? C43 C48 C47 C46 3.7(10) . . . . ? C49 C48 C47 C46 -174.6(6) . . . . ? C13A C8A C9A C10A -1.4(10) . . . . ? C7A C8A C9A C10A -175.3(6) . . . . ? C11A C10A C9A C8A 1.6(11) . . . . ? C9 C10 C11 C12 3.0(11) . . . . ? C13 C12 C11 C10 -1.9(11) . . . . ? C19A C18A C17A C16A -1.2(11) . . . . ? C21A C18A C17A C16A 178.1(7) . . . . ? N2A C40A C39A C38A 2.7(8) . . . . ? C42A C40A C39A C38A -172.5(6) . . . . ? C37A C38A C39A C40A -0.4(9) . . . . ? C48 C43 C44 C45 6.0(9) . . . . ? N1 C43 C44 C45 178.5(5) . . . . ? C48 C43 C44 C51 -177.8(6) . . . . ? N1 C43 C44 C51 -5.3(9) . . . . ? C46 C45 C44 C43 -2.2(9) . . . . ? C46 C45 C44 C51 -178.4(7) . . . . ? C22A C27A C26A C25A 1.4(13) . . . . ? C33A C28A C29A C30A -0.1(11) . . . . ? C21A C28A C29A C30A -178.3(7) . . . . ? C44A C45A C46A C47A 1.8(10) . . . . ? C44A C45A C46A C53A -174.8(6) . . . . ? C48A C47A C46A C45A -1.4(9) . . . . ? C48A C47A C46A C53A 175.1(6) . . . . ? C27 C22 C23 C24 0.8(10) . . . . ? C21 C22 C23 C24 179.7(6) . . . . ? C43A C48A C49A C50A -169.4(6) . . . . ? C47A C48A C49A C50A 11.4(9) . . . . ? C28 C33 C32 C31 -1.0(10) . . . . ? C30 C31 C32 C33 3.7(10) . . . . ? C27A C26A C25A C24A -1.5(13) . . . . ? C9A C8A C13A C12A 1.3(10) . . . . ? C7A C8A C13A C12A 175.7(6) . . . . ? C11A C12A C13A C8A -1.5(11) . . . . ? C22A C23A C24A C25A -1.1(11) . . . . ? C26A C25A C24A C23A 1.4(12) . . . . ? C3A C2A C1A C6A -2.0(11) . . . . ? C3A C2A C1A C7A 177.3(7) . . . . ? C14A C7A C1A C6A 41.3(9) . . . . ? C8A C7A C1A C6A -88.8(8) . . . . ? C14A C7A C1A C2A -137.9(6) . . . . ? C8A C7A C1A C2A 92.0(7) . . . . ? C18A C17A C16A C15A -1.8(12) . . . . ? C18A C17A C16A C20A -179.0(8) . . . . ? C14A C15A C16A C17A 1.7(11) . . . . ? C14A C15A C16A C20A 179.0(8) . . . . ? C28A C29A C30A C31A 1.0(12) . . . . ? C27 C26 C25 C24 -1.5(13) . . . . ? C2A C1A C6A C5A 2.2(11) . . . . ? C7A C1A C6A C5A -177.0(7) . . . . ? C32 C31 C30 C29 -4.2(10) . . . . ? C28 C29 C30 C31 1.8(10) . . . . ? C28A C33A C32A C31A -2.0(11) . . . . ? C43 C44 C51 C52 -179.8(13) . . . . ? C45 C44 C51 C52 -3.7(16) . . . . ? C43 C44 C51 C52' 136.4(14) . . . . ? C45 C44 C51 C52' -47.6(16) . . . . ? C29A C30A C31A C32A -2.4(13) . . . . ? C33A C32A C31A C30A 2.9(12) . . . . ? C22 C23 C24 C25 -2.6(11) . . . . ? C26 C25 C24 C23 2.9(12) . . . . ? C1A C2A C3A C4A 0.9(12) . . . . ? C1A C6A C5A C4A -1.6(13) . . . . ? C6A C5A C4A C3A 0.5(15) . . . . ? C2A C3A C4A C5A -0.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.428 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.003 0.500 1083.6 150.1 2 0.000 0.500 0.000 7.0 0.5 3 0.306 0.812 0.881 171.9 3.1 4 0.113 0.055 0.191 15.5 -1.1 5 0.694 0.188 0.119 171.9 1.6 6 0.887 0.945 0.809 15.4 -1.7 _platon_squeeze_details ; ? ; #==end