# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email a.white@imperial.ac.uk _publ_contact_author_name 'Andrew J.P. White' loop_ _publ_author_name G.Britovsek T.Smit A.Tomov V.Gibson A.White D.Williams data_[Co(1)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253597' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 Cl2 Co N3 O2, C H2 Cl2' _chemical_formula_sum 'C28 H33 Cl4 Co N3 O2' _chemical_formula_weight 644.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.492(8) _cell_length_b 17.191(10) _cell_length_c 25.784(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6867(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 29.85 _exptl_crystal_description plates _exptl_crystal_colour Green _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 6.993 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0410 _exptl_absorpt_correction_T_max 0.4501 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5039 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1864 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 59.96 _reflns_number_total 5039 _reflns_number_gt 1273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5039 _refine_ls_number_parameters 400 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.3039 _refine_ls_R_factor_gt 0.0972 _refine_ls_wR_factor_ref 0.2764 _refine_ls_wR_factor_gt 0.2010 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.31576(15) 0.62627(12) 0.05950(8) 0.0976(7) Uani 1 1 d . . . Cl1 Cl 0.4093(3) 0.6579(2) 0.12214(13) 0.1108(12) Uani 1 1 d . . . Cl2 Cl 0.1958(3) 0.6958(2) 0.04627(17) 0.1259(14) Uani 1 1 d . . . N1 N 0.3557(8) 0.5378(6) 0.0135(4) 0.092(3) Uani 1 1 d . . . C2 C 0.4041(11) 0.5494(8) -0.0285(6) 0.100(5) Uani 1 1 d . . . C3 C 0.4332(9) 0.4897(8) -0.0589(5) 0.095(4) Uani 1 1 d . . . H3A H 0.4655 0.4997 -0.0886 0.114 Uiso 1 1 calc R . . C4 C 0.4135(11) 0.4135(8) -0.0444(6) 0.111(5) Uani 1 1 d . . . H4A H 0.4324 0.3719 -0.0645 0.133 Uiso 1 1 calc R . . C5 C 0.3653(10) 0.4000(8) 0.0003(5) 0.103(4) Uani 1 1 d . . . H5A H 0.3515 0.3500 0.0113 0.124 Uiso 1 1 calc R . . C6 C 0.3392(9) 0.4650(7) 0.0273(5) 0.088(4) Uani 1 1 d . . . C7 C 0.4152(9) 0.6317(10) -0.0411(5) 0.094(4) Uani 1 1 d . . . N7 N 0.3850(7) 0.6843(6) -0.0117(4) 0.090(3) Uani 1 1 d . . . O7 O 0.4575(6) 0.6402(5) -0.0870(4) 0.102(3) Uani 1 1 d . . . C8 C 0.5023(10) 0.7110(7) -0.1032(6) 0.122(5) Uani 1 1 d . . . H8A H 0.5273 0.7032 -0.1369 0.183 Uiso 1 1 calc R . . H8B H 0.5470 0.7231 -0.0788 0.183 Uiso 1 1 calc R . . H8C H 0.4619 0.7533 -0.1048 0.183 Uiso 1 1 calc R . . C9 C 0.2848(9) 0.4585(8) 0.0767(6) 0.091(4) Uani 1 1 d . . . N9 N 0.2630(8) 0.5199(7) 0.1003(4) 0.092(3) Uani 1 1 d . . . O9 O 0.2773(7) 0.3832(5) 0.0883(4) 0.115(3) Uani 1 1 d . . . C10 C 0.2064(12) 0.3537(9) 0.1204(6) 0.147(6) Uani 1 1 d . . . H10A H 0.2111 0.2982 0.1234 0.220 Uiso 1 1 calc R . . H10B H 0.1522 0.3668 0.1045 0.220 Uiso 1 1 calc R . . H10C H 0.2095 0.3768 0.1542 0.220 Uiso 1 1 calc R . . C11 C 0.3788(11) 0.7644(9) -0.0247(7) 0.105(5) Uani 1 1 d . . . C12 C 0.3172(12) 0.7848(8) -0.0626(6) 0.112(5) Uani 1 1 d . . . C13 C 0.3031(10) 0.8633(8) -0.0765(6) 0.113(5) Uani 1 1 d . . . H13A H 0.2622 0.8764 -0.1014 0.135 Uiso 1 1 calc R . . C14 C 0.3526(13) 0.9214(9) -0.0514(8) 0.122(6) Uani 1 1 d . . . C15 C 0.4117(11) 0.9003(9) -0.0148(7) 0.113(5) Uani 1 1 d . . . H15A H 0.4441 0.9391 0.0011 0.135 Uiso 1 1 calc R . . C16 C 0.4259(11) 0.8228(9) -0.0001(6) 0.105(5) Uani 1 1 d . . . C17 C 0.2591(11) 0.7248(10) -0.0888(6) 0.133(6) Uani 1 1 d . . . H17A H 0.2164 0.7511 -0.1094 0.199 Uiso 1 1 calc R . . H17B H 0.2310 0.6938 -0.0629 0.199 Uiso 1 1 calc R . . H17C H 0.2933 0.6919 -0.1107 0.199 Uiso 1 1 calc R . . C18 C 0.3387(12) 1.0075(9) -0.0676(8) 0.172(8) Uani 1 1 d . . . H18A H 0.3331 1.0391 -0.0371 0.257 Uiso 1 1 calc R . . H18B H 0.2871 1.0116 -0.0881 0.257 Uiso 1 1 calc R . . H18C H 0.3872 1.0250 -0.0876 0.257 Uiso 1 1 calc R . . C19 C 0.4969(10) 0.8004(8) 0.0370(6) 0.123(5) Uani 1 1 d . . . H19A H 0.4794 0.7556 0.0566 0.185 Uiso 1 1 calc R . . H19B H 0.5081 0.8429 0.0601 0.185 Uiso 1 1 calc R . . H19C H 0.5483 0.7884 0.0178 0.185 Uiso 1 1 calc R . . C20 C 0.2335(14) 0.5162(8) 0.1529(6) 0.107(5) Uani 1 1 d . . . C21 C 0.2803(12) 0.4994(9) 0.1941(7) 0.110(5) Uani 1 1 d . . . C22 C 0.2472(15) 0.5000(10) 0.2452(6) 0.129(6) Uani 1 1 d . . . H22A H 0.2812 0.4864 0.2735 0.155 Uiso 1 1 calc R . . C23 C 0.1603(15) 0.5222(11) 0.2512(7) 0.129(6) Uani 1 1 d . . . C24 C 0.1099(12) 0.5346(10) 0.2089(8) 0.139(6) Uani 1 1 d . . . H24A H 0.0508 0.5415 0.2135 0.166 Uiso 1 1 calc R . . C25 C 0.1445(15) 0.5374(9) 0.1572(6) 0.116(5) Uani 1 1 d . . . C26 C 0.3781(11) 0.4795(10) 0.1861(6) 0.136(6) Uani 1 1 d . . . H26A H 0.3839 0.4259 0.1765 0.204 Uiso 1 1 calc R . . H26B H 0.4089 0.4888 0.2179 0.204 Uiso 1 1 calc R . . H26C H 0.4015 0.5118 0.1592 0.204 Uiso 1 1 calc R . . C27 C 0.1218(13) 0.5192(13) 0.3069(6) 0.197(10) Uani 1 1 d . . . H27A H 0.0659 0.5434 0.3070 0.296 Uiso 1 1 calc R . . H27B H 0.1593 0.5465 0.3303 0.296 Uiso 1 1 calc R . . H27C H 0.1165 0.4660 0.3178 0.296 Uiso 1 1 calc R . . C28 C 0.0816(11) 0.5496(10) 0.1125(6) 0.134(6) Uani 1 1 d . . . H28A H 0.1014 0.5917 0.0911 0.201 Uiso 1 1 calc R . . H28B H 0.0255 0.5619 0.1261 0.201 Uiso 1 1 calc R . . H28C H 0.0782 0.5030 0.0921 0.201 Uiso 1 1 calc R . . C30A C 0.411(4) 0.287(3) 0.3023(17) 0.119(18) Uiso 0.203(4) 1 d PDU A 1 H30A H 0.3882 0.2557 0.3302 0.143 Uiso 0.203(4) 1 calc PR A 1 H30B H 0.4695 0.2681 0.2964 0.143 Uiso 0.203(4) 1 calc PR A 1 Cl3A Cl 0.361(3) 0.262(2) 0.2545(15) 0.250(15) Uiso 0.203(4) 1 d PDU A 1 Cl4A Cl 0.424(2) 0.3657(17) 0.3256(12) 0.187(11) Uiso 0.203(4) 1 d PDU A 1 C30B C 0.483(5) 0.294(3) 0.293(3) 0.118(19) Uiso 0.184(9) 1 d PDU B 2 H30C H 0.4723 0.2625 0.3233 0.142 Uiso 0.184(9) 1 calc PR B 2 H30D H 0.5433 0.2856 0.2842 0.142 Uiso 0.184(9) 1 calc PR B 2 Cl3B Cl 0.435(3) 0.2520(19) 0.2500(13) 0.201(13) Uiso 0.184(9) 1 d PDU B 2 Cl4B Cl 0.480(2) 0.3752(18) 0.3119(13) 0.176(13) Uiso 0.184(9) 1 d PDU B 2 C30C C 0.199(4) 0.194(3) 0.2486(18) 0.081(14) Uiso 0.210(13) 1 d PDU C 3 H30E H 0.2201 0.1483 0.2299 0.097 Uiso 0.210(13) 1 calc PR C 3 H30F H 0.1581 0.2185 0.2258 0.097 Uiso 0.210(13) 1 calc PR C 3 Cl3C Cl 0.146(3) 0.1610(19) 0.2931(14) 0.175(14) Uiso 0.210(13) 1 d PDU C 3 Cl4C Cl 0.275(3) 0.248(3) 0.2504(18) 0.29(2) Uiso 0.210(13) 1 d PDU C 3 C30D C 0.164(5) 0.209(3) 0.258(3) 0.109(19) Uiso 0.195(15) 1 d PDU D 4 H30G H 0.2198 0.1890 0.2685 0.131 Uiso 0.195(15) 1 calc PR D 4 H30H H 0.1585 0.1977 0.2215 0.131 Uiso 0.195(15) 1 calc PR D 4 Cl3D Cl 0.098(3) 0.156(2) 0.2846(16) 0.174(14) Uiso 0.195(15) 1 d PDU D 4 Cl4D Cl 0.172(3) 0.295(2) 0.2615(17) 0.174(16) Uiso 0.195(15) 1 d PDU D 4 C30E C 0.075(8) 0.221(4) 0.267(5) 0.12(2) Uiso 0.099(11) 1 d PDU E 5 H30I H 0.0789 0.1995 0.2320 0.147 Uiso 0.099(11) 1 calc PR E 5 H30J H 0.0136 0.2219 0.2746 0.147 Uiso 0.099(11) 1 calc PR E 5 Cl3E Cl 0.109(6) 0.156(3) 0.3010(17) 0.14(2) Uiso 0.099(11) 1 d PDU E 5 Cl4E Cl 0.098(5) 0.305(3) 0.260(2) 0.16(2) Uiso 0.099(11) 1 d PDU E 5 C30F C 0.110(5) 0.283(4) 0.244(7) 0.12(2) Uiso 0.109(10) 1 d PDU F 6 H30K H 0.0888 0.2492 0.2713 0.139 Uiso 0.109(10) 1 calc PR F 6 H30L H 0.1089 0.2509 0.2127 0.139 Uiso 0.109(10) 1 calc PR F 6 Cl3F Cl 0.036(4) 0.340(4) 0.235(3) 0.21(2) Uiso 0.109(10) 1 d PDU F 6 Cl4F Cl 0.204(4) 0.292(3) 0.255(3) 0.138(19) Uiso 0.109(10) 1 d PDU F 6 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 Co 0.1151(17) 0.0826(12) 0.0951(13) -0.0069(13) -0.0029(15) 0.0047(13) Cl1 0.131(3) 0.109(2) 0.092(2) -0.008(2) -0.001(2) -0.009(2) Cl2 0.121(3) 0.100(2) 0.156(3) 0.009(2) 0.006(3) 0.015(2) N1 0.116(10) 0.072(7) 0.088(7) -0.009(6) -0.007(7) -0.008(6) C2 0.141(14) 0.078(10) 0.080(9) 0.005(8) -0.038(10) -0.017(9) C3 0.120(12) 0.100(10) 0.066(7) -0.017(9) -0.008(8) -0.009(9) C4 0.170(15) 0.063(8) 0.100(11) 0.000(8) -0.016(11) 0.008(10) C5 0.136(13) 0.088(10) 0.087(9) -0.005(8) 0.002(10) -0.011(9) C6 0.104(11) 0.056(8) 0.105(10) -0.016(8) 0.007(9) 0.002(7) C7 0.090(11) 0.112(12) 0.079(8) 0.010(9) -0.002(8) 0.007(9) N7 0.098(9) 0.075(7) 0.097(7) -0.001(7) -0.004(7) -0.016(6) O7 0.120(8) 0.079(6) 0.108(6) -0.006(6) 0.008(6) -0.009(5) C8 0.140(14) 0.077(9) 0.149(13) 0.021(9) 0.021(11) -0.011(9) C9 0.089(11) 0.084(10) 0.100(10) 0.002(9) -0.016(9) 0.002(8) N9 0.095(9) 0.098(9) 0.083(7) -0.003(7) -0.017(7) -0.005(7) O9 0.149(9) 0.059(5) 0.136(7) 0.010(6) 0.032(7) -0.013(5) C10 0.180(17) 0.119(12) 0.140(13) -0.004(11) 0.044(14) -0.047(12) C11 0.105(12) 0.090(12) 0.119(12) 0.013(10) 0.033(10) -0.001(9) C12 0.152(15) 0.072(9) 0.111(10) 0.023(9) 0.002(12) -0.002(10) C13 0.119(12) 0.095(11) 0.125(11) 0.005(10) 0.005(10) -0.008(10) C14 0.140(15) 0.079(11) 0.148(15) 0.018(12) 0.034(14) -0.003(10) C15 0.127(15) 0.091(12) 0.120(12) 0.002(10) 0.028(12) -0.003(10) C16 0.129(15) 0.083(11) 0.103(10) 0.003(9) 0.034(11) -0.020(10) C17 0.140(14) 0.140(14) 0.118(12) -0.001(12) -0.014(12) 0.016(12) C18 0.168(18) 0.111(13) 0.24(2) 0.019(14) 0.067(17) 0.026(12) C19 0.122(13) 0.106(11) 0.142(13) 0.011(10) -0.032(12) -0.022(10) C20 0.153(17) 0.063(8) 0.103(12) 0.014(9) 0.014(13) 0.013(9) C21 0.118(16) 0.113(11) 0.098(11) 0.020(10) -0.017(11) -0.029(10) C22 0.151(17) 0.147(13) 0.090(11) 0.004(11) -0.026(13) -0.026(13) C23 0.125(16) 0.157(15) 0.106(12) -0.016(12) -0.012(13) -0.020(13) C24 0.107(15) 0.151(15) 0.158(17) -0.019(15) 0.009(14) -0.013(12) C25 0.174(18) 0.090(10) 0.084(10) -0.009(9) 0.004(12) 0.017(11) C26 0.127(16) 0.157(16) 0.123(13) 0.020(12) -0.010(12) 0.024(12) C27 0.22(2) 0.30(3) 0.080(10) -0.022(14) 0.060(13) -0.02(2) C28 0.151(16) 0.146(14) 0.104(12) -0.001(11) -0.014(12) -0.002(12) _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 Co N1 2.026(11) . ? Co Cl2 2.236(5) . ? Co Cl1 2.237(4) . ? Co N9 2.261(11) . ? Co N7 2.348(11) . ? N1 C6 1.325(14) . ? N1 C2 1.331(17) . ? C2 C3 1.367(17) . ? C2 C7 1.462(19) . ? C3 C4 1.397(17) . ? C4 C5 1.391(18) . ? C5 C6 1.377(16) . ? C6 C9 1.532(17) . ? C7 N7 1.271(15) . ? C7 O7 1.360(14) . ? N7 C11 1.419(17) . ? O7 C8 1.463(14) . ? C9 N9 1.264(15) . ? C9 O9 1.333(14) . ? N9 C20 1.433(17) . ? O9 C10 1.466(15) . ? C11 C16 1.394(19) . ? C11 C12 1.410(19) . ? C12 C13 1.412(18) . ? C12 C17 1.527(19) . ? C13 C14 1.42(2) . ? C14 C15 1.36(2) . ? C14 C18 1.55(2) . ? C15 C16 1.403(19) . ? C16 C19 1.507(19) . ? C20 C21 1.317(19) . ? C20 C25 1.43(2) . ? C21 C22 1.41(2) . ? C21 C26 1.57(2) . ? C22 C23 1.41(2) . ? C23 C24 1.36(2) . ? C23 C27 1.56(2) . ? C24 C25 1.44(2) . ? C25 C28 1.52(2) . ? C30A Cl4A 1.49(3) . ? C30A Cl3A 1.52(3) . ? C30B Cl4B 1.49(3) . ? C30B Cl3B 1.51(3) . ? C30C Cl4C 1.50(3) . ? C30C Cl3C 1.52(3) . ? C30D Cl4D 1.50(3) . ? C30D Cl3D 1.53(3) . ? C30E Cl4E 1.49(3) . ? C30E Cl3E 1.52(3) . ? C30F Cl4F 1.49(3) . ? C30F Cl3F 1.52(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co Cl2 124.5(3) . . ? N1 Co Cl1 114.0(3) . . ? Cl2 Co Cl1 121.25(17) . . ? N1 Co N9 77.0(5) . . ? Cl2 Co N9 101.7(3) . . ? Cl1 Co N9 95.4(3) . . ? N1 Co N7 73.9(5) . . ? Cl2 Co N7 91.9(3) . . ? Cl1 Co N7 99.5(3) . . ? N9 Co N7 150.7(4) . . ? C6 N1 C2 117.9(12) . . ? C6 N1 Co 119.5(10) . . ? C2 N1 Co 122.4(10) . . ? N1 C2 C3 122.7(13) . . ? N1 C2 C7 113.1(15) . . ? C3 C2 C7 124.0(15) . . ? C2 C3 C4 118.5(13) . . ? C5 C4 C3 119.7(14) . . ? C6 C5 C4 116.1(13) . . ? N1 C6 C5 125.0(13) . . ? N1 C6 C9 113.4(11) . . ? C5 C6 C9 121.5(13) . . ? N7 C7 O7 128.3(14) . . ? N7 C7 C2 120.8(14) . . ? O7 C7 C2 110.8(14) . . ? C7 N7 C11 125.1(12) . . ? C7 N7 Co 109.4(9) . . ? C11 N7 Co 124.4(10) . . ? C7 O7 C8 124.6(12) . . ? N9 C9 O9 132.8(14) . . ? N9 C9 C6 119.1(13) . . ? O9 C9 C6 107.8(13) . . ? C9 N9 C20 120.2(13) . . ? C9 N9 Co 110.8(10) . . ? C20 N9 Co 126.3(9) . . ? C9 O9 C10 121.9(12) . . ? C16 C11 C12 119.3(14) . . ? C16 C11 N7 123.8(16) . . ? C12 C11 N7 116.9(15) . . ? C11 C12 C13 121.3(16) . . ? C11 C12 C17 122.5(13) . . ? C13 C12 C17 116.2(16) . . ? C12 C13 C14 118.3(16) . . ? C15 C14 C13 119.5(15) . . ? C15 C14 C18 122.2(18) . . ? C13 C14 C18 118.4(18) . . ? C14 C15 C16 123.0(16) . . ? C11 C16 C15 118.7(16) . . ? C11 C16 C19 119.1(14) . . ? C15 C16 C19 121.9(16) . . ? C21 C20 C25 121.5(18) . . ? C21 C20 N9 126.7(18) . . ? C25 C20 N9 111.7(16) . . ? C20 C21 C22 123.4(18) . . ? C20 C21 C26 118.3(17) . . ? C22 C21 C26 118.3(17) . . ? C23 C22 C21 116.8(18) . . ? C24 C23 C22 120.3(19) . . ? C24 C23 C27 122(2) . . ? C22 C23 C27 117.3(19) . . ? C23 C24 C25 122.3(18) . . ? C20 C25 C24 115.1(17) . . ? C20 C25 C28 126.4(17) . . ? C24 C25 C28 117.8(19) . . ? Cl4A C30A Cl3A 130(3) . . ? Cl4B C30B Cl3B 132(3) . . ? Cl4C C30C Cl3C 129(3) . . ? Cl4D C30D Cl3D 129(3) . . ? Cl4E C30E Cl3E 134(4) . . ? Cl4F C30F Cl3F 133(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 59.96 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.304 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.061 #===END data_[Fe(2)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253598' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C27 H31 Cl2 Fe N3 S2, C H2 Cl2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H33 Cl4 Fe N3 S2' _chemical_formula_weight 673.34 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2849(8) _cell_length_b 16.2809(4) _cell_length_c 17.6654(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.957(3) _cell_angle_gamma 90.00 _cell_volume 6405.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293 _cell_measurement_reflns_used 38 _cell_measurement_theta_min 10.61 _cell_measurement_theta_max 27.49 _exptl_crystal_description prisms _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method ? _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 8.237 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.0585 _exptl_absorpt_correction_T_max 0.1784 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4875 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4743 _reflns_number_gt 3194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 436 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4307 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_all 0.1494 _refine_ls_wR_factor_ref 0.1265 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.74922(3) 0.46021(5) 0.48562(4) 0.0564(2) Uani 1 d . . Cl1 Cl 0.67474(7) 0.38112(13) 0.50669(9) 0.0896(5) Uani 1 d . . Cl2 Cl 0.76612(8) 0.57640(10) 0.56141(8) 0.0779(4) Uani 1 d . . N1 N 0.7933(2) 0.4222(3) 0.4019(2) 0.0536(9) Uani 1 d . . C2 C 0.7698(2) 0.4429(3) 0.3250(3) 0.0574(12) Uani 1 d . . C3 C 0.7918(2) 0.4077(4) 0.2679(3) 0.0659(14) Uani 1 d . . H3A H 0.7766 0.4234 0.2152 0.079 Uiso 1 calc R . C4 C 0.8359(3) 0.3497(4) 0.2893(3) 0.077(2) Uani 1 d . . H4A H 0.8497 0.3241 0.2508 0.092 Uiso 1 calc R . C5 C 0.8597(3) 0.3290(4) 0.3667(3) 0.071(2) Uani 1 d . . H5A H 0.8898 0.2896 0.3815 0.086 Uiso 1 calc R . C6 C 0.8383(2) 0.3681(3) 0.4239(3) 0.0562(11) Uani 1 d . . C7 C 0.7203(2) 0.5053(3) 0.3092(3) 0.0556(11) Uani 1 d . . N7 N 0.7009(2) 0.5217(3) 0.3688(2) 0.0534(10) Uani 1 d . . S7 S 0.70288(7) 0.54428(12) 0.21363(8) 0.0809(5) Uani 1 d . . C8 C 0.6340(4) 0.5996(5) 0.1898(4) 0.102(3) Uani 1 d . . H8A H 0.6252 0.6206 0.1368 0.153 Uiso 1 calc R . H8B H 0.6374 0.6444 0.2261 0.153 Uiso 1 calc R . H8C H 0.6023 0.5636 0.1935 0.153 Uiso 1 calc R . C9 C 0.8632(2) 0.3576(3) 0.5112(3) 0.0579(12) Uani 1 d . . N9 N 0.8331(2) 0.3898(3) 0.5537(2) 0.0568(10) Uani 1 d . . S9 S 0.93299(7) 0.30792(12) 0.53666(10) 0.0811(5) Uani 1 d . . C10 C 0.9496(4) 0.2701(6) 0.6347(5) 0.109(3) Uani 1 d . . H10A H 0.9879 0.2429 0.6486 0.163 Uiso 1 calc R . H10B H 0.9191 0.2319 0.6382 0.163 Uiso 1 calc R . H10C H 0.9510 0.3151 0.6704 0.163 Uiso 1 calc R . C11 C 0.6547(2) 0.5818(3) 0.3644(3) 0.0551(11) Uani 1 d . . C12 C 0.6696(2) 0.6642(4) 0.3783(3) 0.0607(12) Uani 1 d . . C13 C 0.6240(3) 0.7195(4) 0.3784(3) 0.075(2) Uani 1 d . . H13A H 0.6332 0.7748 0.3879 0.090 Uiso 1 calc R . C14 C 0.5652(3) 0.6936(5) 0.3645(4) 0.080(2) Uani 1 d . . C15 C 0.5520(3) 0.6115(5) 0.3498(4) 0.081(2) Uani 1 d . . H15A H 0.5123 0.5944 0.3393 0.097 Uiso 1 calc R . C16 C 0.5955(2) 0.5535(4) 0.3500(3) 0.0657(14) Uani 1 d . . C17 C 0.7332(3) 0.6947(4) 0.3897(4) 0.0695(14) Uani 1 d . . H17A H 0.7372 0.7494 0.4110 0.104 Uiso 1 calc R . H17B H 0.7417 0.6951 0.3397 0.104 Uiso 1 calc R . H17C H 0.7610 0.6590 0.4257 0.104 Uiso 1 calc R . C18 C 0.5160(4) 0.7536(6) 0.3669(6) 0.123(3) Uani 1 d . . H18A H 0.4806 0.7238 0.3678 0.185 Uiso 1 calc R . H18B H 0.5069 0.7881 0.3208 0.185 Uiso 1 calc R . H18C H 0.5292 0.7870 0.4135 0.185 Uiso 1 calc R . C19 C 0.5793(3) 0.4651(5) 0.3318(4) 0.084(2) Uani 1 d . . H19A H 0.6035 0.4312 0.3734 0.126 Uiso 1 calc R . H19B H 0.5864 0.4504 0.2826 0.126 Uiso 1 calc R . H19C H 0.5377 0.4570 0.3277 0.126 Uiso 1 calc R . C20 C 0.8552(2) 0.3966(4) 0.6379(3) 0.0615(13) Uani 1 d . . C21 C 0.8330(3) 0.3437(4) 0.6853(3) 0.0709(14) Uani 1 d . . C22 C 0.8529(3) 0.3570(5) 0.7667(4) 0.082(2) Uani 1 d . . H22A H 0.8386 0.3229 0.7994 0.099 Uiso 1 calc R . C23 C 0.8931(3) 0.4190(5) 0.8012(4) 0.089(2) Uani 1 d . . C24 C 0.9133(3) 0.4686(5) 0.7516(4) 0.083(2) Uani 1 d . . H24A H 0.9402 0.5104 0.7738 0.100 Uiso 1 calc R . C25 C 0.8957(3) 0.4597(4) 0.6705(3) 0.0706(14) Uani 1 d . . C26 C 0.7911(3) 0.2748(5) 0.6497(4) 0.093(2) Uani 1 d . . H26A H 0.8109 0.2371 0.6240 0.139 Uiso 1 calc R . H26B H 0.7561 0.2966 0.6118 0.139 Uiso 1 calc R . H26C H 0.7795 0.2467 0.6907 0.139 Uiso 1 calc R . C27 C 0.9119(4) 0.4322(7) 0.8897(4) 0.127(4) Uani 1 d . . H27A H 0.8909 0.3943 0.9136 0.191 Uiso 1 calc R . H27B H 0.9025 0.4874 0.9010 0.191 Uiso 1 calc R . H27C H 0.9544 0.4232 0.9106 0.191 Uiso 1 calc R . C28 C 0.9192(3) 0.5170(5) 0.6191(5) 0.093(2) Uani 1 d . . H28A H 0.8862 0.5383 0.5775 0.140 Uiso 1 calc R . H28B H 0.9459 0.4875 0.5965 0.140 Uiso 1 calc R . H28C H 0.9404 0.5616 0.6507 0.140 Uiso 1 calc R . C30 C 0.3894(5) 0.3922(7) 0.4375(5) 0.121(3) Uani 1 d . . H30A H 0.3610 0.4355 0.4383 0.145 Uiso 0.70 calc PR 1 H30B H 0.3917 0.3552 0.4813 0.145 Uiso 0.70 calc PR 1 H30C H 0.3571 0.4271 0.4091 0.145 Uiso 0.30 d PR 2 H30D H 0.3858 0.3860 0.4899 0.145 Uiso 0.30 d PR 2 Cl31 Cl 0.4559(3) 0.4316(6) 0.4454(5) 0.201(4) Uani 0.70 d P 1 Cl32 Cl 0.3668(3) 0.3397(4) 0.3492(4) 0.185(2) Uani 0.70 d P 1 Cl33 Cl 0.4774(9) 0.3942(13) 0.4674(8) 0.186(8) Uani 0.30 d P 2 Cl34 Cl 0.3838(9) 0.2888(12) 0.4171(13) 0.245(9) Uani 0.30 d P 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 Fe 0.0556(4) 0.0727(5) 0.0473(4) -0.0043(4) 0.0248(3) 0.0048(4) Cl1 0.0691(8) 0.1332(14) 0.0730(8) 0.0083(9) 0.0311(7) -0.0181(9) Cl2 0.1063(11) 0.0737(9) 0.0556(7) -0.0084(6) 0.0263(7) 0.0077(8) N1 0.049(2) 0.061(2) 0.056(2) -0.005(2) 0.025(2) -0.001(2) C2 0.055(3) 0.072(3) 0.051(3) -0.005(2) 0.024(2) -0.002(2) C3 0.066(3) 0.084(4) 0.058(3) -0.007(3) 0.033(2) 0.007(3) C4 0.074(4) 0.103(5) 0.062(3) -0.021(3) 0.033(3) 0.009(3) C5 0.064(3) 0.084(4) 0.076(4) -0.020(3) 0.035(3) 0.010(3) C6 0.049(2) 0.064(3) 0.059(3) -0.003(2) 0.022(2) 0.001(2) C7 0.054(3) 0.069(3) 0.046(2) -0.003(2) 0.019(2) -0.004(2) N7 0.057(2) 0.063(3) 0.046(2) 0.001(2) 0.024(2) 0.005(2) S7 0.0776(9) 0.1211(13) 0.0523(7) 0.0139(8) 0.0320(6) 0.0198(9) C8 0.117(6) 0.134(7) 0.059(3) 0.020(4) 0.033(4) 0.043(5) C9 0.053(3) 0.066(3) 0.059(3) -0.001(2) 0.023(2) -0.001(2) N9 0.051(2) 0.062(3) 0.060(2) 0.002(2) 0.021(2) -0.001(2) S9 0.0587(8) 0.1022(12) 0.0848(9) 0.0043(8) 0.0247(7) 0.0189(8) C10 0.097(5) 0.120(7) 0.108(6) 0.022(5) 0.029(4) 0.052(5) C11 0.059(3) 0.073(3) 0.039(2) 0.002(2) 0.024(2) 0.008(2) C12 0.067(3) 0.074(3) 0.049(2) 0.003(2) 0.030(2) 0.004(3) C13 0.086(4) 0.079(4) 0.074(3) 0.004(3) 0.047(3) 0.016(3) C14 0.074(4) 0.092(5) 0.085(4) 0.012(3) 0.039(3) 0.026(3) C15 0.055(3) 0.109(5) 0.084(4) 0.010(4) 0.030(3) 0.006(3) C16 0.055(3) 0.083(4) 0.060(3) 0.004(3) 0.020(2) 0.002(3) C17 0.066(3) 0.075(4) 0.073(3) 0.000(3) 0.030(3) -0.005(3) C18 0.099(5) 0.127(7) 0.167(8) 0.016(6) 0.075(6) 0.043(5) C19 0.065(3) 0.095(5) 0.085(4) -0.003(4) 0.013(3) -0.008(3) C20 0.057(3) 0.072(3) 0.058(3) 0.006(2) 0.019(2) 0.012(2) C21 0.066(3) 0.084(4) 0.066(3) 0.013(3) 0.024(3) 0.009(3) C22 0.085(4) 0.100(5) 0.070(4) 0.020(3) 0.037(3) 0.026(4) C23 0.074(4) 0.122(6) 0.065(3) -0.005(4) 0.014(3) 0.036(4) C24 0.069(3) 0.090(5) 0.082(4) -0.011(4) 0.008(3) 0.011(3) C25 0.063(3) 0.080(4) 0.064(3) 0.000(3) 0.013(2) 0.007(3) C26 0.087(4) 0.098(5) 0.097(5) 0.021(4) 0.034(4) -0.011(4) C27 0.106(6) 0.203(11) 0.065(4) 0.000(5) 0.014(4) 0.061(6) C28 0.078(4) 0.092(5) 0.105(5) 0.009(4) 0.019(4) -0.015(4) C30 0.131(7) 0.139(8) 0.096(5) 0.008(5) 0.040(5) 0.012(6) Cl31 0.131(4) 0.276(10) 0.198(6) 0.024(6) 0.053(4) -0.069(5) Cl32 0.222(6) 0.165(5) 0.168(4) -0.067(4) 0.053(4) -0.011(4) Cl33 0.254(20) 0.223(16) 0.107(7) -0.022(9) 0.095(10) -0.004(13) Cl34 0.259(20) 0.227(18) 0.250(18) -0.135(15) 0.074(16) -0.084(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.123(4) . ? Fe N7 2.274(4) . ? Fe Cl1 2.276(2) . ? Fe N9 2.281(4) . ? Fe Cl2 2.284(2) . ? N1 C6 1.338(6) . ? N1 C2 1.350(6) . ? C2 C3 1.383(7) . ? C2 C7 1.499(7) . ? C3 C4 1.365(8) . ? C4 C5 1.359(8) . ? C5 C6 1.403(7) . ? C6 C9 1.491(7) . ? C7 N7 1.289(6) . ? C7 S7 1.738(5) . ? N7 C11 1.439(6) . ? S7 C8 1.779(7) . ? C9 N9 1.281(6) . ? C9 S9 1.752(5) . ? N9 C20 1.428(7) . ? S9 C10 1.771(8) . ? C11 C12 1.390(8) . ? C11 C16 1.405(7) . ? C12 C13 1.392(8) . ? C12 C17 1.519(8) . ? C13 C14 1.384(9) . ? C14 C15 1.379(10) . ? C14 C18 1.517(9) . ? C15 C16 1.383(9) . ? C16 C19 1.499(9) . ? C20 C25 1.400(9) . ? C20 C21 1.402(8) . ? C21 C22 1.393(9) . ? C21 C26 1.498(10) . ? C22 C23 1.391(11) . ? C23 C24 1.372(11) . ? C23 C27 1.510(9) . ? C24 C25 1.379(9) . ? C25 C28 1.511(9) . ? C30 Cl31 1.644(12) . ? C30 Cl34 1.72(2) . ? C30 Cl32 1.721(11) . ? C30 Cl33 1.96(2) . ? 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 N1 Fe N7 73.01(15) . . ? N1 Fe Cl1 119.67(13) . . ? N7 Fe Cl1 101.46(11) . . ? N1 Fe N9 73.02(15) . . ? N7 Fe N9 145.15(14) . . ? Cl1 Fe N9 101.83(12) . . ? N1 Fe Cl2 127.88(12) . . ? N7 Fe Cl2 97.01(11) . . ? Cl1 Fe Cl2 112.45(7) . . ? N9 Fe Cl2 97.62(12) . . ? C6 N1 C2 120.6(4) . . ? C6 N1 Fe 119.1(3) . . ? C2 N1 Fe 119.5(3) . . ? N1 C2 C3 120.2(5) . . ? N1 C2 C7 114.8(4) . . ? C3 C2 C7 125.0(5) . . ? C4 C3 C2 119.6(5) . . ? C5 C4 C3 120.2(5) . . ? C4 C5 C6 119.1(5) . . ? N1 C6 C5 120.2(5) . . ? N1 C6 C9 114.3(4) . . ? C5 C6 C9 125.5(5) . . ? N7 C7 C2 115.0(4) . . ? N7 C7 S7 132.8(4) . . ? C2 C7 S7 112.2(3) . . ? C7 N7 C11 122.1(4) . . ? C7 N7 Fe 116.8(3) . . ? C11 N7 Fe 120.8(3) . . ? C7 S7 C8 110.8(3) . . ? N9 C9 C6 116.4(5) . . ? N9 C9 S9 131.6(4) . . ? C6 C9 S9 111.8(3) . . ? C9 N9 C20 123.3(4) . . ? C9 N9 Fe 115.3(3) . . ? C20 N9 Fe 120.2(3) . . ? C9 S9 C10 109.5(3) . . ? C12 C11 C16 122.0(5) . . ? C12 C11 N7 120.1(5) . . ? C16 C11 N7 117.8(5) . . ? C11 C12 C13 118.2(5) . . ? C11 C12 C17 121.5(5) . . ? C13 C12 C17 120.2(6) . . ? C14 C13 C12 121.2(6) . . ? C15 C14 C13 118.9(5) . . ? C15 C14 C18 120.1(7) . . ? C13 C14 C18 121.0(7) . . ? C14 C15 C16 122.5(6) . . ? C15 C16 C11 117.2(6) . . ? C15 C16 C19 121.1(5) . . ? C11 C16 C19 121.7(5) . . ? C25 C20 C21 121.8(5) . . ? C25 C20 N9 118.7(5) . . ? C21 C20 N9 119.3(5) . . ? C22 C21 C20 116.8(6) . . ? C22 C21 C26 121.9(6) . . ? C20 C21 C26 121.2(5) . . ? C23 C22 C21 123.0(6) . . ? C24 C23 C22 117.3(6) . . ? C24 C23 C27 121.8(8) . . ? C22 C23 C27 120.8(8) . . ? C23 C24 C25 123.3(7) . . ? C24 C25 C20 117.7(6) . . ? C24 C25 C28 120.6(6) . . ? C20 C25 C28 121.6(5) . . ? Cl31 C30 Cl32 107.6(6) . . ? Cl34 C30 Cl33 94.8(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.363 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.055 #===END data_[Fe(3)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253599' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C37 H35 Cl2 Fe N3 O2, C4 H8 O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H43 Cl2 Fe N3 O3' _chemical_formula_weight 752.53 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.114(2) _cell_length_b 8.9394(7) _cell_length_c 27.383(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.828(14) _cell_angle_gamma 90.00 _cell_volume 3886.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.12 _cell_measurement_theta_max 20.83 _exptl_crystal_description needles _exptl_crystal_colour 'Pale olive' _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method ? _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 4.696 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6189 _exptl_absorpt_correction_T_max 0.7792 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5881 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 60.00 _reflns_number_total 5661 _reflns_number_gt 3381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 684 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00030(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4977 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_all 0.1604 _refine_ls_wR_factor_ref 0.1274 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.146 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.32173(5) 0.61376(9) 0.14226(3) 0.0454(2) Uani 1 d . . Cl1 Cl 0.35178(11) 0.7152(2) 0.21908(7) 0.0955(7) Uani 1 d . . Cl2 Cl 0.30888(12) 0.7671(2) 0.07619(7) 0.0837(6) Uani 1 d . . N1 N 0.2986(2) 0.3840(5) 0.14446(15) 0.0416(9) Uani 1 d . . C2 C 0.2204(3) 0.3325(5) 0.1439(2) 0.0433(12) Uani 1 d . . C3 C 0.2041(4) 0.1824(6) 0.1500(2) 0.0564(15) Uani 1 d . . H3A H 0.1495 0.1493 0.1504 0.068 Uiso 1 calc R . C4 C 0.2701(4) 0.0833(6) 0.1554(3) 0.064(2) Uani 1 d . . H4A H 0.2603 -0.0183 0.1589 0.076 Uiso 1 calc R . C5 C 0.3506(3) 0.1340(6) 0.1555(2) 0.0515(14) Uani 1 d . . H5A H 0.3958 0.0680 0.1592 0.062 Uiso 1 calc R . C6 C 0.3626(3) 0.2867(6) 0.1500(2) 0.0419(11) Uani 1 d . . C7 C 0.1546(3) 0.4518(6) 0.1363(2) 0.0493(13) Uani 1 d . . N7 N 0.1757(3) 0.5866(4) 0.1367(2) 0.0427(10) Uani 1 d . . O8 O 0.0751(2) 0.3922(5) 0.1271(2) 0.0713(13) Uani 1 d . . C9 C 0.4465(3) 0.3573(6) 0.1503(2) 0.0471(13) Uani 1 d . . N9 N 0.4509(2) 0.4976(5) 0.1448(2) 0.0438(10) Uani 1 d . . O10 O 0.5090(2) 0.2546(4) 0.1585(2) 0.0637(11) Uani 1 d . . C11 C 0.1150(3) 0.7037(5) 0.1246(2) 0.0421(11) Uani 1 d . . C12 C 0.0794(4) 0.7270(6) 0.0748(2) 0.0534(13) Uani 1 d . . C13 C 0.0238(4) 0.8446(6) 0.0641(2) 0.059(2) Uani 1 d . . H13A H -0.0012 0.8603 0.0313 0.071 Uiso 1 calc R . C14 C 0.0034(4) 0.9400(6) 0.0998(2) 0.0562(15) Uani 1 d . . C15 C 0.0404(3) 0.9148(6) 0.1479(2) 0.0542(14) Uani 1 d . . H15A H 0.0271 0.9780 0.1724 0.065 Uiso 1 calc R . C16 C 0.0969(3) 0.7990(6) 0.1617(2) 0.0461(12) Uani 1 d . . C17 C 0.0989(5) 0.6268(8) 0.0338(2) 0.076(2) Uani 1 d . . H17A H 0.0865 0.5249 0.0410 0.115 Uiso 1 d R . H17B H 0.1575 0.6356 0.0314 0.115 Uiso 1 d R . H17C H 0.0652 0.6561 0.0029 0.115 Uiso 1 d R . C18 C -0.0576(5) 1.0700(8) 0.0865(3) 0.091(2) Uani 1 d . . H18A H -0.0926 1.0799 0.1113 0.137 Uiso 1 d R . H18B H -0.0922 1.0511 0.0549 0.137 Uiso 1 d R . H18C H -0.0263 1.1607 0.0847 0.137 Uiso 1 d R . C19 C 0.1339(4) 0.7781(8) 0.2154(2) 0.064(2) Uani 1 d . . H19A H 0.1873 0.7284 0.2181 0.096 Uiso 1 d R . H19B H 0.0965 0.7187 0.2312 0.096 Uiso 1 d R . H19C H 0.1417 0.8740 0.2314 0.096 Uiso 1 d R . C20 C 0.5289(3) 0.5792(5) 0.1519(2) 0.0419(12) Uani 1 d . . C21 C 0.5743(3) 0.5987(6) 0.1999(2) 0.0471(12) Uani 1 d . . C22 C 0.6433(3) 0.6935(7) 0.2056(2) 0.0582(15) Uani 1 d . . H22A H 0.6750 0.7053 0.2371 0.070 Uiso 1 calc R . C23 C 0.6667(4) 0.7705(6) 0.1670(3) 0.060(2) Uani 1 d . . C24 C 0.6216(4) 0.7459(7) 0.1197(2) 0.061(2) Uani 1 d . . H24A H 0.6386 0.7937 0.0930 0.073 Uiso 1 calc R . C25 C 0.5525(3) 0.6529(6) 0.1113(2) 0.0496(13) Uani 1 d . . C26 C 0.5497(4) 0.5243(8) 0.2440(2) 0.066(2) Uani 1 d . . H26A H 0.5582 0.4183 0.2420 0.099 Uiso 1 d R . H26B H 0.4914 0.5441 0.2448 0.099 Uiso 1 d R . H26C H 0.5837 0.5625 0.2736 0.099 Uiso 1 d R . C27 C 0.7397(4) 0.8794(9) 0.1753(3) 0.094(2) Uani 1 d . . H27A H 0.7202 0.9769 0.1639 0.141 Uiso 1 d R . H27B H 0.7824 0.8466 0.1572 0.141 Uiso 1 d R . H27C H 0.7627 0.8839 0.2100 0.141 Uiso 1 d R . C28 C 0.5061(4) 0.6293(9) 0.0597(2) 0.070(2) Uani 1 d . . H28A H 0.4581 0.6945 0.0537 0.106 Uiso 1 d R . H28B H 0.4878 0.5272 0.0558 0.106 Uiso 1 d R . H28C H 0.5428 0.6512 0.0364 0.106 Uiso 1 d R . C29 C 0.0188(2) 0.4465(5) 0.20032(15) 0.081(2) Uani 1 d G . H29A H 0.0675 0.4095 0.21972 0.097 Uiso 1 calc R . C30 C -0.0477(3) 0.4955(6) 0.22254(13) 0.097(3) Uani 1 d G . H30A H -0.0434 0.4914 0.25682 0.117 Uiso 1 calc R . C31 C -0.1205(3) 0.5507(6) 0.1935(2) 0.089(2) Uani 1 d G . H31A H -0.1650 0.5835 0.2084 0.107 Uiso 1 calc R . C32 C -0.1268(2) 0.5568(5) 0.1423(2) 0.083(2) Uani 1 d G . H32A H -0.1756 0.5937 0.1229 0.099 Uiso 1 calc R . C33 C -0.0604(2) 0.5078(5) 0.12009(13) 0.069(2) Uani 1 d G . H33A H -0.0646 0.5119 0.08582 0.082 Uiso 1 calc R . C34 C 0.0124(2) 0.4526(4) 0.1491(2) 0.0528(14) Uani 1 d G . C35 C 0.6578(2) 0.2735(5) 0.16267(11) 0.064(2) Uani 1 d G . H35A H 0.6641 0.2781 0.19704 0.077 Uiso 1 calc R . C36 C 0.7285(2) 0.2736(5) 0.1398(2) 0.079(2) Uani 1 d G . H36A H 0.7820 0.2783 0.1588 0.095 Uiso 1 calc R . C37 C 0.7191(2) 0.2667(6) 0.0884(2) 0.084(2) Uani 1 d G . H37A H 0.7663 0.2668 0.0731 0.101 Uiso 1 calc R . C38 C 0.6390(3) 0.2596(6) 0.05995(12) 0.087(2) Uani 1 d G . H38A H 0.6327 0.2550 0.02559 0.105 Uiso 1 calc R . C39 C 0.5684(2) 0.2595(5) 0.08284(13) 0.077(2) Uani 1 d G . H39A H 0.5148 0.2548 0.0638 0.092 Uiso 1 calc R . C40 C 0.5778(2) 0.2664(5) 0.13420(14) 0.0527(14) Uani 1 d G . O50 O 0.3582(4) 0.2708(6) 0.0315(2) 0.102(2) Uani 1 d . . C51 C 0.2906(5) 0.3580(9) 0.0082(3) 0.096(2) Uani 1 d . . H51A H 0.3029 0.3987 -0.0226 0.115 Uiso 1 calc R . H51B H 0.2804 0.4404 0.0295 0.115 Uiso 1 calc R . C52 C 0.2151(6) 0.2585(13) -0.0017(4) 0.131(4) Uani 1 d . . H52A H 0.1797 0.2718 0.0233 0.157 Uiso 1 calc R . H52B H 0.1820 0.2790 -0.0341 0.157 Uiso 1 calc R . C53 C 0.2499(7) 0.1076(12) 0.0003(4) 0.136(4) Uani 1 d . . H53A H 0.2408 0.0633 -0.0326 0.164 Uiso 1 calc R . H53B H 0.2230 0.0450 0.0219 0.164 Uiso 1 calc R . C54 C 0.3399(6) 0.1203(9) 0.0193(3) 0.097(2) Uani 1 d . . H54A H 0.3549 0.0580 0.0485 0.116 Uiso 1 calc R . H54B H 0.3721 0.0873 -0.0055 0.116 Uiso 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 Fe 0.0481(5) 0.0302(4) 0.0575(5) -0.0021(4) 0.0080(4) -0.0035(4) Cl1 0.0715(11) 0.1099(15) 0.0951(13) -0.0600(12) -0.0145(9) 0.0142(10) Cl2 0.0979(13) 0.0626(10) 0.0999(13) 0.0371(9) 0.0438(10) 0.0179(9) N1 0.038(2) 0.037(2) 0.049(2) -0.004(2) 0.006(2) 0.000(2) C2 0.045(3) 0.036(3) 0.049(3) -0.003(2) 0.007(2) -0.004(2) C3 0.047(3) 0.038(3) 0.085(4) -0.005(3) 0.016(3) -0.004(2) C4 0.065(4) 0.029(3) 0.100(5) 0.000(3) 0.021(3) -0.006(3) C5 0.054(3) 0.029(3) 0.073(4) 0.003(2) 0.016(3) 0.004(2) C6 0.039(3) 0.038(3) 0.049(3) 0.002(2) 0.008(2) -0.002(2) C7 0.042(3) 0.040(3) 0.065(4) -0.008(3) 0.010(3) -0.002(2) N7 0.042(2) 0.034(3) 0.051(3) -0.006(2) 0.004(2) 0.002(2) O8 0.034(2) 0.050(2) 0.128(4) -0.024(3) 0.008(2) -0.009(2) C9 0.036(3) 0.048(3) 0.057(3) 0.007(3) 0.008(2) 0.005(2) N9 0.041(2) 0.040(2) 0.051(2) 0.004(2) 0.008(2) 0.001(2) O10 0.046(2) 0.051(2) 0.097(3) 0.024(2) 0.021(2) 0.014(2) C11 0.040(3) 0.033(3) 0.054(3) -0.002(2) 0.008(2) -0.004(2) C12 0.058(3) 0.046(3) 0.054(3) -0.009(3) 0.002(3) -0.001(3) C13 0.057(3) 0.049(3) 0.065(4) -0.005(3) -0.006(3) 0.007(3) C14 0.054(3) 0.037(3) 0.079(4) 0.006(3) 0.017(3) 0.005(2) C15 0.058(3) 0.044(3) 0.065(4) -0.007(3) 0.021(3) -0.001(3) C16 0.042(3) 0.045(3) 0.053(3) -0.007(3) 0.013(2) -0.006(2) C17 0.096(5) 0.073(4) 0.056(4) -0.016(4) -0.002(3) 0.016(4) C18 0.086(5) 0.064(4) 0.120(6) 0.004(4) 0.004(5) 0.031(4) C19 0.064(4) 0.071(4) 0.058(4) -0.004(3) 0.015(3) 0.004(3) C20 0.038(3) 0.038(3) 0.051(3) -0.002(2) 0.012(2) -0.003(2) C21 0.042(3) 0.049(3) 0.050(3) 0.001(3) 0.007(2) 0.000(3) C22 0.044(3) 0.061(4) 0.066(4) -0.005(3) 0.000(3) -0.002(3) C23 0.048(3) 0.043(3) 0.090(5) -0.002(3) 0.014(3) -0.005(3) C24 0.055(3) 0.058(4) 0.072(4) 0.013(3) 0.022(3) -0.003(3) C25 0.051(3) 0.052(3) 0.046(3) 0.004(3) 0.011(2) 0.003(2) C26 0.053(3) 0.092(5) 0.054(3) 0.016(3) 0.008(3) -0.001(3) C27 0.064(4) 0.066(4) 0.152(8) -0.009(5) 0.016(4) -0.021(4) C28 0.069(4) 0.092(5) 0.053(3) 0.005(4) 0.014(3) -0.004(4) C29 0.062(4) 0.075(4) 0.102(6) 0.041(4) 0.007(4) 0.000(3) C30 0.088(6) 0.114(7) 0.094(6) 0.021(5) 0.027(5) -0.022(5) C31 0.066(5) 0.085(5) 0.122(7) 0.002(5) 0.034(5) -0.006(4) C32 0.041(3) 0.083(5) 0.121(7) 0.007(5) 0.002(4) 0.014(3) C33 0.049(3) 0.066(4) 0.086(5) 0.012(4) -0.002(3) -0.001(3) C34 0.034(3) 0.041(3) 0.082(4) 0.008(3) 0.005(3) 0.001(2) C35 0.053(3) 0.064(4) 0.073(4) 0.002(3) 0.007(3) 0.006(3) C36 0.043(3) 0.079(5) 0.115(6) 0.016(4) 0.013(3) 0.002(3) C37 0.069(4) 0.078(5) 0.113(6) 0.014(5) 0.036(4) 0.022(4) C38 0.086(5) 0.107(6) 0.074(5) -0.011(4) 0.028(4) 0.021(5) C39 0.062(4) 0.089(5) 0.077(5) -0.017(4) 0.002(3) 0.018(4) C40 0.042(3) 0.039(3) 0.079(4) 0.002(3) 0.015(3) 0.006(2) O50 0.094(4) 0.081(4) 0.126(5) 0.007(3) 0.003(3) -0.008(3) C51 0.097(6) 0.079(5) 0.112(6) 0.002(5) 0.020(5) 0.005(5) C52 0.098(7) 0.136(9) 0.150(10) 0.009(8) -0.002(6) 0.004(7) C53 0.127(8) 0.099(7) 0.161(10) 0.008(7) -0.036(7) -0.041(7) C54 0.134(7) 0.061(4) 0.093(6) 0.001(4) 0.015(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.090(4) . ? Fe Cl2 2.251(2) . ? Fe Cl1 2.266(2) . ? Fe N9 2.317(4) . ? Fe N7 2.345(4) . ? N1 C6 1.338(6) . ? N1 C2 1.339(6) . ? C2 C3 1.383(7) . ? C2 C7 1.492(7) . ? C3 C4 1.373(8) . ? C4 C5 1.372(8) . ? C5 C6 1.391(7) . ? C6 C9 1.491(7) . ? C7 N7 1.251(7) . ? C7 O8 1.370(6) . ? N7 C11 1.433(6) . ? O8 C34 1.373(5) . ? C9 N9 1.267(7) . ? C9 O10 1.354(6) . ? N9 C20 1.437(6) . ? O10 C40 1.390(5) . ? C11 C16 1.394(7) . ? C11 C12 1.403(7) . ? C12 C13 1.380(8) . ? C12 C17 1.511(8) . ? C13 C14 1.379(8) . ? C14 C15 1.368(8) . ? C14 C18 1.525(8) . ? C15 C16 1.387(8) . ? C16 C19 1.503(7) . ? C20 C25 1.400(7) . ? C20 C21 1.403(7) . ? C21 C22 1.385(8) . ? C21 C26 1.490(8) . ? C22 C23 1.368(8) . ? C23 C24 1.391(9) . ? C23 C27 1.514(8) . ? C24 C25 1.376(8) . ? C25 C28 1.496(7) . ? C29 C30 1.39 . ? C29 C34 1.39 . ? C30 C31 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C35 C36 1.39 . ? C35 C40 1.39 . ? C36 C37 1.39 . ? C37 C38 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? O50 C51 1.401(9) . ? O50 C54 1.405(9) . ? C51 C52 1.494(12) . ? C52 C53 1.458(14) . ? C53 C54 1.460(12) . ? 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 N1 Fe Cl2 128.99(13) . . ? N1 Fe Cl1 112.18(13) . . ? Cl2 Fe Cl1 118.56(9) . . ? N1 Fe N9 73.91(15) . . ? Cl2 Fe N9 104.80(12) . . ? Cl1 Fe N9 95.93(12) . . ? N1 Fe N7 73.62(14) . . ? Cl2 Fe N7 93.27(12) . . ? Cl1 Fe N7 98.93(12) . . ? N9 Fe N7 147.39(15) . . ? C6 N1 C2 118.9(4) . . ? C6 N1 Fe 120.3(3) . . ? C2 N1 Fe 120.6(3) . . ? N1 C2 C3 122.0(5) . . ? N1 C2 C7 113.6(4) . . ? C3 C2 C7 124.4(5) . . ? C4 C3 C2 118.7(5) . . ? C5 C4 C3 120.1(5) . . ? C4 C5 C6 118.2(5) . . ? N1 C6 C5 122.1(5) . . ? N1 C6 C9 114.0(4) . . ? C5 C6 C9 124.0(5) . . ? N7 C7 O8 128.3(5) . . ? N7 C7 C2 120.1(5) . . ? O8 C7 C2 111.5(4) . . ? C7 N7 C11 121.9(4) . . ? C7 N7 Fe 111.6(3) . . ? C11 N7 Fe 125.3(3) . . ? C7 O8 C34 120.0(4) . . ? N9 C9 O10 129.5(5) . . ? N9 C9 C6 119.2(5) . . ? O10 C9 C6 111.2(4) . . ? C9 N9 C20 123.5(4) . . ? C9 N9 Fe 112.2(3) . . ? C20 N9 Fe 122.5(3) . . ? C9 O10 C40 120.0(4) . . ? C16 C11 C12 121.1(5) . . ? C16 C11 N7 119.9(5) . . ? C12 C11 N7 118.9(5) . . ? C13 C12 C11 117.5(5) . . ? C13 C12 C17 120.3(5) . . ? C11 C12 C17 122.1(5) . . ? C14 C13 C12 123.1(6) . . ? C15 C14 C13 117.6(5) . . ? C15 C14 C18 120.9(6) . . ? C13 C14 C18 121.5(6) . . ? C14 C15 C16 122.9(5) . . ? C15 C16 C11 117.9(5) . . ? C15 C16 C19 119.5(5) . . ? C11 C16 C19 122.7(5) . . ? C25 C20 C21 121.2(5) . . ? C25 C20 N9 118.7(5) . . ? C21 C20 N9 119.6(4) . . ? C22 C21 C20 117.5(5) . . ? C22 C21 C26 120.1(5) . . ? C20 C21 C26 122.5(5) . . ? C23 C22 C21 122.9(5) . . ? C22 C23 C24 118.1(5) . . ? C22 C23 C27 121.2(6) . . ? C24 C23 C27 120.7(6) . . ? C25 C24 C23 122.1(5) . . ? C24 C25 C20 118.1(5) . . ? C24 C25 C28 120.2(5) . . ? C20 C25 C28 121.6(5) . . ? C30 C29 C34 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? O8 C34 C33 120.1(4) . . ? O8 C34 C29 119.7(4) . . ? C33 C34 C29 120.0 . . ? C36 C35 C40 120.0 . . ? C37 C36 C35 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? O10 C40 C39 121.5(3) . . ? O10 C40 C35 118.3(3) . . ? C39 C40 C35 120.0 . . ? C51 O50 C54 108.1(6) . . ? O50 C51 C52 107.3(7) . . ? C53 C52 C51 104.4(8) . . ? C52 C53 C54 107.1(8) . . ? O50 C54 C53 108.3(8) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.232 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.053 #===END data_[Fe(4)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253600' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Cl2 Fe N3 S2, C H2 Cl2' _chemical_formula_sum 'C38 H37 Cl4 Fe N3 S2' _chemical_formula_weight 797.48 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' S S 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.148(4) _cell_length_b 20.564(4) _cell_length_c 22.319(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7870(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 4.96 _cell_measurement_theta_max 12.50 _exptl_crystal_description prisms _exptl_crystal_colour Red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4939 _exptl_absorpt_correction_T_max 0.8383 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.62 _diffrn_reflns_number 5750 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1295 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.49 _reflns_number_total 5750 _reflns_number_gt 2556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5750 _refine_ls_number_parameters 451 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1875 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.25790(7) 0.67031(6) 0.44843(5) 0.0539(3) Uani 1 1 d . . . Cl1 Cl 0.35472(19) 0.59590(14) 0.43251(12) 0.0959(9) Uani 1 1 d . . . Cl2 Cl 0.13350(14) 0.63839(13) 0.46154(11) 0.0765(7) Uani 1 1 d . . . N1 N 0.3247(4) 0.7571(3) 0.4462(3) 0.0459(15) Uani 1 1 d . . . C2 C 0.3673(5) 0.7690(4) 0.4945(4) 0.053(2) Uani 1 1 d . . . C3 C 0.4419(5) 0.7986(4) 0.4915(4) 0.054(2) Uani 1 1 d . . . H3A H 0.4719 0.8054 0.5256 0.064 Uiso 1 1 calc R . . C4 C 0.4678(5) 0.8168(4) 0.4351(4) 0.056(2) Uani 1 1 d . . . H4A H 0.5164 0.8364 0.4311 0.067 Uiso 1 1 calc R . . C5 C 0.4225(5) 0.8064(4) 0.3850(4) 0.052(2) Uani 1 1 d . . . H5A H 0.4398 0.8192 0.3473 0.063 Uiso 1 1 calc R . . C6 C 0.3501(5) 0.7761(4) 0.3921(3) 0.048(2) Uani 1 1 d . . . C7 C 0.3318(5) 0.7455(4) 0.5523(4) 0.053(2) Uani 1 1 d . . . N7 N 0.2862(4) 0.6961(3) 0.5458(3) 0.0552(17) Uani 1 1 d . . . S8 S 0.35370(15) 0.78248(12) 0.62116(10) 0.0660(7) Uani 1 1 d . . . C9 C 0.2974(5) 0.7571(4) 0.3424(3) 0.049(2) Uani 1 1 d . . . N9 N 0.2519(4) 0.7087(3) 0.3521(3) 0.0528(16) Uani 1 1 d . . . S10 S 0.29730(17) 0.80025(12) 0.27399(10) 0.0682(7) Uani 1 1 d . . . C11 C 0.2453(5) 0.6696(4) 0.5966(3) 0.0503(19) Uani 1 1 d . . . C12 C 0.2696(5) 0.6107(4) 0.6214(4) 0.058(2) Uani 1 1 d . . . C13 C 0.2245(5) 0.5832(5) 0.6662(4) 0.066(3) Uani 1 1 d . . . H13A H 0.2405 0.5440 0.6829 0.080 Uiso 1 1 calc R . . C14 C 0.1573(6) 0.6116(6) 0.6868(4) 0.073(3) Uani 1 1 d . . . C15 C 0.1347(5) 0.6703(5) 0.6620(4) 0.065(2) Uani 1 1 d . . . H15A H 0.0900 0.6906 0.6763 0.078 Uiso 1 1 calc R . . C16 C 0.1766(5) 0.6999(4) 0.6164(4) 0.057(2) Uani 1 1 d . . . C17 C 0.3442(6) 0.5789(5) 0.5994(5) 0.095(4) Uani 1 1 d . . . H17A H 0.3369 0.5637 0.5591 0.143 Uiso 1 1 calc R . . H17B H 0.3570 0.5429 0.6249 0.143 Uiso 1 1 calc R . . H17C H 0.3859 0.6101 0.6002 0.143 Uiso 1 1 calc R . . C18 C 0.1083(6) 0.5787(6) 0.7341(4) 0.093(4) Uani 1 1 d . . . H18A H 0.0558 0.5742 0.7198 0.140 Uiso 1 1 calc R . . H18B H 0.1084 0.6046 0.7699 0.140 Uiso 1 1 calc R . . H18C H 0.1295 0.5366 0.7427 0.140 Uiso 1 1 calc R . . C19 C 0.1482(6) 0.7620(4) 0.5887(4) 0.077(3) Uani 1 1 d . . . H19A H 0.1600 0.7620 0.5466 0.116 Uiso 1 1 calc R . . H19B H 0.1735 0.7983 0.6075 0.116 Uiso 1 1 calc R . . H19C H 0.0928 0.7656 0.5941 0.116 Uiso 1 1 calc R . . C20 C 0.1994(6) 0.6881(4) 0.3043(4) 0.065(3) Uani 1 1 d . . . C21 C 0.1214(6) 0.7109(5) 0.3047(5) 0.076(3) Uani 1 1 d . . . C22 C 0.0719(7) 0.6865(6) 0.2621(5) 0.090(4) Uani 1 1 d . . . H22A H 0.0206 0.7012 0.2616 0.107 Uiso 1 1 calc R . . C23 C 0.0938(9) 0.6416(7) 0.2204(6) 0.099(4) Uani 1 1 d . . . C24 C 0.1722(9) 0.6198(5) 0.2203(5) 0.099(4) Uani 1 1 d . . . H24A H 0.1887 0.5903 0.1914 0.119 Uiso 1 1 calc R . . C25 C 0.2252(6) 0.6423(5) 0.2633(4) 0.070(3) Uani 1 1 d . . . C26 C 0.0956(6) 0.7606(6) 0.3484(5) 0.101(4) Uani 1 1 d . . . H26A H 0.1227 0.8006 0.3409 0.151 Uiso 1 1 calc R . . H26B H 0.1070 0.7459 0.3883 0.151 Uiso 1 1 calc R . . H26C H 0.0405 0.7674 0.3443 0.151 Uiso 1 1 calc R . . C27 C 0.0378(9) 0.6129(7) 0.1742(5) 0.157(7) Uani 1 1 d . . . H27A H 0.0333 0.6421 0.1408 0.235 Uiso 1 1 calc R . . H27B H -0.0125 0.6068 0.1922 0.235 Uiso 1 1 calc R . . H27C H 0.0575 0.5718 0.1605 0.235 Uiso 1 1 calc R . . C28 C 0.3068(7) 0.6180(5) 0.2645(4) 0.084(3) Uani 1 1 d . . . H28A H 0.3420 0.6531 0.2559 0.126 Uiso 1 1 calc R . . H28B H 0.3130 0.5844 0.2350 0.126 Uiso 1 1 calc R . . H28C H 0.3183 0.6007 0.3035 0.126 Uiso 1 1 calc R . . C29 C 0.4376(6) 0.8959(5) 0.6138(4) 0.074(3) Uani 1 1 d . . . H29A H 0.4754 0.8738 0.6357 0.089 Uiso 1 1 calc R . . C30 C 0.4506(7) 0.9589(6) 0.5964(5) 0.092(4) Uani 1 1 d . . . H30A H 0.4969 0.9795 0.6071 0.111 Uiso 1 1 calc R . . C31 C 0.3967(8) 0.9912(5) 0.5639(5) 0.094(4) Uani 1 1 d . . . H31A H 0.4068 1.0337 0.5518 0.113 Uiso 1 1 calc R . . C32 C 0.3265(7) 0.9623(6) 0.5482(5) 0.097(4) Uani 1 1 d . . . H32A H 0.2900 0.9849 0.5256 0.116 Uiso 1 1 calc R . . C33 C 0.3113(7) 0.8980(5) 0.5671(5) 0.082(3) Uani 1 1 d . . . H33A H 0.2641 0.8779 0.5583 0.098 Uiso 1 1 calc R . . C34 C 0.3694(5) 0.8653(4) 0.5992(4) 0.061(2) Uani 1 1 d . . . C35 C 0.3786(6) 0.9143(5) 0.2706(4) 0.076(3) Uani 1 1 d . . . H35A H 0.4076 0.8947 0.2404 0.092 Uiso 1 1 calc R . . C36 C 0.3953(7) 0.9781(6) 0.2891(6) 0.100(4) Uani 1 1 d . . . H36A H 0.4362 1.0010 0.2716 0.120 Uiso 1 1 calc R . . C37 C 0.3515(11) 1.0061(6) 0.3324(8) 0.125(6) Uani 1 1 d . . . H37A H 0.3622 1.0486 0.3438 0.150 Uiso 1 1 calc R . . C38 C 0.2913(8) 0.9730(6) 0.3602(6) 0.102(4) Uani 1 1 d . . . H38A H 0.2626 0.9927 0.3905 0.123 Uiso 1 1 calc R . . C39 C 0.2743(6) 0.9105(5) 0.3423(4) 0.075(3) Uani 1 1 d . . . H39A H 0.2333 0.8880 0.3600 0.090 Uiso 1 1 calc R . . C40 C 0.3180(5) 0.8813(4) 0.2983(4) 0.061(3) Uani 1 1 d . . . C50 C 0.0637(18) 0.9434(16) 0.4589(9) 0.118(11) Uiso 0.446(4) 1 d PDU A 1 H50A H 0.0163 0.9287 0.4782 0.142 Uiso 0.446(4) 1 calc PR A 1 H50B H 0.0745 0.9873 0.4724 0.142 Uiso 0.446(4) 1 calc PR A 1 Cl3 Cl 0.0517(8) 0.9429(6) 0.3841(5) 0.105(3) Uiso 0.446(4) 1 d PDU A 1 Cl4 Cl 0.1389(9) 0.8937(8) 0.4777(7) 0.205(5) Uiso 0.446(4) 1 d PDU A 1 C50' C 0.038(3) 0.938(2) 0.4630(12) 0.109(11) Uiso 0.325(7) 1 d PDU B 2 H50C H -0.0159 0.9319 0.4749 0.131 Uiso 0.325(7) 1 calc PR B 2 H50D H 0.0547 0.9808 0.4756 0.131 Uiso 0.325(7) 1 calc PR B 2 Cl3' Cl 0.0468(18) 0.9304(13) 0.3886(10) 0.180(8) Uiso 0.325(7) 1 d PDU B 2 Cl4' Cl 0.0944(12) 0.8807(9) 0.4949(8) 0.174(6) Uiso 0.325(7) 1 d PDU B 2 C50" C 0.0223(17) 0.894(2) 0.5048(17) 0.090(11) Uiso 0.229(6) 1 d PDU C 3 H50E H 0.0051 0.8657 0.5371 0.108 Uiso 0.229(6) 1 calc PR C 3 H50F H -0.0172 0.9267 0.4978 0.108 Uiso 0.229(6) 1 calc PR C 3 Cl3" Cl 0.0386(16) 0.8505(12) 0.4422(11) 0.222(8) Uiso 0.229(6) 1 d PDU C 3 Cl4" Cl 0.1084(12) 0.9289(10) 0.5221(8) 0.150(6) Uiso 0.229(6) 1 d PDU C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0524(7) 0.0506(6) 0.0587(6) -0.0010(6) -0.0004(7) -0.0054(6) Cl1 0.108(2) 0.090(2) 0.0890(18) -0.0042(15) 0.0019(16) 0.0417(17) Cl2 0.0634(15) 0.0877(17) 0.0783(17) -0.0008(13) 0.0066(13) -0.0165(13) N1 0.049(4) 0.044(4) 0.045(4) -0.006(3) -0.004(3) -0.004(3) C2 0.054(5) 0.054(5) 0.050(5) 0.003(4) 0.000(4) -0.007(4) C3 0.044(5) 0.063(6) 0.054(5) -0.009(4) -0.011(4) -0.003(4) C4 0.045(5) 0.056(5) 0.066(6) 0.003(4) 0.002(4) -0.006(4) C5 0.040(5) 0.064(6) 0.053(5) -0.002(4) -0.001(4) -0.003(4) C6 0.049(5) 0.043(5) 0.053(5) 0.002(4) -0.004(4) -0.007(4) C7 0.048(5) 0.059(5) 0.053(5) 0.000(4) -0.003(4) -0.003(4) N7 0.046(4) 0.059(4) 0.061(4) -0.007(4) -0.002(4) 0.010(3) S8 0.0752(17) 0.0741(16) 0.0488(12) -0.0012(11) -0.0087(12) -0.0170(14) C9 0.051(5) 0.049(5) 0.046(5) 0.001(4) -0.003(4) 0.004(4) N9 0.056(4) 0.049(4) 0.053(4) -0.001(3) -0.003(4) -0.016(4) S10 0.0917(18) 0.0639(15) 0.0491(12) 0.0061(11) -0.0099(13) -0.0204(14) C11 0.045(5) 0.065(5) 0.042(4) -0.003(4) -0.006(4) -0.006(5) C12 0.058(6) 0.068(6) 0.049(5) 0.005(4) -0.013(4) -0.001(5) C13 0.068(7) 0.067(6) 0.064(6) 0.019(5) -0.015(5) -0.008(5) C14 0.052(6) 0.114(9) 0.052(5) 0.002(6) 0.000(5) -0.022(6) C15 0.054(6) 0.082(7) 0.060(6) -0.013(5) -0.008(5) -0.007(6) C16 0.053(6) 0.062(6) 0.056(5) -0.007(5) 0.002(4) -0.007(5) C17 0.081(8) 0.107(9) 0.098(8) 0.028(7) 0.010(7) 0.030(7) C18 0.083(8) 0.125(9) 0.071(7) 0.021(7) 0.000(6) -0.037(7) C19 0.079(7) 0.064(6) 0.089(7) -0.014(5) 0.004(6) -0.001(6) C20 0.082(7) 0.059(6) 0.054(5) 0.009(5) -0.003(5) -0.033(5) C21 0.055(6) 0.086(8) 0.089(7) 0.013(6) -0.023(6) -0.019(6) C22 0.070(8) 0.098(9) 0.101(9) 0.036(7) -0.021(7) -0.030(7) C23 0.106(11) 0.109(10) 0.082(8) 0.038(8) -0.033(8) -0.057(9) C24 0.157(14) 0.080(8) 0.061(7) 0.000(5) -0.002(8) -0.053(9) C25 0.086(8) 0.072(6) 0.051(6) 0.010(5) -0.010(5) -0.029(6) C26 0.065(7) 0.102(9) 0.135(10) -0.003(8) -0.014(7) 0.001(7) C27 0.208(16) 0.163(13) 0.098(9) 0.037(9) -0.081(10) -0.133(13) C28 0.105(9) 0.078(7) 0.069(7) -0.019(5) 0.009(6) -0.007(7) C29 0.069(7) 0.079(7) 0.073(6) 0.002(5) -0.026(5) -0.017(6) C30 0.094(9) 0.076(8) 0.107(9) -0.006(7) -0.005(7) -0.036(7) C31 0.120(11) 0.062(7) 0.099(9) -0.007(6) -0.007(8) -0.007(7) C32 0.103(10) 0.094(9) 0.093(8) -0.024(7) -0.007(7) 0.017(8) C33 0.083(8) 0.069(7) 0.094(8) -0.006(6) -0.010(6) -0.007(6) C34 0.055(6) 0.069(6) 0.059(5) -0.007(5) -0.001(5) -0.004(5) C35 0.081(7) 0.059(6) 0.089(7) 0.016(6) -0.022(6) -0.007(6) C36 0.082(9) 0.069(8) 0.148(12) 0.034(8) -0.043(8) -0.015(7) C37 0.145(15) 0.053(8) 0.177(16) 0.001(9) -0.075(13) 0.017(9) C38 0.118(11) 0.069(8) 0.120(10) -0.030(8) -0.040(9) 0.037(8) C39 0.061(7) 0.086(8) 0.078(7) 0.007(6) -0.011(5) 0.015(6) C40 0.061(6) 0.050(6) 0.071(6) 0.012(5) -0.027(5) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.121(6) . ? Fe Cl2 2.251(3) . ? Fe Cl1 2.286(3) . ? Fe N7 2.289(7) . ? Fe N9 2.293(6) . ? N1 C2 1.326(10) . ? N1 C6 1.342(9) . ? C2 C3 1.418(11) . ? C2 C7 1.507(11) . ? C3 C4 1.385(11) . ? C4 C5 1.378(11) . ? C5 C6 1.399(11) . ? C6 C9 1.483(11) . ? C7 N7 1.291(10) . ? C7 S8 1.754(9) . ? N7 C11 1.438(10) . ? S8 C34 1.793(9) . ? C9 N9 1.283(10) . ? C9 S10 1.765(8) . ? N9 C20 1.460(11) . ? S10 C40 1.789(9) . ? C11 C12 1.396(11) . ? C11 C16 1.404(11) . ? C12 C13 1.384(12) . ? C12 C17 1.519(13) . ? C13 C14 1.372(13) . ? C14 C15 1.384(13) . ? C14 C18 1.509(12) . ? C15 C16 1.386(12) . ? C16 C19 1.502(12) . ? C20 C25 1.384(13) . ? C20 C21 1.418(14) . ? C21 C22 1.371(14) . ? C21 C26 1.479(14) . ? C22 C23 1.364(16) . ? C23 C24 1.417(18) . ? C23 C27 1.528(15) . ? C24 C25 1.400(14) . ? C25 C28 1.488(14) . ? C29 C34 1.368(12) . ? C29 C30 1.371(13) . ? C30 C31 1.351(15) . ? C31 C32 1.388(15) . ? C32 C33 1.411(14) . ? C33 C34 1.399(13) . ? C35 C40 1.387(13) . ? C35 C36 1.404(15) . ? C36 C37 1.352(18) . ? C37 C38 1.384(19) . ? C38 C39 1.378(15) . ? C39 C40 1.372(12) . ? C50 Cl3 1.681(16) . ? C50 Cl4 1.699(16) . ? C50' Cl3' 1.675(17) . ? C50' Cl4' 1.680(17) . ? C50" Cl3" 1.680(19) . ? C50" Cl4" 1.687(19) . ? 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 N1 Fe Cl2 139.46(19) . . ? N1 Fe Cl1 99.6(2) . . ? Cl2 Fe Cl1 120.89(12) . . ? N1 Fe N7 73.3(3) . . ? Cl2 Fe N7 98.33(19) . . ? Cl1 Fe N7 98.54(18) . . ? N1 Fe N9 73.3(2) . . ? Cl2 Fe N9 100.37(19) . . ? Cl1 Fe N9 96.7(2) . . ? N7 Fe N9 145.1(2) . . ? C2 N1 C6 119.9(6) . . ? C2 N1 Fe 115.8(5) . . ? C6 N1 Fe 116.2(5) . . ? N1 C2 C3 122.5(7) . . ? N1 C2 C7 114.5(7) . . ? C3 C2 C7 122.9(7) . . ? C4 C3 C2 116.7(7) . . ? C5 C4 C3 120.9(8) . . ? C4 C5 C6 118.6(8) . . ? N1 C6 C5 121.3(7) . . ? N1 C6 C9 113.5(7) . . ? C5 C6 C9 125.0(7) . . ? N7 C7 C2 113.6(7) . . ? N7 C7 S8 124.7(7) . . ? C2 C7 S8 121.6(6) . . ? C7 N7 C11 120.3(7) . . ? C7 N7 Fe 114.7(6) . . ? C11 N7 Fe 123.8(5) . . ? C7 S8 C34 101.8(4) . . ? N9 C9 C6 116.6(7) . . ? N9 C9 S10 122.3(6) . . ? C6 C9 S10 121.1(6) . . ? C9 N9 C20 118.4(7) . . ? C9 N9 Fe 113.5(5) . . ? C20 N9 Fe 127.9(5) . . ? C9 S10 C40 101.9(4) . . ? C12 C11 C16 120.6(8) . . ? C12 C11 N7 119.7(8) . . ? C16 C11 N7 119.3(8) . . ? C13 C12 C11 118.3(9) . . ? C13 C12 C17 121.9(9) . . ? C11 C12 C17 119.7(8) . . ? C14 C13 C12 122.5(9) . . ? C13 C14 C15 118.1(9) . . ? C13 C14 C18 120.8(10) . . ? C15 C14 C18 121.0(10) . . ? C14 C15 C16 122.1(9) . . ? C15 C16 C11 118.2(8) . . ? C15 C16 C19 120.5(9) . . ? C11 C16 C19 121.3(8) . . ? C25 C20 C21 122.0(9) . . ? C25 C20 N9 118.9(9) . . ? C21 C20 N9 118.7(9) . . ? C22 C21 C20 117.3(11) . . ? C22 C21 C26 121.7(11) . . ? C20 C21 C26 121.0(9) . . ? C23 C22 C21 123.4(12) . . ? C22 C23 C24 118.4(11) . . ? C22 C23 C27 123.3(15) . . ? C24 C23 C27 118.3(15) . . ? C25 C24 C23 120.7(12) . . ? C20 C25 C24 118.1(11) . . ? C20 C25 C28 121.1(9) . . ? C24 C25 C28 120.8(11) . . ? C34 C29 C30 120.4(10) . . ? C31 C30 C29 120.4(11) . . ? C30 C31 C32 121.2(11) . . ? C31 C32 C33 119.1(11) . . ? C34 C33 C32 118.1(10) . . ? C29 C34 C33 120.7(9) . . ? C29 C34 S8 120.0(8) . . ? C33 C34 S8 119.4(7) . . ? C40 C35 C36 118.6(11) . . ? C37 C36 C35 119.6(13) . . ? C36 C37 C38 121.7(13) . . ? C39 C38 C37 119.1(13) . . ? C40 C39 C38 120.0(11) . . ? C39 C40 C35 120.9(9) . . ? C39 C40 S10 121.1(8) . . ? C35 C40 S10 118.0(8) . . ? Cl3 C50 Cl4 109.6(13) . . ? Cl3' C50' Cl4' 107.7(15) . . ? Cl3" C50" Cl4" 105.7(16) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.402 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.071 #===END data_[V(4)Cl3] _database_code_depnum_ccdc_archive 'CCDC 253601' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Cl3 N3 S2 V, 1.5(C H2 Cl2)' _chemical_formula_sum 'C38.50 H38 Cl6 N3 S2 V' _chemical_formula_weight 870.48 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' S S 0.1246 0.1234 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3896(16) _cell_length_b 19.617(2) _cell_length_c 16.797(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.449(16) _cell_angle_gamma 90.00 _cell_volume 4064.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 203 _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.51 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.97 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7842 _exptl_absorpt_correction_T_max 0.9410 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203 _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 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7507 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7157 _reflns_number_gt 4726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7157 _refine_ls_number_parameters 486 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.988 _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 V V 0.45689(5) 0.26360(3) 0.72708(4) 0.02408(15) Uani 1 1 d . . . Cl1 Cl 0.30642(9) 0.29664(6) 0.79231(6) 0.0376(2) Uani 1 1 d . . . Cl2 Cl 0.55098(9) 0.22032(6) 0.83968(6) 0.0394(2) Uani 1 1 d . . . Cl3 Cl 0.58831(8) 0.23643(6) 0.64174(6) 0.0370(2) Uani 1 1 d . . . N1 N 0.3653(3) 0.30109(17) 0.62687(19) 0.0267(7) Uani 1 1 d . . . C2 C 0.2943(3) 0.2595(2) 0.5854(2) 0.0299(8) Uani 1 1 d . . . C3 C 0.2390(4) 0.2811(3) 0.5145(3) 0.0416(11) Uani 1 1 d . . . H3A H 0.1894 0.2520 0.4854 0.050 Uiso 1 1 calc R . . C4 C 0.2577(4) 0.3460(3) 0.4873(3) 0.0476(12) Uani 1 1 d . . . H4A H 0.2208 0.3613 0.4392 0.057 Uiso 1 1 calc R . . C5 C 0.3309(4) 0.3888(2) 0.5307(3) 0.0418(11) Uani 1 1 d . . . H5A H 0.3439 0.4332 0.5128 0.050 Uiso 1 1 calc R . . C6 C 0.3842(3) 0.3641(2) 0.6014(2) 0.0309(8) Uani 1 1 d . . . C7 C 0.2921(3) 0.1898(2) 0.6199(2) 0.0284(8) Uani 1 1 d . . . N7 N 0.3657(3) 0.17485(17) 0.67722(19) 0.0287(7) Uani 1 1 d . . . S8 S 0.19907(9) 0.12885(6) 0.57651(7) 0.0412(3) Uani 1 1 d . . . C9 C 0.4630(3) 0.4027(2) 0.6570(2) 0.0295(8) Uani 1 1 d . . . N9 N 0.5025(2) 0.37248(17) 0.7219(2) 0.0274(7) Uani 1 1 d . . . S10 S 0.47922(10) 0.48792(6) 0.62522(8) 0.0445(3) Uani 1 1 d . . . C11 C 0.3820(3) 0.1038(2) 0.6990(3) 0.0339(9) Uani 1 1 d . . . C12 C 0.3502(4) 0.0798(2) 0.7713(3) 0.0402(10) Uani 1 1 d . . . C13 C 0.3703(4) 0.0116(3) 0.7916(4) 0.0532(14) Uani 1 1 d . . . H13A H 0.3493 -0.0048 0.8404 0.064 Uiso 1 1 calc R . . C14 C 0.4199(4) -0.0322(3) 0.7422(4) 0.0575(16) Uani 1 1 d . . . C15 C 0.4507(4) -0.0071(2) 0.6697(4) 0.0538(14) Uani 1 1 d . . . H15A H 0.4849 -0.0364 0.6357 0.065 Uiso 1 1 calc R . . C16 C 0.4318(4) 0.0606(2) 0.6470(3) 0.0449(11) Uani 1 1 d . . . C17 C 0.2891(6) 0.1236(3) 0.8257(3) 0.0575(14) Uani 1 1 d . . . H17A H 0.3372 0.1582 0.8504 0.086 Uiso 1 1 calc R . . H17B H 0.2622 0.0953 0.8669 0.086 Uiso 1 1 calc R . . H17C H 0.2285 0.1454 0.7948 0.086 Uiso 1 1 calc R . . C18 C 0.4419(6) -0.1053(3) 0.7671(6) 0.095(3) Uani 1 1 d . . . H18A H 0.5007 -0.1066 0.8095 0.143 Uiso 1 1 calc R . . H18B H 0.4620 -0.1312 0.7216 0.143 Uiso 1 1 calc R . . H18C H 0.3772 -0.1248 0.7861 0.143 Uiso 1 1 calc R . . C19 C 0.4656(5) 0.0842(3) 0.5678(3) 0.0564(14) Uani 1 1 d . . . H19A H 0.5190 0.0529 0.5500 0.085 Uiso 1 1 calc R . . H19B H 0.4969 0.1295 0.5737 0.085 Uiso 1 1 calc R . . H19C H 0.4028 0.0854 0.5287 0.085 Uiso 1 1 calc R . . C20 C 0.5568(3) 0.41135(19) 0.7869(2) 0.0281(8) Uani 1 1 d . . . C21 C 0.6682(3) 0.4010(2) 0.8089(2) 0.0306(8) Uani 1 1 d . . . C22 C 0.7189(4) 0.4418(2) 0.8688(3) 0.0374(9) Uani 1 1 d . . . H22A H 0.7939 0.4369 0.8822 0.045 Uiso 1 1 calc R . . C23 C 0.6621(4) 0.4900(2) 0.9100(3) 0.0388(10) Uani 1 1 d . . . C24 C 0.5522(4) 0.4950(2) 0.8901(3) 0.0409(10) Uani 1 1 d . . . H24A H 0.5124 0.5253 0.9194 0.049 Uiso 1 1 calc R . . C25 C 0.4966(4) 0.4574(2) 0.8284(3) 0.0341(9) Uani 1 1 d . . . C26 C 0.7346(4) 0.3505(2) 0.7661(3) 0.0408(10) Uani 1 1 d . . . H26A H 0.8110 0.3611 0.7773 0.061 Uiso 1 1 calc R . . H26B H 0.7145 0.3534 0.7089 0.061 Uiso 1 1 calc R . . H26C H 0.7208 0.3048 0.7846 0.061 Uiso 1 1 calc R . . C27 C 0.7208(5) 0.5363(3) 0.9717(3) 0.0550(13) Uani 1 1 d . . . H27A H 0.6690 0.5561 1.0048 0.082 Uiso 1 1 calc R . . H27B H 0.7569 0.5724 0.9449 0.082 Uiso 1 1 calc R . . H27C H 0.7741 0.5102 1.0049 0.082 Uiso 1 1 calc R . . C28 C 0.3774(4) 0.4698(3) 0.8082(3) 0.0470(12) Uani 1 1 d . . . H28A H 0.3672 0.5102 0.7750 0.070 Uiso 1 1 calc R . . H28B H 0.3428 0.4765 0.8571 0.070 Uiso 1 1 calc R . . H28C H 0.3452 0.4308 0.7794 0.070 Uiso 1 1 calc R . . C29 C 0.0466(4) 0.2041(3) 0.6486(3) 0.0488(12) Uani 1 1 d . . . H29A H 0.0942 0.2021 0.6956 0.059 Uiso 1 1 calc R . . C30 C -0.0533(5) 0.2359(3) 0.6486(4) 0.0633(15) Uani 1 1 d . . . H30A H -0.0729 0.2562 0.6959 0.076 Uiso 1 1 calc R . . C31 C -0.1235(4) 0.2383(4) 0.5808(4) 0.0638(15) Uani 1 1 d . . . H31A H -0.1911 0.2599 0.5817 0.077 Uiso 1 1 calc R . . C32 C -0.0956(4) 0.2088(3) 0.5109(3) 0.0562(14) Uani 1 1 d . . . H32A H -0.1445 0.2103 0.4646 0.067 Uiso 1 1 calc R . . C33 C 0.0047(4) 0.1769(3) 0.5086(3) 0.0443(11) Uani 1 1 d . . . H33A H 0.0240 0.1571 0.4611 0.053 Uiso 1 1 calc R . . C34 C 0.0753(4) 0.1750(2) 0.5779(3) 0.0355(9) Uani 1 1 d . . . C35 C 0.6142(5) 0.5723(3) 0.7171(3) 0.0532(13) Uani 1 1 d . . . H35A H 0.5503 0.5917 0.7330 0.064 Uiso 1 1 calc R . . C36 C 0.7138(6) 0.5998(3) 0.7437(4) 0.072(2) Uani 1 1 d . . . H36A H 0.7178 0.6385 0.7770 0.087 Uiso 1 1 calc R . . C37 C 0.8075(6) 0.5703(4) 0.7212(4) 0.077(2) Uani 1 1 d . . . H37A H 0.8754 0.5881 0.7407 0.093 Uiso 1 1 calc R . . C38 C 0.8023(5) 0.5155(4) 0.6707(4) 0.073(2) Uani 1 1 d . . . H38A H 0.8664 0.4959 0.6552 0.087 Uiso 1 1 calc R . . C39 C 0.7018(4) 0.4885(3) 0.6421(3) 0.0532(13) Uani 1 1 d . . . H39A H 0.6976 0.4518 0.6060 0.064 Uiso 1 1 calc R . . C40 C 0.6089(4) 0.5164(2) 0.6674(3) 0.0408(11) Uani 1 1 d . . . C50 C 0.4068(7) 0.7346(5) 0.5642(6) 0.068(2) Uani 0.805(14) 1 d PDU A 1 H50A H 0.3539 0.7407 0.6034 0.081 Uiso 0.805(14) 1 calc PR A 1 H50B H 0.3843 0.7631 0.5176 0.081 Uiso 0.805(14) 1 calc PR A 1 Cl4 Cl 0.5357(3) 0.7607(5) 0.6063(3) 0.129(2) Uani 0.805(14) 1 d PDU A 1 Cl5 Cl 0.4085(3) 0.6488(2) 0.5348(3) 0.0913(13) Uani 0.805(14) 1 d PDU A 1 C50' C 0.404(2) 0.7611(15) 0.567(3) 0.075(9) Uiso 0.195(14) 1 d PDU A 2 H50C H 0.3805 0.7779 0.5128 0.090 Uiso 0.195(14) 1 calc PR A 2 H50D H 0.3486 0.7734 0.6021 0.090 Uiso 0.195(14) 1 calc PR A 2 Cl4' Cl 0.5287(14) 0.7978(11) 0.6014(11) 0.102(5) Uiso 0.195(14) 1 d PDU A 2 Cl5' Cl 0.4198(18) 0.6718(13) 0.5648(16) 0.133(7) Uiso 0.195(14) 1 d PDU A 2 C60 C 0.4994(19) -0.0702(12) 1.0197(18) 0.082(7) Uiso 0.280(7) 1 d PDU B -1 H60A H 0.4414 -0.1001 0.9964 0.099 Uiso 0.280(7) 1 calc PR B -1 H60B H 0.5092 -0.0793 1.0772 0.099 Uiso 0.280(7) 1 calc PR B -1 Cl6 Cl 0.6233(9) -0.0916(5) 0.9767(6) 0.113(4) Uiso 0.280(7) 1 d PD B -1 Cl7 Cl 0.4577(19) 0.0154(11) 1.0049(13) 0.199(8) Uiso 0.280(7) 1 d PD B -1 C60' C 0.555(2) 0.0449(10) 0.996(2) 0.075(10) Uiso 0.220(7) 1 d PD B -2 H60C H 0.5714 0.0554 0.9412 0.091 Uiso 0.220(7) 1 calc PR B -2 H60D H 0.6241 0.0436 1.0299 0.091 Uiso 0.220(7) 1 calc PR B -2 Cl6' Cl 0.4916(9) -0.0348(6) 0.9976(6) 0.074(3) Uiso 0.220(7) 1 d PDU B -2 Cl7' Cl 0.4709(17) 0.1098(9) 1.0305(11) 0.154(7) Uiso 0.220(7) 1 d PD 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 V 0.0247(3) 0.0255(3) 0.0214(3) 0.0005(2) -0.0008(2) 0.0038(3) Cl1 0.0358(5) 0.0387(5) 0.0398(5) 0.0016(4) 0.0116(4) 0.0084(4) Cl2 0.0428(5) 0.0445(6) 0.0288(5) 0.0037(4) -0.0072(4) 0.0124(4) Cl3 0.0315(5) 0.0458(6) 0.0345(5) -0.0081(4) 0.0072(4) 0.0016(4) N1 0.0261(16) 0.0297(17) 0.0239(15) 0.0037(13) -0.0004(12) 0.0009(13) C2 0.0285(18) 0.033(2) 0.0275(18) 0.0014(16) -0.0017(15) -0.0043(16) C3 0.037(2) 0.048(3) 0.038(2) 0.0075(19) -0.0069(18) -0.0135(19) C4 0.050(3) 0.049(3) 0.039(2) 0.019(2) -0.020(2) -0.014(2) C5 0.048(3) 0.039(2) 0.036(2) 0.0144(19) -0.011(2) -0.008(2) C6 0.0282(19) 0.033(2) 0.031(2) 0.0084(16) -0.0019(16) -0.0038(16) C7 0.0283(19) 0.029(2) 0.0274(19) -0.0029(15) 0.0020(15) -0.0025(15) N7 0.0295(17) 0.0288(17) 0.0277(16) -0.0008(13) 0.0017(13) 0.0022(13) S8 0.0382(6) 0.0307(5) 0.0520(7) -0.0039(5) -0.0095(5) -0.0041(4) C9 0.0294(19) 0.0261(19) 0.032(2) 0.0025(16) -0.0026(16) -0.0010(16) N9 0.0214(15) 0.0288(16) 0.0313(17) 0.0008(13) -0.0011(13) 0.0008(13) S10 0.0429(6) 0.0337(5) 0.0528(7) 0.0157(5) -0.0169(5) -0.0095(5) C11 0.031(2) 0.0275(19) 0.041(2) 0.0004(17) -0.0104(17) 0.0022(16) C12 0.043(2) 0.033(2) 0.043(2) 0.0042(18) -0.0045(19) -0.0004(19) C13 0.050(3) 0.036(2) 0.069(3) 0.016(2) -0.022(3) -0.007(2) C14 0.038(3) 0.032(2) 0.096(4) 0.005(3) -0.026(3) -0.001(2) C15 0.036(2) 0.033(2) 0.090(4) -0.022(3) -0.011(3) 0.007(2) C16 0.032(2) 0.038(2) 0.063(3) -0.016(2) -0.006(2) 0.0018(19) C17 0.084(4) 0.045(3) 0.046(3) 0.005(2) 0.018(3) -0.009(3) C18 0.062(4) 0.033(3) 0.181(9) 0.012(4) -0.039(5) 0.004(3) C19 0.055(3) 0.057(3) 0.059(3) -0.025(3) 0.014(3) 0.001(3) C20 0.0269(19) 0.0247(18) 0.032(2) 0.0030(15) -0.0017(16) -0.0020(15) C21 0.028(2) 0.030(2) 0.032(2) 0.0054(16) -0.0007(16) 0.0012(16) C22 0.032(2) 0.041(2) 0.037(2) 0.0043(18) -0.0071(18) -0.0028(18) C23 0.048(3) 0.032(2) 0.034(2) -0.0001(17) -0.0051(19) -0.0061(19) C24 0.048(3) 0.034(2) 0.041(2) -0.0092(18) 0.008(2) 0.0000(19) C25 0.036(2) 0.027(2) 0.037(2) -0.0001(16) -0.0017(18) 0.0029(17) C26 0.029(2) 0.046(3) 0.046(3) -0.005(2) -0.0031(18) -0.0003(19) C27 0.063(3) 0.044(3) 0.055(3) -0.011(2) -0.011(3) -0.008(2) C28 0.037(2) 0.042(3) 0.062(3) -0.013(2) 0.004(2) 0.010(2) C29 0.049(3) 0.054(3) 0.042(3) 0.000(2) -0.004(2) -0.011(2) C30 0.051(3) 0.071(4) 0.069(4) -0.022(3) 0.015(3) -0.010(3) C31 0.035(3) 0.074(4) 0.083(4) -0.003(3) 0.012(3) -0.004(3) C32 0.033(2) 0.077(4) 0.057(3) 0.008(3) -0.005(2) -0.002(2) C33 0.040(2) 0.053(3) 0.039(2) 0.005(2) -0.0007(19) -0.010(2) C34 0.032(2) 0.033(2) 0.040(2) 0.0064(17) -0.0018(17) -0.0083(17) C35 0.061(3) 0.034(2) 0.062(3) 0.010(2) -0.008(3) -0.011(2) C36 0.083(5) 0.048(3) 0.078(4) 0.019(3) -0.038(4) -0.033(3) C37 0.065(4) 0.079(4) 0.080(4) 0.043(4) -0.037(3) -0.045(4) C38 0.041(3) 0.091(5) 0.085(5) 0.045(4) 0.001(3) -0.011(3) C39 0.051(3) 0.056(3) 0.052(3) 0.021(2) 0.000(2) -0.004(2) C40 0.039(2) 0.037(2) 0.043(2) 0.0150(19) -0.0098(19) -0.0141(19) C50 0.080(5) 0.069(6) 0.059(4) -0.001(5) 0.025(4) 0.017(4) Cl4 0.098(2) 0.166(5) 0.117(3) -0.057(3) -0.0124(18) 0.008(3) Cl5 0.111(2) 0.074(2) 0.096(2) 0.0182(16) 0.0459(17) -0.0018(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V N1 2.074(3) . ? V N7 2.198(3) . ? V N9 2.213(3) . ? V Cl2 2.2889(12) . ? V Cl3 2.3309(12) . ? V Cl1 2.3418(12) . ? N1 C6 1.335(5) . ? N1 C2 1.345(5) . ? C2 C3 1.383(6) . ? C2 C7 1.486(6) . ? C3 C4 1.380(7) . ? C4 C5 1.390(7) . ? C5 C6 1.390(6) . ? C6 C9 1.493(5) . ? C7 N7 1.295(5) . ? C7 S8 1.769(4) . ? N7 C11 1.451(5) . ? S8 C34 1.782(5) . ? C9 N9 1.296(5) . ? C9 S10 1.772(4) . ? N9 C20 1.444(5) . ? S10 C40 1.783(4) . ? C11 C12 1.393(7) . ? C11 C16 1.402(7) . ? C12 C13 1.397(7) . ? C12 C17 1.509(7) . ? C13 C14 1.380(9) . ? C14 C15 1.400(9) . ? C14 C18 1.509(7) . ? C15 C16 1.395(7) . ? C16 C19 1.505(8) . ? C20 C25 1.399(6) . ? C20 C21 1.409(6) . ? C21 C22 1.389(6) . ? C21 C26 1.512(6) . ? C22 C23 1.399(7) . ? C23 C24 1.375(7) . ? C23 C27 1.511(6) . ? C24 C25 1.400(6) . ? C25 C28 1.504(6) . ? C29 C30 1.386(8) . ? C29 C34 1.395(7) . ? C30 C31 1.367(9) . ? C31 C32 1.382(9) . ? C32 C33 1.395(8) . ? C33 C34 1.388(6) . ? C35 C40 1.376(7) . ? C35 C36 1.382(8) . ? C36 C37 1.382(11) . ? C37 C38 1.369(11) . ? C38 C39 1.395(8) . ? C39 C40 1.378(8) . ? C50 Cl5 1.755(8) . ? C50 Cl4 1.760(8) . ? C50' Cl4' 1.755(17) . ? C50' Cl5' 1.763(17) . ? C60 Cl7 1.767(18) . ? C60 Cl6 1.807(17) . ? C60' Cl6' 1.754(19) . ? C60' Cl7' 1.781(19) . ? 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 N1 V N7 75.50(13) . . ? N1 V N9 75.41(12) . . ? N7 V N9 150.88(12) . . ? N1 V Cl2 177.42(10) . . ? N7 V Cl2 102.96(9) . . ? N9 V Cl2 106.16(9) . . ? N1 V Cl3 86.70(10) . . ? N7 V Cl3 87.05(9) . . ? N9 V Cl3 90.04(9) . . ? Cl2 V Cl3 95.32(5) . . ? N1 V Cl1 83.28(10) . . ? N7 V Cl1 89.67(10) . . ? N9 V Cl1 88.21(9) . . ? Cl2 V Cl1 94.68(5) . . ? Cl3 V Cl1 169.94(5) . . ? C6 N1 C2 121.4(3) . . ? C6 N1 V 119.3(3) . . ? C2 N1 V 119.0(3) . . ? N1 C2 C3 120.4(4) . . ? N1 C2 C7 113.1(3) . . ? C3 C2 C7 126.3(4) . . ? C4 C3 C2 118.8(4) . . ? C3 C4 C5 120.4(4) . . ? C4 C5 C6 118.0(4) . . ? N1 C6 C5 120.9(4) . . ? N1 C6 C9 113.2(3) . . ? C5 C6 C9 125.9(4) . . ? N7 C7 C2 117.4(3) . . ? N7 C7 S8 122.6(3) . . ? C2 C7 S8 119.7(3) . . ? C7 N7 C11 118.5(3) . . ? C7 N7 V 113.8(3) . . ? C11 N7 V 127.6(2) . . ? C7 S8 C34 100.34(19) . . ? N9 C9 C6 117.8(3) . . ? N9 C9 S10 129.8(3) . . ? C6 C9 S10 112.1(3) . . ? C9 N9 C20 120.4(3) . . ? C9 N9 V 113.4(3) . . ? C20 N9 V 125.6(2) . . ? C9 S10 C40 107.5(2) . . ? C12 C11 C16 121.2(4) . . ? C12 C11 N7 120.0(4) . . ? C16 C11 N7 118.8(4) . . ? C11 C12 C13 118.5(5) . . ? C11 C12 C17 122.4(4) . . ? C13 C12 C17 119.0(5) . . ? C14 C13 C12 122.0(6) . . ? C13 C14 C15 118.5(5) . . ? C13 C14 C18 120.3(7) . . ? C15 C14 C18 121.2(7) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C11 118.5(5) . . ? C15 C16 C19 118.8(5) . . ? C11 C16 C19 122.8(5) . . ? C25 C20 C21 121.2(4) . . ? C25 C20 N9 119.0(3) . . ? C21 C20 N9 119.8(4) . . ? C22 C21 C20 118.1(4) . . ? C22 C21 C26 119.5(4) . . ? C20 C21 C26 122.2(4) . . ? C21 C22 C23 122.2(4) . . ? C24 C23 C22 117.5(4) . . ? C24 C23 C27 121.6(5) . . ? C22 C23 C27 120.9(4) . . ? C23 C24 C25 123.2(4) . . ? C20 C25 C24 117.5(4) . . ? C20 C25 C28 123.4(4) . . ? C24 C25 C28 119.0(4) . . ? C30 C29 C34 119.0(5) . . ? C31 C30 C29 120.8(5) . . ? C30 C31 C32 120.2(5) . . ? C31 C32 C33 120.4(5) . . ? C34 C33 C32 118.8(5) . . ? C33 C34 C29 120.7(5) . . ? C33 C34 S8 118.6(4) . . ? C29 C34 S8 120.6(3) . . ? C40 C35 C36 119.8(6) . . ? C37 C36 C35 119.7(6) . . ? C38 C37 C36 120.5(5) . . ? C37 C38 C39 120.0(7) . . ? C40 C39 C38 119.2(6) . . ? C35 C40 C39 120.7(5) . . ? C35 C40 S10 118.7(4) . . ? C39 C40 S10 120.0(4) . . ? Cl5 C50 Cl4 110.9(5) . . ? Cl4' C50' Cl5' 108.5(15) . . ? Cl7 C60 Cl6 114.4(15) . . ? Cl6' C60' Cl7' 110.6(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.630 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.072 #===END data_[Cr(4)Cl3] _database_code_depnum_ccdc_archive 'CCDC 253602' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Cl3 N3 S2 Cr, 1.5(C H2 Cl2)' _chemical_formula_sum 'C38.50 H38 Cl6 Cr N3 S2' _chemical_formula_weight 871.54 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' S S 0.1246 0.1234 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3561(14) _cell_length_b 19.623(2) _cell_length_c 16.750(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.756(15) _cell_angle_gamma 90.00 _cell_volume 4040.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 203 _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.49 _exptl_crystal_description 'tabular needles' _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.97 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6395 _exptl_absorpt_correction_T_max 0.8943 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203 _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 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7433 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7085 _reflns_number_gt 5317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.3368P] 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 7085 _refine_ls_number_parameters 486 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.45169(3) 0.26425(2) 0.72187(2) 0.02202(11) Uani 1 1 d . . . Cl1 Cl 0.30447(6) 0.29538(4) 0.78986(4) 0.03478(17) Uani 1 1 d . . . Cl2 Cl 0.54793(6) 0.22214(4) 0.83498(4) 0.03561(17) Uani 1 1 d . . . Cl3 Cl 0.58611(6) 0.23559(4) 0.64120(4) 0.03481(17) Uani 1 1 d . . . N1 N 0.36260(18) 0.29985(12) 0.62380(13) 0.0255(5) Uani 1 1 d . . . C2 C 0.2912(2) 0.25853(15) 0.58309(16) 0.0279(6) Uani 1 1 d . . . C3 C 0.2341(3) 0.27954(17) 0.51120(18) 0.0378(7) Uani 1 1 d . . . H3A H 0.1841 0.2505 0.4822 0.045 Uiso 1 1 calc R . . C4 C 0.2535(3) 0.3445(2) 0.4838(2) 0.0482(9) Uani 1 1 d . . . H4A H 0.2168 0.3598 0.4353 0.058 Uiso 1 1 calc R . . C5 C 0.3267(3) 0.38719(18) 0.5274(2) 0.0417(8) Uani 1 1 d . . . H5A H 0.3393 0.4315 0.5092 0.050 Uiso 1 1 calc R . . C6 C 0.3811(2) 0.36320(15) 0.59845(17) 0.0289(6) Uani 1 1 d . . . C7 C 0.2898(2) 0.18909(14) 0.61861(17) 0.0280(6) Uani 1 1 d . . . N7 N 0.36472(19) 0.17588(12) 0.67616(14) 0.0261(5) Uani 1 1 d . . . S8 S 0.19598(7) 0.12768(4) 0.57732(5) 0.03889(19) Uani 1 1 d . . . C9 C 0.4603(2) 0.40136(14) 0.65507(17) 0.0279(6) Uani 1 1 d . . . N9 N 0.49891(17) 0.36978(12) 0.71961(14) 0.0252(5) Uani 1 1 d . . . S10 S 0.47772(7) 0.48608(4) 0.62372(5) 0.0427(2) Uani 1 1 d . . . C11 C 0.3833(2) 0.10489(15) 0.69872(19) 0.0320(6) Uani 1 1 d . . . C12 C 0.3526(3) 0.08099(16) 0.7716(2) 0.0390(7) Uani 1 1 d . . . C13 C 0.3741(3) 0.01246(18) 0.7907(2) 0.0503(9) Uani 1 1 d . . . H13A H 0.3538 -0.0047 0.8394 0.060 Uiso 1 1 calc R . . C14 C 0.4239(3) -0.03088(17) 0.7406(3) 0.0549(11) Uani 1 1 d . . . C15 C 0.4513(3) -0.00551(18) 0.6686(3) 0.0533(10) Uani 1 1 d . . . H15A H 0.4839 -0.0349 0.6337 0.064 Uiso 1 1 calc R . . C16 C 0.4324(3) 0.06240(17) 0.6454(2) 0.0417(8) Uani 1 1 d . . . C17 C 0.2929(4) 0.1243(2) 0.8257(2) 0.0548(10) Uani 1 1 d . . . H17A H 0.3415 0.1588 0.8503 0.082 Uiso 1 1 calc R . . H17B H 0.2665 0.0961 0.8672 0.082 Uiso 1 1 calc R . . H17C H 0.2318 0.1461 0.7949 0.082 Uiso 1 1 calc R . . C18 C 0.4457(4) -0.1046(2) 0.7655(4) 0.0847(18) Uani 1 1 d . . . H18A H 0.5103 -0.1068 0.8034 0.127 Uiso 1 1 calc R . . H18B H 0.4568 -0.1316 0.7185 0.127 Uiso 1 1 calc R . . H18C H 0.3840 -0.1223 0.7904 0.127 Uiso 1 1 calc R . . C19 C 0.4649(3) 0.0860(2) 0.5657(2) 0.0533(9) Uani 1 1 d . . . H19A H 0.5120 0.0522 0.5448 0.080 Uiso 1 1 calc R . . H19B H 0.5033 0.1290 0.5726 0.080 Uiso 1 1 calc R . . H19C H 0.4003 0.0919 0.5284 0.080 Uiso 1 1 calc R . . C20 C 0.5544(2) 0.40813(14) 0.78600(17) 0.0282(6) Uani 1 1 d . . . C21 C 0.6663(2) 0.39856(15) 0.80751(17) 0.0293(6) Uani 1 1 d . . . C22 C 0.7166(3) 0.43945(16) 0.86807(19) 0.0352(7) Uani 1 1 d . . . H22A H 0.7918 0.4343 0.8822 0.042 Uiso 1 1 calc R . . C23 C 0.6600(3) 0.48767(16) 0.90855(19) 0.0376(7) Uani 1 1 d . . . C24 C 0.5492(3) 0.49281(16) 0.8888(2) 0.0392(7) Uani 1 1 d . . . H24A H 0.5094 0.5233 0.9178 0.047 Uiso 1 1 calc R . . C25 C 0.4937(2) 0.45429(15) 0.82731(19) 0.0326(6) Uani 1 1 d . . . C26 C 0.7320(2) 0.34815(18) 0.7649(2) 0.0396(7) Uani 1 1 d . . . H26A H 0.8088 0.3581 0.7768 0.059 Uiso 1 1 calc R . . H26B H 0.7124 0.3514 0.7075 0.059 Uiso 1 1 calc R . . H26C H 0.7172 0.3024 0.7829 0.059 Uiso 1 1 calc R . . C27 C 0.7193(3) 0.53454(19) 0.9698(2) 0.0528(9) Uani 1 1 d . . . H27A H 0.6671 0.5570 1.0004 0.079 Uiso 1 1 calc R . . H27B H 0.7593 0.5685 0.9425 0.079 Uiso 1 1 calc R . . H27C H 0.7697 0.5082 1.0057 0.079 Uiso 1 1 calc R . . C28 C 0.3732(3) 0.46686(18) 0.8063(2) 0.0441(8) Uani 1 1 d . . . H28A H 0.3631 0.5080 0.7742 0.066 Uiso 1 1 calc R . . H28B H 0.3381 0.4722 0.8551 0.066 Uiso 1 1 calc R . . H28C H 0.3413 0.4285 0.7759 0.066 Uiso 1 1 calc R . . C29 C 0.0437(3) 0.20425(19) 0.6479(2) 0.0445(8) Uani 1 1 d . . . H29A H 0.0919 0.2022 0.6950 0.053 Uiso 1 1 calc R . . C30 C -0.0553(3) 0.2365(2) 0.6484(3) 0.0584(10) Uani 1 1 d . . . H30A H -0.0746 0.2568 0.6958 0.070 Uiso 1 1 calc R . . C31 C -0.1268(3) 0.2392(2) 0.5786(3) 0.0593(10) Uani 1 1 d . . . H31A H -0.1946 0.2609 0.5790 0.071 Uiso 1 1 calc R . . C32 C -0.0978(3) 0.2100(2) 0.5091(2) 0.0537(9) Uani 1 1 d . . . H32A H -0.1458 0.2123 0.4619 0.064 Uiso 1 1 calc R . . C33 C 0.0015(3) 0.17709(18) 0.5078(2) 0.0399(7) Uani 1 1 d . . . H33A H 0.0206 0.1568 0.4603 0.048 Uiso 1 1 calc R . . C34 C 0.0721(2) 0.17467(15) 0.57748(19) 0.0341(6) Uani 1 1 d . . . C35 C 0.6102(4) 0.57142(18) 0.7177(2) 0.0526(9) Uani 1 1 d . . . H35A H 0.5454 0.5900 0.7333 0.063 Uiso 1 1 calc R . . C36 C 0.7099(4) 0.6000(2) 0.7449(3) 0.0689(14) Uani 1 1 d . . . H36A H 0.7128 0.6385 0.7785 0.083 Uiso 1 1 calc R . . C37 C 0.8049(4) 0.5719(3) 0.7225(3) 0.0744(16) Uani 1 1 d . . . H37A H 0.8725 0.5908 0.7413 0.089 Uiso 1 1 calc R . . C38 C 0.8002(3) 0.5164(3) 0.6728(3) 0.0710(14) Uani 1 1 d . . . H38A H 0.8651 0.4972 0.6584 0.085 Uiso 1 1 calc R . . C39 C 0.7009(3) 0.4877(2) 0.6431(2) 0.0507(9) Uani 1 1 d . . . H39A H 0.6980 0.4506 0.6074 0.061 Uiso 1 1 calc R . . C40 C 0.6071(3) 0.51533(16) 0.6675(2) 0.0403(8) Uani 1 1 d . . . C50 C 0.4075(5) 0.7326(4) 0.5651(4) 0.0610(15) Uani 0.822(12) 1 d PDU A 1 H50A H 0.3545 0.7387 0.6043 0.073 Uiso 0.822(12) 1 calc PR A 1 H50B H 0.3853 0.7616 0.5187 0.073 Uiso 0.822(12) 1 calc PR A 1 Cl4 Cl 0.5369(2) 0.7580(3) 0.6082(2) 0.1165(13) Uani 0.822(12) 1 d PDU A 1 Cl5 Cl 0.4078(2) 0.64693(15) 0.5347(2) 0.0828(9) Uani 0.822(12) 1 d PDU A 1 C50' C 0.4034(18) 0.7571(13) 0.566(2) 0.053(7) Uiso 0.178(12) 1 d PDU A 2 H50C H 0.3792 0.7757 0.5134 0.063 Uiso 0.178(12) 1 calc PR A 2 H50D H 0.3488 0.7686 0.6029 0.063 Uiso 0.178(12) 1 calc PR A 2 Cl4' Cl 0.5292(10) 0.7924(9) 0.6020(8) 0.091(4) Uiso 0.178(12) 1 d PDU A 2 Cl5' Cl 0.4174(14) 0.6682(11) 0.5606(13) 0.123(5) Uiso 0.178(12) 1 d PDU A 2 C60 C 0.5003(13) -0.0748(9) 1.0194(12) 0.072(5) Uiso 0.276(5) 1 d PDU B -1 H60A H 0.4461 -0.1078 0.9970 0.087 Uiso 0.276(5) 1 calc PR B -1 H60B H 0.5130 -0.0835 1.0772 0.087 Uiso 0.276(5) 1 calc PR B -1 Cl6 Cl 0.6251(6) -0.0904(4) 0.9758(4) 0.108(3) Uiso 0.276(5) 1 d PD B -1 Cl7 Cl 0.4464(12) 0.0050(8) 1.0059(9) 0.181(5) Uiso 0.276(5) 1 d PD B -1 C60' C 0.5544(16) 0.0439(8) 0.9937(12) 0.053(5) Uiso 0.224(5) 1 d PD B -2 H60C H 0.5669 0.0544 0.9382 0.064 Uiso 0.224(5) 1 calc PR B -2 H60D H 0.6252 0.0431 1.0258 0.064 Uiso 0.224(5) 1 calc PR B -2 Cl6' Cl 0.4955(7) -0.0357(4) 0.9967(4) 0.083(2) Uiso 0.224(5) 1 d PDU B -2 Cl7' Cl 0.4717(12) 0.1101(7) 1.0311(8) 0.158(5) Uiso 0.224(5) 1 d PD 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 Cr 0.0229(2) 0.0222(2) 0.0206(2) 0.00040(16) 0.00040(15) 0.00346(16) Cl1 0.0341(4) 0.0348(4) 0.0372(4) 0.0001(3) 0.0119(3) 0.0077(3) Cl2 0.0396(4) 0.0386(4) 0.0269(3) 0.0033(3) -0.0053(3) 0.0096(3) Cl3 0.0298(3) 0.0430(4) 0.0326(3) -0.0066(3) 0.0080(3) 0.0026(3) N1 0.0241(11) 0.0274(12) 0.0246(11) 0.0027(9) 0.0004(9) 0.0000(9) C2 0.0259(13) 0.0325(14) 0.0249(13) 0.0026(11) 0.0004(10) -0.0033(11) C3 0.0369(16) 0.0462(18) 0.0283(15) 0.0071(13) -0.0070(12) -0.0101(13) C4 0.0500(19) 0.052(2) 0.0380(18) 0.0190(15) -0.0174(15) -0.0126(16) C5 0.0434(18) 0.0398(17) 0.0393(17) 0.0166(14) -0.0086(14) -0.0094(14) C6 0.0254(13) 0.0315(15) 0.0292(14) 0.0062(11) -0.0004(11) -0.0021(11) C7 0.0290(14) 0.0275(14) 0.0274(14) -0.0021(11) 0.0028(11) -0.0015(11) N7 0.0279(12) 0.0251(11) 0.0258(11) -0.0012(9) 0.0047(9) 0.0021(9) S8 0.0360(4) 0.0279(4) 0.0503(5) -0.0040(3) -0.0079(3) -0.0039(3) C9 0.0260(13) 0.0259(13) 0.0313(14) 0.0050(11) 0.0006(11) -0.0008(11) N9 0.0221(11) 0.0254(11) 0.0275(11) 0.0012(9) 0.0001(9) 0.0015(9) S10 0.0417(4) 0.0307(4) 0.0518(5) 0.0157(3) -0.0151(4) -0.0097(3) C11 0.0304(14) 0.0246(14) 0.0390(16) -0.0005(12) -0.0057(12) 0.0032(11) C12 0.0427(17) 0.0298(16) 0.0426(17) 0.0064(13) -0.0053(14) -0.0010(13) C13 0.050(2) 0.0359(18) 0.061(2) 0.0155(16) -0.0178(17) -0.0072(15) C14 0.0369(18) 0.0244(16) 0.098(3) -0.0005(18) -0.0226(19) 0.0031(13) C15 0.0356(17) 0.0304(17) 0.091(3) -0.0185(19) -0.0096(18) 0.0056(14) C16 0.0310(16) 0.0343(16) 0.058(2) -0.0136(15) -0.0034(14) 0.0022(13) C17 0.080(3) 0.0428(19) 0.044(2) 0.0088(16) 0.0213(19) -0.0062(19) C18 0.057(3) 0.0289(19) 0.161(5) 0.013(3) -0.028(3) 0.0033(18) C19 0.049(2) 0.054(2) 0.059(2) -0.0260(18) 0.0159(17) -0.0010(17) C20 0.0298(14) 0.0251(13) 0.0291(14) 0.0015(11) -0.0006(11) -0.0020(11) C21 0.0297(14) 0.0291(14) 0.0282(14) 0.0030(11) -0.0017(11) -0.0008(11) C22 0.0338(15) 0.0339(15) 0.0361(16) 0.0061(12) -0.0056(12) -0.0032(12) C23 0.0482(18) 0.0276(15) 0.0355(16) 0.0000(12) -0.0035(14) -0.0079(13) C24 0.0490(18) 0.0281(15) 0.0409(17) -0.0067(13) 0.0070(14) 0.0018(13) C25 0.0332(15) 0.0265(14) 0.0376(16) -0.0035(12) 0.0010(12) 0.0017(12) C26 0.0260(15) 0.0446(18) 0.0471(18) -0.0039(14) -0.0015(13) 0.0030(13) C27 0.063(2) 0.0405(19) 0.051(2) -0.0095(16) -0.0115(18) -0.0078(17) C28 0.0350(17) 0.0381(17) 0.059(2) -0.0151(15) 0.0031(15) 0.0093(14) C29 0.0435(18) 0.051(2) 0.0386(17) -0.0048(14) 0.0007(14) -0.0097(15) C30 0.050(2) 0.069(3) 0.058(2) -0.019(2) 0.0161(18) -0.0046(19) C31 0.0344(18) 0.069(3) 0.075(3) 0.002(2) 0.0106(18) 0.0022(18) C32 0.0371(18) 0.074(3) 0.048(2) 0.0088(18) -0.0053(15) -0.0032(17) C33 0.0354(16) 0.0506(19) 0.0324(16) 0.0016(13) -0.0029(12) -0.0066(14) C34 0.0323(15) 0.0294(15) 0.0396(16) 0.0041(12) -0.0010(12) -0.0083(12) C35 0.061(2) 0.0345(18) 0.059(2) 0.0092(16) -0.0101(18) -0.0133(16) C36 0.081(3) 0.047(2) 0.072(3) 0.018(2) -0.030(2) -0.032(2) C37 0.067(3) 0.071(3) 0.077(3) 0.039(3) -0.032(2) -0.042(3) C38 0.040(2) 0.092(4) 0.080(3) 0.046(3) 0.000(2) -0.009(2) C39 0.049(2) 0.052(2) 0.051(2) 0.0199(17) 0.0022(16) -0.0077(17) C40 0.0382(17) 0.0337(16) 0.0461(18) 0.0136(14) -0.0098(14) -0.0115(13) C50 0.074(4) 0.062(4) 0.049(3) 0.006(3) 0.019(2) 0.014(3) Cl4 0.0955(15) 0.140(4) 0.1091(17) -0.0489(19) -0.0127(12) 0.0099(16) Cl5 0.1009(14) 0.0673(13) 0.0860(16) 0.0140(10) 0.0387(11) -0.0034(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr N1 2.009(2) . ? Cr N7 2.141(2) . ? Cr N9 2.153(2) . ? Cr Cl2 2.2880(8) . ? Cr Cl3 2.3133(8) . ? Cr Cl1 2.3226(9) . ? N1 C2 1.334(4) . ? N1 C6 1.341(4) . ? C2 C3 1.395(4) . ? C2 C7 1.488(4) . ? C3 C4 1.384(5) . ? C4 C5 1.385(5) . ? C5 C6 1.389(4) . ? C6 C9 1.494(4) . ? C7 N7 1.294(4) . ? C7 S8 1.764(3) . ? N7 C11 1.455(4) . ? S8 C34 1.787(3) . ? C9 N9 1.295(4) . ? C9 S10 1.763(3) . ? N9 C20 1.456(4) . ? S10 C40 1.785(3) . ? C11 C12 1.395(5) . ? C11 C16 1.404(5) . ? C12 C13 1.402(5) . ? C12 C17 1.491(5) . ? C13 C14 1.382(6) . ? C14 C15 1.379(7) . ? C14 C18 1.521(5) . ? C15 C16 1.401(5) . ? C16 C19 1.504(6) . ? C20 C25 1.402(4) . ? C20 C21 1.406(4) . ? C21 C22 1.390(4) . ? C21 C26 1.505(4) . ? C22 C23 1.393(5) . ? C23 C24 1.380(5) . ? C23 C27 1.511(4) . ? C24 C25 1.401(4) . ? C25 C28 1.515(4) . ? C29 C30 1.379(6) . ? C29 C34 1.391(5) . ? C30 C31 1.393(6) . ? C31 C32 1.379(6) . ? C32 C33 1.388(5) . ? C33 C34 1.386(4) . ? C35 C40 1.384(5) . ? C35 C36 1.388(6) . ? C36 C37 1.383(8) . ? C37 C38 1.368(8) . ? C38 C39 1.395(6) . ? C39 C40 1.378(6) . ? C50 Cl5 1.758(7) . ? C50 Cl4 1.759(6) . ? C50' Cl4' 1.751(15) . ? C50' Cl5' 1.758(15) . ? C60 Cl7 1.707(16) . ? C60 Cl6 1.798(15) . ? C60' Cl6' 1.727(16) . ? C60' Cl7' 1.804(16) . ? 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 N1 Cr N7 76.99(9) . . ? N1 Cr N9 77.20(9) . . ? N7 Cr N9 154.17(9) . . ? N1 Cr Cl2 178.06(7) . . ? N7 Cr Cl2 101.78(7) . . ? N9 Cr Cl2 104.05(6) . . ? N1 Cr Cl3 88.48(7) . . ? N7 Cr Cl3 87.60(6) . . ? N9 Cr Cl3 90.68(6) . . ? Cl2 Cr Cl3 92.97(3) . . ? N1 Cr Cl1 85.28(7) . . ? N7 Cr Cl1 89.92(7) . . ? N9 Cr Cl1 89.00(6) . . ? Cl2 Cr Cl1 93.24(3) . . ? Cl3 Cr Cl1 173.67(3) . . ? C2 N1 C6 121.8(2) . . ? C2 N1 Cr 119.13(19) . . ? C6 N1 Cr 118.98(18) . . ? N1 C2 C3 120.8(3) . . ? N1 C2 C7 112.7(2) . . ? C3 C2 C7 126.2(3) . . ? C4 C3 C2 118.0(3) . . ? C3 C4 C5 120.5(3) . . ? C4 C5 C6 118.7(3) . . ? N1 C6 C5 120.2(3) . . ? N1 C6 C9 112.7(2) . . ? C5 C6 C9 127.2(3) . . ? N7 C7 C2 116.4(2) . . ? N7 C7 S8 123.2(2) . . ? C2 C7 S8 120.2(2) . . ? C7 N7 C11 117.9(2) . . ? C7 N7 Cr 113.59(19) . . ? C11 N7 Cr 128.47(18) . . ? C7 S8 C34 100.13(14) . . ? N9 C9 C6 116.9(2) . . ? N9 C9 S10 130.9(2) . . ? C6 C9 S10 112.0(2) . . ? C9 N9 C20 119.7(2) . . ? C9 N9 Cr 113.41(18) . . ? C20 N9 Cr 126.26(17) . . ? C9 S10 C40 108.17(14) . . ? C12 C11 C16 122.0(3) . . ? C12 C11 N7 120.0(3) . . ? C16 C11 N7 118.0(3) . . ? C11 C12 C13 117.4(3) . . ? C11 C12 C17 122.3(3) . . ? C13 C12 C17 120.1(3) . . ? C14 C13 C12 122.5(4) . . ? C15 C14 C13 118.2(3) . . ? C15 C14 C18 122.0(4) . . ? C13 C14 C18 119.8(5) . . ? C14 C15 C16 122.5(4) . . ? C15 C16 C11 117.3(4) . . ? C15 C16 C19 119.2(3) . . ? C11 C16 C19 123.6(3) . . ? C25 C20 C21 121.4(3) . . ? C25 C20 N9 118.5(2) . . ? C21 C20 N9 120.2(3) . . ? C22 C21 C20 117.8(3) . . ? C22 C21 C26 120.2(3) . . ? C20 C21 C26 122.0(3) . . ? C21 C22 C23 122.5(3) . . ? C24 C23 C22 117.9(3) . . ? C24 C23 C27 121.3(3) . . ? C22 C23 C27 120.7(3) . . ? C23 C24 C25 122.5(3) . . ? C24 C25 C20 117.7(3) . . ? C24 C25 C28 118.7(3) . . ? C20 C25 C28 123.5(3) . . ? C30 C29 C34 119.8(3) . . ? C29 C30 C31 120.1(4) . . ? C32 C31 C30 119.7(4) . . ? C31 C32 C33 120.8(3) . . ? C34 C33 C32 119.0(3) . . ? C33 C34 C29 120.6(3) . . ? C33 C34 S8 118.9(3) . . ? C29 C34 S8 120.4(3) . . ? C40 C35 C36 119.4(5) . . ? C37 C36 C35 119.9(5) . . ? C38 C37 C36 119.9(4) . . ? C37 C38 C39 121.3(5) . . ? C40 C39 C38 118.2(4) . . ? C39 C40 C35 121.3(3) . . ? C39 C40 S10 119.8(3) . . ? C35 C40 S10 118.3(3) . . ? Cl5 C50 Cl4 111.2(4) . . ? Cl4' C50' Cl5' 108.8(13) . . ? Cl7 C60 Cl6 116.2(12) . . ? Cl6' C60' Cl7' 112.8(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.693 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.063 #===END data_[Mn(4)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253603' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Cl2 Mn N3 S2, C H2 Cl2' _chemical_formula_sum 'C38 H37 Cl4 Mn N3 S2' _chemical_formula_weight 796.57 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' S S 0.1246 0.1234 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.056(3) _cell_length_b 20.693(7) _cell_length_c 22.231(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7846(3) _cell_formula_units_Z 8 _cell_measurement_temperature 203 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 4.87 _cell_measurement_theta_max 12.01 _exptl_crystal_description tablets _exptl_crystal_colour Orange _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6537 _exptl_absorpt_correction_T_max 0.8992 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203 _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 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.33 _diffrn_reflns_number 6908 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1495 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6908 _reflns_number_gt 3264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6908 _refine_ls_number_parameters 439 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.25836(5) 0.66558(5) 0.45018(4) 0.0393(2) Uani 1 1 d . . . Cl1 Cl 0.35991(13) 0.59123(11) 0.43570(9) 0.0700(6) Uani 1 1 d . . . Cl2 Cl 0.12907(10) 0.63414(10) 0.46216(8) 0.0559(4) Uani 1 1 d . . . N1 N 0.3239(3) 0.7578(2) 0.4486(2) 0.0377(11) Uani 1 1 d . . . C2 C 0.3670(4) 0.7691(3) 0.4982(3) 0.0402(14) Uani 1 1 d . . . C3 C 0.4409(4) 0.7996(3) 0.4934(3) 0.0428(15) Uani 1 1 d . . . H3A H 0.4715 0.8066 0.5280 0.051 Uiso 1 1 calc R . . C4 C 0.4678(4) 0.8188(3) 0.4385(3) 0.0440(15) Uani 1 1 d . . . H4A H 0.5165 0.8397 0.4350 0.053 Uiso 1 1 calc R . . C5 C 0.4225(4) 0.8072(3) 0.3876(3) 0.0432(15) Uani 1 1 d . . . H5A H 0.4404 0.8197 0.3494 0.052 Uiso 1 1 calc R . . C6 C 0.3501(4) 0.7767(3) 0.3942(3) 0.0384(14) Uani 1 1 d . . . C7 C 0.3302(3) 0.7464(3) 0.5544(3) 0.0422(14) Uani 1 1 d . . . N7 N 0.2852(3) 0.6973(3) 0.5493(2) 0.0421(12) Uani 1 1 d . . . S8 S 0.35127(11) 0.78417(9) 0.62394(7) 0.0498(4) Uani 1 1 d . . . C9 C 0.2972(4) 0.7574(3) 0.3436(3) 0.0413(15) Uani 1 1 d . . . N9 N 0.2538(3) 0.7079(2) 0.3525(2) 0.0420(12) Uani 1 1 d . . . S10 S 0.29650(12) 0.80078(9) 0.27533(7) 0.0509(4) Uani 1 1 d . . . C11 C 0.2432(4) 0.6703(3) 0.5999(2) 0.0434(14) Uani 1 1 d . . . C12 C 0.2691(4) 0.6124(4) 0.6250(3) 0.0502(17) Uani 1 1 d . . . C13 C 0.2237(4) 0.5835(4) 0.6692(3) 0.0536(18) Uani 1 1 d . . . H13A H 0.2400 0.5440 0.6859 0.064 Uiso 1 1 calc R . . C14 C 0.1552(5) 0.6116(4) 0.6892(3) 0.0578(19) Uani 1 1 d . . . C15 C 0.1310(4) 0.6694(4) 0.6649(3) 0.0549(17) Uani 1 1 d . . . H15A H 0.0851 0.6893 0.6793 0.066 Uiso 1 1 calc R . . C16 C 0.1741(4) 0.6989(3) 0.6190(3) 0.0432(15) Uani 1 1 d . . . C17 C 0.3439(5) 0.5817(5) 0.6043(3) 0.069(2) Uani 1 1 d . . . H17A H 0.3567 0.5457 0.6305 0.103 Uiso 1 1 calc R . . H17B H 0.3858 0.6133 0.6056 0.103 Uiso 1 1 calc R . . H17C H 0.3375 0.5662 0.5634 0.103 Uiso 1 1 calc R . . C18 C 0.1058(5) 0.5786(5) 0.7379(3) 0.078(3) Uani 1 1 d . . . H18A H 0.0848 0.5384 0.7223 0.116 Uiso 1 1 calc R . . H18B H 0.0630 0.6068 0.7494 0.116 Uiso 1 1 calc R . . H18C H 0.1383 0.5697 0.7727 0.116 Uiso 1 1 calc R . . C19 C 0.1455(4) 0.7617(4) 0.5921(3) 0.0577(19) Uani 1 1 d . . . H19A H 0.1809 0.7964 0.6032 0.086 Uiso 1 1 calc R . . H19B H 0.0933 0.7712 0.6071 0.086 Uiso 1 1 calc R . . H19C H 0.1438 0.7578 0.5486 0.086 Uiso 1 1 calc R . . C20 C 0.2024(4) 0.6852(3) 0.3047(3) 0.0472(17) Uani 1 1 d . . . C21 C 0.1247(5) 0.7071(4) 0.3026(3) 0.0583(19) Uani 1 1 d . . . C22 C 0.0757(6) 0.6818(5) 0.2593(4) 0.084(3) Uani 1 1 d . . . H22A H 0.0235 0.6962 0.2582 0.101 Uiso 1 1 calc R . . C23 C 0.0987(7) 0.6372(5) 0.2182(4) 0.089(4) Uani 1 1 d . . . C24 C 0.1774(6) 0.6164(4) 0.2205(3) 0.076(3) Uani 1 1 d . . . H24A H 0.1950 0.5852 0.1929 0.091 Uiso 1 1 calc R . . C25 C 0.2303(5) 0.6412(4) 0.2631(3) 0.065(2) Uani 1 1 d . . . C26 C 0.0961(5) 0.7572(5) 0.3467(4) 0.077(3) Uani 1 1 d . . . H26A H 0.1182 0.7989 0.3363 0.115 Uiso 1 1 calc R . . H26B H 0.1124 0.7453 0.3870 0.115 Uiso 1 1 calc R . . H26C H 0.0394 0.7595 0.3450 0.115 Uiso 1 1 calc R . . C27 C 0.0432(8) 0.6073(6) 0.1721(5) 0.135(6) Uani 1 1 d . . . H27A H 0.0064 0.5790 0.1924 0.202 Uiso 1 1 calc R . . H27B H 0.0732 0.5826 0.1430 0.202 Uiso 1 1 calc R . . H27C H 0.0147 0.6414 0.1515 0.202 Uiso 1 1 calc R . . C28 C 0.3135(6) 0.6170(4) 0.2663(4) 0.077(3) Uani 1 1 d . . . H28A H 0.3494 0.6527 0.2595 0.116 Uiso 1 1 calc R . . H28B H 0.3216 0.5842 0.2358 0.116 Uiso 1 1 calc R . . H28C H 0.3232 0.5986 0.3057 0.116 Uiso 1 1 calc R . . C29 C 0.4363(2) 0.8969(2) 0.6165(2) 0.0558(18) Uani 1 1 d G . . H29A H 0.4746 0.8749 0.6390 0.067 Uiso 1 1 calc R . . C30 C 0.4495(3) 0.9602(2) 0.5983(2) 0.073(2) Uani 1 1 d G . . H30A H 0.4966 0.9811 0.6085 0.088 Uiso 1 1 calc R . . C31 C 0.3929(3) 0.99278(17) 0.5650(3) 0.072(2) Uani 1 1 d G . . H31A H 0.4018 1.0356 0.5527 0.087 Uiso 1 1 calc R . . C32 C 0.3232(3) 0.9620(2) 0.5500(2) 0.074(2) Uani 1 1 d G . . H32A H 0.2849 0.9840 0.5275 0.089 Uiso 1 1 calc R . . C33 C 0.3100(2) 0.8986(2) 0.5682(2) 0.0562(18) Uani 1 1 d G . . H33A H 0.2629 0.8778 0.5580 0.067 Uiso 1 1 calc R . . C34 C 0.3666(3) 0.86610(17) 0.6014(2) 0.0473(16) Uani 1 1 d G . . C35 C 0.3764(2) 0.9151(2) 0.27264(18) 0.0528(16) Uani 1 1 d G . . H35A H 0.4061 0.8960 0.2418 0.063 Uiso 1 1 calc R . . C36 C 0.3922(3) 0.9782(2) 0.2904(2) 0.073(3) Uani 1 1 d G . . H36A H 0.4325 1.0017 0.2716 0.088 Uiso 1 1 calc R . . C37 C 0.3484(3) 1.00655(17) 0.3361(3) 0.073(3) Uani 1 1 d G . . H37A H 0.3591 1.0492 0.3481 0.088 Uiso 1 1 calc R . . C38 C 0.2888(3) 0.9718(2) 0.3640(2) 0.077(3) Uani 1 1 d G . . H38A H 0.2592 0.9910 0.3948 0.092 Uiso 1 1 calc R . . C39 C 0.2731(2) 0.9088(2) 0.3462(2) 0.060(2) Uani 1 1 d G . . H39A H 0.2328 0.8853 0.3650 0.072 Uiso 1 1 calc R . . C40 C 0.3169(3) 0.88041(17) 0.30050(19) 0.0471(16) Uani 1 1 d G . . C50 C 0.0490(12) 0.5627(9) 0.9622(6) 0.089(9) Uani 0.60 1 d PD A 1 H50A H -0.0030 0.5751 0.9769 0.107 Uiso 0.60 1 calc PR A 1 H50B H 0.0614 0.5194 0.9773 0.107 Uiso 0.60 1 calc PR A 1 Cl3 Cl 0.0512(3) 0.5637(3) 0.8822(2) 0.0839(16) Uani 0.60 1 d PD A 1 Cl4 Cl 0.1203(6) 0.6188(4) 0.9863(3) 0.169(3) Uani 0.60 1 d PD A 1 C50' C 0.036(4) 0.566(2) 0.967(3) 0.17(4) Uiso 0.30 1 d PD B 2 H50C H -0.0159 0.5610 0.9845 0.204 Uiso 0.30 1 calc PR B 2 H50D H 0.0472 0.5283 0.9413 0.204 Uiso 0.30 1 calc PR B 2 Cl3' Cl 0.0432(14) 0.6385(12) 0.9251(9) 0.241(10) Uiso 0.30 1 d PD B 2 Cl4' Cl 0.1082(7) 0.5735(6) 1.0235(5) 0.119(3) Uiso 0.30 1 d PD B 2 C50" C 0.085(3) 0.5625(18) 0.9662(15) 0.012(10) Uiso 0.10 1 d PD C 3 H50E H 0.0694 0.5301 0.9960 0.015 Uiso 0.10 1 calc PR C 3 H50F H 0.1421 0.5602 0.9608 0.015 Uiso 0.10 1 calc PR C 3 Cl3" Cl 0.0363(15) 0.5495(11) 0.8972(10) 0.047(6) Uiso 0.10 1 d PD C 3 Cl4" Cl 0.057(3) 0.641(2) 0.990(2) 0.163(19) Uiso 0.10 1 d PD C 3 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 Mn 0.0403(5) 0.0399(4) 0.0379(4) -0.0010(4) -0.0009(4) -0.0038(4) Cl1 0.0697(13) 0.0730(13) 0.0673(11) -0.0052(11) 0.0022(10) 0.0270(11) Cl2 0.0432(9) 0.0672(10) 0.0574(10) -0.0039(9) 0.0051(8) -0.0095(8) N1 0.033(2) 0.045(3) 0.035(2) 0.001(2) 0.000(2) -0.004(2) C2 0.040(3) 0.042(4) 0.038(3) -0.003(3) -0.011(3) 0.003(3) C3 0.042(3) 0.046(4) 0.040(3) -0.008(3) -0.002(3) 0.001(3) C4 0.036(3) 0.046(4) 0.050(4) 0.003(3) 0.002(3) -0.005(3) C5 0.038(3) 0.052(4) 0.040(3) 0.004(3) 0.004(3) -0.002(3) C6 0.037(3) 0.037(3) 0.041(3) -0.004(3) -0.005(3) -0.008(3) C7 0.035(3) 0.047(4) 0.045(3) -0.005(3) -0.007(3) 0.000(3) N7 0.039(3) 0.051(3) 0.036(2) -0.002(3) -0.004(2) 0.003(2) S8 0.0577(10) 0.0580(10) 0.0336(7) -0.0024(8) -0.0053(8) -0.0108(9) C9 0.039(3) 0.047(4) 0.038(3) 0.007(3) -0.001(3) 0.000(3) N9 0.047(3) 0.041(3) 0.038(2) 0.003(2) -0.008(2) -0.007(3) S10 0.0677(11) 0.0490(10) 0.0359(7) 0.0035(8) -0.0095(8) -0.0153(9) C11 0.040(3) 0.059(4) 0.032(3) -0.007(3) -0.003(3) -0.009(3) C12 0.050(4) 0.059(4) 0.041(3) 0.003(3) -0.005(3) -0.002(3) C13 0.058(5) 0.061(4) 0.043(3) 0.013(3) -0.009(3) -0.015(4) C14 0.055(4) 0.078(5) 0.040(3) 0.001(4) -0.006(3) -0.017(4) C15 0.047(4) 0.069(5) 0.049(4) -0.005(4) 0.001(3) -0.008(4) C16 0.046(4) 0.044(4) 0.040(3) -0.008(3) -0.012(3) -0.005(3) C17 0.062(5) 0.084(6) 0.060(4) 0.012(5) 0.002(4) 0.017(5) C18 0.066(5) 0.108(7) 0.058(5) 0.003(5) 0.001(4) -0.028(5) C19 0.051(4) 0.067(5) 0.055(4) -0.019(4) -0.003(4) 0.002(4) C20 0.064(4) 0.044(4) 0.033(3) 0.005(3) -0.008(3) -0.024(3) C21 0.059(5) 0.061(5) 0.055(4) 0.016(4) -0.021(4) -0.018(4) C22 0.079(6) 0.093(7) 0.081(6) 0.044(6) -0.045(5) -0.043(5) C23 0.119(9) 0.088(7) 0.059(5) 0.033(5) -0.048(6) -0.068(7) C24 0.127(9) 0.065(5) 0.035(4) 0.006(4) -0.006(5) -0.045(6) C25 0.094(6) 0.058(4) 0.043(4) 0.001(3) -0.005(4) -0.040(4) C26 0.056(5) 0.084(6) 0.092(6) 0.012(5) -0.011(5) -0.009(5) C27 0.164(12) 0.156(12) 0.084(7) 0.016(8) -0.056(8) -0.090(10) C28 0.105(7) 0.070(6) 0.058(5) -0.014(4) 0.021(5) -0.009(5) C29 0.049(4) 0.064(5) 0.054(4) -0.007(4) -0.004(3) -0.011(3) C30 0.084(6) 0.059(5) 0.078(6) -0.004(4) -0.009(5) -0.024(5) C31 0.082(6) 0.048(4) 0.086(6) -0.007(4) -0.013(5) -0.004(4) C32 0.085(6) 0.075(6) 0.061(5) 0.000(5) -0.006(5) 0.016(5) C33 0.055(4) 0.060(5) 0.054(4) -0.005(3) -0.006(4) -0.005(3) C34 0.053(4) 0.057(4) 0.032(3) -0.011(3) 0.002(3) -0.006(3) C35 0.052(4) 0.049(4) 0.058(4) 0.010(4) -0.012(3) -0.004(3) C36 0.073(6) 0.054(5) 0.093(7) 0.009(5) -0.023(5) -0.011(4) C37 0.083(6) 0.043(4) 0.095(6) -0.001(4) -0.037(5) 0.006(4) C38 0.088(6) 0.053(5) 0.090(6) -0.017(5) -0.019(5) 0.021(5) C39 0.062(5) 0.066(5) 0.051(4) 0.000(4) 0.001(3) 0.008(4) C40 0.049(4) 0.052(4) 0.041(3) 0.005(3) -0.004(3) -0.007(3) C50 0.033(7) 0.093(13) 0.14(2) 0.069(13) 0.000(9) -0.016(7) Cl3 0.067(3) 0.105(4) 0.080(3) 0.011(3) 0.006(2) -0.014(2) Cl4 0.212(9) 0.195(8) 0.099(4) -0.028(5) -0.054(5) -0.065(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 Mn N1 2.213(5) . ? Mn Cl2 2.315(2) . ? Mn Cl1 2.339(2) . ? Mn N9 2.343(5) . ? Mn N7 2.343(5) . ? N1 C2 1.345(8) . ? N1 C6 1.348(8) . ? C2 C3 1.414(9) . ? C2 C7 1.475(9) . ? C3 C4 1.364(9) . ? C4 C5 1.390(9) . ? C5 C6 1.394(9) . ? C6 C9 1.496(9) . ? C7 N7 1.280(8) . ? C7 S8 1.768(7) . ? N7 C11 1.447(8) . ? S8 C34 1.787(4) . ? C9 N9 1.280(8) . ? C9 S10 1.763(6) . ? N9 C20 1.455(8) . ? S10 C40 1.775(4) . ? C11 C16 1.386(9) . ? C11 C12 1.393(10) . ? C12 C13 1.386(9) . ? C12 C17 1.498(10) . ? C13 C14 1.378(11) . ? C14 C15 1.375(11) . ? C14 C18 1.533(10) . ? C15 C16 1.397(9) . ? C16 C19 1.513(10) . ? C20 C25 1.381(11) . ? C20 C21 1.401(11) . ? C21 C22 1.378(11) . ? C21 C26 1.507(12) . ? C22 C23 1.358(15) . ? C23 C24 1.410(15) . ? C23 C27 1.526(12) . ? C24 C25 1.404(11) . ? C25 C28 1.507(13) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C50 Cl4 1.764(11) . ? C50 Cl3 1.779(14) . ? C50' Cl4' 1.763(18) . ? C50' Cl3' 1.771(17) . ? C50" Cl4" 1.765(17) . ? C50" Cl3" 1.767(17) . ? 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 N1 Mn Cl2 136.54(14) . . ? N1 Mn Cl1 101.01(15) . . ? Cl2 Mn Cl1 122.45(9) . . ? N1 Mn N9 71.34(18) . . ? Cl2 Mn N9 100.38(15) . . ? Cl1 Mn N9 98.21(15) . . ? N1 Mn N7 70.99(19) . . ? Cl2 Mn N7 99.02(13) . . ? Cl1 Mn N7 99.71(14) . . ? N9 Mn N7 140.63(18) . . ? C2 N1 C6 120.3(5) . . ? C2 N1 Mn 114.4(4) . . ? C6 N1 Mn 115.5(4) . . ? N1 C2 C3 120.2(6) . . ? N1 C2 C7 114.0(5) . . ? C3 C2 C7 125.8(5) . . ? C4 C3 C2 119.7(6) . . ? C3 C4 C5 119.5(6) . . ? C4 C5 C6 119.0(6) . . ? N1 C6 C5 121.2(5) . . ? N1 C6 C9 113.5(5) . . ? C5 C6 C9 125.2(6) . . ? N7 C7 C2 115.6(6) . . ? N7 C7 S8 123.4(5) . . ? C2 C7 S8 120.9(4) . . ? C7 N7 C11 122.3(6) . . ? C7 N7 Mn 115.1(4) . . ? C11 N7 Mn 121.8(4) . . ? C7 S8 C34 101.8(3) . . ? N9 C9 C6 116.5(5) . . ? N9 C9 S10 122.5(5) . . ? C6 C9 S10 121.0(5) . . ? C9 N9 C20 119.6(5) . . ? C9 N9 Mn 115.0(4) . . ? C20 N9 Mn 125.2(4) . . ? C9 S10 C40 101.5(3) . . ? C16 C11 C12 120.9(6) . . ? C16 C11 N7 119.6(6) . . ? C12 C11 N7 119.2(6) . . ? C13 C12 C11 118.6(7) . . ? C13 C12 C17 120.7(7) . . ? C11 C12 C17 120.7(6) . . ? C14 C13 C12 121.3(7) . . ? C15 C14 C13 119.7(7) . . ? C15 C14 C18 119.9(8) . . ? C13 C14 C18 120.4(8) . . ? C14 C15 C16 120.5(7) . . ? C11 C16 C15 119.0(7) . . ? C11 C16 C19 121.4(6) . . ? C15 C16 C19 119.6(6) . . ? C25 C20 C21 121.1(7) . . ? C25 C20 N9 119.6(7) . . ? C21 C20 N9 119.3(7) . . ? C22 C21 C20 118.3(9) . . ? C22 C21 C26 121.3(8) . . ? C20 C21 C26 120.4(6) . . ? C23 C22 C21 123.6(10) . . ? C22 C23 C24 117.2(8) . . ? C22 C23 C27 123.3(12) . . ? C24 C23 C27 119.5(12) . . ? C25 C24 C23 121.7(9) . . ? C20 C25 C24 118.1(9) . . ? C20 C25 C28 120.8(7) . . ? C24 C25 C28 121.0(8) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 S8 120.5(3) . . ? C29 C34 S8 119.5(3) . . ? C36 C35 C40 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 S10 121.1(3) . . ? C35 C40 S10 118.9(3) . . ? Cl4 C50 Cl3 106.4(7) . . ? Cl4' C50' Cl3' 104.6(14) . . ? Cl4" C50" Cl3" 105.4(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.376 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.073 #===END data_[Ni(4)Br2] _database_code_depnum_ccdc_archive 'CCDC 253604' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Br2 N3 Ni S2, C4 H8 O' _chemical_formula_sum 'C41 H43 Br2 N3 Ni O S2' _chemical_formula_weight 876.43 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.540(3) _cell_length_b 20.405(4) _cell_length_c 22.230(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7956(3) _cell_formula_units_Z 8 _cell_measurement_temperature 203 _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.05 _cell_measurement_theta_max 11.49 _exptl_crystal_description plates _exptl_crystal_colour Orange-red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 2.637 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3565 _exptl_absorpt_correction_T_max 0.7727 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203 _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 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 21.92 _diffrn_reflns_number 5835 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1665 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 23.49 _reflns_number_total 5835 _reflns_number_gt 2824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5835 _refine_ls_number_parameters 457 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1832 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.1878 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _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 Ni Ni 0.25009(10) 0.32012(9) 0.55635(7) 0.0332(4) Uani 1 1 d . . . Br1 Br 0.14861(10) 0.39727(9) 0.57525(7) 0.0542(4) Uani 1 1 d . . . Br2 Br 0.37169(8) 0.36797(8) 0.54352(7) 0.0484(4) Uani 1 1 d . . . N1 N 0.1804(6) 0.2423(5) 0.5582(5) 0.034(2) Uani 1 1 d . . . C2 C 0.1369(7) 0.2310(6) 0.5083(5) 0.030(3) Uani 1 1 d . . . C3 C 0.0654(8) 0.2015(7) 0.5125(6) 0.038(3) Uani 1 1 d . . . H3A H 0.0358 0.1941 0.4779 0.046 Uiso 1 1 calc R . . C4 C 0.0394(7) 0.1834(7) 0.5678(5) 0.038(3) Uani 1 1 d . . . H4A H -0.0092 0.1642 0.5714 0.045 Uiso 1 1 calc R . . C5 C 0.0843(8) 0.1931(6) 0.6201(6) 0.037(3) Uani 1 1 d . . . H5A H 0.0671 0.1796 0.6582 0.044 Uiso 1 1 calc R . . C6 C 0.1544(8) 0.2231(7) 0.6128(5) 0.034(3) Uani 1 1 d . . . C7 C 0.1760(7) 0.2567(7) 0.4521(5) 0.033(3) Uani 1 1 d . . . N7 N 0.2224(6) 0.3027(5) 0.4612(5) 0.033(3) Uani 1 1 d . . . S8 S 0.1524(2) 0.22408(19) 0.38197(14) 0.0434(9) Uani 1 1 d . . . C9 C 0.2085(7) 0.2425(7) 0.6622(5) 0.033(3) Uani 1 1 d . . . N9 N 0.2551(6) 0.2877(5) 0.6502(4) 0.031(2) Uani 1 1 d . . . S10 S 0.2044(2) 0.2033(2) 0.73315(14) 0.0473(10) Uani 1 1 d . . . C11 C 0.2650(8) 0.3315(7) 0.4095(5) 0.039(3) Uani 1 1 d . . . C12 C 0.2370(8) 0.3890(7) 0.3842(6) 0.038(3) Uani 1 1 d . . . C13 C 0.2780(8) 0.4164(8) 0.3383(6) 0.047(4) Uani 1 1 d . . . H13A H 0.2615 0.4563 0.3217 0.056 Uiso 1 1 calc R . . C14 C 0.3434(7) 0.3871(7) 0.3153(6) 0.039(3) Uani 1 1 d . . . C15 C 0.3688(7) 0.3304(8) 0.3410(5) 0.042(3) Uani 1 1 d . . . H15A H 0.4135 0.3106 0.3262 0.050 Uiso 1 1 calc R . . C16 C 0.3295(8) 0.3004(6) 0.3897(5) 0.035(3) Uani 1 1 d . . . C17 C 0.1628(10) 0.4206(9) 0.4065(7) 0.060(5) Uani 1 1 d . . . H17A H 0.1483 0.4558 0.3794 0.090 Uiso 1 1 calc R . . H17B H 0.1706 0.4382 0.4466 0.090 Uiso 1 1 calc R . . H17C H 0.1227 0.3879 0.4075 0.090 Uiso 1 1 calc R . . C18 C 0.3905(10) 0.4219(10) 0.2657(6) 0.065(5) Uani 1 1 d . . . H18A H 0.4179 0.3895 0.2421 0.098 Uiso 1 1 calc R . . H18B H 0.4267 0.4517 0.2842 0.098 Uiso 1 1 calc R . . H18C H 0.3565 0.4464 0.2396 0.098 Uiso 1 1 calc R . . C19 C 0.3577(9) 0.2382(7) 0.4164(7) 0.053(4) Uani 1 1 d . . . H19A H 0.3178 0.2054 0.4145 0.079 Uiso 1 1 calc R . . H19B H 0.3718 0.2457 0.4581 0.079 Uiso 1 1 calc R . . H19C H 0.4019 0.2231 0.3941 0.079 Uiso 1 1 calc R . . C20 C 0.3096(8) 0.3098(8) 0.6964(6) 0.045(4) Uani 1 1 d . . . C21 C 0.3832(8) 0.2866(8) 0.6946(7) 0.048(4) Uani 1 1 d . . . C22 C 0.4343(10) 0.3091(10) 0.7380(8) 0.071(6) Uani 1 1 d . . . H22A H 0.4844 0.2929 0.7379 0.085 Uiso 1 1 calc R . . C23 C 0.4136(11) 0.3544(9) 0.7812(8) 0.062(5) Uani 1 1 d . . . C24 C 0.3369(13) 0.3760(9) 0.7823(7) 0.069(6) Uani 1 1 d . . . H24A H 0.3210 0.4054 0.8123 0.083 Uiso 1 1 calc R . . C25 C 0.2845(9) 0.3542(7) 0.7394(6) 0.047(4) Uani 1 1 d . . . C26 C 0.4081(9) 0.2363(9) 0.6508(9) 0.064(5) Uani 1 1 d . . . H26A H 0.4002 0.2524 0.6102 0.096 Uiso 1 1 calc R . . H26B H 0.3788 0.1965 0.6568 0.096 Uiso 1 1 calc R . . H26C H 0.4618 0.2270 0.6568 0.096 Uiso 1 1 calc R . . C27 C 0.4717(12) 0.3820(11) 0.8246(8) 0.086(7) Uani 1 1 d U . . H27A H 0.5057 0.4115 0.8033 0.129 Uiso 1 1 calc R . . H27B H 0.5010 0.3464 0.8420 0.129 Uiso 1 1 calc R . . H27C H 0.4457 0.4058 0.8563 0.129 Uiso 1 1 calc R . . C28 C 0.2022(9) 0.3801(8) 0.7385(7) 0.052(4) Uani 1 1 d . . . H28A H 0.1670 0.3437 0.7422 0.077 Uiso 1 1 calc R . . H28B H 0.1930 0.4029 0.7009 0.077 Uiso 1 1 calc R . . H28C H 0.1948 0.4102 0.7718 0.077 Uiso 1 1 calc R . . C29 C 0.0638(9) 0.1127(9) 0.3823(7) 0.055(4) Uani 1 1 d . . . H29A H 0.0268 0.1366 0.3609 0.066 Uiso 1 1 calc R . . C30 C 0.0518(9) 0.0468(8) 0.3985(7) 0.053(4) Uani 1 1 d . . . H30A H 0.0061 0.0268 0.3863 0.064 Uiso 1 1 calc R . . C31 C 0.1022(10) 0.0106(9) 0.4306(8) 0.064(5) Uani 1 1 d . . . H31A H 0.0910 -0.0328 0.4418 0.077 Uiso 1 1 calc R . . C32 C 0.1712(11) 0.0398(9) 0.4466(9) 0.076(6) Uani 1 1 d . . . H32A H 0.2077 0.0154 0.4680 0.091 Uiso 1 1 calc R . . C33 C 0.1861(9) 0.1027(8) 0.4317(8) 0.054(4) Uani 1 1 d . . . H33A H 0.2329 0.1213 0.4431 0.065 Uiso 1 1 calc R . . C34 C 0.1332(8) 0.1414(8) 0.3993(6) 0.045(4) Uani 1 1 d . . . C35 C 0.1165(9) 0.0932(8) 0.7428(7) 0.051(4) Uani 1 1 d . . . H35A H 0.0904 0.1157 0.7735 0.062 Uiso 1 1 calc R . . C36 C 0.0944(10) 0.0277(9) 0.7267(11) 0.075(6) Uani 1 1 d . . . H36A H 0.0523 0.0075 0.7450 0.089 Uiso 1 1 calc R . . C37 C 0.1359(12) -0.0045(10) 0.6842(10) 0.072(6) Uani 1 1 d . . . H37A H 0.1214 -0.0474 0.6740 0.087 Uiso 1 1 calc R . . C38 C 0.1946(14) 0.0210(9) 0.6568(9) 0.077(6) Uani 1 1 d . . . H38A H 0.2219 -0.0035 0.6282 0.092 Uiso 1 1 calc R . . C39 C 0.2169(9) 0.0863(8) 0.6707(7) 0.051(4) Uani 1 1 d . . . H39A H 0.2594 0.1044 0.6509 0.062 Uiso 1 1 calc R . . C40 C 0.1783(8) 0.1239(8) 0.7120(6) 0.045(4) Uani 1 1 d . . . O50 O 0.3754(11) 0.0842(10) 0.6021(8) 0.125(6) Uani 1 1 d U . . C51 C 0.4534(13) 0.0697(14) 0.5933(10) 0.101(7) Uani 1 1 d U . . H51A H 0.4617 0.0224 0.5897 0.122 Uiso 1 1 calc R . . H51B H 0.4846 0.0867 0.6264 0.122 Uiso 1 1 calc R . . C52 C 0.472(2) 0.105(2) 0.5334(15) 0.168(14) Uani 1 1 d U . . H52A H 0.5207 0.0911 0.5159 0.202 Uiso 1 1 calc R . . H52B H 0.4715 0.1532 0.5375 0.202 Uiso 1 1 calc R . . C53 C 0.3987(18) 0.0775(17) 0.4966(14) 0.142(11) Uani 1 1 d U . . H53A H 0.3873 0.1040 0.4609 0.170 Uiso 1 1 calc R . . H53B H 0.4053 0.0316 0.4848 0.170 Uiso 1 1 calc R . . C54 C 0.3394(16) 0.0853(15) 0.5442(10) 0.114(8) Uani 1 1 d U . . H54A H 0.3124 0.1270 0.5386 0.136 Uiso 1 1 calc R . . H54B H 0.3021 0.0497 0.5413 0.136 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 Ni 0.0308(7) 0.0407(9) 0.0282(7) 0.0006(7) 0.0019(7) -0.0053(8) Br1 0.0573(9) 0.0646(10) 0.0408(7) -0.0015(8) 0.0023(7) 0.0204(8) Br2 0.0394(7) 0.0640(9) 0.0417(7) -0.0002(7) 0.0018(7) -0.0171(7) N1 0.038(6) 0.031(6) 0.032(6) 0.001(5) 0.001(5) -0.005(5) C2 0.031(7) 0.033(7) 0.026(6) -0.008(5) 0.005(5) 0.000(6) C3 0.040(8) 0.047(9) 0.028(7) 0.001(6) -0.016(6) -0.008(7) C4 0.030(6) 0.047(8) 0.036(7) -0.002(7) 0.005(5) -0.014(6) C5 0.043(8) 0.035(8) 0.032(7) 0.007(6) 0.004(6) 0.004(6) C6 0.039(7) 0.045(8) 0.017(6) 0.004(5) 0.009(5) 0.005(6) C7 0.032(6) 0.051(8) 0.017(6) -0.001(6) -0.012(5) 0.001(7) N7 0.024(5) 0.048(7) 0.026(5) 0.003(5) -0.001(4) 0.000(5) S8 0.049(2) 0.058(2) 0.0241(16) 0.0004(15) -0.0032(15) -0.0114(18) C9 0.037(7) 0.045(8) 0.018(6) 0.008(6) 0.000(5) -0.002(7) N9 0.030(5) 0.049(6) 0.013(4) 0.000(4) 0.002(4) -0.006(6) S10 0.066(2) 0.052(2) 0.0236(16) 0.0057(15) -0.0052(16) -0.016(2) C11 0.040(8) 0.049(9) 0.029(7) -0.011(6) 0.000(6) 0.007(7) C12 0.039(8) 0.037(8) 0.040(8) 0.005(6) -0.010(6) -0.008(6) C13 0.049(9) 0.065(11) 0.027(7) -0.006(7) -0.006(6) -0.020(8) C14 0.026(7) 0.059(10) 0.031(7) -0.002(7) -0.001(6) -0.022(7) C15 0.027(7) 0.066(10) 0.033(7) -0.010(7) -0.007(6) -0.003(7) C16 0.046(8) 0.030(7) 0.030(7) -0.002(6) -0.002(6) -0.011(6) C17 0.057(10) 0.075(12) 0.048(9) 0.016(8) 0.007(7) 0.039(9) C18 0.059(10) 0.103(15) 0.033(8) 0.013(8) 0.008(7) -0.040(10) C19 0.048(9) 0.048(9) 0.062(9) -0.011(8) 0.003(8) 0.026(8) C20 0.043(8) 0.058(10) 0.034(7) 0.002(7) 0.005(6) -0.020(7) C21 0.043(9) 0.045(9) 0.056(9) 0.013(7) -0.013(7) -0.018(7) C22 0.045(9) 0.097(16) 0.071(12) 0.038(12) -0.029(9) -0.033(10) C23 0.064(11) 0.061(12) 0.061(11) 0.021(9) -0.023(9) -0.033(10) C24 0.117(17) 0.062(12) 0.029(8) 0.008(7) -0.012(9) -0.043(12) C25 0.070(10) 0.053(10) 0.018(7) 0.010(6) 0.003(6) -0.030(8) C26 0.033(8) 0.062(12) 0.098(13) 0.022(10) -0.009(9) -0.006(8) C27 0.090(12) 0.113(15) 0.055(9) 0.024(10) -0.040(9) -0.043(11) C28 0.058(10) 0.060(12) 0.037(8) -0.005(7) 0.001(7) -0.010(8) C29 0.045(9) 0.076(13) 0.042(8) 0.000(8) -0.003(7) 0.008(8) C30 0.040(9) 0.060(11) 0.060(10) -0.017(8) -0.009(7) -0.013(8) C31 0.068(12) 0.057(11) 0.067(11) -0.009(9) 0.008(9) -0.008(9) C32 0.073(12) 0.059(12) 0.097(14) -0.018(11) -0.020(11) 0.039(10) C33 0.046(8) 0.040(9) 0.077(11) -0.010(9) -0.008(8) -0.001(7) C34 0.041(8) 0.058(10) 0.036(7) -0.009(6) -0.014(6) -0.006(8) C35 0.040(8) 0.064(10) 0.051(9) 0.011(8) 0.005(7) 0.006(8) C36 0.037(9) 0.058(12) 0.128(18) 0.050(12) -0.019(11) -0.017(9) C37 0.060(12) 0.059(12) 0.099(15) 0.019(11) -0.040(12) -0.012(11) C38 0.113(18) 0.045(11) 0.072(12) -0.006(9) -0.016(12) 0.024(12) C39 0.046(8) 0.056(11) 0.053(9) 0.007(8) 0.008(7) 0.024(8) C40 0.040(8) 0.060(10) 0.035(7) 0.012(7) -0.016(6) -0.021(7) O50 0.102(11) 0.159(14) 0.114(11) -0.002(11) -0.015(10) 0.010(11) C51 0.080(12) 0.139(16) 0.085(12) -0.010(12) -0.001(10) 0.036(12) C52 0.136(19) 0.21(2) 0.155(19) 0.007(17) 0.020(16) -0.001(17) C53 0.143(18) 0.151(19) 0.131(17) -0.026(15) 0.024(15) 0.009(15) C54 0.118(15) 0.144(17) 0.079(12) 0.015(12) -0.016(12) 0.006(14) _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 Ni N1 2.005(10) . ? Ni N9 2.191(9) . ? Ni N7 2.200(10) . ? Ni Br2 2.363(2) . ? Ni Br1 2.413(2) . ? N1 C6 1.355(16) . ? N1 C2 1.366(16) . ? C2 C3 1.394(18) . ? C2 C7 1.518(17) . ? C3 C4 1.364(18) . ? C4 C5 1.418(18) . ? C5 C6 1.383(19) . ? C6 C9 1.504(18) . ? C7 N7 1.258(17) . ? C7 S8 1.746(12) . ? N7 C11 1.491(17) . ? S8 C34 1.763(16) . ? C9 N9 1.260(17) . ? C9 S10 1.769(12) . ? N9 C20 1.474(17) . ? S10 C40 1.748(16) . ? C11 C16 1.370(19) . ? C11 C12 1.39(2) . ? C12 C13 1.37(2) . ? C12 C17 1.53(2) . ? C13 C14 1.39(2) . ? C14 C15 1.37(2) . ? C14 C18 1.551(18) . ? C15 C16 1.421(19) . ? C16 C19 1.484(19) . ? C20 C21 1.37(2) . ? C20 C25 1.39(2) . ? C21 C22 1.40(2) . ? C21 C26 1.48(2) . ? C22 C23 1.38(3) . ? C23 C24 1.41(3) . ? C23 C27 1.51(2) . ? C24 C25 1.40(2) . ? C25 C28 1.54(2) . ? C29 C34 1.40(2) . ? C29 C30 1.41(2) . ? C30 C31 1.36(2) . ? C31 C32 1.39(3) . ? C32 C33 1.35(2) . ? C33 C34 1.42(2) . ? C35 C40 1.43(2) . ? C35 C36 1.44(3) . ? C36 C37 1.36(3) . ? C37 C38 1.31(3) . ? C38 C39 1.42(3) . ? C39 C40 1.37(2) . ? O50 C51 1.41(3) . ? O50 C54 1.44(3) . ? C51 C52 1.55(4) . ? C52 C53 1.63(4) . ? C53 C54 1.49(4) . ? 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 N1 Ni N9 76.4(4) . . ? N1 Ni N7 75.9(4) . . ? N9 Ni N7 151.2(4) . . ? N1 Ni Br2 151.7(3) . . ? N9 Ni Br2 101.8(3) . . ? N7 Ni Br2 98.6(3) . . ? N1 Ni Br1 93.6(3) . . ? N9 Ni Br1 93.5(3) . . ? N7 Ni Br1 96.3(3) . . ? Br2 Ni Br1 114.66(9) . . ? C6 N1 C2 119.5(11) . . ? C6 N1 Ni 116.9(9) . . ? C2 N1 Ni 117.2(8) . . ? N1 C2 C3 121.3(11) . . ? N1 C2 C7 110.9(10) . . ? C3 C2 C7 127.7(11) . . ? C4 C3 C2 118.6(11) . . ? C3 C4 C5 121.0(12) . . ? C6 C5 C4 117.4(11) . . ? N1 C6 C5 122.1(12) . . ? N1 C6 C9 111.4(11) . . ? C5 C6 C9 126.3(11) . . ? N7 C7 C2 114.8(11) . . ? N7 C7 S8 125.5(10) . . ? C2 C7 S8 119.7(9) . . ? C7 N7 C11 119.7(11) . . ? C7 N7 Ni 114.7(8) . . ? C11 N7 Ni 124.5(8) . . ? C7 S8 C34 102.4(6) . . ? N9 C9 C6 116.5(11) . . ? N9 C9 S10 123.1(10) . . ? C6 C9 S10 120.4(10) . . ? C9 N9 C20 119.8(10) . . ? C9 N9 Ni 113.4(8) . . ? C20 N9 Ni 126.6(8) . . ? C40 S10 C9 100.9(6) . . ? C16 C11 C12 123.5(13) . . ? C16 C11 N7 118.7(12) . . ? C12 C11 N7 117.8(11) . . ? C13 C12 C11 117.4(14) . . ? C13 C12 C17 121.0(14) . . ? C11 C12 C17 121.6(12) . . ? C12 C13 C14 122.2(15) . . ? C15 C14 C13 118.6(13) . . ? C15 C14 C18 120.9(14) . . ? C13 C14 C18 120.2(15) . . ? C14 C15 C16 121.7(13) . . ? C11 C16 C15 116.5(13) . . ? C11 C16 C19 122.8(13) . . ? C15 C16 C19 120.8(13) . . ? C21 C20 C25 122.8(14) . . ? C21 C20 N9 119.0(13) . . ? C25 C20 N9 118.2(14) . . ? C20 C21 C22 118.0(17) . . ? C20 C21 C26 122.4(13) . . ? C22 C21 C26 119.5(16) . . ? C23 C22 C21 122.1(18) . . ? C22 C23 C24 118.0(15) . . ? C22 C23 C27 121.0(19) . . ? C24 C23 C27 121.0(19) . . ? C25 C24 C23 121.0(18) . . ? C20 C25 C24 118.0(17) . . ? C20 C25 C28 120.9(13) . . ? C24 C25 C28 121.2(16) . . ? C34 C29 C30 117.3(15) . . ? C31 C30 C29 124.0(15) . . ? C30 C31 C32 117.8(17) . . ? C33 C32 C31 120.7(17) . . ? C32 C33 C34 121.9(16) . . ? C29 C34 C33 118.2(15) . . ? C29 C34 S8 120.4(12) . . ? C33 C34 S8 121.3(11) . . ? C40 C35 C36 119.5(16) . . ? C37 C36 C35 118.6(16) . . ? C38 C37 C36 124(2) . . ? C37 C38 C39 119(2) . . ? C40 C39 C38 122.1(17) . . ? C39 C40 C35 116.7(15) . . ? C39 C40 S10 124.6(12) . . ? C35 C40 S10 118.4(12) . . ? C51 O50 C54 107.7(19) . . ? O50 C51 C52 103(2) . . ? C51 C52 C53 96(3) . . ? C54 C53 C52 99(2) . . ? O50 C54 C53 109(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.702 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.136 #===END data_[Fe(5)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253605' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C43 H47 Cl2 Fe N3 O2, 1.5(C H2 Cl2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44.50 H50 Cl5 Fe N3 O2' _chemical_formula_weight 891.98 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2178(11) _cell_length_b 29.170(2) _cell_length_c 16.7749(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.674(7) _cell_angle_gamma 90.00 _cell_volume 4505.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.99 _cell_measurement_theta_max 24.99 _exptl_crystal_description prisms _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method ? _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 5.714 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3069 _exptl_absorpt_correction_T_max 0.5715 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7077 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 60.00 _reflns_number_total 6599 _reflns_number_gt 4730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 552 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0804P)^2^+2.4115P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6047 _refine_ls_number_parameters 491 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_all 0.1567 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.59294(7) 0.19859(2) 0.28881(4) 0.0234(2) Uani 1 d . . Cl1 Cl 0.63383(14) 0.22779(4) 0.16448(7) 0.0416(3) Uani 1 d . . Cl2 Cl 0.78480(12) 0.16825(4) 0.35838(7) 0.0383(3) Uani 1 d . . N1 N 0.3711(4) 0.21399(12) 0.2858(2) 0.0238(8) Uani 1 d . . C2 C 0.2734(5) 0.18087(15) 0.2666(3) 0.0272(9) Uani 1 d . . C3 C 0.1241(5) 0.1888(2) 0.2670(3) 0.0359(11) Uani 1 d . . H3A H 0.0566 0.1651 0.2534 0.043 Uiso 1 calc R . C4 C 0.0773(5) 0.2318(2) 0.2877(3) 0.0386(11) Uani 1 d . . H4A H -0.0237 0.2383 0.2876 0.046 Uiso 1 calc R . C5 C 0.1781(5) 0.2657(2) 0.3089(3) 0.0325(10) Uani 1 d . . H5A H 0.1472 0.2954 0.3244 0.039 Uiso 1 calc R . C6 C 0.3245(5) 0.25524(15) 0.3069(2) 0.0234(9) Uani 1 d . . C7 C 0.3416(5) 0.1360(2) 0.2561(3) 0.0298(10) Uani 1 d . . N7 N 0.4786(4) 0.13224(12) 0.2676(2) 0.0289(8) Uani 1 d . . O8 O 0.2498(4) 0.09962(12) 0.2441(2) 0.0443(9) Uani 1 d . . C9 C 0.4466(5) 0.28429(14) 0.3384(2) 0.0228(9) Uani 1 d . . N9 N 0.5696(4) 0.26531(12) 0.3503(2) 0.0236(8) Uani 1 d . . O10 O 0.4228(3) 0.32754(10) 0.3656(2) 0.0302(7) Uani 1 d . . C11 C 0.5438(6) 0.0873(2) 0.2725(3) 0.0386(12) Uani 1 d . . C12 C 0.6125(7) 0.0693(2) 0.2070(3) 0.0471(14) Uani 1 d . . C13 C 0.6763(11) 0.0263(2) 0.2164(4) 0.085(3) Uani 1 d . . H13A H 0.7244 0.0128 0.1733 0.101 Uiso 1 calc R . C14 C 0.6700(13) 0.0029(3) 0.2882(5) 0.109(4) Uani 1 d . . H14A H 0.7131 -0.0266 0.2933 0.130 Uiso 1 calc R . C15 C 0.6035(12) 0.0213(2) 0.3516(4) 0.090(3) Uani 1 d . . H15A H 0.5984 0.0043 0.3997 0.107 Uiso 1 calc R . C16 C 0.5436(9) 0.0645(2) 0.3460(4) 0.059(2) Uani 1 d . . C17 C 0.6228(6) 0.0952(2) 0.1295(3) 0.0457(13) Uani 1 d . . H17A H 0.5555 0.1221 0.1312 0.055 Uiso 1 calc R . C18 C 0.7767(7) 0.1140(3) 0.1194(5) 0.068(2) Uani 1 d . . H18A H 0.7796 0.1305 0.0686 0.102 Uiso 1 calc R . H18B H 0.8459 0.0884 0.1196 0.102 Uiso 1 calc R . H18C H 0.8028 0.1349 0.1635 0.102 Uiso 1 calc R . C19 C 0.5743(8) 0.0658(2) 0.0567(4) 0.057(2) Uani 1 d . . H19A H 0.5826 0.0838 0.0078 0.085 Uiso 1 calc R . H19B H 0.4731 0.0563 0.0616 0.085 Uiso 1 calc R . H19C H 0.6363 0.0386 0.0545 0.085 Uiso 1 calc R . C20 C 0.4723(9) 0.0842(2) 0.4187(4) 0.060(2) Uani 1 d . . H20A H 0.4419 0.1163 0.4050 0.073 Uiso 1 calc R . C21 C 0.3353(10) 0.0578(3) 0.4367(5) 0.085(2) Uani 1 d . . H21A H 0.2703 0.0568 0.3889 0.128 Uiso 1 calc R . H21B H 0.2862 0.0730 0.4800 0.128 Uiso 1 calc R . H21C H 0.3614 0.0264 0.4529 0.128 Uiso 1 calc R . C22 C 0.5789(10) 0.0871(2) 0.4905(4) 0.075(2) Uani 1 d . . H22A H 0.6650 0.1044 0.4761 0.112 Uiso 1 calc R . H22B H 0.6077 0.0561 0.5073 0.112 Uiso 1 calc R . H22C H 0.5326 0.1027 0.5344 0.112 Uiso 1 calc R . C23 C 0.6923(5) 0.28729(14) 0.3908(3) 0.0241(9) Uani 1 d . . C24 C 0.7253(5) 0.27155(15) 0.4688(3) 0.0272(9) Uani 1 d . . C25 C 0.8552(5) 0.2873(2) 0.5058(3) 0.0310(10) Uani 1 d . . H25A H 0.8811 0.2776 0.5587 0.037 Uiso 1 calc R . C26 C 0.9461(5) 0.3166(2) 0.4674(3) 0.0343(11) Uani 1 d . . H26A H 1.0360 0.3255 0.4927 0.041 Uiso 1 calc R . C27 C 0.9071(5) 0.3328(2) 0.3923(3) 0.0323(10) Uani 1 d . . H27A H 0.9682 0.3544 0.3679 0.039 Uiso 1 calc R . C28 C 0.7795(5) 0.31833(14) 0.3511(3) 0.0257(9) Uani 1 d . . C29 C 0.6193(5) 0.2424(2) 0.5124(3) 0.0319(10) Uani 1 d . . H29A H 0.5675 0.2223 0.4721 0.038 Uiso 1 calc R . C30 C 0.6917(6) 0.2115(2) 0.5759(3) 0.0471(13) Uani 1 d . . H30A H 0.6173 0.1936 0.6018 0.071 Uiso 1 calc R . H30B H 0.7447 0.2304 0.6158 0.071 Uiso 1 calc R . H30C H 0.7594 0.1907 0.5508 0.071 Uiso 1 calc R . C31 C 0.5054(6) 0.2729(2) 0.5500(3) 0.0422(12) Uani 1 d . . H31A H 0.4372 0.2536 0.5781 0.063 Uiso 1 calc R . H31B H 0.4523 0.2903 0.5080 0.063 Uiso 1 calc R . H31C H 0.5537 0.2941 0.5878 0.063 Uiso 1 calc R . C32 C 0.7384(5) 0.3382(2) 0.2697(3) 0.0327(10) Uani 1 d . . H32A H 0.6495 0.3219 0.2483 0.039 Uiso 1 calc R . C33 C 0.7005(7) 0.3891(2) 0.2784(4) 0.0472(13) Uani 1 d . . H33A H 0.6740 0.4020 0.2258 0.071 Uiso 1 calc R . H33B H 0.7848 0.4056 0.3019 0.071 Uiso 1 calc R . H33C H 0.6186 0.3923 0.3132 0.071 Uiso 1 calc R . C34 C 0.8575(6) 0.3320(2) 0.2098(3) 0.0467(13) Uani 1 d . . H34A H 0.8254 0.3455 0.1584 0.070 Uiso 1 calc R . H34B H 0.8768 0.2993 0.2028 0.070 Uiso 1 calc R . H34C H 0.9465 0.3474 0.2299 0.070 Uiso 1 calc R . C35 C 0.2208(4) 0.11517(9) 0.1016(2) 0.0434(12) Uani 1 d G . H35A H 0.2489 0.14625 0.1094 0.052 Uiso 1 calc R . C36 C 0.1835(5) 0.09922(13) 0.0253(2) 0.055(2) Uani 1 d G . H36A H 0.1860 0.1194 -0.0190 0.067 Uiso 1 calc R . C37 C 0.1424(6) 0.05375(14) 0.0139(2) 0.071(2) Uani 1 d G . H37A H 0.1169 0.0429 -0.0382 0.086 Uiso 1 calc R . C38 C 0.1387(6) 0.02423(10) 0.0789(2) 0.078(2) Uani 1 d G . H38A H 0.1106 -0.00684 0.0711 0.094 Uiso 1 calc R . C39 C 0.1760(5) 0.04018(10) 0.1552(2) 0.058(2) Uani 1 d G . H39A H 0.1735 0.02001 0.1995 0.069 Uiso 1 calc R . C40 C 0.2171(4) 0.08565(10) 0.16655(15) 0.0354(11) Uani 1 d G . C41 C 0.3355(3) 0.35920(10) 0.23753(15) 0.0341(10) Uani 1 d G . H41A H 0.3866 0.33676 0.20887 0.041 Uiso 1 calc R . C42 C 0.2564(4) 0.39306(11) 0.19655(14) 0.0438(13) Uani 1 d G . H42A H 0.2535 0.3938 0.13988 0.053 Uiso 1 calc R . C43 C 0.1817(4) 0.42589(10) 0.2385(2) 0.0516(15) Uani 1 d G . H43A H 0.1277 0.44903 0.2105 0.062 Uiso 1 calc R . C44 C 0.1861(4) 0.42488(10) 0.3214(2) 0.0519(15) Uani 1 d G . H44A H 0.1350 0.44732 0.3501 0.062 Uiso 1 calc R . C45 C 0.2651(4) 0.39102(10) 0.36239(14) 0.0372(11) Uani 1 d G . H45A H 0.2681 0.39033 0.41906 0.045 Uiso 1 calc R . C46 C 0.3398(3) 0.35819(9) 0.32045(15) 0.0288(10) Uani 1 d G . C50 C 0.5857(6) 0.3142(2) 0.0087(4) 0.0498(14) Uani 1 d . . H50A H 0.5769 0.2892 0.0481 0.060 Uiso 1 calc R . H50B H 0.5162 0.3080 -0.0367 0.060 Uiso 1 calc R . Cl3 Cl 0.7613(2) 0.31476(6) -0.02496(9) 0.0584(4) Uani 1 d . . Cl4 Cl 0.5403(2) 0.36661(6) 0.05328(11) 0.0686(5) Uani 1 d . . C60 C 0.5392(28) 0.5387(8) 0.0868(13) 0.134(8) Uani 0.50 d PDU -1 H60A H 0.6413 0.5455 0.1034 0.161 Uiso 0.50 calc PR -1 H60B H 0.4792 0.5663 0.0946 0.161 Uiso 0.50 calc PR -1 Cl5 Cl 0.4692(6) 0.4887(2) 0.1430(5) 0.144(3) Uani 0.50 d PDU -1 Cl6 Cl 0.5232(15) 0.5183(3) -0.0205(9) 0.240(6) Uani 0.50 d PDU -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0212(3) 0.0222(3) 0.0263(3) 0.0005(3) -0.0045(2) -0.0011(3) Cl1 0.0489(7) 0.0480(7) 0.0276(5) 0.0058(5) -0.0014(5) -0.0059(5) Cl2 0.0298(6) 0.0396(6) 0.0444(6) 0.0050(5) -0.0100(5) 0.0049(5) N1 0.025(2) 0.024(2) 0.022(2) 0.0006(14) -0.0052(14) -0.0055(15) C2 0.026(2) 0.027(2) 0.028(2) 0.006(2) -0.005(2) -0.008(2) C3 0.026(2) 0.045(3) 0.036(3) 0.010(2) -0.007(2) -0.012(2) C4 0.023(2) 0.046(3) 0.047(3) 0.010(2) -0.003(2) -0.004(2) C5 0.025(2) 0.034(2) 0.038(2) 0.004(2) 0.001(2) -0.001(2) C6 0.020(2) 0.026(2) 0.024(2) 0.004(2) -0.002(2) 0.000(2) C7 0.034(3) 0.026(2) 0.029(2) 0.003(2) -0.008(2) -0.010(2) N7 0.035(2) 0.021(2) 0.031(2) -0.0005(15) -0.002(2) -0.004(2) O8 0.057(2) 0.033(2) 0.041(2) 0.0058(15) -0.013(2) -0.024(2) C9 0.025(2) 0.024(2) 0.019(2) 0.001(2) -0.005(2) 0.002(2) N9 0.025(2) 0.023(2) 0.022(2) -0.0006(14) -0.0048(14) -0.0003(15) O10 0.034(2) 0.026(2) 0.030(2) -0.0026(13) -0.0087(13) 0.0049(13) C11 0.054(3) 0.021(2) 0.040(3) -0.006(2) -0.007(2) 0.003(2) C12 0.064(4) 0.032(3) 0.045(3) -0.006(2) -0.008(3) 0.013(2) C13 0.145(8) 0.054(4) 0.054(4) -0.013(3) -0.004(4) 0.050(5) C14 0.186(11) 0.051(4) 0.086(6) -0.009(4) -0.020(6) 0.070(6) C15 0.175(9) 0.038(4) 0.053(4) 0.005(3) -0.019(5) 0.037(5) C16 0.108(6) 0.026(3) 0.042(3) -0.001(2) -0.008(3) 0.013(3) C17 0.052(3) 0.045(3) 0.040(3) -0.010(2) 0.000(2) 0.013(3) C18 0.047(4) 0.074(5) 0.083(5) -0.021(4) 0.008(3) 0.004(3) C19 0.068(4) 0.055(4) 0.046(3) -0.010(3) -0.001(3) 0.002(3) C20 0.103(5) 0.029(3) 0.049(3) 0.013(2) 0.006(3) 0.009(3) C21 0.102(7) 0.084(6) 0.069(5) 0.015(4) 0.002(4) 0.004(5) C22 0.129(7) 0.051(4) 0.043(3) 0.000(3) -0.001(4) -0.009(4) C23 0.020(2) 0.024(2) 0.028(2) -0.003(2) -0.004(2) 0.000(2) C24 0.031(2) 0.024(2) 0.026(2) -0.007(2) -0.006(2) 0.003(2) C25 0.033(3) 0.032(2) 0.027(2) -0.006(2) -0.012(2) 0.005(2) C26 0.026(2) 0.038(3) 0.038(3) -0.009(2) -0.012(2) 0.000(2) C27 0.028(2) 0.028(2) 0.040(3) -0.004(2) -0.003(2) -0.006(2) C28 0.025(2) 0.023(2) 0.028(2) -0.003(2) -0.004(2) -0.001(2) C29 0.033(3) 0.035(3) 0.027(2) 0.006(2) -0.008(2) -0.001(2) C30 0.047(3) 0.053(3) 0.041(3) 0.016(2) -0.003(2) 0.006(3) C31 0.036(3) 0.057(3) 0.035(3) 0.003(2) 0.007(2) 0.001(2) C32 0.031(2) 0.030(2) 0.036(3) 0.007(2) -0.004(2) -0.008(2) C33 0.054(3) 0.029(3) 0.057(3) 0.008(2) -0.012(3) -0.007(2) C34 0.037(3) 0.068(4) 0.034(3) 0.008(3) -0.004(2) -0.008(3) C35 0.051(3) 0.036(3) 0.041(3) 0.001(2) -0.011(2) -0.009(2) C36 0.056(4) 0.068(4) 0.041(3) -0.003(3) -0.012(3) -0.017(3) C37 0.082(5) 0.075(5) 0.055(4) -0.019(4) -0.021(3) -0.025(4) C38 0.088(6) 0.047(4) 0.097(6) -0.028(4) -0.026(4) -0.019(4) C39 0.068(4) 0.033(3) 0.069(4) 0.003(3) -0.026(3) -0.015(3) C40 0.033(3) 0.030(2) 0.042(3) -0.007(2) -0.015(2) -0.005(2) C41 0.033(3) 0.030(2) 0.038(3) 0.003(2) -0.008(2) 0.003(2) C42 0.046(3) 0.038(3) 0.046(3) 0.011(2) -0.013(2) -0.002(2) C43 0.043(3) 0.034(3) 0.077(4) 0.011(3) -0.013(3) 0.004(2) C44 0.045(3) 0.027(3) 0.084(5) -0.001(3) 0.005(3) 0.012(2) C45 0.039(3) 0.027(2) 0.045(3) -0.006(2) 0.005(2) 0.005(2) C46 0.028(2) 0.023(2) 0.035(2) -0.003(2) -0.006(2) 0.002(2) C50 0.048(3) 0.055(4) 0.046(3) 0.005(3) -0.005(3) -0.005(3) Cl3 0.0474(8) 0.0796(10) 0.0480(8) -0.0086(7) 0.0015(6) 0.0054(7) Cl4 0.0537(9) 0.0773(11) 0.0754(11) -0.0148(9) 0.0110(8) 0.0048(8) C60 0.111(11) 0.145(12) 0.146(12) 0.006(9) -0.001(9) 0.018(9) Cl5 0.088(3) 0.116(4) 0.231(8) 0.063(5) 0.034(4) 0.012(3) Cl6 0.248(10) 0.152(8) 0.333(13) 0.032(8) 0.144(10) 0.082(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.092(4) . ? Fe N9 2.218(3) . ? Fe N7 2.225(4) . ? Fe Cl2 2.2539(13) . ? Fe Cl1 2.3002(13) . ? N1 C6 1.331(6) . ? N1 C2 1.349(6) . ? C2 C3 1.396(7) . ? C2 C7 1.465(7) . ? C3 C4 1.376(8) . ? C4 C5 1.393(7) . ? C5 C6 1.386(6) . ? C6 C9 1.486(6) . ? C7 N7 1.273(6) . ? C7 O8 1.367(6) . ? N7 C11 1.444(6) . ? O8 C40 1.383(4) . ? C9 N9 1.270(6) . ? C9 O10 1.363(5) . ? N9 C23 1.442(5) . ? O10 C46 1.380(4) . ? C11 C12 1.395(8) . ? C11 C16 1.399(8) . ? C12 C13 1.392(8) . ? C12 C17 1.512(8) . ? C13 C14 1.388(12) . ? C14 C15 1.362(12) . ? C15 C16 1.378(9) . ? C16 C20 1.525(9) . ? C17 C18 1.537(9) . ? C17 C19 1.540(8) . ? C20 C22 1.521(10) . ? C20 C21 1.522(11) . ? C23 C28 1.400(6) . ? C23 C24 1.407(6) . ? C24 C25 1.401(6) . ? C24 C29 1.509(7) . ? C25 C26 1.378(7) . ? C26 C27 1.378(7) . ? C27 C28 1.402(6) . ? C28 C32 1.515(6) . ? C29 C30 1.526(6) . ? C29 C31 1.534(7) . ? C32 C33 1.533(7) . ? C32 C34 1.534(7) . ? C35 C36 1.39 . ? C35 C40 1.39 . ? C36 C37 1.39 . ? C37 C38 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C41 C42 1.39 . ? C41 C46 1.39 . ? C42 C43 1.39 . ? C43 C44 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C50 Cl3 1.739(6) . ? C50 Cl4 1.760(6) . ? C60 Cl5 1.87(2) . ? C60 Cl6 1.89(2) . ? 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 N1 Fe N9 72.97(13) . . ? N1 Fe N7 74.18(14) . . ? N9 Fe N7 141.48(14) . . ? N1 Fe Cl2 147.08(10) . . ? N9 Fe Cl2 101.21(10) . . ? N7 Fe Cl2 95.50(11) . . ? N1 Fe Cl1 95.73(10) . . ? N9 Fe Cl1 96.90(10) . . ? N7 Fe Cl1 105.89(10) . . ? Cl2 Fe Cl1 117.20(5) . . ? C6 N1 C2 119.4(4) . . ? C6 N1 Fe 121.0(3) . . ? C2 N1 Fe 119.5(3) . . ? N1 C2 C3 121.9(4) . . ? N1 C2 C7 112.5(4) . . ? C3 C2 C7 125.2(4) . . ? C4 C3 C2 118.2(4) . . ? C3 C4 C5 120.0(4) . . ? C6 C5 C4 118.4(4) . . ? N1 C6 C5 122.2(4) . . ? N1 C6 C9 111.2(4) . . ? C5 C6 C9 126.0(4) . . ? N7 C7 O8 123.9(4) . . ? N7 C7 C2 119.2(4) . . ? O8 C7 C2 116.4(4) . . ? C7 N7 C11 119.7(4) . . ? C7 N7 Fe 114.1(3) . . ? C11 N7 Fe 126.0(3) . . ? C7 O8 C40 118.3(3) . . ? N9 C9 O10 120.5(4) . . ? N9 C9 C6 117.6(4) . . ? O10 C9 C6 121.1(4) . . ? C9 N9 C23 123.7(4) . . ? C9 N9 Fe 114.5(3) . . ? C23 N9 Fe 121.2(3) . . ? C9 O10 C46 120.6(3) . . ? C12 C11 C16 122.3(5) . . ? C12 C11 N7 119.9(5) . . ? C16 C11 N7 117.6(5) . . ? C13 C12 C11 117.0(6) . . ? C13 C12 C17 120.3(6) . . ? C11 C12 C17 122.6(5) . . ? C14 C13 C12 120.4(7) . . ? C15 C14 C13 121.5(6) . . ? C14 C15 C16 120.1(7) . . ? C15 C16 C11 118.5(6) . . ? C15 C16 C20 118.5(6) . . ? C11 C16 C20 123.0(5) . . ? C12 C17 C18 111.6(5) . . ? C12 C17 C19 112.1(5) . . ? C18 C17 C19 110.2(5) . . ? C22 C20 C21 112.5(6) . . ? C22 C20 C16 111.6(6) . . ? C21 C20 C16 111.1(6) . . ? C28 C23 C24 123.3(4) . . ? C28 C23 N9 121.3(4) . . ? C24 C23 N9 115.1(4) . . ? C25 C24 C23 116.7(4) . . ? C25 C24 C29 121.9(4) . . ? C23 C24 C29 121.2(4) . . ? C26 C25 C24 121.4(4) . . ? C25 C26 C27 120.2(4) . . ? C26 C27 C28 121.6(4) . . ? C23 C28 C27 116.6(4) . . ? C23 C28 C32 123.5(4) . . ? C27 C28 C32 119.8(4) . . ? C24 C29 C30 113.6(4) . . ? C24 C29 C31 110.2(4) . . ? C30 C29 C31 109.9(4) . . ? C28 C32 C33 109.5(4) . . ? C28 C32 C34 112.9(4) . . ? C33 C32 C34 110.5(4) . . ? C36 C35 C40 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? O8 C40 C39 117.2(2) . . ? O8 C40 C35 122.8(2) . . ? C39 C40 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C46 120.0 . . ? O10 C46 C45 116.3(2) . . ? O10 C46 C41 123.6(2) . . ? C45 C46 C41 120.0 . . ? Cl3 C50 Cl4 111.9(3) . . ? Cl5 C60 Cl6 102.8(12) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.862 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.070 #===END data_[Co(5)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253606' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H47 Cl2 Co N3 O2, 1.25(C H2 Cl2)' _chemical_formula_sum 'C44.25 H49.50 Cl4.50 Co N3 O2' _chemical_formula_weight 873.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8687(6) _cell_length_b 19.6515(16) _cell_length_c 18.0924(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.931(4) _cell_angle_gamma 90.00 _cell_volume 4574.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 183 _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.80 _cell_measurement_theta_max 24.95 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1822 _exptl_absorpt_coefficient_mu 5.650 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1975 _exptl_absorpt_correction_T_max 0.7983 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 47 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6635 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 59.99 _reflns_number_total 6320 _reflns_number_gt 4184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00053(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6320 _refine_ls_number_parameters 527 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.65745(5) 0.15696(4) 0.70720(4) 0.0330(2) Uani 1 1 d . . . Cl1 Cl 0.54146(9) 0.07317(7) 0.67412(8) 0.0495(3) Uani 1 1 d . . . Cl2 Cl 0.70528(11) 0.15944(9) 0.82618(7) 0.0598(4) Uani 1 1 d . . . N1 N 0.6619(3) 0.1848(2) 0.5982(2) 0.0360(9) Uani 1 1 d . . . C2 C 0.5975(4) 0.2321(3) 0.5723(3) 0.0400(11) Uani 1 1 d . . . C3 C 0.5954(5) 0.2508(3) 0.4982(3) 0.0513(13) Uani 1 1 d . . . H3A H 0.5496 0.2852 0.4802 0.062 Uiso 1 1 calc R . . C4 C 0.6631(5) 0.2174(3) 0.4513(3) 0.0502(13) Uani 1 1 d . . . H4A H 0.6636 0.2284 0.4002 0.060 Uiso 1 1 calc R . . C5 C 0.7289(4) 0.1685(3) 0.4788(3) 0.0434(11) Uani 1 1 d . . . H5A H 0.7757 0.1458 0.4470 0.052 Uiso 1 1 calc R . . C6 C 0.7270(3) 0.1524(3) 0.5534(3) 0.0374(10) Uani 1 1 d . . . C7 C 0.5402(4) 0.2654(3) 0.6329(3) 0.0433(12) Uani 1 1 d . . . N7 N 0.5680(3) 0.2520(2) 0.6992(2) 0.0367(9) Uani 1 1 d . . . O8 O 0.4708(3) 0.3160(2) 0.6159(2) 0.0596(11) Uani 1 1 d . . . C9 C 0.7985(3) 0.1068(2) 0.5950(3) 0.0353(10) Uani 1 1 d . . . N9 N 0.8020(3) 0.1132(2) 0.6656(2) 0.0362(9) Uani 1 1 d . . . O10 O 0.8643(3) 0.0657(2) 0.55833(19) 0.0460(9) Uani 1 1 d . . . C11 C 0.5285(3) 0.2927(3) 0.7592(3) 0.0400(11) Uani 1 1 d . . . C12 C 0.4518(4) 0.2656(3) 0.8043(3) 0.0442(12) Uani 1 1 d . . . C13 C 0.4223(4) 0.3051(3) 0.8648(3) 0.0507(13) Uani 1 1 d . . . H13A H 0.3715 0.2881 0.8975 0.061 Uiso 1 1 calc R . . C14 C 0.4656(4) 0.3681(3) 0.8777(3) 0.0536(14) Uani 1 1 d . . . H14A H 0.4440 0.3942 0.9189 0.064 Uiso 1 1 calc R . . C15 C 0.5397(4) 0.3936(3) 0.8316(3) 0.0505(13) Uani 1 1 d . . . H15A H 0.5684 0.4373 0.8414 0.061 Uiso 1 1 calc R . . C16 C 0.5735(4) 0.3571(3) 0.7710(3) 0.0459(12) Uani 1 1 d . . . C17 C 0.3994(4) 0.1987(3) 0.7882(3) 0.0518(13) Uani 1 1 d . . . H17A H 0.4329 0.1784 0.7438 0.062 Uiso 1 1 calc R . . C18 C 0.4138(5) 0.1488(3) 0.8522(4) 0.0709(18) Uani 1 1 d . . . H18A H 0.4882 0.1426 0.8628 0.106 Uiso 1 1 calc R . . H18B H 0.3827 0.1049 0.8388 0.106 Uiso 1 1 calc R . . H18C H 0.3799 0.1669 0.8962 0.106 Uiso 1 1 calc R . . C19 C 0.2854(5) 0.2093(4) 0.7697(4) 0.0716(19) Uani 1 1 d . . . H19A H 0.2525 0.1652 0.7595 0.107 Uiso 1 1 calc R . . H19B H 0.2785 0.2386 0.7260 0.107 Uiso 1 1 calc R . . H19C H 0.2513 0.2310 0.8116 0.107 Uiso 1 1 calc R . . C20 C 0.6592(4) 0.3847(3) 0.7227(3) 0.0498(13) Uani 1 1 d . . . H20A H 0.6556 0.3601 0.6743 0.060 Uiso 1 1 calc R . . C21 C 0.6489(7) 0.4601(3) 0.7072(5) 0.080(2) Uani 1 1 d . . . H21A H 0.5818 0.4691 0.6827 0.120 Uiso 1 1 calc R . . H21B H 0.7052 0.4747 0.6750 0.120 Uiso 1 1 calc R . . H21C H 0.6530 0.4854 0.7538 0.120 Uiso 1 1 calc R . . C22 C 0.7647(6) 0.3703(5) 0.7580(6) 0.102(3) Uani 1 1 d . . . H22A H 0.7721 0.3212 0.7665 0.153 Uiso 1 1 calc R . . H22B H 0.7706 0.3944 0.8053 0.153 Uiso 1 1 calc R . . H22C H 0.8195 0.3859 0.7251 0.153 Uiso 1 1 calc R . . C23 C 0.8802(3) 0.0813(3) 0.7123(3) 0.0374(11) Uani 1 1 d . . . C24 C 0.9529(4) 0.1257(3) 0.7437(3) 0.0448(12) Uani 1 1 d . . . C25 C 1.0286(4) 0.0981(3) 0.7908(3) 0.0518(14) Uani 1 1 d . . . H25A H 1.0803 0.1269 0.8121 0.062 Uiso 1 1 calc R . . C26 C 1.0292(4) 0.0298(3) 0.8069(3) 0.0552(14) Uani 1 1 d . . . H26A H 1.0819 0.0116 0.8385 0.066 Uiso 1 1 calc R . . C27 C 0.9544(4) -0.0123(3) 0.7776(3) 0.0559(14) Uani 1 1 d . . . H27A H 0.9552 -0.0592 0.7902 0.067 Uiso 1 1 calc R . . C28 C 0.8770(4) 0.0122(3) 0.7295(3) 0.0439(12) Uani 1 1 d . . . C29 C 0.9526(4) 0.2008(3) 0.7253(4) 0.0569(15) Uani 1 1 d . . . H29A H 0.8794 0.2131 0.7118 0.068 Uiso 1 1 calc R . . C30 C 0.9843(5) 0.2457(4) 0.7902(5) 0.079(2) Uani 1 1 d . . . H30A H 0.9416 0.2346 0.8329 0.118 Uiso 1 1 calc R . . H30B H 0.9740 0.2935 0.7769 0.118 Uiso 1 1 calc R . . H30C H 1.0577 0.2378 0.8028 0.118 Uiso 1 1 calc R . . C31 C 1.0189(6) 0.2148(4) 0.6565(5) 0.082(2) Uani 1 1 d . . . H31A H 0.9962 0.1849 0.6160 0.123 Uiso 1 1 calc R . . H31B H 1.0922 0.2061 0.6684 0.123 Uiso 1 1 calc R . . H31C H 1.0102 0.2624 0.6414 0.123 Uiso 1 1 calc R . . C32 C 0.7911(4) -0.0355(3) 0.7020(3) 0.0471(12) Uani 1 1 d . . . H32A H 0.7439 -0.0089 0.6684 0.056 Uiso 1 1 calc R . . C33 C 0.8352(5) -0.0950(3) 0.6576(4) 0.0631(16) Uani 1 1 d . . . H33A H 0.7783 -0.1244 0.6406 0.095 Uiso 1 1 calc R . . H33B H 0.8833 -0.1212 0.6890 0.095 Uiso 1 1 calc R . . H33C H 0.8724 -0.0773 0.6148 0.095 Uiso 1 1 calc R . . C34 C 0.7271(5) -0.0601(4) 0.7672(4) 0.0650(17) Uani 1 1 d . . . H34A H 0.7000 -0.0208 0.7940 0.098 Uiso 1 1 calc R . . H34B H 0.7713 -0.0874 0.8005 0.098 Uiso 1 1 calc R . . H34C H 0.6691 -0.0881 0.7488 0.098 Uiso 1 1 calc R . . C35 C 0.3460(4) 0.2325(3) 0.5684(3) 0.0562(15) Uani 1 1 d . . . H35A H 0.3866 0.1956 0.5868 0.067 Uiso 1 1 calc R . . C36 C 0.2525(5) 0.2209(4) 0.5315(4) 0.0702(18) Uani 1 1 d . . . H36A H 0.2291 0.1755 0.5245 0.084 Uiso 1 1 calc R . . C37 C 0.1931(5) 0.2735(6) 0.5051(5) 0.091(3) Uani 1 1 d . . . H37A H 0.1293 0.2649 0.4797 0.110 Uiso 1 1 calc R . . C38 C 0.2276(6) 0.3398(6) 0.5161(5) 0.096(3) Uani 1 1 d . . . H38A H 0.1862 0.3765 0.4983 0.116 Uiso 1 1 calc R . . C39 C 0.3220(5) 0.3539(4) 0.5528(4) 0.0703(19) Uani 1 1 d . . . H39A H 0.3457 0.3992 0.5602 0.084 Uiso 1 1 calc R . . C40 C 0.3788(4) 0.2983(3) 0.5777(3) 0.0526(15) Uani 1 1 d . . . C41 C 0.7203(4) 0.0022(3) 0.5030(3) 0.0453(12) Uani 1 1 d . . . H41A H 0.6780 0.0119 0.5442 0.054 Uiso 1 1 calc R . . C42 C 0.6823(5) -0.0366(3) 0.4440(3) 0.0590(15) Uani 1 1 d . . . H42A H 0.6123 -0.0519 0.4438 0.071 Uiso 1 1 calc R . . C43 C 0.7458(6) -0.0527(3) 0.3858(4) 0.0676(17) Uani 1 1 d . . . H43A H 0.7198 -0.0799 0.3462 0.081 Uiso 1 1 calc R . . C44 C 0.8471(7) -0.0295(4) 0.3850(3) 0.070(2) Uani 1 1 d . . . H44A H 0.8903 -0.0409 0.3448 0.084 Uiso 1 1 calc R . . C45 C 0.8861(5) 0.0103(3) 0.4423(3) 0.0542(14) Uani 1 1 d . . . H45A H 0.9556 0.0266 0.4420 0.065 Uiso 1 1 calc R . . C46 C 0.8202(4) 0.0257(3) 0.5001(3) 0.0438(12) Uani 1 1 d . . . C50 C 0.8502(16) 0.4115(11) 0.4624(9) 0.100(7) Uani 0.513(4) 1 d PDU A 1 H50A H 0.8158 0.3916 0.4180 0.120 Uiso 0.513(4) 1 calc PR A 1 H50B H 0.9014 0.4454 0.4453 0.120 Uiso 0.513(4) 1 calc PR A 1 Cl3 Cl 0.9151(9) 0.3480(7) 0.5092(6) 0.204(5) Uani 0.513(4) 1 d PD A 1 Cl4 Cl 0.7580(9) 0.4527(6) 0.5138(5) 0.206(5) Uani 0.513(4) 1 d PDU A 1 C50' C 0.883(4) 0.3954(10) 0.4767(16) 0.128(9) Uiso 0.360(8) 1 d PDU B 2 H50C H 0.8275 0.3909 0.4381 0.154 Uiso 0.360(8) 1 calc PR B 2 H50D H 0.9481 0.3796 0.4545 0.154 Uiso 0.360(8) 1 calc PR B 2 Cl3' Cl 0.8534(15) 0.3405(9) 0.5463(10) 0.209(7) Uiso 0.360(8) 1 d PD B 2 Cl4' Cl 0.8966(12) 0.4809(7) 0.4955(8) 0.190(6) Uiso 0.360(8) 1 d PD B 2 C50" C 0.866(5) 0.425(5) 0.455(4) 0.092(11) Uiso 0.127(8) 1 d PDU C 3 H50E H 0.8861 0.4380 0.4041 0.110 Uiso 0.127(8) 1 calc PR C 3 H50F H 0.8287 0.3813 0.4520 0.110 Uiso 0.127(8) 1 calc PR C 3 Cl3" Cl 0.975(2) 0.4167(15) 0.5093(15) 0.133(10) Uiso 0.127(8) 1 d PD C 3 Cl4" Cl 0.784(3) 0.486(3) 0.488(3) 0.217(12) Uiso 0.127(8) 1 d PDU C 3 C60 C 0.490(2) 0.4983(16) 0.4704(13) 0.088(9) Uiso 0.25 1 d PD D -4 H60A H 0.5222 0.5306 0.4355 0.105 Uiso 0.25 1 calc PR D -4 H60B H 0.4418 0.4690 0.4418 0.105 Uiso 0.25 1 calc PR D -4 Cl5 Cl 0.4233(16) 0.5422(11) 0.5324(13) 0.190(8) Uiso 0.25 1 d PD D -4 Cl6 Cl 0.5842(13) 0.4495(9) 0.5081(11) 0.158(6) Uiso 0.25 1 d PD D -4 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 Co 0.0335(3) 0.0341(4) 0.0314(4) -0.0017(3) -0.0001(3) 0.0018(3) Cl1 0.0442(6) 0.0439(7) 0.0604(8) -0.0062(6) 0.0019(5) -0.0085(5) Cl2 0.0666(8) 0.0779(10) 0.0345(6) -0.0114(7) -0.0081(5) 0.0280(7) N1 0.0379(19) 0.034(2) 0.036(2) -0.0012(17) 0.0006(16) 0.0018(16) C2 0.050(3) 0.034(3) 0.036(3) -0.005(2) -0.003(2) 0.000(2) C3 0.070(3) 0.041(3) 0.043(3) 0.003(2) -0.009(2) 0.006(2) C4 0.066(3) 0.048(3) 0.037(3) 0.002(2) 0.001(2) -0.002(3) C5 0.054(3) 0.042(3) 0.034(2) -0.004(2) 0.004(2) -0.002(2) C6 0.039(2) 0.038(3) 0.035(2) 0.000(2) 0.0023(18) -0.006(2) C7 0.044(3) 0.036(3) 0.049(3) -0.005(2) -0.003(2) 0.007(2) N7 0.0387(19) 0.035(2) 0.036(2) -0.0060(17) -0.0022(16) 0.0009(16) O8 0.072(3) 0.046(2) 0.060(2) -0.0087(19) -0.022(2) 0.0275(19) C9 0.030(2) 0.039(3) 0.037(3) 0.001(2) 0.0026(18) -0.0005(18) N9 0.0326(18) 0.041(2) 0.035(2) 0.0013(18) -0.0015(15) -0.0023(16) O10 0.0366(16) 0.064(2) 0.0375(18) -0.0097(17) 0.0017(13) 0.0107(16) C11 0.036(2) 0.038(3) 0.046(3) -0.007(2) -0.002(2) 0.0085(19) C12 0.038(2) 0.049(3) 0.046(3) -0.007(2) 0.003(2) 0.006(2) C13 0.044(3) 0.060(4) 0.048(3) -0.004(3) 0.005(2) 0.014(2) C14 0.054(3) 0.053(3) 0.054(3) -0.018(3) 0.000(3) 0.016(3) C15 0.053(3) 0.042(3) 0.056(3) -0.013(3) -0.005(2) 0.007(2) C16 0.049(3) 0.039(3) 0.049(3) -0.006(2) -0.005(2) 0.007(2) C17 0.041(3) 0.058(4) 0.057(3) -0.016(3) 0.008(2) -0.002(2) C18 0.065(4) 0.058(4) 0.090(5) -0.005(4) 0.006(3) -0.011(3) C19 0.042(3) 0.090(5) 0.083(5) -0.022(4) -0.006(3) -0.010(3) C20 0.061(3) 0.033(3) 0.056(3) -0.007(2) 0.006(3) -0.004(2) C21 0.099(5) 0.047(4) 0.093(5) 0.013(4) 0.005(4) 0.001(4) C22 0.052(4) 0.105(6) 0.149(9) 0.049(6) 0.009(4) 0.001(4) C23 0.029(2) 0.046(3) 0.037(2) -0.002(2) 0.0015(18) 0.0042(19) C24 0.033(2) 0.054(3) 0.048(3) -0.009(2) 0.001(2) 0.005(2) C25 0.038(3) 0.071(4) 0.046(3) -0.013(3) -0.006(2) 0.003(2) C26 0.044(3) 0.071(4) 0.050(3) 0.005(3) -0.012(2) 0.011(3) C27 0.051(3) 0.055(4) 0.061(4) 0.011(3) -0.007(3) 0.007(3) C28 0.042(2) 0.042(3) 0.048(3) 0.001(2) -0.004(2) 0.005(2) C29 0.043(3) 0.054(4) 0.074(4) -0.008(3) -0.008(3) -0.007(2) C30 0.056(4) 0.069(5) 0.110(6) -0.021(4) -0.025(4) -0.008(3) C31 0.070(4) 0.079(5) 0.097(6) 0.027(4) 0.002(4) -0.017(4) C32 0.044(3) 0.039(3) 0.057(3) 0.005(2) -0.002(2) 0.000(2) C33 0.067(4) 0.044(3) 0.079(4) -0.005(3) -0.005(3) 0.006(3) C34 0.054(3) 0.073(4) 0.068(4) 0.013(3) 0.002(3) -0.012(3) C35 0.048(3) 0.068(4) 0.052(3) 0.009(3) 0.003(2) 0.016(3) C36 0.044(3) 0.099(5) 0.068(4) 0.012(4) 0.002(3) -0.001(3) C37 0.045(3) 0.136(8) 0.093(6) 0.025(6) 0.000(3) 0.011(4) C38 0.054(4) 0.140(8) 0.096(6) 0.038(6) 0.002(4) 0.044(5) C39 0.064(4) 0.086(5) 0.061(4) 0.013(4) 0.006(3) 0.033(4) C40 0.049(3) 0.071(4) 0.038(3) 0.000(3) 0.001(2) 0.027(3) C41 0.050(3) 0.043(3) 0.043(3) -0.004(2) -0.004(2) 0.001(2) C42 0.080(4) 0.048(3) 0.049(3) -0.010(3) -0.012(3) 0.001(3) C43 0.099(5) 0.050(4) 0.053(4) -0.014(3) -0.012(3) 0.007(3) C44 0.114(6) 0.064(4) 0.033(3) -0.008(3) 0.003(3) 0.037(4) C45 0.055(3) 0.068(4) 0.039(3) -0.003(3) 0.008(2) 0.020(3) C46 0.049(3) 0.048(3) 0.035(3) -0.005(2) 0.000(2) 0.015(2) C50 0.098(11) 0.123(13) 0.079(9) -0.023(10) -0.031(8) 0.003(10) Cl3 0.182(8) 0.255(12) 0.175(8) 0.049(8) -0.026(6) 0.101(9) Cl4 0.238(10) 0.237(10) 0.147(7) -0.044(7) 0.066(6) 0.034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N1 2.048(4) . ? Co N9 2.194(4) . ? Co N7 2.197(4) . ? Co Cl2 2.2300(14) . ? Co Cl1 2.2954(15) . ? N1 C2 1.326(6) . ? N1 C6 1.336(6) . ? C2 C3 1.391(7) . ? C2 C7 1.483(7) . ? C3 C4 1.390(8) . ? C4 C5 1.369(8) . ? C5 C6 1.387(7) . ? C6 C9 1.480(7) . ? C7 N7 1.273(7) . ? C7 O8 1.369(6) . ? N7 C11 1.447(6) . ? O8 C40 1.405(7) . ? C9 N9 1.285(6) . ? C9 O10 1.352(6) . ? N9 C23 1.446(6) . ? O10 C46 1.424(6) . ? C11 C12 1.398(7) . ? C11 C16 1.406(7) . ? C12 C13 1.398(7) . ? C12 C17 1.505(8) . ? C13 C14 1.377(8) . ? C14 C15 1.372(9) . ? C15 C16 1.387(8) . ? C16 C20 1.518(8) . ? C17 C19 1.514(8) . ? C17 C18 1.527(9) . ? C20 C21 1.514(8) . ? C20 C22 1.518(9) . ? C23 C24 1.393(7) . ? C23 C28 1.394(7) . ? C24 C25 1.395(8) . ? C24 C29 1.513(8) . ? C25 C26 1.373(9) . ? C26 C27 1.370(9) . ? C27 C28 1.397(8) . ? C28 C32 1.526(7) . ? C29 C30 1.519(9) . ? C29 C31 1.546(9) . ? C32 C34 1.527(8) . ? C32 C33 1.533(8) . ? C35 C40 1.370(9) . ? C35 C36 1.386(9) . ? C36 C37 1.367(11) . ? C37 C38 1.389(13) . ? C38 C39 1.402(12) . ? C39 C40 1.385(9) . ? C41 C46 1.368(8) . ? C41 C42 1.394(8) . ? C42 C43 1.380(9) . ? C43 C44 1.382(11) . ? C44 C45 1.386(9) . ? C45 C46 1.391(7) . ? C50 Cl3 1.717(14) . ? C50 Cl4 1.721(14) . ? C50' Cl3' 1.704(16) . ? C50' Cl4' 1.723(16) . ? C50" Cl4" 1.706(18) . ? C50" Cl3" 1.710(18) . ? C60 Cl5 1.666(16) . ? C60 Cl6 1.678(16) . ? 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 N1 Co N9 74.79(15) . . ? N1 Co N7 74.49(15) . . ? N9 Co N7 139.18(15) . . ? N1 Co Cl2 155.81(12) . . ? N9 Co Cl2 96.72(11) . . ? N7 Co Cl2 100.43(11) . . ? N1 Co Cl1 88.19(12) . . ? N9 Co Cl1 100.43(11) . . ? N7 Co Cl1 104.78(11) . . ? Cl2 Co Cl1 115.82(7) . . ? C2 N1 C6 121.0(4) . . ? C2 N1 Co 120.0(3) . . ? C6 N1 Co 118.9(3) . . ? N1 C2 C3 121.9(5) . . ? N1 C2 C7 111.3(4) . . ? C3 C2 C7 126.5(5) . . ? C4 C3 C2 117.4(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 119.6(5) . . ? N1 C6 C5 120.1(5) . . ? N1 C6 C9 111.8(4) . . ? C5 C6 C9 127.7(4) . . ? N7 C7 O8 122.3(5) . . ? N7 C7 C2 118.1(4) . . ? O8 C7 C2 119.0(5) . . ? C7 N7 C11 119.7(4) . . ? C7 N7 Co 112.1(3) . . ? C11 N7 Co 127.6(3) . . ? C7 O8 C40 118.2(4) . . ? N9 C9 O10 122.3(4) . . ? N9 C9 C6 117.2(4) . . ? O10 C9 C6 120.2(4) . . ? C9 N9 C23 123.5(4) . . ? C9 N9 Co 111.3(3) . . ? C23 N9 Co 123.8(3) . . ? C9 O10 C46 116.6(4) . . ? C12 C11 C16 123.1(5) . . ? C12 C11 N7 119.2(4) . . ? C16 C11 N7 117.6(4) . . ? C11 C12 C13 116.7(5) . . ? C11 C12 C17 122.5(5) . . ? C13 C12 C17 120.7(5) . . ? C14 C13 C12 121.2(5) . . ? C15 C14 C13 120.6(5) . . ? C14 C15 C16 121.4(5) . . ? C15 C16 C11 116.9(5) . . ? C15 C16 C20 120.7(5) . . ? C11 C16 C20 122.3(4) . . ? C12 C17 C19 110.6(5) . . ? C12 C17 C18 111.4(5) . . ? C19 C17 C18 111.2(5) . . ? C21 C20 C22 109.7(6) . . ? C21 C20 C16 113.2(5) . . ? C22 C20 C16 110.1(5) . . ? C24 C23 C28 122.8(5) . . ? C24 C23 N9 115.0(4) . . ? C28 C23 N9 122.0(4) . . ? C23 C24 C25 117.6(5) . . ? C23 C24 C29 121.5(5) . . ? C25 C24 C29 120.8(5) . . ? C26 C25 C24 120.7(5) . . ? C27 C26 C25 120.5(5) . . ? C26 C27 C28 121.5(6) . . ? C23 C28 C27 116.8(5) . . ? C23 C28 C32 123.3(5) . . ? C27 C28 C32 119.8(5) . . ? C24 C29 C30 113.4(6) . . ? C24 C29 C31 110.6(5) . . ? C30 C29 C31 112.0(6) . . ? C28 C32 C34 109.9(5) . . ? C28 C32 C33 111.5(5) . . ? C34 C32 C33 111.8(5) . . ? C40 C35 C36 118.5(6) . . ? C37 C36 C35 121.3(8) . . ? C36 C37 C38 118.9(7) . . ? C37 C38 C39 121.7(7) . . ? C40 C39 C38 116.5(8) . . ? C35 C40 C39 123.0(6) . . ? C35 C40 O8 123.3(5) . . ? C39 C40 O8 113.6(6) . . ? C46 C41 C42 118.3(5) . . ? C43 C42 C41 120.3(6) . . ? C42 C43 C44 120.2(6) . . ? C43 C44 C45 120.6(6) . . ? C44 C45 C46 117.8(6) . . ? C41 C46 C45 122.7(5) . . ? C41 C46 O10 121.4(4) . . ? C45 C46 O10 115.8(5) . . ? Cl3 C50 Cl4 114.1(12) . . ? Cl3' C50' Cl4' 119.7(18) . . ? Cl4" C50" Cl3" 111.6(18) . . ? Cl5 C60 Cl6 113.6(14) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.646 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.061 #===END data_[Fe(6)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253607' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H47 Cl2 Fe N3 S2, 1.5(C H2 Cl2)' _chemical_formula_sum 'C44.50 H50 Cl5 Fe N3 S2' _chemical_formula_weight 924.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.005(3) _cell_length_b 10.0092(11) _cell_length_c 27.105(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.482(7) _cell_angle_gamma 90.00 _cell_volume 9197.3(17) _cell_formula_units_Z 8 _cell_measurement_temperature 183 _cell_measurement_reflns_used 26 _cell_measurement_theta_min 10.75 _cell_measurement_theta_max 24.98 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Blue-green dichroic' _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3848 _exptl_absorpt_coefficient_mu 6.410 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4993 _exptl_absorpt_correction_T_max 0.8406 _exptl_absorpt_process_details 'Bruker XPREP ver 5.1 (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6871 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 59.99 _reflns_number_total 6741 _reflns_number_gt 4615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+1.0399P] 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 6741 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.62423(2) 0.36836(7) 0.54931(2) 0.02515(17) Uani 1 1 d . . . Cl1 Cl 0.55690(3) 0.36834(14) 0.53501(4) 0.0389(3) Uani 1 1 d . . . Cl2 Cl 0.64856(4) 0.56688(13) 0.57598(5) 0.0441(3) Uani 1 1 d . . . N1 N 0.62937(10) 0.1692(4) 0.52717(13) 0.0250(8) Uani 1 1 d . . . C2 C 0.63879(12) 0.1398(5) 0.48086(15) 0.0258(9) Uani 1 1 d . . . C3 C 0.64536(14) 0.0089(5) 0.46730(17) 0.0320(10) Uani 1 1 d . . . H3A H 0.6518 -0.0110 0.4346 0.038 Uiso 1 1 calc R . . C4 C 0.64261(15) -0.0921(5) 0.50103(19) 0.0359(11) Uani 1 1 d . . . H4A H 0.6473 -0.1820 0.4919 0.043 Uiso 1 1 calc R . . C5 C 0.63298(15) -0.0623(5) 0.54837(18) 0.0345(10) Uani 1 1 d . . . H5A H 0.6307 -0.1308 0.5722 0.041 Uiso 1 1 calc R . . C6 C 0.62673(13) 0.0710(5) 0.56020(17) 0.0294(10) Uani 1 1 d . . . C7 C 0.64486(12) 0.2617(5) 0.45139(16) 0.0261(9) Uani 1 1 d . . . N7 N 0.64623(10) 0.3729(4) 0.47525(13) 0.0241(7) Uani 1 1 d . . . S8 S 0.65587(4) 0.25629(13) 0.38881(4) 0.0352(3) Uani 1 1 d . . . C9 C 0.62179(13) 0.1213(5) 0.61121(17) 0.0305(10) Uani 1 1 d . . . N9 N 0.63302(11) 0.2413(4) 0.62013(14) 0.0295(8) Uani 1 1 d . . . S10 S 0.60320(4) 0.01077(14) 0.65461(4) 0.0408(3) Uani 1 1 d . . . C11 C 0.65637(13) 0.4935(5) 0.44976(15) 0.0240(9) Uani 1 1 d . . . C12 C 0.62739(14) 0.5686(5) 0.42294(16) 0.0298(10) Uani 1 1 d . . . C13 C 0.63962(16) 0.6808(5) 0.39799(18) 0.0375(11) Uani 1 1 d . . . H13A H 0.6205 0.7333 0.3793 0.045 Uiso 1 1 calc R . . C14 C 0.67887(16) 0.7178(5) 0.39968(18) 0.0360(11) Uani 1 1 d . . . H14A H 0.6866 0.7933 0.3815 0.043 Uiso 1 1 calc R . . C15 C 0.70666(15) 0.6452(5) 0.42769(18) 0.0372(11) Uani 1 1 d . . . H15A H 0.7335 0.6729 0.4295 0.045 Uiso 1 1 calc R . . C16 C 0.69633(14) 0.5321(5) 0.45342(17) 0.0292(10) Uani 1 1 d . . . C17 C 0.58391(14) 0.5307(6) 0.42040(18) 0.0391(12) Uani 1 1 d . . . H17A H 0.5813 0.4473 0.4402 0.047 Uiso 1 1 calc R . . C18 C 0.55988(19) 0.6409(8) 0.4432(3) 0.0630(18) Uani 1 1 d . . . H18A H 0.5703 0.6566 0.4774 0.094 Uiso 1 1 calc R . . H18B H 0.5322 0.6133 0.4426 0.094 Uiso 1 1 calc R . . H18C H 0.5618 0.7233 0.4240 0.094 Uiso 1 1 calc R . . C19 C 0.56864(18) 0.5014(8) 0.3668(2) 0.0626(18) Uani 1 1 d . . . H19A H 0.5844 0.4299 0.3535 0.094 Uiso 1 1 calc R . . H19B H 0.5708 0.5823 0.3468 0.094 Uiso 1 1 calc R . . H19C H 0.5410 0.4734 0.3658 0.094 Uiso 1 1 calc R . . C20 C 0.72791(15) 0.4553(6) 0.4850(2) 0.0422(12) Uani 1 1 d . . . H20A H 0.7145 0.3811 0.5019 0.051 Uiso 1 1 calc R . . C21 C 0.75786(17) 0.3927(6) 0.4528(3) 0.0570(16) Uani 1 1 d . . . H21A H 0.7441 0.3357 0.4276 0.086 Uiso 1 1 calc R . . H21B H 0.7767 0.3386 0.4735 0.086 Uiso 1 1 calc R . . H21C H 0.7721 0.4634 0.4366 0.086 Uiso 1 1 calc R . . C22 C 0.74808(17) 0.5439(8) 0.5249(2) 0.0581(17) Uani 1 1 d . . . H22A H 0.7282 0.5824 0.5450 0.087 Uiso 1 1 calc R . . H22B H 0.7623 0.6158 0.5094 0.087 Uiso 1 1 calc R . . H22C H 0.7668 0.4905 0.5460 0.087 Uiso 1 1 calc R . . C23 C 0.63686(14) 0.2896(5) 0.67051(16) 0.0303(10) Uani 1 1 d . . . C24 C 0.67496(17) 0.2917(6) 0.69395(19) 0.0401(12) Uani 1 1 d . . . C25 C 0.68019(18) 0.3427(7) 0.7421(2) 0.0511(14) Uani 1 1 d . . . H25A H 0.7057 0.3420 0.7591 0.061 Uiso 1 1 calc R . . C26 C 0.6488(2) 0.3939(6) 0.76538(19) 0.0535(16) Uani 1 1 d . . . H26A H 0.6528 0.4305 0.7977 0.064 Uiso 1 1 calc R . . C27 C 0.61164(18) 0.3916(6) 0.74139(19) 0.0448(13) Uani 1 1 d . . . H27A H 0.5901 0.4267 0.7576 0.054 Uiso 1 1 calc R . . C28 C 0.60484(15) 0.3392(5) 0.69408(17) 0.0329(10) Uani 1 1 d . . . C29 C 0.71042(17) 0.2401(7) 0.6685(2) 0.0538(15) Uani 1 1 d . . . H29A H 0.7008 0.2114 0.6343 0.065 Uiso 1 1 calc R . . C30 C 0.7403(2) 0.3503(10) 0.6637(4) 0.092(3) Uani 1 1 d . . . H30A H 0.7628 0.3156 0.6472 0.138 Uiso 1 1 calc R . . H30B H 0.7494 0.3831 0.6967 0.138 Uiso 1 1 calc R . . H30C H 0.7280 0.4238 0.6442 0.138 Uiso 1 1 calc R . . C31 C 0.7284(3) 0.1204(10) 0.6949(4) 0.115(4) Uani 1 1 d . . . H31A H 0.7509 0.0890 0.6777 0.173 Uiso 1 1 calc R . . H31B H 0.7086 0.0491 0.6953 0.173 Uiso 1 1 calc R . . H31C H 0.7373 0.1449 0.7289 0.173 Uiso 1 1 calc R . . C32 C 0.56365(16) 0.3438(6) 0.66848(18) 0.0398(12) Uani 1 1 d . . . H32A H 0.5643 0.2963 0.6361 0.048 Uiso 1 1 calc R . . C33 C 0.53329(19) 0.2732(8) 0.6980(2) 0.0638(19) Uani 1 1 d . . . H33A H 0.5415 0.1805 0.7043 0.096 Uiso 1 1 calc R . . H33B H 0.5075 0.2742 0.6791 0.096 Uiso 1 1 calc R . . H33C H 0.5313 0.3194 0.7296 0.096 Uiso 1 1 calc R . . C34 C 0.5518(2) 0.4899(7) 0.6574(3) 0.069(2) Uani 1 1 d . . . H34A H 0.5717 0.5321 0.6381 0.104 Uiso 1 1 calc R . . H34B H 0.5502 0.5384 0.6885 0.104 Uiso 1 1 calc R . . H34C H 0.5261 0.4922 0.6383 0.104 Uiso 1 1 calc R . . C35 C 0.58653(16) 0.1117(6) 0.36995(19) 0.0450(13) Uani 1 1 d . . . H35A H 0.5746 0.1706 0.3918 0.054 Uiso 1 1 calc R . . C36 C 0.5645(2) 0.0118(8) 0.3456(2) 0.0609(17) Uani 1 1 d . . . H36A H 0.5377 -0.0005 0.3519 0.073 Uiso 1 1 calc R . . C37 C 0.5814(2) -0.0693(7) 0.3126(2) 0.0634(18) Uani 1 1 d . . . H37A H 0.5660 -0.1366 0.2957 0.076 Uiso 1 1 calc R . . C38 C 0.6203(2) -0.0549(6) 0.3035(2) 0.0529(15) Uani 1 1 d . . . H38A H 0.6317 -0.1115 0.2804 0.064 Uiso 1 1 calc R . . C39 C 0.64272(18) 0.0428(5) 0.32837(18) 0.0399(12) Uani 1 1 d . . . H39A H 0.6697 0.0535 0.3222 0.048 Uiso 1 1 calc R . . C40 C 0.62621(15) 0.1249(5) 0.36204(16) 0.0338(10) Uani 1 1 d . . . C41 C 0.53483(18) 0.0272(6) 0.5933(2) 0.0485(14) Uani 1 1 d . . . H41A H 0.5364 0.1208 0.5987 0.058 Uiso 1 1 calc R . . C42 C 0.50413(19) -0.0255(8) 0.5624(2) 0.0582(17) Uani 1 1 d . . . H42A H 0.4849 0.0325 0.5467 0.070 Uiso 1 1 calc R . . C43 C 0.5014(2) -0.1602(8) 0.5545(2) 0.070(2) Uani 1 1 d . . . H43A H 0.4803 -0.1959 0.5335 0.084 Uiso 1 1 calc R . . C44 C 0.5297(2) -0.2443(7) 0.5774(2) 0.0624(18) Uani 1 1 d . . . H44A H 0.5278 -0.3378 0.5718 0.075 Uiso 1 1 calc R . . C45 C 0.5609(2) -0.1937(7) 0.6086(2) 0.0557(16) Uani 1 1 d . . . H45A H 0.5802 -0.2515 0.6242 0.067 Uiso 1 1 calc R . . C46 C 0.56288(17) -0.0560(6) 0.61602(19) 0.0405(12) Uani 1 1 d . . . C50 C 0.6823(3) 0.6747(10) 0.6903(3) 0.101(3) Uani 1 1 d . . . H50A H 0.6610 0.6610 0.6638 0.121 Uiso 1 1 calc R . . H50B H 0.6908 0.5855 0.7029 0.121 Uiso 1 1 calc R . . Cl3 Cl 0.66349(11) 0.7603(3) 0.73712(10) 0.1175(10) Uani 1 1 d . . . Cl4 Cl 0.72192(10) 0.7499(3) 0.66470(10) 0.1137(10) Uani 1 1 d . . . C60 C 0.5201(8) 0.709(3) 0.7655(12) 0.135(10) Uani 0.50 1 d P A -1 H60A H 0.5264 0.6649 0.7979 0.163 Uiso 0.50 1 calc PR A -1 H60B H 0.5098 0.6387 0.7421 0.163 Uiso 0.50 1 calc PR A -1 Cl5 Cl 0.5615(3) 0.7652(6) 0.7460(2) 0.133(2) Uani 0.50 1 d P A -1 Cl6 Cl 0.4827(3) 0.8217(14) 0.7722(4) 0.211(5) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0234(3) 0.0252(4) 0.0267(3) -0.0033(3) 0.0016(2) -0.0031(3) Cl1 0.0235(5) 0.0508(7) 0.0419(6) 0.0021(5) -0.0005(4) -0.0016(5) Cl2 0.0515(7) 0.0347(6) 0.0463(7) -0.0122(5) 0.0057(5) -0.0111(5) N1 0.0227(18) 0.0231(19) 0.0292(18) -0.0014(15) 0.0013(14) -0.0044(14) C2 0.019(2) 0.030(2) 0.027(2) -0.0055(18) -0.0008(15) -0.0018(18) C3 0.029(2) 0.035(3) 0.032(2) -0.0038(19) -0.0016(18) 0.000(2) C4 0.035(3) 0.029(3) 0.045(3) -0.008(2) 0.005(2) 0.001(2) C5 0.040(3) 0.026(2) 0.037(2) 0.004(2) 0.004(2) 0.000(2) C6 0.023(2) 0.033(2) 0.032(2) -0.002(2) 0.0003(18) -0.0045(18) C7 0.020(2) 0.033(3) 0.026(2) -0.0035(18) 0.0017(16) 0.0000(18) N7 0.0187(16) 0.0259(19) 0.0276(17) 0.0011(16) 0.0019(13) -0.0016(15) S8 0.0394(6) 0.0387(7) 0.0284(5) -0.0054(5) 0.0086(5) -0.0089(5) C9 0.031(2) 0.028(2) 0.033(2) -0.0005(19) 0.0010(18) -0.002(2) N9 0.0281(19) 0.030(2) 0.0312(19) -0.0007(16) 0.0048(15) -0.0020(16) S10 0.0503(7) 0.0398(7) 0.0322(6) 0.0064(5) 0.0029(5) -0.0129(6) C11 0.024(2) 0.025(2) 0.0232(19) -0.0001(16) 0.0045(16) -0.0012(17) C12 0.024(2) 0.035(2) 0.031(2) 0.0020(19) 0.0010(17) 0.001(2) C13 0.046(3) 0.036(3) 0.031(2) 0.006(2) 0.009(2) 0.008(2) C14 0.045(3) 0.031(3) 0.034(2) 0.0056(19) 0.011(2) -0.001(2) C15 0.033(2) 0.036(3) 0.042(3) -0.003(2) 0.007(2) -0.007(2) C16 0.026(2) 0.026(2) 0.036(2) -0.0024(19) 0.0023(18) -0.0055(18) C17 0.024(2) 0.057(3) 0.036(3) 0.009(2) 0.0008(19) 0.004(2) C18 0.044(3) 0.074(5) 0.074(4) 0.008(4) 0.023(3) 0.020(3) C19 0.038(3) 0.094(5) 0.053(4) 0.001(4) -0.014(3) -0.001(3) C20 0.022(2) 0.041(3) 0.062(3) 0.013(3) -0.002(2) 0.000(2) C21 0.034(3) 0.047(4) 0.088(5) -0.016(3) -0.007(3) 0.009(3) C22 0.034(3) 0.085(5) 0.054(3) -0.007(3) -0.005(2) -0.002(3) C23 0.035(3) 0.029(2) 0.026(2) 0.0005(18) 0.0002(18) -0.0044(19) C24 0.041(3) 0.044(3) 0.034(2) -0.005(2) -0.001(2) -0.003(2) C25 0.051(3) 0.061(4) 0.040(3) -0.004(3) -0.009(2) -0.012(3) C26 0.079(4) 0.053(4) 0.029(2) -0.004(2) 0.005(3) -0.017(3) C27 0.056(3) 0.047(3) 0.033(2) -0.001(2) 0.013(2) -0.005(3) C28 0.042(3) 0.030(3) 0.027(2) -0.0003(18) 0.0087(19) -0.002(2) C29 0.034(3) 0.066(4) 0.060(3) -0.019(3) -0.009(2) 0.001(3) C30 0.045(4) 0.098(7) 0.138(8) -0.034(6) 0.039(5) -0.009(4) C31 0.124(9) 0.080(7) 0.141(9) -0.017(6) 0.008(7) 0.048(7) C32 0.043(3) 0.043(3) 0.035(2) 0.007(2) 0.015(2) 0.005(2) C33 0.047(4) 0.088(5) 0.060(4) 0.016(4) 0.021(3) -0.005(3) C34 0.072(5) 0.052(4) 0.085(5) 0.011(4) 0.017(4) 0.029(4) C35 0.040(3) 0.058(4) 0.036(2) -0.007(2) -0.002(2) -0.002(3) C36 0.053(4) 0.082(5) 0.046(3) -0.006(3) -0.010(3) -0.021(3) C37 0.076(5) 0.060(4) 0.049(3) -0.004(3) -0.027(3) -0.019(4) C38 0.084(5) 0.038(3) 0.035(3) -0.009(2) -0.002(3) -0.004(3) C39 0.054(3) 0.034(3) 0.032(2) 0.001(2) 0.006(2) -0.002(2) C40 0.039(3) 0.033(2) 0.028(2) -0.005(2) -0.0005(18) -0.006(2) C41 0.054(3) 0.049(3) 0.043(3) -0.001(2) 0.005(2) -0.012(3) C42 0.047(4) 0.079(5) 0.048(3) -0.004(3) -0.002(3) -0.015(3) C43 0.068(5) 0.090(6) 0.052(3) -0.012(4) 0.001(3) -0.040(4) C44 0.081(5) 0.053(4) 0.053(3) -0.006(3) 0.010(3) -0.031(4) C45 0.066(4) 0.045(4) 0.056(3) 0.003(3) 0.009(3) -0.021(3) C46 0.044(3) 0.041(3) 0.037(2) 0.004(2) 0.009(2) -0.016(2) C50 0.131(9) 0.093(7) 0.082(6) -0.032(5) 0.031(6) -0.042(6) Cl3 0.170(3) 0.0908(18) 0.0945(17) -0.0120(14) 0.0298(17) 0.0352(19) Cl4 0.143(2) 0.109(2) 0.0913(15) -0.0185(14) 0.0208(15) -0.0599(19) C60 0.13(2) 0.14(2) 0.14(2) 0.00(2) 0.030(18) 0.010(19) Cl5 0.203(7) 0.101(4) 0.088(3) -0.035(3) -0.029(4) -0.015(4) Cl6 0.172(9) 0.312(16) 0.152(7) -0.009(9) 0.034(6) -0.077(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.093(4) . ? Fe N7 2.197(3) . ? Fe Cl2 2.2499(15) . ? Fe Cl1 2.2920(13) . ? Fe N9 2.303(4) . ? N1 C6 1.337(6) . ? N1 C2 1.352(6) . ? C2 C3 1.384(7) . ? C2 C7 1.481(7) . ? C3 C4 1.371(7) . ? C4 C5 1.382(7) . ? C5 C6 1.392(7) . ? C6 C9 1.493(6) . ? C7 N7 1.286(6) . ? C7 S8 1.766(4) . ? N7 C11 1.446(6) . ? S8 C40 1.777(5) . ? C9 N9 1.277(7) . ? C9 S10 1.768(5) . ? N9 C23 1.445(6) . ? S10 C46 1.788(6) . ? C11 C12 1.397(6) . ? C11 C16 1.409(6) . ? C12 C13 1.392(7) . ? C12 C17 1.523(6) . ? C13 C14 1.383(8) . ? C14 C15 1.373(7) . ? C15 C16 1.389(7) . ? C16 C20 1.527(7) . ? C17 C18 1.531(8) . ? C17 C19 1.532(7) . ? C20 C22 1.519(8) . ? C20 C21 1.527(8) . ? C23 C28 1.396(7) . ? C23 C24 1.398(7) . ? C24 C25 1.400(7) . ? C24 C29 1.525(8) . ? C25 C26 1.380(9) . ? C26 C27 1.375(9) . ? C27 C28 1.388(7) . ? C28 C32 1.515(7) . ? C29 C31 1.500(11) . ? C29 C30 1.512(10) . ? C32 C33 1.528(7) . ? C32 C34 1.540(8) . ? C35 C36 1.384(9) . ? C35 C40 1.389(7) . ? C36 C37 1.368(10) . ? C37 C38 1.370(10) . ? C38 C39 1.383(8) . ? C39 C40 1.380(7) . ? C41 C46 1.375(9) . ? C41 C42 1.389(8) . ? C42 C43 1.367(11) . ? C43 C44 1.387(11) . ? C44 C45 1.400(9) . ? C45 C46 1.393(9) . ? C50 Cl3 1.697(9) . ? C50 Cl4 1.734(9) . ? C60 Cl5 1.64(3) . ? C60 Cl6 1.72(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe N7 73.48(14) . . ? N1 Fe Cl2 153.69(11) . . ? N7 Fe Cl2 97.61(11) . . ? N1 Fe Cl1 93.22(11) . . ? N7 Fe Cl1 104.63(10) . . ? Cl2 Fe Cl1 113.07(6) . . ? N1 Fe N9 72.82(14) . . ? N7 Fe N9 137.88(14) . . ? Cl2 Fe N9 101.51(11) . . ? Cl1 Fe N9 101.76(10) . . ? C6 N1 C2 119.7(4) . . ? C6 N1 Fe 119.8(3) . . ? C2 N1 Fe 120.3(3) . . ? N1 C2 C3 120.5(4) . . ? N1 C2 C7 112.0(4) . . ? C3 C2 C7 127.2(4) . . ? C4 C3 C2 120.0(4) . . ? C3 C4 C5 119.6(5) . . ? C4 C5 C6 118.2(5) . . ? N1 C6 C5 122.1(4) . . ? N1 C6 C9 113.0(4) . . ? C5 C6 C9 124.5(4) . . ? N7 C7 C2 116.3(4) . . ? N7 C7 S8 120.5(4) . . ? C2 C7 S8 122.8(3) . . ? C7 N7 C11 118.9(3) . . ? C7 N7 Fe 116.1(3) . . ? C11 N7 Fe 124.4(3) . . ? C7 S8 C40 105.0(2) . . ? N9 C9 C6 116.0(4) . . ? N9 C9 S10 125.4(4) . . ? C6 C9 S10 118.5(4) . . ? C9 N9 C23 119.8(4) . . ? C9 N9 Fe 110.1(3) . . ? C23 N9 Fe 126.8(3) . . ? C9 S10 C46 98.2(2) . . ? C12 C11 C16 121.7(4) . . ? C12 C11 N7 120.9(4) . . ? C16 C11 N7 117.4(4) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 C17 120.4(5) . . ? C11 C12 C17 122.2(4) . . ? C14 C13 C12 121.7(5) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 121.3(5) . . ? C15 C16 C11 117.9(4) . . ? C15 C16 C20 119.8(4) . . ? C11 C16 C20 122.2(4) . . ? C12 C17 C18 110.4(5) . . ? C12 C17 C19 110.3(4) . . ? C18 C17 C19 111.6(5) . . ? C22 C20 C21 111.2(5) . . ? C22 C20 C16 111.3(5) . . ? C21 C20 C16 110.9(5) . . ? C28 C23 C24 121.0(4) . . ? C28 C23 N9 122.4(4) . . ? C24 C23 N9 116.5(4) . . ? C23 C24 C25 118.4(5) . . ? C23 C24 C29 121.8(5) . . ? C25 C24 C29 119.9(5) . . ? C26 C25 C24 121.0(6) . . ? C27 C26 C25 119.5(5) . . ? C26 C27 C28 121.6(5) . . ? C27 C28 C23 118.5(5) . . ? C27 C28 C32 119.5(5) . . ? C23 C28 C32 121.8(4) . . ? C31 C29 C30 111.9(7) . . ? C31 C29 C24 111.2(7) . . ? C30 C29 C24 110.5(6) . . ? C28 C32 C33 112.6(5) . . ? C28 C32 C34 109.7(5) . . ? C33 C32 C34 111.4(5) . . ? C36 C35 C40 119.4(6) . . ? C37 C36 C35 120.1(6) . . ? C36 C37 C38 121.0(6) . . ? C37 C38 C39 119.4(6) . . ? C40 C39 C38 120.3(6) . . ? C39 C40 C35 119.7(5) . . ? C39 C40 S8 117.6(4) . . ? C35 C40 S8 122.3(4) . . ? C46 C41 C42 120.2(6) . . ? C43 C42 C41 120.4(7) . . ? C42 C43 C44 119.5(7) . . ? C43 C44 C45 121.1(7) . . ? C46 C45 C44 118.1(7) . . ? C41 C46 C45 120.7(6) . . ? C41 C46 S10 120.6(4) . . ? C45 C46 S10 118.7(5) . . ? Cl3 C50 Cl4 115.5(5) . . ? Cl5 C60 Cl6 117.8(18) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.623 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.070 #===END data_[Co(6)Cl2] _database_code_depnum_ccdc_archive 'CCDC 253608' #TrackingRef 'CST 08-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H47 Cl2 Co N3 S2, 1.5(C H2 Cl2)' _chemical_formula_sum 'C44.50 H50 Cl5 Co N3 S2' _chemical_formula_weight 927.18 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' S S 0.1246 0.1234 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.234(6) _cell_length_b 10.0665(10) _cell_length_c 27.315(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.888(12) _cell_angle_gamma 90.00 _cell_volume 9392(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293 _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 12.49 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 90.67 _diffrn_reflns_number 2459 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2339 _reflns_number_gt 1576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2339 _refine_ls_number_parameters 454 _refine_ls_number_restraints 452 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.62388(12) 0.36547(10) 0.54941(4) 0.041(2) Uani 1 1 d U . . Cl1 Cl 0.5577(3) 0.3607(3) 0.53588(10) 0.055(5) Uani 1 1 d U . . Cl2 Cl 0.64588(16) 0.5625(2) 0.57736(7) 0.059(3) Uani 1 1 d U . . N1 N 0.6295(3) 0.1716(3) 0.52822(13) 0.035(6) Uani 1 1 d GU . . C2 C 0.6399(3) 0.1418(3) 0.48113(13) 0.037(10) Uani 1 1 d GU . . C3 C 0.6467(3) 0.0108(4) 0.46809(15) 0.045(11) Uani 1 1 d GU . . H3A H 0.6536 -0.0092 0.4366 0.054 Uiso 1 1 calc R . . C4 C 0.6432(3) -0.0904(3) 0.50213(17) 0.063(11) Uani 1 1 d GU . . H4A H 0.6477 -0.1780 0.4934 0.076 Uiso 1 1 calc R . . C5 C 0.6328(3) -0.0606(3) 0.54922(15) 0.050(11) Uani 1 1 d GU . . H5A H 0.6304 -0.1283 0.5720 0.060 Uiso 1 1 calc R . . C6 C 0.6260(3) 0.0704(4) 0.56226(13) 0.036(11) Uani 1 1 d GU . . C7 C 0.6442(5) 0.2616(7) 0.4532(2) 0.036(6) Uani 1 1 d U . . N7 N 0.6453(4) 0.3729(6) 0.47621(19) 0.033(6) Uani 1 1 d U . . S8 S 0.65615(16) 0.2587(2) 0.39060(7) 0.058(3) Uani 1 1 d U . . C9 C 0.6219(5) 0.1217(7) 0.6119(2) 0.036(6) Uani 1 1 d U . . N9 N 0.6330(4) 0.2400(6) 0.6209(2) 0.052(9) Uani 1 1 d U . . S10 S 0.60287(17) 0.0113(2) 0.65467(7) 0.063(3) Uani 1 1 d U . . C11 C 0.6563(4) 0.4936(5) 0.4523(2) 0.032(12) Uani 1 1 d GU . . C12 C 0.6282(3) 0.5675(7) 0.4251(3) 0.055(8) Uani 1 1 d GU . . C13 C 0.6392(4) 0.6794(6) 0.3996(2) 0.043(12) Uani 1 1 d GU . . H13A H 0.6204 0.7288 0.3814 0.051 Uiso 1 1 calc R . . C14 C 0.6784(4) 0.7172(4) 0.40119(18) 0.048(12) Uani 1 1 d GU . . H14A H 0.6857 0.7921 0.3841 0.057 Uiso 1 1 calc R . . C15 C 0.7064(3) 0.6433(6) 0.4283(2) 0.054(7) Uani 1 1 d GU . . H15A H 0.7326 0.6686 0.4294 0.064 Uiso 1 1 calc R . . C16 C 0.6954(4) 0.5314(5) 0.45387(18) 0.036(7) Uani 1 1 d GU . . C17 C 0.5856(9) 0.5355(12) 0.4232(4) 0.063(14) Uani 1 1 d U . . H17A H 0.5831 0.4540 0.4423 0.075 Uiso 1 1 calc R . . C18 C 0.5605(7) 0.6400(13) 0.4464(4) 0.078(16) Uani 1 1 d U . . H18A H 0.5708 0.6577 0.4793 0.116 Uiso 1 1 calc R . . H18B H 0.5341 0.6078 0.4471 0.116 Uiso 1 1 calc R . . H18C H 0.5606 0.7203 0.4274 0.116 Uiso 1 1 calc R . . C19 C 0.5692(6) 0.5029(14) 0.3697(4) 0.106(8) Uani 1 1 d U . . H19A H 0.5417 0.4827 0.3697 0.160 Uiso 1 1 calc R . . H19B H 0.5828 0.4277 0.3576 0.160 Uiso 1 1 calc R . . H19C H 0.5728 0.5781 0.3489 0.160 Uiso 1 1 calc R . . C20 C 0.7269(7) 0.4560(11) 0.4849(4) 0.068(13) Uani 1 1 d U . . H20A H 0.7138 0.3827 0.5007 0.081 Uiso 1 1 calc R . . C21 C 0.7564(7) 0.3962(11) 0.4548(5) 0.078(15) Uani 1 1 d U . . H21A H 0.7755 0.3497 0.4756 0.117 Uiso 1 1 calc R . . H21B H 0.7690 0.4648 0.4373 0.117 Uiso 1 1 calc R . . H21C H 0.7437 0.3351 0.4318 0.117 Uiso 1 1 calc R . . C22 C 0.7457(6) 0.5419(12) 0.5256(4) 0.088(7) Uani 1 1 d U . . H22A H 0.7656 0.4918 0.5440 0.132 Uiso 1 1 calc R . . H22B H 0.7261 0.5697 0.5470 0.132 Uiso 1 1 calc R . . H22C H 0.7573 0.6187 0.5116 0.132 Uiso 1 1 calc R . . C23 C 0.6365(4) 0.2866(6) 0.67051(17) 0.056(17) Uani 1 1 d GU . . C24 C 0.6740(4) 0.2878(6) 0.6936(3) 0.068(16) Uani 1 1 d GU . . C25 C 0.6801(4) 0.3387(7) 0.7408(3) 0.067(13) Uani 1 1 d GU . . H25A H 0.7051 0.3395 0.7563 0.080 Uiso 1 1 calc R . . C26 C 0.6487(4) 0.3885(6) 0.76492(17) 0.081(13) Uani 1 1 d GU . . H26A H 0.6528 0.4225 0.7965 0.097 Uiso 1 1 calc R . . C27 C 0.6113(4) 0.3873(6) 0.7418(2) 0.062(7) Uani 1 1 d GU . . H27A H 0.5903 0.4206 0.7580 0.074 Uiso 1 1 calc R . . C28 C 0.6052(4) 0.3364(7) 0.6946(2) 0.066(16) Uani 1 1 d GU . . C29 C 0.7096(9) 0.2395(13) 0.6683(4) 0.080(16) Uani 1 1 d U . . H29A H 0.6999 0.2109 0.6355 0.096 Uiso 1 1 calc R . . C30 C 0.7392(9) 0.3459(19) 0.6608(7) 0.166(10) Uani 1 1 d U . . H30A H 0.7610 0.3084 0.6453 0.249 Uiso 1 1 calc R . . H30B H 0.7481 0.3830 0.6919 0.249 Uiso 1 1 calc R . . H30C H 0.7274 0.4144 0.6402 0.249 Uiso 1 1 calc R . . C31 C 0.7289(8) 0.1158(15) 0.6933(6) 0.154(15) Uani 1 1 d U . . H31A H 0.7515 0.0910 0.6766 0.231 Uiso 1 1 calc R . . H31B H 0.7105 0.0437 0.6919 0.231 Uiso 1 1 calc R . . H31C H 0.7365 0.1359 0.7270 0.231 Uiso 1 1 calc R . . C32 C 0.5654(8) 0.3462(9) 0.6702(4) 0.093(15) Uani 1 1 d U . . H32A H 0.5663 0.3016 0.6384 0.112 Uiso 1 1 calc R . . C33 C 0.5330(7) 0.2740(14) 0.6985(4) 0.096(8) Uani 1 1 d U . . H33A H 0.5081 0.2834 0.6804 0.144 Uiso 1 1 calc R . . H33B H 0.5318 0.3130 0.7304 0.144 Uiso 1 1 calc R . . H33C H 0.5394 0.1814 0.7018 0.144 Uiso 1 1 calc R . . C34 C 0.5519(6) 0.4876(12) 0.6596(5) 0.108(8) Uani 1 1 d U . . H34A H 0.5258 0.4863 0.6443 0.162 Uiso 1 1 calc R . . H34B H 0.5692 0.5294 0.6381 0.162 Uiso 1 1 calc R . . H34C H 0.5521 0.5365 0.6898 0.162 Uiso 1 1 calc R . . C35 C 0.5877(4) 0.1109(6) 0.3720(2) 0.067(13) Uani 1 1 d GU . . H35A H 0.5760 0.1653 0.3943 0.081 Uiso 1 1 calc R . . C36 C 0.5660(3) 0.0121(8) 0.3472(3) 0.083(15) Uani 1 1 d GU . . H36A H 0.5397 0.0005 0.3528 0.100 Uiso 1 1 calc R . . C37 C 0.5835(4) -0.0693(6) 0.3139(2) 0.086(14) Uani 1 1 d GU . . H37A H 0.5690 -0.1353 0.2973 0.104 Uiso 1 1 calc R . . C38 C 0.6228(4) -0.0519(5) 0.30546(18) 0.063(13) Uani 1 1 d GU . . H38A H 0.6345 -0.1064 0.2832 0.076 Uiso 1 1 calc R . . C39 C 0.6445(4) 0.0468(6) 0.3303(2) 0.056(13) Uani 1 1 d GU . . H39A H 0.6708 0.0584 0.3246 0.067 Uiso 1 1 calc R . . C40 C 0.6270(4) 0.1282(5) 0.36356(18) 0.041(7) Uani 1 1 d GU . . C41 C 0.5355(3) 0.0264(5) 0.5930(3) 0.072(12) Uani 1 1 d GU . . H41A H 0.5369 0.1178 0.5976 0.086 Uiso 1 1 calc R . . C42 C 0.5053(3) -0.0278(8) 0.5628(3) 0.088(7) Uani 1 1 d GU . . H42A H 0.4865 0.0273 0.5472 0.106 Uiso 1 1 calc R . . C43 C 0.5031(3) -0.1645(9) 0.5559(3) 0.078(12) Uani 1 1 d GU . . H43A H 0.4829 -0.2008 0.5357 0.093 Uiso 1 1 calc R . . C44 C 0.5312(3) -0.2470(5) 0.5792(3) 0.095(13) Uani 1 1 d GU . . H44A H 0.5297 -0.3384 0.5746 0.115 Uiso 1 1 calc R . . C45 C 0.5613(3) -0.1927(6) 0.6094(3) 0.077(12) Uani 1 1 d GU . . H45A H 0.5801 -0.2479 0.6250 0.093 Uiso 1 1 calc R . . C46 C 0.5635(3) -0.0560(6) 0.6163(2) 0.052(7) Uani 1 1 d GU . . C50 C 0.6795(8) 0.6773(17) 0.6917(5) 0.132(16) Uani 1 1 d U . . H50A H 0.6594 0.6666 0.6653 0.158 Uiso 1 1 calc R . . H50B H 0.6865 0.5891 0.7036 0.158 Uiso 1 1 calc R . . Cl3 Cl 0.6605(3) 0.7555(4) 0.73538(16) 0.221(7) Uani 1 1 d U . . Cl4 Cl 0.7212(3) 0.7458(6) 0.66619(19) 0.186(6) Uani 1 1 d U . . C60 C 0.5083(11) 0.702(3) 0.7746(13) 0.137(14) Uani 0.50 1 d PDU A -1 H60A H 0.5116 0.6744 0.8087 0.164 Uiso 0.50 1 calc PR A -1 H60B H 0.4960 0.6312 0.7549 0.164 Uiso 0.50 1 calc PR A -1 Cl5 Cl 0.5529(8) 0.7568(16) 0.7515(5) 0.228(14) Uani 0.50 1 d PDU A -1 Cl6 Cl 0.4821(10) 0.856(2) 0.7673(9) 0.335(15) Uani 0.50 1 d PDU A -1 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 Co 0.048(8) 0.0385(5) 0.0366(6) -0.0049(4) 0.0035(12) -0.0050(12) Cl1 0.031(16) 0.0750(15) 0.0601(14) 0.0038(11) 0.001(3) -0.005(3) Cl2 0.066(10) 0.0508(11) 0.0602(12) -0.0165(9) 0.010(2) -0.018(2) N1 0.025(18) 0.043(3) 0.036(3) -0.006(2) 0.001(5) -0.012(6) C2 0.03(3) 0.040(4) 0.041(4) -0.007(3) 0.000(7) 0.000(8) C3 0.04(4) 0.046(5) 0.049(4) -0.009(4) 0.008(8) -0.002(8) C4 0.10(4) 0.036(4) 0.057(5) -0.004(3) 0.012(9) 0.014(8) C5 0.06(4) 0.041(4) 0.049(4) 0.005(3) 0.015(8) -0.014(8) C6 0.03(3) 0.035(4) 0.040(4) -0.005(3) 0.002(8) -0.007(8) C7 0.030(19) 0.047(4) 0.031(3) -0.003(3) 0.017(6) -0.004(7) N7 0.023(18) 0.038(3) 0.037(3) 0.002(3) 0.001(5) -0.007(6) S8 0.075(11) 0.0592(13) 0.0412(10) -0.0108(9) 0.021(2) -0.015(2) C9 0.029(19) 0.037(4) 0.044(4) 0.001(3) 0.009(7) 0.011(7) N9 0.07(3) 0.046(4) 0.044(3) 0.004(3) 0.010(6) 0.014(6) S10 0.091(11) 0.0550(12) 0.0438(10) 0.0088(9) 0.011(2) -0.015(2) C11 0.03(4) 0.032(4) 0.040(4) 0.001(4) 0.027(9) -0.010(10) C12 0.05(2) 0.071(7) 0.043(5) 0.002(5) 0.018(11) 0.006(12) C13 0.03(4) 0.051(6) 0.050(5) 0.019(4) -0.005(9) -0.016(11) C14 0.04(4) 0.038(5) 0.064(5) 0.008(4) 0.021(11) 0.007(11) C15 0.05(2) 0.047(5) 0.063(5) -0.003(4) 0.022(9) -0.010(9) C16 0.03(2) 0.039(5) 0.042(4) 0.009(4) 0.020(8) -0.018(10) C17 0.06(4) 0.084(8) 0.050(5) 0.029(5) 0.022(12) 0.028(15) C18 0.02(5) 0.113(9) 0.100(8) 0.025(7) 0.041(14) 0.021(15) C19 0.10(2) 0.144(10) 0.078(6) 0.015(7) -0.001(10) -0.012(13) C20 0.06(4) 0.071(6) 0.076(7) 0.008(6) 0.004(11) -0.005(12) C21 0.04(5) 0.080(7) 0.119(9) -0.017(6) 0.010(15) 0.004(12) C22 0.07(2) 0.115(8) 0.078(6) -0.012(6) 0.013(10) 0.017(12) C23 0.09(5) 0.041(5) 0.036(5) -0.008(4) 0.004(12) -0.008(11) C24 0.10(5) 0.057(6) 0.048(6) -0.009(5) 0.014(12) -0.017(12) C25 0.04(4) 0.097(8) 0.061(6) -0.008(6) -0.001(11) -0.050(13) C26 0.12(4) 0.070(6) 0.049(6) -0.002(5) -0.003(11) -0.016(11) C27 0.08(2) 0.071(5) 0.039(5) 0.000(4) 0.015(9) 0.002(10) C28 0.11(5) 0.050(5) 0.033(5) 0.011(4) -0.010(11) 0.008(11) C29 0.06(5) 0.093(9) 0.080(7) -0.019(6) -0.037(13) 0.018(15) C30 0.16(2) 0.141(12) 0.196(14) -0.029(11) 0.029(15) -0.008(15) C31 0.16(5) 0.123(12) 0.180(14) -0.004(10) 0.039(19) 0.057(18) C32 0.18(5) 0.054(6) 0.048(6) 0.006(4) 0.035(11) 0.008(12) C33 0.08(2) 0.121(9) 0.086(7) 0.010(7) 0.021(11) 0.008(13) C34 0.11(2) 0.105(8) 0.113(8) 0.004(7) 0.000(12) 0.027(12) C35 0.07(4) 0.080(7) 0.052(6) -0.016(5) -0.013(11) 0.005(13) C36 0.04(5) 0.110(9) 0.098(8) -0.008(8) -0.022(14) -0.025(15) C37 0.12(4) 0.066(6) 0.068(7) -0.002(5) -0.009(13) -0.019(13) C38 0.08(4) 0.065(6) 0.048(5) -0.006(5) 0.006(11) -0.024(12) C39 0.07(4) 0.055(5) 0.044(4) -0.006(4) 0.014(8) 0.000(9) C40 0.03(2) 0.056(5) 0.038(4) -0.001(4) 0.014(9) -0.008(9) C41 0.07(4) 0.084(7) 0.065(6) 0.002(6) 0.005(11) -0.023(12) C42 0.09(2) 0.109(8) 0.069(6) -0.002(6) 0.006(10) -0.012(11) C43 0.05(4) 0.115(10) 0.069(6) -0.012(6) 0.015(11) -0.027(14) C44 0.13(4) 0.080(7) 0.076(7) -0.004(6) 0.005(12) -0.031(13) C45 0.11(4) 0.061(6) 0.068(6) 0.003(4) 0.026(11) -0.031(10) C46 0.05(2) 0.056(5) 0.048(4) 0.006(4) 0.008(8) -0.023(8) C50 0.12(5) 0.179(15) 0.099(9) -0.014(9) 0.043(16) -0.11(2) Cl3 0.40(2) 0.135(3) 0.128(3) -0.025(2) 0.017(6) 0.063(6) Cl4 0.23(2) 0.179(4) 0.147(4) -0.028(3) 0.029(6) -0.094(7) C60 0.133(18) 0.149(16) 0.128(15) 0.019(9) 0.014(10) -0.007(10) Cl5 0.24(4) 0.242(13) 0.201(11) -0.132(11) 0.026(16) 0.00(2) Cl6 0.330(18) 0.358(16) 0.318(17) -0.028(9) 0.028(10) -0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N1 2.048(3) . ? Co N7 2.178(8) . ? Co Cl2 2.237(3) . ? Co Cl1 2.271(7) . ? Co N9 2.330(6) . ? N1 C2 1.3900 . ? N1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C7 1.440(8) . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C9 1.467(8) . ? C7 N7 1.284(9) . ? C7 S8 1.785(8) . ? N7 C11 1.442(9) . ? S8 C40 1.781(8) . ? C9 N9 1.269(11) . ? C9 S10 1.768(10) . ? N9 C23 1.430(7) . ? S10 C46 1.784(9) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 C17 1.49(3) . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C20 1.528(18) . ? C17 C18 1.52(2) . ? C17 C19 1.565(17) . ? C20 C21 1.47(2) . ? C20 C22 1.517(17) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C24 C29 1.52(3) . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C32 1.48(3) . ? C29 C30 1.50(3) . ? C29 C31 1.55(2) . ? C32 C34 1.519(17) . ? C32 C33 1.57(3) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C50 Cl3 1.603(18) . ? C50 Cl4 1.77(2) . ? C60 Cl5 1.78(3) . ? C60 Cl6 1.79(2) . ? 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 N1 Co N7 74.3(2) . . ? N1 Co Cl2 154.8(4) . . ? N7 Co Cl2 99.0(2) . . ? N1 Co Cl1 92.6(3) . . ? N7 Co Cl1 104.3(4) . . ? Cl2 Co Cl1 112.56(19) . . ? N1 Co N9 73.19(19) . . ? N7 Co N9 139.0(4) . . ? Cl2 Co N9 99.9(2) . . ? Cl1 Co N9 101.5(4) . . ? C2 N1 C6 120.0 . . ? C2 N1 Co 120.1(2) . . ? C6 N1 Co 119.7(2) . . ? C3 C2 N1 120.0 . . ? C3 C2 C7 129.3(4) . . ? N1 C2 C7 110.6(4) . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 N1 120.0 . . ? C5 C6 C9 126.8(4) . . ? N1 C6 C9 112.3(4) . . ? N7 C7 C2 118.2(6) . . ? N7 C7 S8 118.8(6) . . ? C2 C7 S8 122.2(5) . . ? C7 N7 C11 120.9(6) . . ? C7 N7 Co 114.8(6) . . ? C11 N7 Co 124.1(4) . . ? C40 S8 C7 104.5(5) . . ? N9 C9 C6 117.6(8) . . ? N9 C9 S10 125.5(6) . . ? C6 C9 S10 116.9(6) . . ? C9 N9 C23 119.8(7) . . ? C9 N9 Co 108.9(5) . . ? C23 N9 Co 127.9(4) . . ? C9 S10 C46 98.5(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 N7 120.1(9) . . ? C16 C11 N7 119.8(9) . . ? C13 C12 C11 120.0 . . ? C13 C12 C17 117.1(8) . . ? C11 C12 C17 122.9(8) . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 C20 118.4(9) . . ? C11 C16 C20 121.5(9) . . ? C12 C17 C18 114.6(14) . . ? C12 C17 C19 111.6(16) . . ? C18 C17 C19 110.8(18) . . ? C21 C20 C22 111.8(18) . . ? C21 C20 C16 112.1(9) . . ? C22 C20 C16 111.8(10) . . ? C24 C23 C28 120.0 . . ? C24 C23 N9 116.7(9) . . ? C28 C23 N9 123.2(9) . . ? C25 C24 C23 120.0 . . ? C25 C24 C29 117.6(9) . . ? C23 C24 C29 122.3(9) . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 C32 118.0(8) . . ? C23 C28 C32 121.8(8) . . ? C30 C29 C24 113.9(13) . . ? C30 C29 C31 111(2) . . ? C24 C29 C31 112.8(15) . . ? C28 C32 C34 114.1(15) . . ? C28 C32 C33 113.9(10) . . ? C34 C32 C33 108.1(18) . . ? C36 C35 C40 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 S8 116.8(5) . . ? C35 C40 S8 123.1(5) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 S10 119.2(5) . . ? C41 C46 S10 120.8(5) . . ? Cl3 C50 Cl4 118.8(11) . . ? Cl5 C60 Cl6 97.3(19) . . ? _diffrn_measured_fraction_theta_max 0.381 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.381 _refine_diff_density_max 0.292 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.042 #===END