# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2368a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 Br2 Cd N4 O4 S4,4(C H Cl3)' _chemical_formula_sum 'C68 H72 Br2 Cd Cl12 N4 O4 S4' _chemical_formula_weight 1835.16 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 27.1683(11) _cell_length_b 15.3846(5) _cell_length_c 19.2713(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.162(2) _cell_angle_gamma 90.00 _cell_volume 7973.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.57 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8674 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details sadabs _exptl_special_details ; Because of the flopiness of the solvent and the tertiobutyl the command DFIX and EAD was used One of the two independent CHCL3 molecules show severe positional disorder. This disorder has been modeled accordingly over two positions. The corresponding atoms have been thus refined using EADP command and hydrogen atom was not introduced on this atom. Note however that the hydrogen atoms have been introduced in the formula and the moiety of the compound. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65819 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 29.44 _reflns_number_total 11034 _reflns_number_gt 7878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+66.7564P] 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 11034 _refine_ls_number_parameters 448 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2548 _refine_ls_wR_factor_gt 0.2313 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.073 _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 Cd1 Cd 0.2500 0.7500 0.5000 0.02537(16) Uani 1 2 d S . 1 Br1 Br 0.18388(2) 0.64376(4) 0.42336(3) 0.03679(18) Uani 1 1 d . A 1 S1 S 0.5000 0.88248(11) 0.2500 0.0258(4) Uani 1 2 d S . 1 C1 C 0.53018(16) 0.8135(3) 0.3163(3) 0.0222(9) Uani 1 1 d . . 1 C2 C 0.50538(16) 0.7491(3) 0.3487(3) 0.0217(9) Uani 1 1 d . . 1 C3 C 0.53214(17) 0.7008(3) 0.4027(3) 0.0228(9) Uani 1 1 d . . 1 C4 C 0.58149(17) 0.7226(3) 0.4275(3) 0.0253(10) Uani 1 1 d . . 1 H4 H 0.5993 0.6895 0.4645 0.030 Uiso 1 1 calc R . 1 C5 C 0.60506(17) 0.7921(3) 0.3991(3) 0.0256(10) Uani 1 1 d . . 1 C6 C 0.57943(17) 0.8344(3) 0.3425(3) 0.0234(10) Uani 1 1 d . . 1 H6 H 0.5956 0.8792 0.3204 0.028 Uiso 1 1 calc R . 1 O1 O 0.45509(12) 0.7359(2) 0.3299(2) 0.0242(7) Uani 1 1 d . . 1 C7 C 0.42888(19) 0.7922(4) 0.3731(3) 0.0335(12) Uani 1 1 d . . 1 H7A H 0.4360 0.8538 0.3635 0.040 Uiso 1 1 calc R . 1 H7B H 0.4404 0.7807 0.4233 0.040 Uiso 1 1 calc R . 1 C8 C 0.37373(18) 0.7756(4) 0.3570(3) 0.0320(12) Uani 1 1 d . . 1 C9 C 0.34609(18) 0.7747(4) 0.4116(3) 0.0304(11) Uani 1 1 d . . 1 H9 H 0.3630 0.7806 0.4580 0.036 Uiso 1 1 calc R . 1 N1 N 0.29627(16) 0.7657(3) 0.4027(3) 0.0314(10) Uani 1 1 d . . 1 C10 C 0.2733(2) 0.7568(4) 0.3376(4) 0.0386(14) Uani 1 1 d . . 1 H10 H 0.2382 0.7503 0.3303 0.046 Uiso 1 1 calc R . 1 C11 C 0.2982(2) 0.7566(6) 0.2802(4) 0.0509(19) Uani 1 1 d . . 1 H11 H 0.2805 0.7508 0.2343 0.061 Uiso 1 1 calc R . 1 C12 C 0.3497(2) 0.7648(5) 0.2904(4) 0.0457(17) Uani 1 1 d . . 1 H12 H 0.3678 0.7629 0.2517 0.055 Uiso 1 1 calc R . 1 C13 C 0.65810(19) 0.8188(4) 0.4305(3) 0.0327(12) Uani 1 1 d . . 1 C14 C 0.6933(2) 0.7430(4) 0.4247(4) 0.0413(15) Uani 1 1 d . . 1 H14A H 0.7275 0.7613 0.4413 0.062 Uiso 1 1 calc R . 1 H14B H 0.6908 0.7245 0.3756 0.062 Uiso 1 1 calc R . 1 H14C H 0.6844 0.6945 0.4534 0.062 Uiso 1 1 calc R . 1 C15 C 0.6768(2) 0.8973(4) 0.3919(4) 0.0452(16) Uani 1 1 d . . 1 H15A H 0.6540 0.9463 0.3937 0.068 Uiso 1 1 calc R . 1 H15B H 0.6782 0.8817 0.3430 0.068 Uiso 1 1 calc R . 1 H15C H 0.7100 0.9137 0.4147 0.068 Uiso 1 1 calc R . 1 C16 C 0.6586(3) 0.8439(5) 0.5078(4) 0.0517(18) Uani 1 1 d . . 1 H16A H 0.6437 0.7970 0.5322 0.077 Uiso 1 1 calc R . 1 H16B H 0.6395 0.8975 0.5106 0.077 Uiso 1 1 calc R . 1 H16C H 0.6930 0.8531 0.5298 0.077 Uiso 1 1 calc R . 1 S2 S 0.50367(5) 0.62185(9) 0.45109(7) 0.0286(3) Uani 1 1 d . . 1 C17 C 0.47130(17) 0.5506(3) 0.3877(3) 0.0228(9) Uani 1 1 d . . 1 C18 C 0.49685(17) 0.4967(3) 0.3474(3) 0.0234(10) Uani 1 1 d . . 1 C19 C 0.46976(18) 0.4367(3) 0.3021(3) 0.0246(10) Uani 1 1 d . . 1 C20 C 0.41910(18) 0.4283(3) 0.3012(3) 0.0269(10) Uani 1 1 d . . 1 H20 H 0.4013 0.3875 0.2702 0.032 Uiso 1 1 calc R . 1 C21 C 0.39324(17) 0.4782(3) 0.3446(3) 0.0250(10) Uani 1 1 d . . 1 C22 C 0.42005(17) 0.5412(3) 0.3857(3) 0.0233(9) Uani 1 1 d . . 1 H22 H 0.4030 0.5790 0.4132 0.028 Uiso 1 1 calc R . 1 O2 O 0.54803(12) 0.5009(2) 0.3523(2) 0.0264(8) Uani 1 1 d . . 1 C23 C 0.57046(19) 0.4376(4) 0.4017(3) 0.0357(13) Uani 1 1 d . . 1 H23A H 0.5594 0.3787 0.3859 0.043 Uiso 1 1 calc R . 1 H23B H 0.5598 0.4481 0.4480 0.043 Uiso 1 1 calc R . 1 C24 C 0.62610(18) 0.4431(4) 0.4082(3) 0.0277(11) Uani 1 1 d . . 1 C25 C 0.65373(19) 0.3726(4) 0.4343(3) 0.0294(11) Uani 1 1 d . . 1 H25 H 0.6365 0.3207 0.4425 0.035 Uiso 1 1 calc R . 1 N2 N 0.70376(16) 0.3724(3) 0.4491(3) 0.0311(10) Uani 1 1 d . . 1 C26 C 0.72732(19) 0.4449(4) 0.4340(3) 0.0330(12) Uani 1 1 d . . 1 H26 H 0.7626 0.4466 0.4442 0.040 Uiso 1 1 calc R . 1 C27 C 0.7029(2) 0.5168(4) 0.4045(4) 0.0392(14) Uani 1 1 d . . 1 H27 H 0.7211 0.5660 0.3926 0.047 Uiso 1 1 calc R . 1 C28 C 0.6513(2) 0.5168(4) 0.3922(4) 0.0356(13) Uani 1 1 d . . 1 H28 H 0.6336 0.5666 0.3732 0.043 Uiso 1 1 calc R . 1 C29 C 0.3379(3) 0.4624(8) 0.3481(6) 0.0833(16) Uani 1 1 d . . 1 C30 C 0.3350(3) 0.3907(8) 0.4025(6) 0.0833(16) Uani 1 1 d . . 1 H30A H 0.3534 0.4087 0.4476 0.125 Uiso 1 1 calc R . 1 H30B H 0.3495 0.3371 0.3868 0.125 Uiso 1 1 calc R . 1 H30C H 0.3001 0.3804 0.4078 0.125 Uiso 1 1 calc R . 1 C31 C 0.3115(3) 0.4254(8) 0.2832(6) 0.0833(16) Uani 1 1 d . . 1 H31A H 0.3255 0.3682 0.2750 0.125 Uiso 1 1 calc R . 1 H31B H 0.3152 0.4640 0.2439 0.125 Uiso 1 1 calc R . 1 H31C H 0.2761 0.4192 0.2875 0.125 Uiso 1 1 calc R . 1 C32 C 0.3121(3) 0.5377(8) 0.3760(6) 0.0833(16) Uani 1 1 d . . 1 H32A H 0.3201 0.5911 0.3521 0.125 Uiso 1 1 calc R . 1 H32B H 0.3231 0.5435 0.4264 0.125 Uiso 1 1 calc R . 1 H32C H 0.2761 0.5281 0.3677 0.125 Uiso 1 1 calc R . 1 S3 S 0.5000 0.36429(12) 0.2500 0.0316(4) Uani 1 2 d S . 1 C33 C 0.4464(4) 0.8874(7) 0.5842(5) 0.093(4) Uani 1 1 d D B 1 H33 H 0.4133 0.8729 0.5983 0.112 Uiso 1 1 calc R B 1 Cl1 Cl 0.4761(3) 0.7945(3) 0.5682(2) 0.160(2) Uani 1 1 d D B 1 Cl2 Cl 0.4793(3) 0.9486(5) 0.6474(5) 0.273(5) Uani 1 1 d D B 1 Cl3 Cl 0.4372(2) 0.9551(3) 0.5058(4) 0.174(2) Uani 1 1 d D B 1 C34 C 0.1515(4) 0.5946(6) 0.2403(5) 0.091(4) Uani 1 1 d D C 1 Cl4 Cl 0.1946(3) 0.6380(5) 0.1965(4) 0.092(3) Uani 0.517(12) 1 d PD C 1 Cl5 Cl 0.1328(8) 0.5003(6) 0.2057(7) 0.245(12) Uani 0.517(12) 1 d PD C 1 Cl6 Cl 0.1025(3) 0.6705(9) 0.2116(13) 0.276(13) Uani 0.517(12) 1 d PD C 1 Cl4A Cl 0.1977(5) 0.557(2) 0.1987(8) 0.37(2) Uani 0.483(12) 1 d PD C 2 Cl5A Cl 0.1376(12) 0.6852(6) 0.2089(9) 0.43(3) Uani 0.483(12) 1 d PD C 2 Cl6A Cl 0.1081(4) 0.5189(8) 0.2228(8) 0.170(8) Uani 0.483(12) 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0138(2) 0.0280(3) 0.0353(3) -0.0005(2) 0.00708(19) 0.00086(17) Br1 0.0280(3) 0.0381(3) 0.0445(4) -0.0087(2) 0.0062(2) -0.0076(2) S1 0.0219(8) 0.0231(8) 0.0310(10) 0.000 -0.0009(6) 0.000 C1 0.0158(19) 0.023(2) 0.027(3) -0.0017(18) 0.0028(17) 0.0013(16) C2 0.0131(18) 0.026(2) 0.026(3) -0.0056(18) 0.0035(17) -0.0008(16) C3 0.020(2) 0.027(2) 0.022(3) -0.0013(18) 0.0034(17) -0.0029(17) C4 0.017(2) 0.029(2) 0.029(3) 0.000(2) -0.0022(18) -0.0015(18) C5 0.0151(19) 0.029(2) 0.032(3) -0.004(2) -0.0006(18) -0.0032(17) C6 0.017(2) 0.023(2) 0.030(3) 0.0010(19) 0.0033(18) -0.0026(17) O1 0.0114(14) 0.0330(18) 0.028(2) -0.0007(14) 0.0037(12) -0.0015(12) C7 0.019(2) 0.040(3) 0.043(4) -0.009(2) 0.011(2) -0.003(2) C8 0.015(2) 0.040(3) 0.043(4) 0.007(2) 0.010(2) 0.003(2) C9 0.017(2) 0.035(3) 0.040(3) 0.003(2) 0.005(2) 0.0028(19) N1 0.0179(19) 0.038(2) 0.040(3) 0.004(2) 0.0108(18) -0.0002(17) C10 0.018(2) 0.058(4) 0.040(4) 0.014(3) 0.005(2) 0.002(2) C11 0.025(3) 0.091(6) 0.036(4) 0.012(3) 0.003(2) 0.001(3) C12 0.027(3) 0.076(5) 0.037(4) 0.010(3) 0.014(2) -0.004(3) C13 0.019(2) 0.035(3) 0.042(3) 0.004(2) -0.005(2) -0.008(2) C14 0.022(2) 0.047(4) 0.054(4) 0.005(3) -0.001(2) -0.001(2) C15 0.027(3) 0.040(3) 0.065(5) 0.004(3) -0.006(3) -0.014(2) C16 0.041(4) 0.064(5) 0.047(4) -0.017(3) -0.006(3) -0.010(3) S2 0.0274(6) 0.0344(7) 0.0241(7) 0.0013(5) 0.0040(5) -0.0097(5) C17 0.018(2) 0.026(2) 0.024(3) 0.0039(18) 0.0028(17) -0.0036(17) C18 0.0165(19) 0.026(2) 0.029(3) 0.0073(19) 0.0067(18) -0.0009(16) C19 0.021(2) 0.023(2) 0.030(3) 0.0020(19) 0.0078(19) 0.0020(17) C20 0.019(2) 0.027(2) 0.035(3) 0.002(2) 0.0040(19) -0.0041(17) C21 0.019(2) 0.026(2) 0.031(3) 0.0053(19) 0.0050(18) -0.0008(17) C22 0.018(2) 0.027(2) 0.024(3) -0.0006(18) 0.0043(17) -0.0009(17) O2 0.0147(14) 0.0313(18) 0.034(2) 0.0088(15) 0.0046(13) -0.0002(13) C23 0.017(2) 0.044(3) 0.046(4) 0.021(3) 0.006(2) 0.001(2) C24 0.018(2) 0.032(3) 0.034(3) 0.003(2) 0.0074(19) 0.0025(18) C25 0.021(2) 0.030(3) 0.038(3) 0.001(2) 0.005(2) 0.0013(19) N2 0.0188(19) 0.033(2) 0.042(3) -0.001(2) 0.0055(18) 0.0004(16) C26 0.018(2) 0.033(3) 0.049(4) 0.001(2) 0.007(2) 0.0000(19) C27 0.024(2) 0.033(3) 0.061(4) 0.002(3) 0.009(3) -0.005(2) C28 0.022(2) 0.031(3) 0.054(4) 0.008(2) 0.008(2) 0.003(2) C29 0.0272(17) 0.114(4) 0.112(4) -0.009(3) 0.021(2) -0.013(2) C30 0.0272(17) 0.114(4) 0.112(4) -0.009(3) 0.021(2) -0.013(2) C31 0.0272(17) 0.114(4) 0.112(4) -0.009(3) 0.021(2) -0.013(2) C32 0.0272(17) 0.114(4) 0.112(4) -0.009(3) 0.021(2) -0.013(2) S3 0.0305(9) 0.0215(8) 0.0466(12) 0.000 0.0183(8) 0.000 C33 0.055(5) 0.140(11) 0.085(8) -0.049(7) 0.010(5) -0.002(6) Cl1 0.285(7) 0.087(2) 0.107(3) -0.028(2) 0.023(3) 0.031(3) Cl2 0.242(8) 0.219(7) 0.317(10) -0.194(7) -0.104(7) 0.071(6) Cl3 0.187(5) 0.108(3) 0.244(7) 0.014(4) 0.091(5) 0.019(3) C34 0.096(8) 0.104(9) 0.069(7) 0.008(6) 0.004(6) -0.053(7) Cl4 0.103(6) 0.103(5) 0.071(4) -0.006(3) 0.018(3) -0.043(4) Cl5 0.52(3) 0.076(5) 0.118(8) 0.008(5) -0.032(15) -0.144(12) Cl6 0.067(5) 0.165(12) 0.59(4) 0.098(17) 0.012(10) 0.028(6) Cl4A 0.108(9) 0.90(7) 0.122(10) 0.06(2) 0.041(8) 0.16(2) Cl5A 0.95(7) 0.064(6) 0.196(15) 0.055(8) -0.17(3) -0.153(19) Cl6A 0.126(7) 0.175(11) 0.182(13) 0.112(10) -0.075(7) -0.102(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 Cd1 N2 2.395(5) 3_455 ? Cd1 N2 2.395(5) 5_666 ? Cd1 N1 2.414(5) 7_566 ? Cd1 N1 2.414(5) . ? Cd1 Br1 2.7066(6) 7_566 ? Cd1 Br1 2.7067(6) . ? S1 C1 1.770(5) . ? S1 C1 1.770(5) 2_655 ? C1 C2 1.394(7) . ? C1 C6 1.399(6) . ? C2 O1 1.378(5) . ? C2 C3 1.396(7) . ? C3 C4 1.399(6) . ? C3 S2 1.774(5) . ? C4 C5 1.398(7) . ? C4 H4 0.9500 . ? C5 C6 1.372(7) . ? C5 C13 1.538(7) . ? C6 H6 0.9500 . ? O1 C7 1.456(6) . ? C7 C8 1.508(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.365(10) . ? C8 C9 1.377(8) . ? C9 N1 1.347(6) . ? C9 H9 0.9500 . ? N1 C10 1.326(9) . ? C10 C11 1.375(9) . ? C10 H10 0.9500 . ? C11 C12 1.390(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.523(9) . ? C13 C16 1.537(10) . ? C13 C15 1.541(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S2 C17 1.779(5) . ? C17 C18 1.387(7) . ? C17 C22 1.395(6) . ? C18 O2 1.382(5) . ? C18 C19 1.404(7) . ? C19 C20 1.380(7) . ? C19 S3 1.777(5) . ? C20 C21 1.396(7) . ? C20 H20 0.9500 . ? C21 C22 1.391(7) . ? C21 C29 1.534(9) . ? C22 H22 0.9500 . ? O2 C23 1.435(6) . ? C23 C24 1.501(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.374(7) . ? C24 C28 1.381(8) . ? C25 N2 1.348(7) . ? C25 H25 0.9500 . ? N2 C26 1.339(7) . ? N2 Cd1 2.395(5) 3_545 ? C26 C27 1.370(8) . ? C26 H26 0.9500 . ? C27 C28 1.389(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C31 1.465(15) . ? C29 C32 1.494(15) . ? C29 C30 1.531(17) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S3 C19 1.777(5) 2_655 ? C33 Cl1 1.691(11) . ? C33 Cl2 1.691(10) . ? C33 Cl3 1.822(12) . ? C33 H33 1.0000 . ? C34 Cl5A 1.544(13) . ? C34 Cl5 1.647(11) . ? C34 Cl6A 1.657(11) . ? C34 Cl4 1.676(10) . ? C34 Cl4A 1.684(14) . ? C34 Cl6 1.796(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 179.996(1) 3_455 5_666 ? N2 Cd1 N1 95.54(16) 3_455 7_566 ? N2 Cd1 N1 84.46(16) 5_666 7_566 ? N2 Cd1 N1 84.46(16) 3_455 . ? N2 Cd1 N1 95.54(16) 5_666 . ? N1 Cd1 N1 179.998(1) 7_566 . ? N2 Cd1 Br1 91.02(12) 3_455 7_566 ? N2 Cd1 Br1 88.98(12) 5_666 7_566 ? N1 Cd1 Br1 90.87(12) 7_566 7_566 ? N1 Cd1 Br1 89.13(12) . 7_566 ? N2 Cd1 Br1 88.98(12) 3_455 . ? N2 Cd1 Br1 91.02(12) 5_666 . ? N1 Cd1 Br1 89.13(12) 7_566 . ? N1 Cd1 Br1 90.87(12) . . ? Br1 Cd1 Br1 180.0 7_566 . ? C1 S1 C1 106.3(3) . 2_655 ? C2 C1 C6 120.0(5) . . ? C2 C1 S1 123.0(4) . . ? C6 C1 S1 116.4(4) . . ? O1 C2 C1 120.8(4) . . ? O1 C2 C3 120.6(4) . . ? C1 C2 C3 118.6(4) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 S2 122.5(4) . . ? C4 C3 S2 116.9(4) . . ? C5 C4 C3 121.3(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C13 121.9(5) . . ? C4 C5 C13 120.4(5) . . ? C5 C6 C1 122.0(5) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C2 O1 C7 108.1(4) . . ? O1 C7 C8 109.5(5) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C12 C8 C9 118.5(5) . . ? C12 C8 C7 122.9(5) . . ? C9 C8 C7 118.6(5) . . ? N1 C9 C8 123.4(6) . . ? N1 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C10 N1 C9 117.4(5) . . ? C10 N1 Cd1 119.9(3) . . ? C9 N1 Cd1 122.4(4) . . ? N1 C10 C11 122.8(5) . . ? N1 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 119.1(7) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C8 C12 C11 118.8(6) . . ? C8 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C16 110.1(6) . . ? C14 C13 C5 109.3(5) . . ? C16 C13 C5 109.1(5) . . ? C14 C13 C15 108.1(5) . . ? C16 C13 C15 108.2(6) . . ? C5 C13 C15 112.0(5) . . ? C3 S2 C17 105.7(2) . . ? C18 C17 C22 120.0(5) . . ? C18 C17 S2 121.0(4) . . ? C22 C17 S2 118.4(4) . . ? O2 C18 C17 120.8(5) . . ? O2 C18 C19 120.4(4) . . ? C17 C18 C19 118.7(4) . . ? C20 C19 C18 120.2(5) . . ? C20 C19 S3 118.3(4) . . ? C18 C19 S3 121.3(4) . . ? C19 C20 C21 121.8(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 117.2(4) . . ? C22 C21 C29 121.5(6) . . ? C20 C21 C29 121.3(6) . . ? C21 C22 C17 121.8(5) . . ? C21 C22 H22 119.1 . . ? C17 C22 H22 119.1 . . ? C18 O2 C23 110.0(4) . . ? O2 C23 C24 110.2(4) . . ? O2 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? O2 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C28 117.9(5) . . ? C25 C24 C23 118.5(5) . . ? C28 C24 C23 123.5(5) . . ? N2 C25 C24 124.1(5) . . ? N2 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? C26 N2 C25 116.8(5) . . ? C26 N2 Cd1 120.3(3) . 3_545 ? C25 N2 Cd1 122.8(4) . 3_545 ? N2 C26 C27 123.0(5) . . ? N2 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C26 C27 C28 119.3(5) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C24 C28 C27 118.8(5) . . ? C24 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C31 C29 C32 114.2(9) . . ? C31 C29 C30 103.7(10) . . ? C32 C29 C30 103.9(9) . . ? C31 C29 C21 112.9(8) . . ? C32 C29 C21 114.0(8) . . ? C30 C29 C21 106.8(8) . . ? C19 S3 C19 102.4(3) . 2_655 ? Cl1 C33 Cl2 112.6(6) . . ? Cl1 C33 Cl3 110.2(6) . . ? Cl2 C33 Cl3 105.9(8) . . ? Cl1 C33 H33 109.4 . . ? Cl2 C33 H33 109.4 . . ? Cl3 C33 H33 109.4 . . ? Cl5A C34 Cl5 126.4(10) . . ? Cl5A C34 Cl6A 115.3(11) . . ? Cl5 C34 Cl4 110.1(9) . . ? Cl6A C34 Cl4 134.8(10) . . ? Cl5A C34 Cl4A 106.3(10) . . ? Cl6A C34 Cl4A 102.6(11) . . ? Cl5 C34 Cl6 106.0(9) . . ? Cl6A C34 Cl6 85.4(8) . . ? Cl4 C34 Cl6 97.2(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.661 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.178 _database_code_depnum_ccdc_archive 'CCDC 970400' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2296a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 Br2 Cd N4 S8, 2(C H Cl3)' _chemical_formula_sum 'C66 H70 Br2 Cd Cl6 N4 S8' _chemical_formula_weight 1660.66 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9112(2) _cell_length_b 14.4800(3) _cell_length_c 20.8500(4) _cell_angle_alpha 74.7320(10) _cell_angle_beta 82.4040(10) _cell_angle_gamma 66.7770(10) _cell_volume 3721.48(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.59 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 1.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8815 _exptl_absorpt_correction_T_max 0.9133 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101938 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 29.11 _reflns_number_total 19836 _reflns_number_gt 13249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+1.9757P] 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 19836 _refine_ls_number_parameters 806 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.005 _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 Cd1 Cd 0.5000 0.5000 0.0000 0.02480(8) Uani 1 2 d S . . Br1 Br 0.40714(3) 0.44848(3) 0.119879(16) 0.03743(9) Uani 1 1 d . . . Cd2 Cd 0.0000 1.0000 0.5000 0.02476(8) Uani 1 2 d S . . Br2 Br 0.01854(3) 1.05928(3) 0.366452(15) 0.03246(9) Uani 1 1 d . . . S1 S 0.91130(6) 0.56109(6) 0.28385(4) 0.02545(17) Uani 1 1 d . . . C1 C 0.8562(2) 0.6498(2) 0.20877(14) 0.0218(6) Uani 1 1 d . . . C2 C 0.7535(2) 0.6743(2) 0.19075(14) 0.0220(6) Uani 1 1 d . . . C3 C 0.7209(2) 0.7418(2) 0.12912(14) 0.0232(6) Uani 1 1 d . . . C4 C 0.7894(2) 0.7808(2) 0.08642(15) 0.0254(7) Uani 1 1 d . . . H4 H 0.7650 0.8271 0.0450 0.030 Uiso 1 1 calc R . . C5 C 0.8918(2) 0.7538(2) 0.10279(15) 0.0252(7) Uani 1 1 d . . . C6 C 0.9234(2) 0.6888(2) 0.16480(15) 0.0247(6) Uani 1 1 d . . . H6 H 0.9928 0.6703 0.1777 0.030 Uiso 1 1 calc R . . S2 S 0.66623(6) 0.62229(6) 0.24268(4) 0.02746(17) Uani 1 1 d . . . C7 C 0.7155(3) 0.4929(2) 0.22719(16) 0.0342(8) Uani 1 1 d . . . H7A H 0.7854 0.4533 0.2467 0.041 Uiso 1 1 calc R . . H7B H 0.6683 0.4574 0.2502 0.041 Uiso 1 1 calc R . . C8 C 0.7244(3) 0.4921(2) 0.15482(17) 0.0296(7) Uani 1 1 d . . . C9 C 0.6419(3) 0.4978(2) 0.12162(15) 0.0278(7) Uani 1 1 d . . . H9 H 0.5780 0.5026 0.1459 0.033 Uiso 1 1 calc R . . N1 N 0.6466(2) 0.4969(2) 0.05697(13) 0.0281(6) Uani 1 1 d . . . C10 C 0.7367(3) 0.4922(3) 0.02350(19) 0.0412(9) Uani 1 1 d . . . H10 H 0.7416 0.4920 -0.0223 0.049 Uiso 1 1 calc R . . C11 C 0.8224(3) 0.4878(4) 0.0520(2) 0.0563(12) Uani 1 1 d . . . H11 H 0.8846 0.4858 0.0263 0.068 Uiso 1 1 calc R . . C12 C 0.8161(3) 0.4862(3) 0.1189(2) 0.0444(10) Uani 1 1 d . . . H12 H 0.8750 0.4810 0.1400 0.053 Uiso 1 1 calc R . . C13 C 0.9664(3) 0.7997(3) 0.05769(17) 0.0328(7) Uani 1 1 d D . . C14 C 1.0120(10) 0.8476(9) 0.0980(4) 0.056(2) Uani 0.546(19) 1 d PD . . H14A H 1.0477 0.8891 0.0677 0.083 Uiso 0.546(19) 1 calc PR . . H14B H 1.0620 0.7924 0.1296 0.083 Uiso 0.546(19) 1 calc PR . . H14C H 0.9551 0.8918 0.1225 0.083 Uiso 0.546(19) 1 calc PR . . C15 C 0.9134(7) 0.8821(8) -0.0035(5) 0.056(2) Uani 0.546(19) 1 d PD . . H15A H 0.9665 0.9007 -0.0338 0.083 Uiso 0.546(19) 1 calc PR . . H15B H 0.8629 0.9435 0.0106 0.083 Uiso 0.546(19) 1 calc PR . . H15C H 0.8770 0.8549 -0.0263 0.083 Uiso 0.546(19) 1 calc PR . . C16 C 1.0567(7) 0.7107(6) 0.0342(6) 0.056(2) Uani 0.546(19) 1 d PD . . H16A H 1.1076 0.7372 0.0073 0.083 Uiso 0.546(19) 1 calc PR . . H16B H 1.0289 0.6810 0.0075 0.083 Uiso 0.546(19) 1 calc PR . . H16C H 1.0909 0.6573 0.0730 0.083 Uiso 0.546(19) 1 calc PR . . S3 S 0.59591(6) 0.77494(6) 0.09744(4) 0.02650(17) Uani 1 1 d . . . C17 C 0.5048(2) 0.8407(2) 0.15465(14) 0.0238(6) Uani 1 1 d . C . C18 C 0.5023(2) 0.9322(2) 0.16649(15) 0.0247(6) Uani 1 1 d . . . C19 C 0.4256(2) 0.9784(2) 0.21122(15) 0.0255(6) Uani 1 1 d . C . C20 C 0.3493(2) 0.9396(2) 0.23793(15) 0.0262(7) Uani 1 1 d . . . H20 H 0.2961 0.9742 0.2666 0.031 Uiso 1 1 calc R C . C21 C 0.3481(2) 0.8510(2) 0.22397(15) 0.0248(6) Uani 1 1 d . C . C22 C 0.4287(2) 0.8012(2) 0.18335(15) 0.0252(6) Uani 1 1 d . . . H22 H 0.4320 0.7386 0.1749 0.030 Uiso 1 1 calc R C . S4 S 0.59283(6) 0.98781(6) 0.12460(4) 0.03188(19) Uani 1 1 d . C . C23 C 0.5054(3) 1.0903(3) 0.06404(17) 0.0343(8) Uani 1 1 d . . . H23A H 0.4832 1.0610 0.0335 0.041 Uiso 1 1 calc R C . H23B H 0.4422 1.1320 0.0867 0.041 Uiso 1 1 calc R . . C24 C 0.5641(2) 1.1567(2) 0.02590(15) 0.0277(7) Uani 1 1 d . C . C25 C 0.5304(2) 1.2583(2) 0.02903(15) 0.0272(7) Uani 1 1 d . . . H25 H 0.4701 1.2846 0.0560 0.033 Uiso 1 1 calc R C . N2 N 0.5778(2) 1.3225(2) -0.00385(13) 0.0273(6) Uani 1 1 d . . . C26 C 0.6636(2) 1.2841(3) -0.04114(16) 0.0312(7) Uani 1 1 d . . . H26 H 0.6983 1.3285 -0.0648 0.037 Uiso 1 1 calc R C . C27 C 0.7034(3) 1.1829(3) -0.04639(18) 0.0397(8) Uani 1 1 d . C . H27 H 0.7652 1.1579 -0.0725 0.048 Uiso 1 1 calc R . . C28 C 0.6532(3) 1.1184(3) -0.01364(17) 0.0368(8) Uani 1 1 d . . . H28 H 0.6786 1.0489 -0.0178 0.044 Uiso 1 1 calc R C . C29 C 0.2627(2) 0.8101(2) 0.25623(16) 0.0298(7) Uani 1 1 d . . . C30 C 0.2667(3) 0.7897(3) 0.33234(17) 0.0406(9) Uani 1 1 d . C . H30A H 0.2168 0.7575 0.3536 0.061 Uiso 1 1 calc R . . H30B H 0.2483 0.8552 0.3451 0.061 Uiso 1 1 calc R . . H30C H 0.3375 0.7433 0.3467 0.061 Uiso 1 1 calc R . . C31 C 0.1565(3) 0.8926(3) 0.23281(18) 0.0366(8) Uani 1 1 d . C . H31A H 0.1562 0.9099 0.1841 0.055 Uiso 1 1 calc R . . H31B H 0.1439 0.9546 0.2485 0.055 Uiso 1 1 calc R . . H31C H 0.1012 0.8660 0.2508 0.055 Uiso 1 1 calc R . . C32 C 0.2774(3) 0.7101(3) 0.2384(2) 0.0430(9) Uani 1 1 d . C . H32A H 0.2220 0.6861 0.2605 0.064 Uiso 1 1 calc R . . H32B H 0.3458 0.6576 0.2531 0.064 Uiso 1 1 calc R . . H32C H 0.2740 0.7221 0.1901 0.064 Uiso 1 1 calc R . . S5 S 0.41506(6) 1.09297(6) 0.23409(4) 0.02907(18) Uani 1 1 d . . . C33 C 0.5395(2) 1.0594(2) 0.26689(15) 0.0250(6) Uani 1 1 d . C . C34 C 0.5750(2) 0.9837(2) 0.32528(15) 0.0244(6) Uani 1 1 d . . . C35 C 0.6730(2) 0.9662(2) 0.34783(14) 0.0227(6) Uani 1 1 d . C . C36 C 0.7306(2) 1.0244(2) 0.31359(15) 0.0246(6) Uani 1 1 d . . . H36 H 0.7955 1.0128 0.3305 0.030 Uiso 1 1 calc R C . C37 C 0.6960(2) 1.0996(2) 0.25493(15) 0.0231(6) Uani 1 1 d . C . C38 C 0.5992(2) 1.1160(2) 0.23329(15) 0.0255(7) Uani 1 1 d . . . H38 H 0.5728 1.1678 0.1942 0.031 Uiso 1 1 calc R C . S6 S 0.50049(6) 0.90965(6) 0.36923(4) 0.02994(18) Uani 1 1 d . C . C39 C 0.4136(3) 0.9972(3) 0.41911(18) 0.0359(8) Uani 1 1 d . . . H39A H 0.4549 1.0190 0.4430 0.043 Uiso 1 1 calc R C . H39B H 0.3649 1.0596 0.3901 0.043 Uiso 1 1 calc R . . C40 C 0.3533(2) 0.9424(2) 0.46795(16) 0.0279(7) Uani 1 1 d . C . C41 C 0.2466(2) 0.9719(2) 0.46210(16) 0.0300(7) Uani 1 1 d . . . H41 H 0.2133 1.0269 0.4259 0.036 Uiso 1 1 calc R C . N3 N 0.1879(2) 0.9272(2) 0.50454(13) 0.0284(6) Uani 1 1 d . C . C42 C 0.2357(3) 0.8485(3) 0.55407(17) 0.0347(8) Uani 1 1 d . . . H42 H 0.1954 0.8152 0.5842 0.042 Uiso 1 1 calc R C . C43 C 0.3418(3) 0.8134(3) 0.56329(18) 0.0413(9) Uani 1 1 d . C . H43 H 0.3735 0.7570 0.5991 0.050 Uiso 1 1 calc R . . C44 C 0.4009(3) 0.8609(3) 0.52015(18) 0.0378(8) Uani 1 1 d . . . H44 H 0.4739 0.8380 0.5261 0.045 Uiso 1 1 calc R C . C45 C 0.7658(2) 1.1563(2) 0.21557(15) 0.0263(7) Uani 1 1 d . . . C46 C 0.7750(3) 1.2271(3) 0.25557(17) 0.0370(8) Uani 1 1 d . C . H46A H 0.8216 1.2617 0.2314 0.055 Uiso 1 1 calc R . . H46B H 0.8038 1.1859 0.2990 0.055 Uiso 1 1 calc R . . H46C H 0.7056 1.2790 0.2619 0.055 Uiso 1 1 calc R . . C47 C 0.8754(3) 1.0772(3) 0.20492(18) 0.0382(8) Uani 1 1 d . C . H47A H 0.8697 1.0268 0.1837 0.057 Uiso 1 1 calc R . . H47B H 0.9083 1.0415 0.2480 0.057 Uiso 1 1 calc R . . H47C H 0.9181 1.1128 0.1763 0.057 Uiso 1 1 calc R . . C48 C 0.7224(3) 1.2207(3) 0.14727(18) 0.0429(9) Uani 1 1 d . C . H48A H 0.6528 1.2727 0.1530 0.064 Uiso 1 1 calc R . . H48B H 0.7173 1.1754 0.1214 0.064 Uiso 1 1 calc R . . H48C H 0.7694 1.2552 0.1237 0.064 Uiso 1 1 calc R . . S7 S 0.72472(6) 0.87585(6) 0.42345(4) 0.02562(17) Uani 1 1 d . . . C49 C 0.7494(2) 0.7538(2) 0.40657(14) 0.0214(6) Uani 1 1 d . C . C50 C 0.8160(2) 0.7170(2) 0.35467(14) 0.0210(6) Uani 1 1 d . . . C51 C 0.8303(2) 0.6184(2) 0.34752(14) 0.0213(6) Uani 1 1 d . C . C52 C 0.7875(2) 0.5560(2) 0.39464(14) 0.0239(6) Uani 1 1 d . . . H52 H 0.7992 0.4892 0.3893 0.029 Uiso 1 1 calc R C . C53 C 0.7282(2) 0.5887(2) 0.44915(15) 0.0232(6) Uani 1 1 d . C . C54 C 0.7074(2) 0.6898(2) 0.45282(14) 0.0243(6) Uani 1 1 d . . . H54 H 0.6633 0.7157 0.4881 0.029 Uiso 1 1 calc R C . S8 S 0.89356(7) 0.78388(6) 0.30606(4) 0.02791(17) Uani 1 1 d . C . C55 C 1.0120(3) 0.7094(3) 0.35339(16) 0.0305(7) Uani 1 1 d . . . H55A H 1.0315 0.6351 0.3555 0.037 Uiso 1 1 calc R C . H55B H 1.0698 0.7297 0.3300 0.037 Uiso 1 1 calc R . . C56 C 0.9991(2) 0.7250(2) 0.42295(16) 0.0274(7) Uani 1 1 d . C . C57 C 1.0082(2) 0.8118(2) 0.43382(16) 0.0277(7) Uani 1 1 d . . . H57 H 1.0248 0.8580 0.3967 0.033 Uiso 1 1 calc R C . N4 N 0.9950(2) 0.8340(2) 0.49327(13) 0.0292(6) Uani 1 1 d . . . C58 C 0.9707(3) 0.7685(3) 0.54505(17) 0.0363(8) Uani 1 1 d . . . H58 H 0.9608 0.7831 0.5878 0.044 Uiso 1 1 calc R C . C59 C 0.9592(3) 0.6803(3) 0.53875(17) 0.0368(8) Uani 1 1 d . C . H59 H 0.9421 0.6355 0.5766 0.044 Uiso 1 1 calc R . . C60 C 0.9731(3) 0.6586(2) 0.47699(16) 0.0315(7) Uani 1 1 d . . . H60 H 0.9650 0.5990 0.4715 0.038 Uiso 1 1 calc R C . C61 C 0.6860(3) 0.5190(2) 0.50392(16) 0.0302(7) Uani 1 1 d . . . C62 C 0.7426(3) 0.4966(3) 0.56747(17) 0.0404(9) Uani 1 1 d . C . H62A H 0.7304 0.5617 0.5791 0.061 Uiso 1 1 calc R . . H62B H 0.8179 0.4602 0.5604 0.061 Uiso 1 1 calc R . . H62C H 0.7160 0.4534 0.6038 0.061 Uiso 1 1 calc R . . C63 C 0.7053(3) 0.4168(3) 0.48654(19) 0.0411(9) Uani 1 1 d . C . H63A H 0.6813 0.3729 0.5238 0.062 Uiso 1 1 calc R . . H63B H 0.7803 0.3817 0.4778 0.062 Uiso 1 1 calc R . . H63C H 0.6667 0.4304 0.4468 0.062 Uiso 1 1 calc R . . C64 C 0.5683(3) 0.5753(3) 0.5149(2) 0.0423(9) Uani 1 1 d . C . H64A H 0.5560 0.6373 0.5306 0.063 Uiso 1 1 calc R . . H64B H 0.5407 0.5294 0.5482 0.063 Uiso 1 1 calc R . . H64C H 0.5329 0.5952 0.4729 0.063 Uiso 1 1 calc R . . C65 C 0.3787(4) 0.3604(3) 0.2878(2) 0.0654(13) Uani 1 1 d . . . H65 H 0.4051 0.3335 0.2467 0.078 Uiso 1 1 calc R . . Cl1 Cl 0.45620(10) 0.42409(10) 0.29969(6) 0.0679(3) Uani 1 1 d . . . Cl2 Cl 0.38766(15) 0.25581(10) 0.35509(7) 0.0940(5) Uani 1 1 d . . . Cl3 Cl 0.24590(11) 0.44680(11) 0.27666(6) 0.0734(4) Uani 1 1 d . . . C66 C 0.1809(4) 0.3150(4) 0.1606(3) 0.0809(17) Uani 1 1 d . . . H66 H 0.2455 0.3096 0.1799 0.097 Uiso 1 1 calc R . . Cl4 Cl 0.21681(14) 0.26882(15) 0.08836(11) 0.1216(7) Uani 1 1 d . . . Cl5 Cl 0.09685(9) 0.44518(10) 0.14153(8) 0.0781(4) Uani 1 1 d . . . Cl6 Cl 0.12052(17) 0.24299(15) 0.21965(13) 0.1451(9) Uani 1 1 d . . . C15A C 0.9297(9) 0.8438(11) -0.0157(5) 0.058(3) Uani 0.454(19) 1 d PD C 2 H15D H 0.8570 0.8929 -0.0163 0.086 Uiso 0.454(19) 1 calc PR C 2 H15E H 0.9346 0.7870 -0.0348 0.086 Uiso 0.454(19) 1 calc PR C 2 H15F H 0.9745 0.8790 -0.0419 0.086 Uiso 0.454(19) 1 calc PR C 2 C14A C 0.9634(12) 0.8898(10) 0.0837(6) 0.058(3) Uani 0.454(19) 1 d PD C 2 H14D H 0.9831 0.8653 0.1304 0.086 Uiso 0.454(19) 1 calc PR C 2 H14E H 0.8925 0.9429 0.0801 0.086 Uiso 0.454(19) 1 calc PR C 2 H14F H 1.0126 0.9192 0.0573 0.086 Uiso 0.454(19) 1 calc PR C 2 C16A C 1.0777(8) 0.7191(8) 0.0582(7) 0.058(3) Uani 0.454(19) 1 d PD C 2 H16D H 1.1092 0.7062 0.1007 0.086 Uiso 0.454(19) 1 calc PR C 2 H16E H 1.1196 0.7447 0.0217 0.086 Uiso 0.454(19) 1 calc PR C 2 H16F H 1.0759 0.6547 0.0526 0.086 Uiso 0.454(19) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02947(17) 0.02598(16) 0.02187(15) -0.00371(12) -0.00067(12) -0.01466(14) Br1 0.0444(2) 0.0453(2) 0.02563(16) -0.00419(14) 0.00424(14) -0.02423(17) Cd2 0.02217(16) 0.03185(17) 0.02386(15) -0.01048(13) 0.00001(12) -0.01159(14) Br2 0.03523(19) 0.03975(19) 0.02474(16) -0.01040(14) -0.00030(13) -0.01490(15) S1 0.0259(4) 0.0225(4) 0.0263(4) -0.0085(3) -0.0036(3) -0.0046(3) C1 0.0221(15) 0.0222(14) 0.0218(14) -0.0095(11) -0.0009(11) -0.0060(12) C2 0.0211(15) 0.0232(14) 0.0250(14) -0.0106(12) 0.0039(11) -0.0101(12) C3 0.0213(15) 0.0263(15) 0.0238(14) -0.0092(12) -0.0015(12) -0.0085(13) C4 0.0262(16) 0.0268(15) 0.0258(15) -0.0076(12) 0.0010(12) -0.0123(13) C5 0.0223(15) 0.0277(15) 0.0300(16) -0.0126(13) 0.0064(12) -0.0125(13) C6 0.0166(14) 0.0287(16) 0.0323(16) -0.0134(13) -0.0009(12) -0.0080(13) S2 0.0297(4) 0.0328(4) 0.0250(4) -0.0071(3) 0.0010(3) -0.0175(4) C7 0.045(2) 0.0273(17) 0.0348(18) -0.0032(14) -0.0122(15) -0.0181(16) C8 0.0334(18) 0.0206(15) 0.0390(18) -0.0093(13) -0.0078(14) -0.0111(14) C9 0.0315(17) 0.0255(15) 0.0302(16) -0.0050(13) -0.0041(13) -0.0146(14) N1 0.0292(14) 0.0266(13) 0.0321(14) -0.0079(11) -0.0018(11) -0.0134(12) C10 0.0339(19) 0.058(2) 0.045(2) -0.0308(19) 0.0034(16) -0.0206(18) C11 0.034(2) 0.089(3) 0.068(3) -0.052(3) 0.0141(19) -0.029(2) C12 0.0315(19) 0.053(2) 0.060(2) -0.033(2) -0.0078(17) -0.0132(18) C13 0.0270(17) 0.0389(19) 0.0374(18) -0.0098(15) 0.0063(14) -0.0192(15) C14 0.045(3) 0.059(4) 0.069(4) -0.012(3) 0.016(3) -0.033(3) C15 0.045(3) 0.059(4) 0.069(4) -0.012(3) 0.016(3) -0.033(3) C16 0.045(3) 0.059(4) 0.069(4) -0.012(3) 0.016(3) -0.033(3) S3 0.0217(4) 0.0379(4) 0.0228(4) -0.0079(3) -0.0019(3) -0.0134(3) C17 0.0192(14) 0.0262(15) 0.0244(15) -0.0031(12) -0.0011(12) -0.0083(13) C18 0.0211(15) 0.0255(15) 0.0273(15) 0.0013(12) -0.0027(12) -0.0125(13) C19 0.0219(15) 0.0214(14) 0.0338(16) -0.0025(13) -0.0064(13) -0.0096(13) C20 0.0204(15) 0.0261(15) 0.0305(16) -0.0054(13) 0.0002(12) -0.0079(13) C21 0.0212(15) 0.0240(15) 0.0300(16) -0.0031(12) -0.0030(12) -0.0106(13) C22 0.0243(15) 0.0247(15) 0.0290(16) -0.0055(12) -0.0009(12) -0.0122(13) S4 0.0268(4) 0.0274(4) 0.0386(5) 0.0029(3) -0.0022(3) -0.0136(3) C23 0.0321(18) 0.0293(17) 0.0403(19) 0.0036(14) -0.0087(15) -0.0153(15) C24 0.0249(16) 0.0282(16) 0.0300(16) -0.0026(13) -0.0068(13) -0.0108(14) C25 0.0230(15) 0.0309(16) 0.0280(16) -0.0026(13) -0.0050(12) -0.0116(14) N2 0.0270(14) 0.0296(14) 0.0273(13) -0.0052(11) -0.0017(11) -0.0133(12) C26 0.0262(17) 0.0354(18) 0.0332(17) -0.0038(14) -0.0009(13) -0.0154(15) C27 0.0334(19) 0.042(2) 0.040(2) -0.0111(16) 0.0087(15) -0.0129(16) C28 0.040(2) 0.0316(18) 0.0399(19) -0.0080(15) -0.0034(16) -0.0138(16) C29 0.0270(17) 0.0282(16) 0.0368(18) -0.0057(14) 0.0051(14) -0.0161(14) C30 0.041(2) 0.047(2) 0.0367(19) -0.0024(16) 0.0036(16) -0.0259(18) C31 0.0243(17) 0.042(2) 0.049(2) -0.0128(17) 0.0021(15) -0.0174(16) C32 0.040(2) 0.0338(19) 0.063(3) -0.0159(18) 0.0177(18) -0.0258(17) S5 0.0220(4) 0.0208(4) 0.0441(5) -0.0064(3) -0.0060(3) -0.0069(3) C33 0.0235(15) 0.0194(14) 0.0320(16) -0.0065(12) -0.0051(13) -0.0063(12) C34 0.0256(16) 0.0195(14) 0.0304(16) -0.0073(12) 0.0035(12) -0.0112(13) C35 0.0276(16) 0.0177(13) 0.0228(14) -0.0058(11) -0.0022(12) -0.0073(12) C36 0.0263(16) 0.0218(14) 0.0292(16) -0.0076(12) -0.0041(12) -0.0106(13) C37 0.0243(15) 0.0165(13) 0.0280(15) -0.0042(12) -0.0007(12) -0.0078(12) C38 0.0259(16) 0.0194(14) 0.0308(16) -0.0042(12) -0.0039(13) -0.0082(13) S6 0.0304(4) 0.0247(4) 0.0364(4) -0.0076(3) 0.0068(3) -0.0141(3) C39 0.0291(18) 0.0292(17) 0.050(2) -0.0149(16) 0.0108(15) -0.0116(15) C40 0.0281(17) 0.0243(15) 0.0337(17) -0.0131(13) 0.0056(13) -0.0103(13) C41 0.0290(17) 0.0287(16) 0.0310(16) -0.0091(13) 0.0020(13) -0.0092(14) N3 0.0240(13) 0.0338(14) 0.0290(14) -0.0092(12) 0.0029(11) -0.0125(12) C42 0.0301(18) 0.0366(18) 0.0336(18) -0.0052(15) 0.0048(14) -0.0121(15) C43 0.0303(18) 0.043(2) 0.0369(19) 0.0007(16) -0.0003(15) -0.0062(16) C44 0.0219(16) 0.043(2) 0.043(2) -0.0105(16) 0.0016(14) -0.0064(15) C45 0.0277(16) 0.0248(15) 0.0289(16) -0.0022(13) -0.0034(13) -0.0143(13) C46 0.045(2) 0.0323(18) 0.042(2) -0.0081(15) 0.0008(16) -0.0236(17) C47 0.0297(18) 0.0383(19) 0.044(2) -0.0073(16) 0.0055(15) -0.0134(16) C48 0.046(2) 0.049(2) 0.039(2) 0.0068(17) -0.0093(17) -0.0310(19) S7 0.0360(4) 0.0192(3) 0.0233(4) -0.0054(3) -0.0031(3) -0.0112(3) C49 0.0244(15) 0.0164(13) 0.0239(14) -0.0030(11) -0.0055(12) -0.0077(12) C50 0.0222(15) 0.0196(14) 0.0217(14) -0.0030(11) -0.0060(11) -0.0080(12) C51 0.0200(14) 0.0233(14) 0.0208(14) -0.0062(11) -0.0044(11) -0.0066(12) C52 0.0258(16) 0.0208(14) 0.0267(15) -0.0043(12) -0.0063(12) -0.0095(13) C53 0.0215(15) 0.0223(14) 0.0280(15) -0.0026(12) -0.0052(12) -0.0112(12) C54 0.0251(15) 0.0218(14) 0.0240(15) -0.0028(12) -0.0024(12) -0.0078(13) S8 0.0381(4) 0.0255(4) 0.0235(4) -0.0043(3) 0.0012(3) -0.0170(3) C55 0.0292(17) 0.0343(17) 0.0370(18) -0.0179(15) 0.0084(14) -0.0181(15) C56 0.0200(15) 0.0313(17) 0.0347(17) -0.0121(14) -0.0015(13) -0.0105(13) C57 0.0254(16) 0.0308(16) 0.0320(17) -0.0109(13) 0.0025(13) -0.0146(14) N4 0.0290(14) 0.0334(15) 0.0313(14) -0.0127(12) 0.0000(11) -0.0151(12) C58 0.041(2) 0.0401(19) 0.0308(17) -0.0093(15) -0.0006(15) -0.0174(17) C59 0.044(2) 0.0356(19) 0.0317(18) -0.0024(15) -0.0020(15) -0.0197(17) C60 0.0339(18) 0.0261(16) 0.0384(18) -0.0067(14) -0.0042(15) -0.0150(15) C61 0.0289(17) 0.0262(16) 0.0358(17) -0.0052(14) 0.0030(14) -0.0130(14) C62 0.044(2) 0.0350(19) 0.0352(19) 0.0011(15) 0.0014(16) -0.0138(17) C63 0.047(2) 0.0270(17) 0.052(2) -0.0076(16) 0.0098(18) -0.0219(17) C64 0.0313(19) 0.040(2) 0.059(2) -0.0102(18) 0.0100(17) -0.0203(17) C65 0.096(4) 0.054(3) 0.039(2) -0.014(2) 0.006(2) -0.022(3) Cl1 0.0699(8) 0.0698(8) 0.0577(7) -0.0115(6) -0.0021(6) -0.0216(6) Cl2 0.1739(16) 0.0451(7) 0.0585(7) -0.0074(6) -0.0053(9) -0.0388(9) Cl3 0.0806(9) 0.0923(9) 0.0509(7) -0.0113(6) -0.0066(6) -0.0382(8) C66 0.048(3) 0.065(3) 0.121(5) -0.039(3) -0.023(3) 0.005(2) Cl4 0.0843(11) 0.1176(14) 0.1695(18) -0.0928(14) -0.0244(11) -0.0008(10) Cl5 0.0473(7) 0.0668(8) 0.1134(11) -0.0311(8) -0.0022(7) -0.0081(6) Cl6 0.1064(14) 0.0922(13) 0.195(2) 0.0117(14) -0.0211(15) -0.0173(11) C15A 0.048(4) 0.065(5) 0.065(4) -0.015(3) 0.024(3) -0.034(4) C14A 0.048(4) 0.065(5) 0.065(4) -0.015(3) 0.024(3) -0.034(4) C16A 0.048(4) 0.065(5) 0.065(4) -0.015(3) 0.024(3) -0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.382(3) 1_545 ? Cd1 N2 2.382(3) 2_675 ? Cd1 N1 2.472(3) 2_665 ? Cd1 N1 2.472(3) . ? Cd1 Br1 2.7198(3) . ? Cd1 Br1 2.7198(3) 2_665 ? Cd2 N3 2.406(3) . ? Cd2 N3 2.406(3) 2_576 ? Cd2 N4 2.473(3) 1_455 ? Cd2 N4 2.473(3) 2_676 ? Cd2 Br2 2.6986(3) 2_576 ? Cd2 Br2 2.6986(3) . ? S1 C51 1.780(3) . ? S1 C1 1.780(3) . ? C1 C6 1.397(4) . ? C1 C2 1.407(4) . ? C2 C3 1.398(4) . ? C2 S2 1.776(3) . ? C3 C4 1.399(4) . ? C3 S3 1.780(3) . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.391(4) . ? C5 C13 1.536(4) . ? C6 H6 0.9500 . ? S2 C7 1.825(3) . ? C7 C8 1.500(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.375(5) . ? C8 C9 1.381(5) . ? C9 N1 1.344(4) . ? C9 H9 0.9500 . ? N1 C10 1.337(4) . ? C10 C11 1.373(5) . ? C10 H10 0.9500 . ? C11 C12 1.380(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14A 1.524(9) . ? C13 C16A 1.527(9) . ? C13 C15 1.532(8) . ? C13 C16 1.539(8) . ? C13 C14 1.545(8) . ? C13 C15A 1.563(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S3 C17 1.784(3) . ? C17 C22 1.391(4) . ? C17 C18 1.397(4) . ? C18 C19 1.399(4) . ? C18 S4 1.771(3) . ? C19 C20 1.379(4) . ? C19 S5 1.791(3) . ? C20 C21 1.396(4) . ? C20 H20 0.9500 . ? C21 C22 1.388(4) . ? C21 C29 1.532(4) . ? C22 H22 0.9500 . ? S4 C23 1.809(3) . ? C23 C24 1.506(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.374(4) . ? C24 C28 1.397(5) . ? C25 N2 1.341(4) . ? C25 H25 0.9500 . ? N2 C26 1.340(4) . ? N2 Cd1 2.382(3) 1_565 ? C26 C27 1.377(5) . ? C26 H26 0.9500 . ? C27 C28 1.370(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C32 1.518(5) . ? C29 C31 1.530(5) . ? C29 C30 1.540(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S5 C33 1.781(3) . ? C33 C38 1.391(4) . ? C33 C34 1.399(4) . ? C34 C35 1.406(4) . ? C34 S6 1.781(3) . ? C35 C36 1.387(4) . ? C35 S7 1.785(3) . ? C36 C37 1.398(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 C45 1.535(4) . ? C38 H38 0.9500 . ? S6 C39 1.818(3) . ? C39 C40 1.498(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.383(5) . ? C40 C41 1.386(4) . ? C41 N3 1.340(4) . ? C41 H41 0.9500 . ? N3 C42 1.331(4) . ? C42 C43 1.380(5) . ? C42 H42 0.9500 . ? C43 C44 1.373(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.531(4) . ? C45 C48 1.532(4) . ? C45 C47 1.534(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S7 C49 1.783(3) . ? C49 C54 1.391(4) . ? C49 C50 1.401(4) . ? C50 C51 1.406(4) . ? C50 S8 1.775(3) . ? C51 C52 1.392(4) . ? C52 C53 1.387(4) . ? C52 H52 0.9500 . ? C53 C54 1.398(4) . ? C53 C61 1.532(4) . ? C54 H54 0.9500 . ? S8 C55 1.822(3) . ? C55 C56 1.503(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C60 1.387(4) . ? C56 C57 1.388(4) . ? C57 N4 1.333(4) . ? C57 H57 0.9500 . ? N4 C58 1.340(4) . ? N4 Cd2 2.473(3) 1_655 ? C58 C59 1.390(5) . ? C58 H58 0.9500 . ? C59 C60 1.376(5) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.526(5) . ? C61 C63 1.529(5) . ? C61 C64 1.531(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 Cl1 1.746(5) . ? C65 Cl2 1.748(4) . ? C65 Cl3 1.781(5) . ? C65 H65 1.0000 . ? C66 Cl4 1.741(6) . ? C66 Cl6 1.747(6) . ? C66 Cl5 1.752(5) . ? C66 H66 1.0000 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.0 1_545 2_675 ? N2 Cd1 N1 85.03(9) 1_545 2_665 ? N2 Cd1 N1 94.97(9) 2_675 2_665 ? N2 Cd1 N1 94.97(9) 1_545 . ? N2 Cd1 N1 85.03(9) 2_675 . ? N1 Cd1 N1 180.0 2_665 . ? N2 Cd1 Br1 89.96(6) 1_545 . ? N2 Cd1 Br1 90.04(6) 2_675 . ? N1 Cd1 Br1 89.99(6) 2_665 . ? N1 Cd1 Br1 90.01(6) . . ? N2 Cd1 Br1 90.04(6) 1_545 2_665 ? N2 Cd1 Br1 89.96(6) 2_675 2_665 ? N1 Cd1 Br1 90.01(6) 2_665 2_665 ? N1 Cd1 Br1 89.99(6) . 2_665 ? Br1 Cd1 Br1 179.999(1) . 2_665 ? N3 Cd2 N3 179.999(2) . 2_576 ? N3 Cd2 N4 91.73(9) . 1_455 ? N3 Cd2 N4 88.26(9) 2_576 1_455 ? N3 Cd2 N4 88.27(9) . 2_676 ? N3 Cd2 N4 91.74(9) 2_576 2_676 ? N4 Cd2 N4 180.0 1_455 2_676 ? N3 Cd2 Br2 91.04(6) . 2_576 ? N3 Cd2 Br2 88.96(6) 2_576 2_576 ? N4 Cd2 Br2 88.22(6) 1_455 2_576 ? N4 Cd2 Br2 91.78(6) 2_676 2_576 ? N3 Cd2 Br2 88.96(6) . . ? N3 Cd2 Br2 91.04(6) 2_576 . ? N4 Cd2 Br2 91.78(6) 1_455 . ? N4 Cd2 Br2 88.22(6) 2_676 . ? Br2 Cd2 Br2 179.999(15) 2_576 . ? C51 S1 C1 103.94(13) . . ? C6 C1 C2 120.3(3) . . ? C6 C1 S1 116.3(2) . . ? C2 C1 S1 123.1(2) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 S2 119.8(2) . . ? C1 C2 S2 122.6(2) . . ? C2 C3 C4 120.8(3) . . ? C2 C3 S3 122.9(2) . . ? C4 C3 S3 116.1(2) . . ? C5 C4 C3 121.9(3) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C13 122.3(3) . . ? C6 C5 C13 120.2(3) . . ? C5 C6 C1 122.1(3) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C2 S2 C7 100.67(15) . . ? C8 C7 S2 113.8(2) . . ? C8 C7 H7A 108.8 . . ? S2 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? S2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C12 C8 C9 117.4(3) . . ? C12 C8 C7 120.6(3) . . ? C9 C8 C7 122.0(3) . . ? N1 C9 C8 123.9(3) . . ? N1 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C10 N1 C9 116.9(3) . . ? C10 N1 Cd1 119.9(2) . . ? C9 N1 Cd1 123.2(2) . . ? N1 C10 C11 123.4(3) . . ? N1 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C8 C12 C11 119.9(3) . . ? C8 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14A C13 C16A 110.6(5) . . ? C14A C13 C15 85.4(5) . . ? C16A C13 C15 125.2(6) . . ? C14A C13 C5 107.1(4) . . ? C16A C13 C5 111.2(5) . . ? C15 C13 C5 113.0(4) . . ? C14A C13 C16 132.7(5) . . ? C15 C13 C16 108.8(5) . . ? C5 C13 C16 107.7(4) . . ? C15 C13 C14 109.0(5) . . ? C5 C13 C14 109.4(4) . . ? C16 C13 C14 108.8(5) . . ? C14A C13 C15A 107.3(6) . . ? C16A C13 C15A 108.8(5) . . ? C5 C13 C15A 111.7(5) . . ? C14 C13 C15A 127.5(6) . . ? C3 S3 C17 104.64(14) . . ? C22 C17 C18 120.4(3) . . ? C22 C17 S3 116.4(2) . . ? C18 C17 S3 123.0(2) . . ? C17 C18 C19 118.0(3) . . ? C17 C18 S4 120.3(2) . . ? C19 C18 S4 121.7(2) . . ? C20 C19 C18 120.6(3) . . ? C20 C19 S5 115.8(2) . . ? C18 C19 S5 123.5(2) . . ? C19 C20 C21 121.7(3) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 117.3(3) . . ? C22 C21 C29 123.1(3) . . ? C20 C21 C29 119.5(3) . . ? C21 C22 C17 121.6(3) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C18 S4 C23 97.86(15) . . ? C24 C23 S4 107.4(2) . . ? C24 C23 H23A 110.2 . . ? S4 C23 H23A 110.2 . . ? C24 C23 H23B 110.2 . . ? S4 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? C25 C24 C28 117.8(3) . . ? C25 C24 C23 120.2(3) . . ? C28 C24 C23 122.0(3) . . ? N2 C25 C24 123.8(3) . . ? N2 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C26 N2 C25 117.5(3) . . ? C26 N2 Cd1 123.3(2) . 1_565 ? C25 N2 Cd1 119.1(2) . 1_565 ? N2 C26 C27 122.5(3) . . ? N2 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C24 118.8(3) . . ? C27 C28 H28 120.6 . . ? C24 C28 H28 120.6 . . ? C32 C29 C31 109.7(3) . . ? C32 C29 C21 112.0(3) . . ? C31 C29 C21 108.3(3) . . ? C32 C29 C30 108.5(3) . . ? C31 C29 C30 109.5(3) . . ? C21 C29 C30 108.8(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 S5 C19 103.76(14) . . ? C38 C33 C34 120.5(3) . . ? C38 C33 S5 116.7(2) . . ? C34 C33 S5 122.8(2) . . ? C33 C34 C35 117.9(3) . . ? C33 C34 S6 121.5(2) . . ? C35 C34 S6 120.7(2) . . ? C36 C35 C34 120.4(3) . . ? C36 C35 S7 117.2(2) . . ? C34 C35 S7 122.2(2) . . ? C35 C36 C37 122.1(3) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C38 C37 C36 116.9(3) . . ? C38 C37 C45 122.6(3) . . ? C36 C37 C45 120.5(3) . . ? C37 C38 C33 122.3(3) . . ? C37 C38 H38 118.9 . . ? C33 C38 H38 118.9 . . ? C34 S6 C39 99.99(14) . . ? C40 C39 S6 108.6(2) . . ? C40 C39 H39A 110.0 . . ? S6 C39 H39A 110.0 . . ? C40 C39 H39B 110.0 . . ? S6 C39 H39B 110.0 . . ? H39A C39 H39B 108.3 . . ? C44 C40 C41 117.4(3) . . ? C44 C40 C39 121.9(3) . . ? C41 C40 C39 120.7(3) . . ? N3 C41 C40 123.7(3) . . ? N3 C41 H41 118.1 . . ? C40 C41 H41 118.1 . . ? C42 N3 C41 117.7(3) . . ? C42 N3 Cd2 120.8(2) . . ? C41 N3 Cd2 121.1(2) . . ? N3 C42 C43 122.4(3) . . ? N3 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C44 C43 C42 119.3(3) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C40 119.4(3) . . ? C43 C44 H44 120.3 . . ? C40 C44 H44 120.3 . . ? C46 C45 C48 109.3(3) . . ? C46 C45 C47 108.7(3) . . ? C48 C45 C47 108.2(3) . . ? C46 C45 C37 109.1(3) . . ? C48 C45 C37 112.1(3) . . ? C47 C45 C37 109.4(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 S7 C35 103.65(13) . . ? C54 C49 C50 120.0(3) . . ? C54 C49 S7 116.0(2) . . ? C50 C49 S7 123.7(2) . . ? C49 C50 C51 118.0(3) . . ? C49 C50 S8 121.4(2) . . ? C51 C50 S8 120.2(2) . . ? C52 C51 C50 120.5(3) . . ? C52 C51 S1 115.8(2) . . ? C50 C51 S1 123.5(2) . . ? C53 C52 C51 121.8(3) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 117.1(3) . . ? C52 C53 C61 122.8(3) . . ? C54 C53 C61 120.1(3) . . ? C49 C54 C53 122.2(3) . . ? C49 C54 H54 118.9 . . ? C53 C54 H54 118.9 . . ? C50 S8 C55 96.43(14) . . ? C56 C55 S8 112.7(2) . . ? C56 C55 H55A 109.1 . . ? S8 C55 H55A 109.1 . . ? C56 C55 H55B 109.1 . . ? S8 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C60 C56 C57 118.0(3) . . ? C60 C56 C55 122.5(3) . . ? C57 C56 C55 119.4(3) . . ? N4 C57 C56 123.9(3) . . ? N4 C57 H57 118.1 . . ? C56 C57 H57 118.1 . . ? C57 N4 C58 117.4(3) . . ? C57 N4 Cd2 118.5(2) . 1_655 ? C58 N4 Cd2 123.8(2) . 1_655 ? N4 C58 C59 122.7(3) . . ? N4 C58 H58 118.7 . . ? C59 C58 H58 118.7 . . ? C60 C59 C58 119.1(3) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C56 118.9(3) . . ? C59 C60 H60 120.5 . . ? C56 C60 H60 120.5 . . ? C62 C61 C63 109.0(3) . . ? C62 C61 C64 109.7(3) . . ? C63 C61 C64 109.1(3) . . ? C62 C61 C53 107.6(3) . . ? C63 C61 C53 112.0(3) . . ? C64 C61 C53 109.5(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Cl1 C65 Cl2 110.5(3) . . ? Cl1 C65 Cl3 110.8(2) . . ? Cl2 C65 Cl3 110.2(3) . . ? Cl1 C65 H65 108.4 . . ? Cl2 C65 H65 108.4 . . ? Cl3 C65 H65 108.4 . . ? Cl4 C66 Cl6 111.5(3) . . ? Cl4 C66 Cl5 109.9(3) . . ? Cl6 C66 Cl5 109.9(3) . . ? Cl4 C66 H66 108.5 . . ? Cl6 C66 H66 108.5 . . ? Cl5 C66 H66 108.5 . . ? H15D C15A H15E 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? H14D C14A H14E 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? H16D C16A H16E 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.545 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 970401' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2393a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C128 H136 Br2 Co N8 S16,2(C H4 O), H2 O' _chemical_formula_sum 'C130 H146 Br2 Co N8 O3 S16' _chemical_formula_weight 2600.26 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' Br Br -0.2901 2.4595 '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' 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 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 28.1970(8) _cell_length_b 15.6401(4) _cell_length_c 15.4989(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.242(2) _cell_angle_gamma 90.00 _cell_volume 6726.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9230 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.08 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2718 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9412 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 102470 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 30.05 _reflns_number_total 19261 _reflns_number_gt 13295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1018P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.058(7) _refine_ls_number_reflns 19261 _refine_ls_number_parameters 734 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _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 Co1 Co 1.0000 0.71548(5) 1.0000 0.02578(18) Uani 1 2 d S . . Br1 Br 0.982220(17) 0.72907(3) 0.82568(3) 0.03893(13) Uani 1 1 d . . . S1 S 0.79011(4) 0.86866(7) 0.60762(8) 0.0307(2) Uani 1 1 d . . . C1 C 0.73908(14) 0.8552(3) 0.6601(3) 0.0237(8) Uani 1 1 d . . . C2 C 0.73987(14) 0.8694(2) 0.7492(3) 0.0214(8) Uani 1 1 d . . . C3 C 0.69827(14) 0.8469(3) 0.7825(3) 0.0228(8) Uani 1 1 d . . . C4 C 0.65949(15) 0.8083(3) 0.7306(3) 0.0272(9) Uani 1 1 d . . . H4 H 0.6324 0.7922 0.7556 0.033 Uiso 1 1 calc R . . C5 C 0.65930(16) 0.7924(3) 0.6417(3) 0.0272(9) Uani 1 1 d . . . C6 C 0.69950(16) 0.8178(3) 0.6079(3) 0.0298(9) Uani 1 1 d . . . H6 H 0.6999 0.8094 0.5473 0.036 Uiso 1 1 calc R . . S2 S 0.79121(4) 0.91603(7) 0.81627(7) 0.0275(2) Uani 1 1 d . . . C7 C 0.81478(18) 0.8239(3) 0.8818(4) 0.0413(12) Uani 1 1 d . . . H7A H 0.7912 0.8048 0.9181 0.050 Uiso 1 1 calc R . . H7B H 0.8205 0.7761 0.8430 0.050 Uiso 1 1 calc R . . C8 C 0.86159(15) 0.8492(3) 0.9401(3) 0.0297(9) Uani 1 1 d . . . C9 C 0.90055(15) 0.7939(3) 0.9442(3) 0.0289(9) Uani 1 1 d . . . H9 H 0.8971 0.7450 0.9072 0.035 Uiso 1 1 calc R . . N1 N 0.94317(13) 0.8068(2) 0.9985(3) 0.0304(8) Uani 1 1 d . . . C10 C 0.94772(17) 0.8782(3) 1.0463(3) 0.0375(11) Uani 1 1 d . . . H10 H 0.9774 0.8886 1.0845 0.045 Uiso 1 1 calc R . . C11 C 0.9117(2) 0.9370(4) 1.0428(4) 0.0493(14) Uani 1 1 d . . . H11 H 0.9168 0.9876 1.0771 0.059 Uiso 1 1 calc R . . C12 C 0.86755(18) 0.9225(3) 0.9891(4) 0.0447(13) Uani 1 1 d . . . H12 H 0.8420 0.9625 0.9864 0.054 Uiso 1 1 calc R . . C13 C 0.61597(17) 0.7491(3) 0.5820(3) 0.0402(12) Uani 1 1 d . . . C14 C 0.5721(3) 0.7450(8) 0.6241(5) 0.122(5) Uani 1 1 d . . . H14A H 0.5653 0.8020 0.6452 0.184 Uiso 1 1 calc R . . H14B H 0.5779 0.7051 0.6736 0.184 Uiso 1 1 calc R . . H14C H 0.5445 0.7253 0.5810 0.184 Uiso 1 1 calc R . . C15 C 0.6310(3) 0.6566(4) 0.5637(5) 0.076(2) Uani 1 1 d . . . H15A H 0.6455 0.6292 0.6190 0.114 Uiso 1 1 calc R . . H15B H 0.6544 0.6578 0.5240 0.114 Uiso 1 1 calc R . . H15C H 0.6025 0.6241 0.5365 0.114 Uiso 1 1 calc R . . C16 C 0.6042(2) 0.7923(5) 0.4934(4) 0.0578(16) Uani 1 1 d . . . H16A H 0.5740 0.7690 0.4608 0.087 Uiso 1 1 calc R . . H16B H 0.6302 0.7818 0.4605 0.087 Uiso 1 1 calc R . . H16C H 0.6007 0.8539 0.5016 0.087 Uiso 1 1 calc R . . S3 S 0.69439(4) 0.85070(7) 0.89587(7) 0.0282(2) Uani 1 1 d . . . C17 C 0.70822(15) 0.9544(3) 0.9377(3) 0.0256(9) Uani 1 1 d . . . C18 C 0.68940(14) 1.0316(3) 0.8979(2) 0.0229(8) Uani 1 1 d . . . C19 C 0.70180(15) 1.1075(3) 0.9431(3) 0.0251(9) Uani 1 1 d . . . C20 C 0.72715(16) 1.1067(3) 1.0300(3) 0.0292(9) Uani 1 1 d . . . H20 H 0.7342 1.1593 1.0602 0.035 Uiso 1 1 calc R . . C21 C 0.74199(16) 1.0310(3) 1.0725(3) 0.0276(9) Uani 1 1 d . . . C22 C 0.73464(16) 0.9552(3) 1.0231(3) 0.0287(9) Uani 1 1 d . . . H22 H 0.7480 0.9032 1.0483 0.034 Uiso 1 1 calc R . . S4 S 0.65012(4) 1.03419(8) 0.79508(6) 0.0296(2) Uani 1 1 d . . . C23 C 0.59754(17) 0.9795(3) 0.8226(3) 0.0351(10) Uani 1 1 d . . . H23A H 0.5694 0.9912 0.7759 0.042 Uiso 1 1 calc R . . H23B H 0.6035 0.9171 0.8233 0.042 Uiso 1 1 calc R . . C24 C 0.91500(16) 0.5055(3) 1.0899(3) 0.0319(10) Uani 1 1 d . . . C25 C 0.93512(16) 0.5840(3) 1.0789(3) 0.0316(10) Uani 1 1 d . . . H25 H 0.9396 0.6225 1.1271 0.038 Uiso 1 1 calc R . . N2 N 0.94876(13) 0.6095(2) 1.0046(2) 0.0289(8) Uani 1 1 d . . . C26 C 0.9396(2) 0.5552(4) 0.9363(3) 0.0464(13) Uani 1 1 d . . . H26 H 0.9487 0.5713 0.8824 0.056 Uiso 1 1 calc R . . C27 C 0.9177(3) 0.4774(4) 0.9414(4) 0.0624(19) Uani 1 1 d . . . H27 H 0.9111 0.4416 0.8912 0.075 Uiso 1 1 calc R . . C28 C 0.9058(2) 0.4522(4) 1.0171(4) 0.0514(14) Uani 1 1 d . . . H28 H 0.8910 0.3981 1.0211 0.062 Uiso 1 1 calc R . . C29 C 0.76686(18) 1.0277(3) 1.1693(3) 0.0352(11) Uani 1 1 d . . . C30 C 0.8187(3) 0.9977(6) 1.1753(4) 0.072(2) Uani 1 1 d . . . H30A H 0.8320 0.9825 1.2362 0.108 Uiso 1 1 calc R . . H30B H 0.8380 1.0438 1.1561 0.108 Uiso 1 1 calc R . . H30C H 0.8195 0.9476 1.1376 0.108 Uiso 1 1 calc R . . C31 C 0.7427(3) 0.9609(4) 1.2197(4) 0.0617(18) Uani 1 1 d . . . H31A H 0.7083 0.9742 1.2141 0.092 Uiso 1 1 calc R . . H31B H 0.7578 0.9620 1.2817 0.092 Uiso 1 1 calc R . . H31C H 0.7465 0.9040 1.1954 0.092 Uiso 1 1 calc R . . C32 C 0.7660(3) 1.1124(4) 1.2146(4) 0.072(2) Uani 1 1 d . . . H32A H 0.7325 1.1303 1.2124 0.109 Uiso 1 1 calc R . . H32B H 0.7828 1.1551 1.1850 0.109 Uiso 1 1 calc R . . H32C H 0.7820 1.1069 1.2758 0.109 Uiso 1 1 calc R . . S5 S 0.68090(4) 1.21024(7) 0.90501(7) 0.0331(3) Uani 1 1 d . . . C33 C 0.68980(15) 1.2224(3) 0.7948(2) 0.0268(8) Uani 1 1 d . . . C34 C 0.73300(15) 1.2068(3) 0.7647(3) 0.0242(8) Uani 1 1 d . . . C35 C 0.73534(14) 1.2307(3) 0.6783(3) 0.0257(8) Uani 1 1 d . . . C36 C 0.69605(16) 1.2694(3) 0.6248(3) 0.0301(9) Uani 1 1 d . . . H36 H 0.6985 1.2848 0.5664 0.036 Uiso 1 1 calc R . . C37 C 0.65330(16) 1.2860(3) 0.6556(3) 0.0286(9) Uani 1 1 d . . . C38 C 0.65061(16) 1.2614(3) 0.7401(3) 0.0306(9) Uani 1 1 d . . . H38 H 0.6216 1.2711 0.7618 0.037 Uiso 1 1 calc R . . S6 S 0.78267(4) 1.15692(7) 0.83286(7) 0.0297(2) Uani 1 1 d . . . C39 C 0.8153(2) 1.2485(4) 0.8788(4) 0.0628(13) Uani 1 1 d . . . H39A H 0.8253 1.2826 0.8313 0.075 Uiso 1 1 calc R . . H39B H 0.7942 1.2847 0.9082 0.075 Uiso 1 1 calc R . . C40 C 0.8584(2) 1.2237(4) 0.9428(4) 0.0628(13) Uani 1 1 d . . . C41 C 0.8562(2) 1.1806(4) 1.0209(4) 0.0602(16) Uani 1 1 d . . . H41 H 0.8260 1.1625 1.0333 0.072 Uiso 1 1 calc R . . C43 C 0.8980(3) 1.1641(4) 1.0805(4) 0.0644(18) Uani 1 1 d . . . H43 H 0.8978 1.1354 1.1345 0.077 Uiso 1 1 calc R . . C42 C 0.9389(3) 1.1915(5) 1.0565(7) 0.098(3) Uani 1 1 d . . . H42 H 0.9680 1.1832 1.0972 0.117 Uiso 1 1 calc R . . N3 N 0.9426(3) 1.2297(6) 0.9796(7) 0.117(3) Uani 1 1 d . . . C44 C 0.9023(3) 1.2454(5) 0.9265(6) 0.075(2) Uani 1 1 d . . . H44 H 0.9039 1.2739 0.8730 0.090 Uiso 1 1 calc R . . C45 C 0.61108(19) 1.3293(4) 0.5953(3) 0.0419(12) Uani 1 1 d . . . C46 C 0.5992(2) 1.2798(4) 0.5077(4) 0.0580(16) Uani 1 1 d . . . H46A H 0.6288 1.2708 0.4842 0.087 Uiso 1 1 calc R . . H46B H 0.5763 1.3129 0.4657 0.087 Uiso 1 1 calc R . . H46C H 0.5850 1.2244 0.5179 0.087 Uiso 1 1 calc R . . C47 C 0.5664(3) 1.3352(7) 0.6347(5) 0.101(4) Uani 1 1 d . . . H47A H 0.5545 1.2775 0.6434 0.152 Uiso 1 1 calc R . . H47B H 0.5416 1.3672 0.5953 0.152 Uiso 1 1 calc R . . H47C H 0.5738 1.3646 0.6914 0.152 Uiso 1 1 calc R . . C48 C 0.6274(3) 1.4211(4) 0.5721(4) 0.071(2) Uani 1 1 d . . . H48A H 0.6349 1.4554 0.6257 0.106 Uiso 1 1 calc R . . H48B H 0.6014 1.4486 0.5311 0.106 Uiso 1 1 calc R . . H48C H 0.6562 1.4167 0.5449 0.106 Uiso 1 1 calc R . . S7 S 0.78900(4) 1.22728(7) 0.63302(7) 0.0308(2) Uani 1 1 d . . . C49 C 0.81477(15) 1.1239(3) 0.6491(3) 0.0249(8) Uani 1 1 d . . . C50 C 0.79000(13) 1.0478(3) 0.6236(2) 0.0228(8) Uani 1 1 d . . . C51 C 0.81590(15) 0.9702(3) 0.6369(3) 0.0255(9) Uani 1 1 d . . . C52 C 0.86557(15) 0.9709(3) 0.6689(3) 0.0271(9) Uani 1 1 d . . . H52 H 0.8825 0.9182 0.6765 0.032 Uiso 1 1 calc R . . C53 C 0.89059(14) 1.0465(3) 0.6897(3) 0.0261(8) Uani 1 1 d . . . C54 C 0.86450(15) 1.1226(3) 0.6816(3) 0.0276(9) Uani 1 1 d . . . H54 H 0.8808 1.1749 0.6983 0.033 Uiso 1 1 calc R . . S8 S 0.72843(4) 1.04939(8) 0.57368(7) 0.0300(2) Uani 1 1 d . . . C55 C 0.73624(18) 1.0388(5) 0.4595(3) 0.0531(15) Uani 1 1 d . . . H55A H 0.7587 1.0832 0.4452 0.064 Uiso 1 1 calc R . . H55B H 0.7498 0.9819 0.4497 0.064 Uiso 1 1 calc R . . C56 C 0.68812(17) 1.0492(4) 0.4031(3) 0.0381(11) Uani 1 1 d . . . C57 C 0.6608(2) 0.9787(4) 0.3756(4) 0.0447(12) Uani 1 1 d . . . H57 H 0.6739 0.9240 0.3926 0.054 Uiso 1 1 calc R . . N4 N 0.61654(18) 0.9822(4) 0.3261(3) 0.0589(14) Uani 1 1 d . . . C58 C 0.5988(2) 1.0602(5) 0.3047(4) 0.0603(17) Uani 1 1 d . . . H58 H 0.5668 1.0643 0.2731 0.072 Uiso 1 1 calc R . . C59 C 0.6230(3) 1.1320(5) 0.3248(4) 0.069(2) Uani 1 1 d . . . H59 H 0.6098 1.1854 0.3035 0.083 Uiso 1 1 calc R . . C60 C 0.6683(3) 1.1278(4) 0.3777(4) 0.0559(15) Uani 1 1 d . . . H60 H 0.6854 1.1788 0.3962 0.067 Uiso 1 1 calc R . . C61 C 0.94511(15) 1.0454(3) 0.7280(3) 0.0350(10) Uani 1 1 d . . . C62 C 0.9492(3) 1.0305(7) 0.8266(5) 0.098(3) Uani 1 1 d . . . H62A H 0.9395 0.9718 0.8370 0.147 Uiso 1 1 calc R . . H62B H 0.9281 1.0707 0.8503 0.147 Uiso 1 1 calc R . . H62C H 0.9826 1.0396 0.8557 0.147 Uiso 1 1 calc R . . C63 C 0.9696(2) 0.9738(7) 0.6897(9) 0.137(5) Uani 1 1 d . . . H63A H 1.0046 0.9814 0.7044 0.206 Uiso 1 1 calc R . . H63B H 0.9596 0.9735 0.6258 0.206 Uiso 1 1 calc R . . H63C H 0.9607 0.9193 0.7137 0.206 Uiso 1 1 calc R . . C64 C 0.9683(2) 1.1295(5) 0.7174(6) 0.085(3) Uani 1 1 d . . . H64A H 1.0031 1.1252 0.7392 0.127 Uiso 1 1 calc R . . H64B H 0.9545 1.1732 0.7509 0.127 Uiso 1 1 calc R . . H64C H 0.9627 1.1454 0.6553 0.127 Uiso 1 1 calc R . . O1 O 0.93290(16) 0.3394(3) 0.7530(3) 0.0690(12) Uani 1 1 d D . . H1 H 0.9181 0.3650 0.7087 0.104 Uiso 1 1 calc R . . C65 C 0.9819(2) 0.3629(5) 0.7672(8) 0.110(4) Uani 1 1 d D . . H65A H 0.9846 0.4243 0.7567 0.165 Uiso 1 1 calc R . . H65B H 0.9984 0.3310 0.7269 0.165 Uiso 1 1 calc R . . H65C H 0.9967 0.3497 0.8278 0.165 Uiso 1 1 calc R . . O2 O 0.5923(4) 0.0335(7) 0.5666(6) 0.079(3) Uani 0.50 1 d P . . 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 Co1 0.0228(3) 0.0241(4) 0.0291(4) 0.000 0.0013(3) 0.000 Br1 0.0421(2) 0.0400(3) 0.0321(2) 0.0018(2) -0.00065(18) -0.0010(2) S1 0.0302(5) 0.0285(6) 0.0368(6) -0.0146(5) 0.0150(4) -0.0055(4) C1 0.0236(18) 0.023(2) 0.025(2) -0.0029(17) 0.0068(15) 0.0021(15) C2 0.0240(18) 0.0163(19) 0.0221(19) -0.0021(16) -0.0010(15) -0.0002(15) C3 0.029(2) 0.0184(19) 0.0201(18) -0.0015(16) 0.0031(15) -0.0032(15) C4 0.028(2) 0.029(2) 0.025(2) -0.0022(18) 0.0057(17) -0.0054(17) C5 0.030(2) 0.030(2) 0.0213(19) -0.0076(17) 0.0023(16) -0.0033(17) C6 0.036(2) 0.031(2) 0.023(2) -0.0088(18) 0.0081(18) -0.0062(18) S2 0.0307(5) 0.0243(5) 0.0247(5) 0.0023(4) -0.0028(4) -0.0060(4) C7 0.034(2) 0.028(2) 0.056(3) 0.008(2) -0.009(2) 0.0033(19) C8 0.027(2) 0.030(2) 0.031(2) 0.0040(19) 0.0002(17) 0.0002(17) C9 0.026(2) 0.026(2) 0.032(2) -0.0051(19) -0.0013(17) -0.0016(17) N1 0.0278(18) 0.0286(19) 0.032(2) -0.0023(16) -0.0011(15) 0.0051(15) C10 0.032(2) 0.039(3) 0.036(3) -0.016(2) -0.0095(19) 0.004(2) C11 0.046(3) 0.043(3) 0.051(3) -0.020(3) -0.011(2) 0.012(2) C12 0.039(3) 0.037(3) 0.053(3) -0.008(3) -0.006(2) 0.014(2) C13 0.033(2) 0.049(3) 0.037(2) -0.018(2) 0.0019(19) -0.016(2) C14 0.057(4) 0.254(14) 0.063(4) -0.063(6) 0.030(3) -0.093(6) C15 0.084(5) 0.044(3) 0.082(5) -0.006(3) -0.034(4) -0.021(3) C16 0.042(3) 0.073(4) 0.052(3) -0.010(3) -0.010(3) -0.012(3) S3 0.0392(6) 0.0257(5) 0.0204(5) 0.0007(4) 0.0075(4) -0.0061(4) C17 0.030(2) 0.029(2) 0.0188(19) -0.0008(17) 0.0063(16) -0.0055(17) C18 0.0251(18) 0.030(2) 0.0146(17) -0.0008(17) 0.0071(14) 0.0017(16) C19 0.036(2) 0.025(2) 0.0162(18) 0.0039(16) 0.0106(16) 0.0050(17) C20 0.042(2) 0.027(2) 0.0198(19) -0.0036(18) 0.0059(17) 0.0013(18) C21 0.037(2) 0.028(2) 0.0173(18) 0.0007(18) 0.0039(16) 0.0011(18) C22 0.039(2) 0.030(2) 0.0153(19) 0.0032(17) 0.0010(16) -0.0011(18) S4 0.0348(5) 0.0369(6) 0.0167(4) 0.0007(5) 0.0033(4) 0.0014(5) C23 0.036(2) 0.035(3) 0.035(2) -0.009(2) 0.0058(19) 0.003(2) C24 0.030(2) 0.030(2) 0.036(2) -0.003(2) 0.0074(18) 0.0023(18) C25 0.031(2) 0.033(2) 0.031(2) -0.003(2) 0.0042(18) -0.0008(18) N2 0.0289(18) 0.030(2) 0.0280(19) -0.0012(16) 0.0059(15) -0.0021(15) C26 0.057(3) 0.051(3) 0.036(3) -0.021(2) 0.022(2) -0.023(3) C27 0.100(5) 0.047(3) 0.053(4) -0.021(3) 0.047(4) -0.036(3) C28 0.060(3) 0.034(3) 0.068(4) -0.011(3) 0.030(3) -0.015(2) C29 0.053(3) 0.034(3) 0.0169(19) 0.0008(19) -0.0002(18) -0.004(2) C30 0.073(4) 0.104(6) 0.031(3) 0.007(3) -0.011(3) 0.007(4) C31 0.118(6) 0.042(3) 0.026(3) 0.003(2) 0.014(3) -0.020(3) C32 0.143(7) 0.040(3) 0.025(3) -0.004(2) -0.013(3) 0.004(4) S5 0.0497(6) 0.0305(6) 0.0205(5) 0.0001(4) 0.0104(4) 0.0162(5) C33 0.041(2) 0.020(2) 0.0194(18) 0.0007(17) 0.0046(16) 0.0063(18) C34 0.0314(19) 0.0169(19) 0.0227(19) 0.0023(16) 0.0007(16) 0.0024(15) C35 0.0278(18) 0.022(2) 0.0275(19) 0.0054(18) 0.0067(15) 0.0018(17) C36 0.040(2) 0.023(2) 0.026(2) 0.0066(18) 0.0049(18) 0.0088(18) C37 0.035(2) 0.025(2) 0.026(2) -0.0003(18) 0.0058(17) 0.0097(17) C38 0.032(2) 0.026(2) 0.035(2) -0.0010(19) 0.0090(18) 0.0104(17) S6 0.0356(6) 0.0249(5) 0.0276(5) 0.0031(4) 0.0029(4) 0.0086(4) C39 0.077(3) 0.032(2) 0.065(3) -0.006(2) -0.029(2) 0.013(2) C40 0.077(3) 0.032(2) 0.065(3) -0.006(2) -0.029(2) 0.013(2) C41 0.065(4) 0.046(3) 0.068(4) -0.008(3) 0.006(3) 0.014(3) C43 0.089(5) 0.049(4) 0.048(4) 0.011(3) -0.006(3) 0.018(3) C42 0.069(5) 0.064(5) 0.135(8) -0.004(5) -0.050(5) 0.011(4) N3 0.086(5) 0.098(6) 0.159(8) 0.034(6) -0.001(5) -0.011(5) C44 0.079(5) 0.051(4) 0.094(5) -0.005(4) 0.016(4) -0.006(4) C45 0.046(3) 0.047(3) 0.033(2) 0.007(2) 0.007(2) 0.020(2) C46 0.046(3) 0.070(4) 0.050(3) -0.012(3) -0.012(3) 0.007(3) C47 0.062(4) 0.195(10) 0.053(4) 0.044(5) 0.025(3) 0.077(6) C48 0.104(6) 0.040(3) 0.057(4) 0.004(3) -0.019(4) 0.023(3) S7 0.0333(5) 0.0254(5) 0.0365(6) 0.0122(5) 0.0137(4) 0.0069(5) C49 0.030(2) 0.027(2) 0.0195(19) 0.0054(17) 0.0093(16) 0.0017(17) C50 0.0217(17) 0.033(2) 0.0149(17) -0.0006(16) 0.0054(14) 0.0034(16) C51 0.0255(19) 0.029(2) 0.024(2) -0.0058(18) 0.0092(16) -0.0038(17) C52 0.027(2) 0.026(2) 0.029(2) -0.0015(18) 0.0078(17) 0.0040(17) C53 0.0247(18) 0.028(2) 0.024(2) 0.0025(18) 0.0022(15) 0.0005(17) C54 0.025(2) 0.028(2) 0.031(2) -0.0025(18) 0.0079(17) -0.0013(17) S8 0.0240(5) 0.0424(7) 0.0234(5) -0.0020(5) 0.0037(4) 0.0027(5) C55 0.036(3) 0.098(5) 0.024(2) -0.002(3) 0.0048(19) -0.003(3) C56 0.041(2) 0.053(3) 0.018(2) 0.000(2) 0.0004(18) 0.005(2) C57 0.051(3) 0.043(3) 0.040(3) 0.009(2) 0.006(2) -0.001(2) N4 0.050(3) 0.073(4) 0.048(3) -0.010(3) -0.004(2) -0.010(3) C58 0.057(3) 0.077(5) 0.039(3) -0.008(3) -0.015(3) 0.018(3) C59 0.094(5) 0.061(4) 0.045(3) 0.011(3) -0.007(3) 0.030(4) C60 0.079(4) 0.045(3) 0.040(3) -0.003(3) 0.004(3) -0.002(3) C61 0.026(2) 0.028(2) 0.048(3) -0.004(2) -0.0012(19) -0.0020(19) C62 0.054(4) 0.162(9) 0.067(5) 0.019(6) -0.020(3) 0.006(5) C63 0.024(3) 0.145(9) 0.234(13) -0.123(9) 0.000(5) 0.018(4) C64 0.033(3) 0.067(5) 0.143(7) 0.049(5) -0.017(4) -0.014(3) O1 0.057(3) 0.072(3) 0.075(3) 0.009(3) 0.003(2) 0.002(2) C65 0.039(3) 0.055(4) 0.232(12) -0.014(6) 0.014(5) 0.009(3) O2 0.102(8) 0.072(6) 0.060(5) 0.007(5) 0.007(5) -0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.144(4) 2_757 ? Co1 N1 2.144(4) . ? Co1 N2 2.208(4) . ? Co1 N2 2.208(4) 2_757 ? Co1 Br1 2.6673(5) 2_757 ? Co1 Br1 2.6674(5) . ? S1 C51 1.772(4) . ? S1 C1 1.787(4) . ? C1 C6 1.386(6) . ? C1 C2 1.394(6) . ? C2 C3 1.407(6) . ? C2 S2 1.781(4) . ? C3 C4 1.376(6) . ? C3 S3 1.781(4) . ? C4 C5 1.399(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(6) . ? C5 C13 1.551(6) . ? C6 H6 0.9500 . ? S2 C7 1.819(5) . ? C7 C8 1.514(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.369(7) . ? C8 C9 1.391(6) . ? C9 N1 1.354(5) . ? C9 H9 0.9500 . ? N1 C10 1.333(6) . ? C10 C11 1.365(7) . ? C10 H10 0.9500 . ? C11 C12 1.387(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.498(8) . ? C13 C16 1.514(8) . ? C13 C15 1.547(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S3 C17 1.765(4) . ? C17 C22 1.398(6) . ? C17 C18 1.415(6) . ? C18 C19 1.391(6) . ? C18 S4 1.773(4) . ? C19 C20 1.409(6) . ? C19 S5 1.775(4) . ? C20 C21 1.383(6) . ? C20 H20 0.9500 . ? C21 C22 1.406(6) . ? C21 C29 1.540(6) . ? C22 H22 0.9500 . ? S4 C23 1.826(5) . ? C23 C24 1.517(7) 4_657 ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.376(7) . ? C24 C28 1.390(7) . ? C24 C23 1.517(7) 4_647 ? C25 N2 1.338(6) . ? C25 H25 0.9500 . ? N2 C26 1.346(6) . ? C26 C27 1.373(8) . ? C26 H26 0.9500 . ? C27 C28 1.337(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C32 1.500(8) . ? C29 C30 1.522(9) . ? C29 C31 1.535(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S5 C33 1.780(4) . ? C33 C34 1.401(6) . ? C33 C38 1.407(6) . ? C34 C35 1.402(6) . ? C34 S6 1.778(4) . ? C35 C36 1.399(6) . ? C35 S7 1.778(4) . ? C36 C37 1.397(6) . ? C36 H36 0.9500 . ? C37 C38 1.380(6) . ? C37 C45 1.534(6) . ? C38 H38 0.9500 . ? S6 C39 1.781(6) . ? C39 C40 1.477(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.350(11) . ? C40 C41 1.397(10) . ? C41 C43 1.387(9) . ? C41 H41 0.9500 . ? C43 C42 1.343(13) . ? C43 H43 0.9500 . ? C42 N3 1.353(13) . ? C42 H42 0.9500 . ? N3 C44 1.302(11) . ? C44 H44 0.9500 . ? C45 C47 1.499(8) . ? C45 C46 1.547(8) . ? C45 C48 1.568(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S7 C49 1.772(4) . ? C49 C50 1.401(6) . ? C49 C54 1.403(6) . ? C50 C51 1.412(6) . ? C50 S8 1.771(4) . ? C51 C52 1.400(6) . ? C52 C53 1.386(6) . ? C52 H52 0.9500 . ? C53 C54 1.393(6) . ? C53 C61 1.546(6) . ? C54 H54 0.9500 . ? S8 C55 1.830(5) . ? C55 C56 1.486(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.369(8) . ? C56 C60 1.379(8) . ? C57 N4 1.345(7) . ? C57 H57 0.9500 . ? N4 C58 1.338(9) . ? C58 C59 1.323(10) . ? C58 H58 0.9500 . ? C59 C60 1.390(9) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C63 1.494(9) . ? C61 C64 1.491(8) . ? C61 C62 1.531(9) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O1 C65 1.408(8) . ? O1 H1 0.8400 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 96.4(2) 2_757 . ? N1 Co1 N2 172.69(14) 2_757 . ? N1 Co1 N2 90.49(14) . . ? N1 Co1 N2 90.49(14) 2_757 2_757 ? N1 Co1 N2 172.70(14) . 2_757 ? N2 Co1 N2 82.70(19) . 2_757 ? N1 Co1 Br1 86.01(10) 2_757 2_757 ? N1 Co1 Br1 87.90(10) . 2_757 ? N2 Co1 Br1 91.92(10) . 2_757 ? N2 Co1 Br1 94.94(10) 2_757 2_757 ? N1 Co1 Br1 87.90(10) 2_757 . ? N1 Co1 Br1 86.01(10) . . ? N2 Co1 Br1 94.95(10) . . ? N2 Co1 Br1 91.92(10) 2_757 . ? Br1 Co1 Br1 170.86(4) 2_757 . ? C51 S1 C1 108.45(19) . . ? C6 C1 C2 121.0(4) . . ? C6 C1 S1 114.4(3) . . ? C2 C1 S1 124.0(3) . . ? C1 C2 C3 117.1(3) . . ? C1 C2 S2 120.7(3) . . ? C3 C2 S2 122.2(3) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 S3 114.2(3) . . ? C2 C3 S3 123.7(3) . . ? C3 C4 C5 121.1(4) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 117.4(4) . . ? C6 C5 C13 120.6(4) . . ? C4 C5 C13 122.0(4) . . ? C1 C6 C5 121.8(4) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C2 S2 C7 100.3(2) . . ? C8 C7 S2 108.6(3) . . ? C8 C7 H7A 110.0 . . ? S2 C7 H7A 110.0 . . ? C8 C7 H7B 110.0 . . ? S2 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? C12 C8 C9 118.5(4) . . ? C12 C8 C7 124.0(4) . . ? C9 C8 C7 117.5(4) . . ? N1 C9 C8 122.8(4) . . ? N1 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C10 N1 C9 117.2(4) . . ? C10 N1 Co1 123.6(3) . . ? C9 N1 Co1 119.1(3) . . ? N1 C10 C11 123.0(4) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C8 C12 C11 118.6(4) . . ? C8 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C16 110.4(6) . . ? C14 C13 C15 108.3(7) . . ? C16 C13 C15 105.9(5) . . ? C14 C13 C5 112.5(4) . . ? C16 C13 C5 111.6(4) . . ? C15 C13 C5 107.8(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 S3 C3 110.18(19) . . ? C22 C17 C18 120.0(4) . . ? C22 C17 S3 113.7(3) . . ? C18 C17 S3 125.6(3) . . ? C19 C18 C17 117.9(3) . . ? C19 C18 S4 119.6(3) . . ? C17 C18 S4 122.5(3) . . ? C18 C19 C20 120.8(4) . . ? C18 C19 S5 124.5(3) . . ? C20 C19 S5 114.1(3) . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 117.4(4) . . ? C20 C21 C29 122.6(4) . . ? C22 C21 C29 120.0(4) . . ? C17 C22 C21 121.6(4) . . ? C17 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C18 S4 C23 100.5(2) . . ? C24 C23 S4 114.3(3) 4_657 . ? C24 C23 H23A 108.7 4_657 . ? S4 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 4_657 . ? S4 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C28 117.1(5) . . ? C25 C24 C23 121.1(4) . 4_647 ? C28 C24 C23 121.7(5) . 4_647 ? N2 C25 C24 124.1(4) . . ? N2 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? C25 N2 C26 116.4(4) . . ? C25 N2 Co1 122.8(3) . . ? C26 N2 Co1 118.9(3) . . ? N2 C26 C27 122.6(5) . . ? N2 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 119.9(5) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C24 119.7(5) . . ? C27 C28 H28 120.1 . . ? C24 C28 H28 120.1 . . ? C32 C29 C30 109.8(5) . . ? C32 C29 C31 108.5(5) . . ? C30 C29 C31 105.5(5) . . ? C32 C29 C21 112.6(4) . . ? C30 C29 C21 109.6(4) . . ? C31 C29 C21 110.6(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C19 S5 C33 108.70(19) . . ? C34 C33 C38 120.7(4) . . ? C34 C33 S5 125.4(3) . . ? C38 C33 S5 113.3(3) . . ? C33 C34 C35 117.6(3) . . ? C33 C34 S6 121.2(3) . . ? C35 C34 S6 121.2(3) . . ? C36 C35 C34 121.0(4) . . ? C36 C35 S7 114.7(3) . . ? C34 C35 S7 123.8(3) . . ? C37 C36 C35 121.2(4) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C38 C37 C36 118.0(4) . . ? C38 C37 C45 122.2(4) . . ? C36 C37 C45 119.8(4) . . ? C37 C38 C33 121.5(4) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? C34 S6 C39 100.5(2) . . ? C40 C39 S6 111.2(4) . . ? C40 C39 H39A 109.4 . . ? S6 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? S6 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C44 C40 C41 117.8(6) . . ? C44 C40 C39 118.7(7) . . ? C41 C40 C39 123.5(7) . . ? C43 C41 C40 120.3(7) . . ? C43 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C42 C43 C41 115.2(7) . . ? C42 C43 H43 122.4 . . ? C41 C43 H43 122.4 . . ? N3 C42 C43 126.1(7) . . ? N3 C42 H42 117.0 . . ? C43 C42 H42 117.0 . . ? C44 N3 C42 116.4(8) . . ? N3 C44 C40 124.1(8) . . ? N3 C44 H44 118.0 . . ? C40 C44 H44 118.0 . . ? C47 C45 C37 113.4(5) . . ? C47 C45 C46 108.8(6) . . ? C37 C45 C46 109.6(4) . . ? C47 C45 C48 109.9(6) . . ? C37 C45 C48 108.5(5) . . ? C46 C45 C48 106.5(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 S7 C35 109.1(2) . . ? C50 C49 C54 120.4(4) . . ? C50 C49 S7 124.3(3) . . ? C54 C49 S7 115.0(3) . . ? C49 C50 C51 118.0(3) . . ? C49 C50 S8 120.8(3) . . ? C51 C50 S8 121.1(3) . . ? C52 C51 C50 120.3(4) . . ? C52 C51 S1 115.9(3) . . ? C50 C51 S1 123.7(3) . . ? C53 C52 C51 121.6(4) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 118.0(4) . . ? C52 C53 C61 120.7(4) . . ? C54 C53 C61 121.1(4) . . ? C53 C54 C49 121.5(4) . . ? C53 C54 H54 119.3 . . ? C49 C54 H54 119.3 . . ? C50 S8 C55 98.3(2) . . ? C56 C55 S8 107.7(3) . . ? C56 C55 H55A 110.2 . . ? S8 C55 H55A 110.2 . . ? C56 C55 H55B 110.2 . . ? S8 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? C57 C56 C60 116.9(5) . . ? C57 C56 C55 119.9(5) . . ? C60 C56 C55 123.2(6) . . ? N4 C57 C56 123.9(5) . . ? N4 C57 H57 118.0 . . ? C56 C57 H57 118.0 . . ? C58 N4 C57 116.5(5) . . ? C59 C58 N4 124.2(6) . . ? C59 C58 H58 117.9 . . ? N4 C58 H58 117.9 . . ? C58 C59 C60 118.7(6) . . ? C58 C59 H59 120.7 . . ? C60 C59 H59 120.7 . . ? C56 C60 C59 119.6(6) . . ? C56 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C63 C61 C64 112.1(7) . . ? C63 C61 C62 108.9(8) . . ? C64 C61 C62 106.7(6) . . ? C63 C61 C53 110.7(4) . . ? C64 C61 C53 112.0(4) . . ? C62 C61 C53 106.2(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 O1 H1 109.5 . . ? O1 C65 H65A 109.5 . . ? O1 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O1 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.426 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.199 _database_code_depnum_ccdc_archive 'CCDC 970402' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2370a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H68 Cl2 Fe N4 S8), C H4 O' _chemical_formula_sum 'C129 H140 Cl4 Fe2 N8 O S16' _chemical_formula_weight 2584.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4791(4) _cell_length_b 14.2338(4) _cell_length_c 21.6211(5) _cell_angle_alpha 87.8170(10) _cell_angle_beta 81.1830(10) _cell_angle_gamma 66.3810(10) _cell_volume 3197.45(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 29.85 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1354 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9517 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60060 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 29.00 _reflns_number_total 16744 _reflns_number_gt 13901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+3.7781P] 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 16744 _refine_ls_number_parameters 747 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.0000 0.0000 0.01920(10) Uani 1 2 d S . 1 Cl1 Cl 1.16273(5) -0.04271(4) 0.06669(3) 0.02848(13) Uani 1 1 d . A 1 Fe2 Fe 0.5000 1.0000 0.5000 0.02362(11) Uani 1 2 d S . 1 Cl2 Cl 0.72257(6) 0.90570(5) 0.45973(3) 0.03376(14) Uani 1 1 d . B 1 S1 S 0.99114(6) 0.37687(5) 0.07865(3) 0.02923(14) Uani 1 1 d . C 1 C1 C 0.8432(2) 0.44408(17) 0.12781(11) 0.0228(4) Uani 1 1 d . C 1 C2 C 0.8092(2) 0.41776(16) 0.18892(11) 0.0211(4) Uani 1 1 d . C 1 C3 C 0.6827(2) 0.47535(16) 0.21897(11) 0.0203(4) Uani 1 1 d . C 1 C4 C 0.5936(2) 0.54910(16) 0.18635(12) 0.0231(4) Uani 1 1 d . C 1 H4 H 0.5081 0.5847 0.2069 0.028 Uiso 1 1 calc R C 1 C5 C 0.6263(2) 0.57211(17) 0.12452(12) 0.0241(4) Uani 1 1 d . C 1 C6 C 0.7529(2) 0.51997(18) 0.09675(12) 0.0252(5) Uani 1 1 d . C 1 H6 H 0.7790 0.5364 0.0554 0.030 Uiso 1 1 calc R C 1 S5 S 0.92151(5) 0.31437(4) 0.22495(3) 0.02522(12) Uani 1 1 d . C 1 C7 C 0.8458(3) 0.22223(17) 0.23204(12) 0.0284(5) Uani 1 1 d . C 1 H7A H 0.9082 0.1551 0.2439 0.034 Uiso 1 1 calc R C 1 H7B H 0.7713 0.2460 0.2660 0.034 Uiso 1 1 calc R C 1 C8 C 0.8014(2) 0.20862(16) 0.17285(12) 0.0246(5) Uani 1 1 d . C 1 C9 C 0.8855(2) 0.13855(16) 0.12632(12) 0.0247(5) Uani 1 1 d . C 1 H9 H 0.9707 0.0988 0.1340 0.030 Uiso 1 1 calc R C 1 N1 N 0.85369(18) 0.12392(14) 0.07173(10) 0.0230(4) Uani 1 1 d . C 1 C10 C 0.7340(2) 0.18302(18) 0.06088(13) 0.0277(5) Uani 1 1 d . C 1 H10 H 0.7099 0.1748 0.0220 0.033 Uiso 1 1 calc R C 1 C11 C 0.6441(2) 0.2554(2) 0.10399(14) 0.0335(6) Uani 1 1 d . C 1 H11 H 0.5605 0.2962 0.0946 0.040 Uiso 1 1 calc R C 1 C12 C 0.6783(2) 0.26737(19) 0.16093(13) 0.0308(5) Uani 1 1 d . C 1 H12 H 0.6176 0.3155 0.1915 0.037 Uiso 1 1 calc R C 1 C13 C 0.5249(2) 0.6533(2) 0.09065(14) 0.0316(5) Uani 1 1 d . C 1 C14 C 0.5826(3) 0.6776(3) 0.02639(16) 0.0434(7) Uani 1 1 d . C 1 H14A H 0.6204 0.6155 -0.0004 0.065 Uiso 1 1 calc R C 1 H14B H 0.6493 0.7019 0.0316 0.065 Uiso 1 1 calc R C 1 H14C H 0.5148 0.7310 0.0070 0.065 Uiso 1 1 calc R C 1 C15 C 0.4222(3) 0.6156(3) 0.0813(2) 0.0576(10) Uani 1 1 d . C 1 H15A H 0.3555 0.6688 0.0612 0.086 Uiso 1 1 calc R C 1 H15B H 0.3836 0.6004 0.1220 0.086 Uiso 1 1 calc R C 1 H15C H 0.4612 0.5533 0.0547 0.086 Uiso 1 1 calc R C 1 C16 C 0.4615(3) 0.7528(2) 0.13058(17) 0.0493(8) Uani 1 1 d . C 1 H16A H 0.5279 0.7751 0.1395 0.074 Uiso 1 1 calc R C 1 H16B H 0.4156 0.7406 0.1700 0.074 Uiso 1 1 calc R C 1 H16C H 0.4008 0.8062 0.1077 0.074 Uiso 1 1 calc R C 1 S2 S 0.61518(5) 0.44900(4) 0.29366(3) 0.02291(12) Uani 1 1 d . C 1 C17 C 0.7232(2) 0.43762(17) 0.34704(11) 0.0224(4) Uani 1 1 d . C 1 C18 C 0.7651(2) 0.51465(16) 0.35863(11) 0.0216(4) Uani 1 1 d . C 1 C19 C 0.8492(2) 0.49429(17) 0.40318(11) 0.0230(4) Uani 1 1 d . C 1 C20 C 0.8807(3) 0.4048(2) 0.43724(13) 0.0291(5) Uani 1 1 d . C 1 H20 H 0.9374 0.3931 0.4671 0.035 Uiso 1 1 calc R C 1 C21 C 0.8316(3) 0.3319(2) 0.42882(13) 0.0310(5) Uani 1 1 d . C 1 C22 C 0.7538(2) 0.34968(18) 0.38282(12) 0.0276(5) Uani 1 1 d . C 1 H22 H 0.7204 0.3006 0.3755 0.033 Uiso 1 1 calc R C 1 S6 S 0.71327(6) 0.63422(4) 0.32156(3) 0.03034(14) Uani 1 1 d . C 1 C23 C 0.5387(3) 0.6778(2) 0.3426(2) 0.0496(9) Uani 1 1 d . C 1 H23A H 0.5032 0.6627 0.3071 0.059 Uiso 1 1 calc R C 1 H23B H 0.5199 0.6388 0.3788 0.059 Uiso 1 1 calc R C 1 C24 C 0.4728(3) 0.7901(2) 0.35877(15) 0.0364(6) Uani 1 1 d . C 1 C25 C 0.5080(3) 0.83457(18) 0.40465(14) 0.0321(5) Uani 1 1 d . C 1 H25 H 0.5816 0.7934 0.4230 0.039 Uiso 1 1 calc R C 1 N2 N 0.4438(2) 0.93226(16) 0.42450(11) 0.0295(4) Uani 1 1 d . C 1 C26 C 0.3415(3) 0.9899(2) 0.39753(15) 0.0367(6) Uani 1 1 d . C 1 H26 H 0.2948 1.0594 0.4112 0.044 Uiso 1 1 calc R C 1 C27 C 0.3012(3) 0.9528(2) 0.35073(16) 0.0442(7) Uani 1 1 d . C 1 H27 H 0.2286 0.9961 0.3324 0.053 Uiso 1 1 calc R C 1 C28 C 0.3677(3) 0.8517(2) 0.33082(16) 0.0441(7) Uani 1 1 d . C 1 H28 H 0.3420 0.8247 0.2984 0.053 Uiso 1 1 calc R C 1 C29 C 0.8684(4) 0.2337(3) 0.46659(19) 0.0555(10) Uani 1 1 d D C 1 C30 C 1.0093(8) 0.1726(6) 0.4529(5) 0.0858(17) Uani 0.563(6) 1 d PD C 1 H30A H 1.0544 0.2069 0.4720 0.129 Uiso 0.563(6) 1 calc PR C 1 H30B H 1.0366 0.1664 0.4075 0.129 Uiso 0.563(6) 1 calc PR C 1 H30C H 1.0298 0.1041 0.4701 0.129 Uiso 0.563(6) 1 calc PR C 1 C31 C 0.8282(10) 0.2709(6) 0.5394(4) 0.0858(17) Uani 0.563(6) 1 d PD C 1 H31A H 0.8331 0.2123 0.5657 0.129 Uiso 0.563(6) 1 calc PR C 1 H31B H 0.7401 0.3235 0.5460 0.129 Uiso 0.563(6) 1 calc PR C 1 H31C H 0.8871 0.2996 0.5506 0.129 Uiso 0.563(6) 1 calc PR C 1 C32 C 0.7934(11) 0.1691(9) 0.4578(6) 0.0858(17) Uani 0.563(6) 1 d PD C 1 H32A H 0.8204 0.1088 0.4842 0.129 Uiso 0.563(6) 1 calc PR C 1 H32B H 0.8103 0.1469 0.4138 0.129 Uiso 0.563(6) 1 calc PR C 1 H32C H 0.7012 0.2101 0.4698 0.129 Uiso 0.563(6) 1 calc PR C 1 S3 S 0.90692(6) 0.58463(5) 0.42564(3) 0.02542(12) Uani 1 1 d . . . C33 C 0.9948(2) 0.60928(17) 0.35639(11) 0.0223(4) Uani 1 1 d . C . C34 C 1.1024(2) 0.53219(16) 0.32154(12) 0.0249(5) Uani 1 1 d . . . C35 C 1.1678(2) 0.56249(16) 0.27020(12) 0.0258(5) Uani 1 1 d . C . C36 C 1.1326(2) 0.66662(17) 0.25663(12) 0.0276(5) Uani 1 1 d . . . H36 H 1.1812 0.6854 0.2226 0.033 Uiso 1 1 calc R C . C37 C 1.0284(2) 0.74297(17) 0.29167(12) 0.0261(5) Uani 1 1 d . C . C38 C 0.9594(2) 0.71212(16) 0.34133(12) 0.0241(4) Uani 1 1 d . . . H38 H 0.8864 0.7626 0.3654 0.029 Uiso 1 1 calc R C . S7 S 1.15640(7) 0.40112(5) 0.34178(4) 0.03869(17) Uani 1 1 d . C . C39 C 1.2697(4) 0.3982(2) 0.39553(18) 0.0619(11) Uani 1 1 d . . . H39A H 1.3028 0.4520 0.3844 0.074 Uiso 1 1 calc R C . H39B H 1.2248 0.4114 0.4392 0.074 Uiso 1 1 calc R . . C40 C 1.3786(4) 0.2949(2) 0.38968(16) 0.0439(7) Uani 1 1 d . C . C41 C 1.3909(3) 0.2226(2) 0.43618(14) 0.0397(7) Uani 1 1 d . . . H41 H 1.3276 0.2399 0.4725 0.048 Uiso 1 1 calc R C . N3 N 1.4879(2) 0.12959(16) 0.43193(11) 0.0301(4) Uani 1 1 d . . . C42 C 1.5757(3) 0.1072(2) 0.38012(14) 0.0368(6) Uani 1 1 d . . . H42 H 1.6461 0.0422 0.3766 0.044 Uiso 1 1 calc R C . C43 C 1.5688(3) 0.1741(3) 0.33168(16) 0.0455(7) Uani 1 1 d . C . H43 H 1.6324 0.1550 0.2955 0.055 Uiso 1 1 calc R . . C44 C 1.4681(4) 0.2690(3) 0.33663(16) 0.0454(8) Uani 1 1 d . . . H44 H 1.4607 0.3160 0.3036 0.055 Uiso 1 1 calc R C . C45 C 0.9826(3) 0.85624(17) 0.27466(13) 0.0321(6) Uani 1 1 d . . . C46 C 0.9765(4) 0.9205(2) 0.33087(15) 0.0423(7) Uani 1 1 d . C . H46A H 1.0624 0.8980 0.3428 0.063 Uiso 1 1 calc R . . H46B H 0.9171 0.9118 0.3661 0.063 Uiso 1 1 calc R . . H46C H 0.9461 0.9929 0.3199 0.063 Uiso 1 1 calc R . . C47 C 1.0721(4) 0.8745(2) 0.21979(16) 0.0534(10) Uani 1 1 d . C . H47A H 1.1596 0.8491 0.2301 0.080 Uiso 1 1 calc R . . H47B H 1.0419 0.9482 0.2119 0.080 Uiso 1 1 calc R . . H47C H 1.0720 0.8380 0.1823 0.080 Uiso 1 1 calc R . . C48 C 0.8475(4) 0.8906(3) 0.2567(2) 0.0575(10) Uani 1 1 d . C . H48A H 0.8164 0.9630 0.2455 0.086 Uiso 1 1 calc R . . H48B H 0.7890 0.8819 0.2923 0.086 Uiso 1 1 calc R . . H48C H 0.8509 0.8489 0.2209 0.086 Uiso 1 1 calc R . . S4 S 1.30267(6) 0.47457(4) 0.22008(3) 0.02796(13) Uani 1 1 d . . . C49 C 1.2481(2) 0.39123(16) 0.18496(12) 0.0229(4) Uani 1 1 d . C . C50 C 1.1411(2) 0.42439(16) 0.15372(11) 0.0232(4) Uani 1 1 d . . . C51 C 1.1183(2) 0.34971(17) 0.12258(11) 0.0236(4) Uani 1 1 d . C . C52 C 1.2033(2) 0.24701(17) 0.12089(12) 0.0254(5) Uani 1 1 d . . . H52 H 1.1883 0.1986 0.0978 0.030 Uiso 1 1 calc R C . C53 C 1.3095(2) 0.21347(16) 0.15203(12) 0.0247(5) Uani 1 1 d . C . C54 C 1.3298(2) 0.28697(17) 0.18432(12) 0.0257(5) Uani 1 1 d . . . H54 H 1.4011 0.2659 0.2065 0.031 Uiso 1 1 calc R C . S8 S 1.03160(6) 0.55434(4) 0.15805(3) 0.03201(15) Uani 1 1 d . C . C55 C 1.0781(2) 0.60055(19) 0.08370(14) 0.0344(6) Uani 1 1 d . . . H55A H 1.1647 0.6007 0.0818 0.041 Uiso 1 1 calc R C . H55B H 1.0807 0.5554 0.0493 0.041 Uiso 1 1 calc R . . C56 C 0.9808(2) 0.70800(17) 0.07664(12) 0.0257(5) Uani 1 1 d . C . C57 C 1.0194(2) 0.78528(17) 0.05460(12) 0.0258(5) Uani 1 1 d . . . H57 H 1.1089 0.7697 0.0460 0.031 Uiso 1 1 calc R C . N4 N 0.93699(19) 0.88107(14) 0.04471(10) 0.0246(4) Uani 1 1 d . . . C58 C 0.8119(3) 0.9022(2) 0.05769(17) 0.0404(7) Uani 1 1 d . . . H58 H 0.7523 0.9693 0.0505 0.048 Uiso 1 1 calc R C . C59 C 0.7653(3) 0.8310(2) 0.0810(2) 0.0601(12) Uani 1 1 d . C . H59 H 0.6752 0.8494 0.0906 0.072 Uiso 1 1 calc R . . C60 C 0.8502(3) 0.7325(2) 0.09053(18) 0.0430(8) Uani 1 1 d . . . H60 H 0.8193 0.6822 0.1064 0.052 Uiso 1 1 calc R C . C61 C 1.3909(3) 0.09801(17) 0.15315(14) 0.0327(6) Uani 1 1 d . . . C62 C 1.3042(4) 0.0467(2) 0.18641(18) 0.0471(8) Uani 1 1 d . C . H62A H 1.2630 0.0806 0.2273 0.071 Uiso 1 1 calc R . . H62B H 1.3563 -0.0259 0.1922 0.071 Uiso 1 1 calc R . . H62C H 1.2380 0.0528 0.1609 0.071 Uiso 1 1 calc R . . C63 C 1.5048(3) 0.0735(2) 0.1884(2) 0.0516(9) Uani 1 1 d . C . H63A H 1.5584 0.1089 0.1693 0.077 Uiso 1 1 calc R . . H63B H 1.5560 -0.0007 0.1864 0.077 Uiso 1 1 calc R . . H63C H 1.4731 0.0964 0.2323 0.077 Uiso 1 1 calc R . . C64 C 1.4399(3) 0.0555(2) 0.08549(17) 0.0463(8) Uani 1 1 d . C . H64A H 1.3665 0.0704 0.0632 0.070 Uiso 1 1 calc R . . H64B H 1.4889 -0.0188 0.0859 0.070 Uiso 1 1 calc R . . H64C H 1.4954 0.0880 0.0643 0.070 Uiso 1 1 calc R . . C65 C 0.4847(7) 0.3720(8) 0.4976(4) 0.064(2) Uani 0.50 1 d PD . . H65A H 0.5532 0.3451 0.5237 0.096 Uiso 0.50 1 calc PR . . H65B H 0.5153 0.3371 0.4564 0.096 Uiso 0.50 1 calc PR . . H65C H 0.4096 0.3600 0.5178 0.096 Uiso 0.50 1 calc PR . . O1 O 0.4533(4) 0.4686(5) 0.4910(2) 0.0571(14) Uani 0.50 1 d PD . . H1 H 0.4123 0.4882 0.4606 0.086 Uiso 0.50 1 calc PR . . C30A C 0.9270(14) 0.2356(8) 0.5225(5) 0.0858(17) Uani 0.437(6) 1 d PD C 2 H30D H 0.9186 0.1833 0.5515 0.129 Uiso 0.437(6) 1 calc PR C 2 H30E H 0.8829 0.3034 0.5433 0.129 Uiso 0.437(6) 1 calc PR C 2 H30F H 1.0182 0.2216 0.5099 0.129 Uiso 0.437(6) 1 calc PR C 2 C32A C 0.7661(13) 0.1918(12) 0.4744(8) 0.0858(17) Uani 0.437(6) 1 d PD C 2 H32D H 0.7949 0.1277 0.4973 0.129 Uiso 0.437(6) 1 calc PR C 2 H32E H 0.7499 0.1785 0.4331 0.129 Uiso 0.437(6) 1 calc PR C 2 H32F H 0.6868 0.2418 0.4978 0.129 Uiso 0.437(6) 1 calc PR C 2 C31A C 0.9911(10) 0.1491(7) 0.4181(5) 0.0858(17) Uani 0.437(6) 1 d PD C 2 H31D H 1.0521 0.1797 0.4019 0.129 Uiso 0.437(6) 1 calc PR C 2 H31E H 0.9581 0.1310 0.3832 0.129 Uiso 0.437(6) 1 calc PR C 2 H31F H 1.0347 0.0872 0.4410 0.129 Uiso 0.437(6) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0213(2) 0.01557(18) 0.0190(3) 0.00226(15) -0.00729(16) -0.00429(15) Cl1 0.0266(3) 0.0289(3) 0.0249(3) -0.0017(2) -0.0111(2) -0.0030(2) Fe2 0.0257(2) 0.0178(2) 0.0231(3) -0.00049(16) -0.00432(17) -0.00398(16) Cl2 0.0284(3) 0.0287(3) 0.0359(4) -0.0042(2) -0.0015(2) -0.0036(2) S1 0.0275(3) 0.0311(3) 0.0197(3) -0.0034(2) -0.0070(2) -0.0004(2) C1 0.0254(10) 0.0210(9) 0.0196(12) -0.0007(8) -0.0080(8) -0.0050(8) C2 0.0241(10) 0.0175(9) 0.0207(12) -0.0001(8) -0.0103(8) -0.0046(7) C3 0.0250(10) 0.0190(9) 0.0180(12) -0.0008(7) -0.0077(8) -0.0081(8) C4 0.0222(9) 0.0206(9) 0.0257(13) 0.0003(8) -0.0082(8) -0.0061(8) C5 0.0242(10) 0.0201(9) 0.0273(14) 0.0040(8) -0.0114(9) -0.0058(8) C6 0.0281(11) 0.0254(10) 0.0204(13) 0.0038(8) -0.0092(9) -0.0071(9) S5 0.0263(3) 0.0223(2) 0.0247(3) 0.0046(2) -0.0114(2) -0.0049(2) C7 0.0396(13) 0.0194(10) 0.0228(14) 0.0009(8) -0.0057(10) -0.0080(9) C8 0.0311(11) 0.0174(9) 0.0241(13) 0.0002(8) -0.0042(9) -0.0086(8) C9 0.0275(10) 0.0180(9) 0.0248(13) 0.0014(8) -0.0053(9) -0.0048(8) N1 0.0261(9) 0.0175(8) 0.0230(11) -0.0003(7) -0.0042(7) -0.0060(7) C10 0.0271(11) 0.0257(11) 0.0284(14) -0.0023(9) -0.0072(9) -0.0072(9) C11 0.0232(11) 0.0315(12) 0.0412(17) -0.0103(11) -0.0072(10) -0.0043(9) C12 0.0276(11) 0.0270(11) 0.0343(15) -0.0100(10) -0.0003(10) -0.0078(9) C13 0.0253(11) 0.0328(12) 0.0341(16) 0.0131(10) -0.0140(10) -0.0068(9) C14 0.0369(14) 0.0495(17) 0.0371(19) 0.0200(13) -0.0149(12) -0.0086(12) C15 0.0519(19) 0.081(3) 0.063(3) 0.041(2) -0.0427(18) -0.0421(19) C16 0.0439(16) 0.0297(13) 0.055(2) 0.0112(13) -0.0087(14) 0.0050(12) S2 0.0266(3) 0.0246(2) 0.0197(3) 0.0001(2) -0.0074(2) -0.0112(2) C17 0.0275(10) 0.0224(10) 0.0182(12) 0.0000(8) -0.0060(8) -0.0098(8) C18 0.0256(10) 0.0197(9) 0.0190(12) 0.0004(8) -0.0038(8) -0.0086(8) C19 0.0275(10) 0.0262(10) 0.0188(12) -0.0001(8) -0.0045(8) -0.0141(8) C20 0.0364(12) 0.0336(12) 0.0258(14) 0.0088(10) -0.0149(10) -0.0199(10) C21 0.0417(14) 0.0306(12) 0.0297(15) 0.0112(10) -0.0170(11) -0.0207(11) C22 0.0365(12) 0.0258(11) 0.0264(14) 0.0038(9) -0.0103(10) -0.0170(9) S6 0.0382(3) 0.0191(2) 0.0339(4) 0.0030(2) -0.0142(3) -0.0088(2) C23 0.0357(14) 0.0257(12) 0.087(3) -0.0151(14) -0.0243(15) -0.0048(11) C24 0.0367(13) 0.0239(11) 0.0458(18) -0.0066(11) -0.0138(12) -0.0061(10) C25 0.0349(12) 0.0220(11) 0.0380(16) 0.0018(10) -0.0145(11) -0.0068(9) N2 0.0324(10) 0.0229(9) 0.0306(13) -0.0017(8) -0.0080(8) -0.0070(8) C26 0.0390(14) 0.0242(11) 0.0396(17) -0.0042(10) -0.0142(12) -0.0018(10) C27 0.0444(16) 0.0315(13) 0.050(2) -0.0031(12) -0.0243(14) -0.0013(11) C28 0.0455(16) 0.0343(14) 0.049(2) -0.0095(13) -0.0227(14) -0.0057(12) C29 0.081(2) 0.0497(18) 0.064(3) 0.0377(17) -0.052(2) -0.0443(18) C30 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) C31 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) C32 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) S3 0.0342(3) 0.0288(3) 0.0191(3) -0.0017(2) -0.0047(2) -0.0182(2) C33 0.0272(10) 0.0211(9) 0.0210(12) 0.0006(8) -0.0050(8) -0.0115(8) C34 0.0283(11) 0.0165(9) 0.0294(14) -0.0003(8) -0.0023(9) -0.0092(8) C35 0.0278(10) 0.0173(9) 0.0306(14) -0.0024(8) -0.0009(9) -0.0083(8) C36 0.0354(12) 0.0195(10) 0.0269(14) -0.0001(8) 0.0002(9) -0.0116(9) C37 0.0359(12) 0.0171(9) 0.0242(13) -0.0004(8) -0.0057(9) -0.0090(8) C38 0.0307(11) 0.0173(9) 0.0225(13) -0.0019(8) -0.0043(9) -0.0074(8) S7 0.0414(3) 0.0170(3) 0.0518(5) 0.0034(2) 0.0055(3) -0.0103(2) C39 0.104(3) 0.0258(14) 0.040(2) 0.0032(12) -0.032(2) -0.0017(16) C40 0.071(2) 0.0218(11) 0.0375(18) 0.0050(11) -0.0210(15) -0.0125(12) C41 0.0572(18) 0.0228(11) 0.0302(16) 0.0026(10) -0.0099(12) -0.0057(11) N3 0.0386(11) 0.0228(9) 0.0284(13) 0.0051(8) -0.0090(9) -0.0107(8) C42 0.0328(13) 0.0459(15) 0.0357(17) 0.0107(12) -0.0109(11) -0.0186(11) C43 0.0420(15) 0.066(2) 0.0409(19) 0.0205(15) -0.0137(13) -0.0333(15) C44 0.070(2) 0.0475(17) 0.0383(19) 0.0189(13) -0.0256(15) -0.0392(16) C45 0.0475(15) 0.0168(10) 0.0257(14) 0.0022(8) -0.0024(11) -0.0073(9) C46 0.069(2) 0.0229(11) 0.0347(17) -0.0020(10) 0.0007(14) -0.0216(13) C47 0.083(3) 0.0232(12) 0.0358(19) 0.0071(11) 0.0118(16) -0.0108(14) C48 0.063(2) 0.0330(15) 0.067(3) 0.0090(15) -0.0307(19) -0.0028(14) S4 0.0260(3) 0.0202(2) 0.0366(4) -0.0047(2) 0.0024(2) -0.0103(2) C49 0.0234(10) 0.0163(9) 0.0256(13) -0.0005(8) 0.0008(8) -0.0059(8) C50 0.0249(10) 0.0159(9) 0.0219(13) 0.0017(8) -0.0007(8) -0.0021(7) C51 0.0237(10) 0.0215(10) 0.0196(12) 0.0004(8) -0.0033(8) -0.0029(8) C52 0.0264(10) 0.0194(10) 0.0251(13) -0.0028(8) -0.0054(9) -0.0028(8) C53 0.0244(10) 0.0163(9) 0.0285(14) -0.0010(8) -0.0049(9) -0.0027(8) C54 0.0221(10) 0.0185(9) 0.0333(14) -0.0009(8) -0.0061(9) -0.0040(8) S8 0.0384(3) 0.0174(2) 0.0265(4) 0.0017(2) -0.0029(2) 0.0021(2) C55 0.0282(11) 0.0211(10) 0.0412(17) 0.0089(10) 0.0027(10) -0.0003(9) C56 0.0264(10) 0.0183(9) 0.0294(14) 0.0041(8) -0.0070(9) -0.0051(8) C57 0.0225(10) 0.0224(10) 0.0286(14) 0.0063(9) -0.0048(8) -0.0052(8) N4 0.0249(9) 0.0190(8) 0.0278(12) 0.0044(7) -0.0053(7) -0.0066(7) C58 0.0256(12) 0.0217(11) 0.071(2) 0.0131(12) -0.0105(12) -0.0059(9) C59 0.0212(12) 0.0320(14) 0.124(4) 0.0295(18) -0.0143(16) -0.0092(11) C60 0.0291(12) 0.0237(12) 0.079(2) 0.0175(13) -0.0150(13) -0.0121(10) C61 0.0334(12) 0.0149(9) 0.0453(17) -0.0018(9) -0.0165(11) -0.0010(8) C62 0.064(2) 0.0257(13) 0.056(2) 0.0101(12) -0.0211(16) -0.0191(13) C63 0.0497(17) 0.0213(12) 0.079(3) -0.0021(13) -0.0373(17) 0.0006(11) C64 0.0399(15) 0.0264(12) 0.056(2) -0.0129(12) -0.0095(13) 0.0063(11) C65 0.049(4) 0.109(7) 0.040(4) -0.028(4) 0.008(3) -0.042(4) O1 0.032(2) 0.104(5) 0.037(3) -0.023(3) 0.0009(18) -0.030(3) C30A 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) C32A 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) C31A 0.118(4) 0.068(3) 0.107(4) 0.056(3) -0.070(3) -0.060(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.2283(19) 2_765 ? Fe1 N4 2.2283(19) 1_545 ? Fe1 N1 2.3179(19) 2_755 ? Fe1 N1 2.3180(19) . ? Fe1 Cl1 2.4056(6) . ? Fe1 Cl1 2.4057(6) 2_755 ? Fe2 N2 2.225(2) . ? Fe2 N2 2.225(2) 2_676 ? Fe2 N3 2.289(2) 1_465 ? Fe2 N3 2.289(2) 2_766 ? Fe2 Cl2 2.3972(6) . ? Fe2 Cl2 2.3972(6) 2_676 ? S1 C51 1.768(2) . ? S1 C1 1.775(2) . ? C1 C6 1.398(3) . ? C1 C2 1.400(3) . ? C2 C3 1.414(3) . ? C2 S5 1.771(2) . ? C3 C4 1.396(3) . ? C3 S2 1.776(2) . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 C13 1.532(3) . ? C6 H6 0.9500 . ? S5 C7 1.832(3) . ? C7 C8 1.494(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.383(3) . ? C8 C9 1.395(3) . ? C9 N1 1.335(3) . ? C9 H9 0.9500 . ? N1 C10 1.345(3) . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.384(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.519(4) . ? C13 C14 1.534(4) . ? C13 C16 1.534(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S2 C17 1.778(2) . ? C17 C22 1.395(3) . ? C17 C18 1.406(3) . ? C18 C19 1.408(3) . ? C18 S6 1.768(2) . ? C19 C20 1.391(3) . ? C19 S3 1.777(2) . ? C20 C21 1.394(3) . ? C20 H20 0.9500 . ? C21 C22 1.387(4) . ? C21 C29 1.531(4) . ? C22 H22 0.9500 . ? S6 C23 1.832(3) . ? C23 C24 1.497(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.387(4) . ? C24 C28 1.387(4) . ? C25 N2 1.337(3) . ? C25 H25 0.9500 . ? N2 C26 1.339(3) . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 C28 1.380(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30A 1.477(9) . ? C29 C30 1.485(9) . ? C29 C32A 1.502(11) . ? C29 C32 1.523(9) . ? C29 C31 1.617(9) . ? C29 C31A 1.678(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S3 C33 1.779(2) . ? C33 C38 1.393(3) . ? C33 C34 1.410(3) . ? C34 C35 1.396(3) . ? C34 S7 1.775(2) . ? C35 C36 1.403(3) . ? C35 S4 1.781(2) . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.398(3) . ? C37 C45 1.532(3) . ? C38 H38 0.9500 . ? S7 C39 1.860(4) . ? C39 C40 1.495(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.369(5) . ? C40 C41 1.392(4) . ? C41 N3 1.341(3) . ? C41 H41 0.9500 . ? N3 C42 1.340(4) . ? N3 Fe2 2.289(2) 1_645 ? C42 C43 1.378(4) . ? C42 H42 0.9500 . ? C43 C44 1.376(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.525(4) . ? C45 C47 1.532(4) . ? C45 C48 1.535(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S4 C49 1.785(2) . ? C49 C50 1.398(3) . ? C49 C54 1.402(3) . ? C50 C51 1.409(3) . ? C50 S8 1.768(2) . ? C51 C52 1.393(3) . ? C52 C53 1.388(3) . ? C52 H52 0.9500 . ? C53 C54 1.392(3) . ? C53 C61 1.532(3) . ? C54 H54 0.9500 . ? S8 C55 1.800(3) . ? C55 C56 1.508(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C60 1.383(4) . ? C56 C57 1.385(3) . ? C57 N4 1.344(3) . ? C57 H57 0.9500 . ? N4 C58 1.330(3) . ? N4 Fe1 2.2283(19) 1_565 ? C58 C59 1.371(4) . ? C58 H58 0.9500 . ? C59 C60 1.379(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C63 1.527(4) . ? C61 C62 1.538(4) . ? C61 C64 1.538(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 O1 1.282(10) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O1 O1 1.739(10) 2_666 ? O1 H1 0.8400 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N4 179.999(1) 2_765 1_545 ? N4 Fe1 N1 91.11(7) 2_765 2_755 ? N4 Fe1 N1 88.89(7) 1_545 2_755 ? N4 Fe1 N1 88.89(7) 2_765 . ? N4 Fe1 N1 91.10(7) 1_545 . ? N1 Fe1 N1 180.0 2_755 . ? N4 Fe1 Cl1 89.82(6) 2_765 . ? N4 Fe1 Cl1 90.18(5) 1_545 . ? N1 Fe1 Cl1 88.86(5) 2_755 . ? N1 Fe1 Cl1 91.14(5) . . ? N4 Fe1 Cl1 90.18(5) 2_765 2_755 ? N4 Fe1 Cl1 89.81(5) 1_545 2_755 ? N1 Fe1 Cl1 91.14(5) 2_755 2_755 ? N1 Fe1 Cl1 88.86(5) . 2_755 ? Cl1 Fe1 Cl1 179.999(2) . 2_755 ? N2 Fe2 N2 179.998(1) . 2_676 ? N2 Fe2 N3 85.38(8) . 1_465 ? N2 Fe2 N3 94.62(8) 2_676 1_465 ? N2 Fe2 N3 94.62(8) . 2_766 ? N2 Fe2 N3 85.38(8) 2_676 2_766 ? N3 Fe2 N3 179.999(2) 1_465 2_766 ? N2 Fe2 Cl2 90.11(6) . . ? N2 Fe2 Cl2 89.89(6) 2_676 . ? N3 Fe2 Cl2 91.36(6) 1_465 . ? N3 Fe2 Cl2 88.64(6) 2_766 . ? N2 Fe2 Cl2 89.89(6) . 2_676 ? N2 Fe2 Cl2 90.11(6) 2_676 2_676 ? N3 Fe2 Cl2 88.64(6) 1_465 2_676 ? N3 Fe2 Cl2 91.36(6) 2_766 2_676 ? Cl2 Fe2 Cl2 180.00(3) . 2_676 ? C51 S1 C1 108.71(11) . . ? C6 C1 C2 120.9(2) . . ? C6 C1 S1 113.09(18) . . ? C2 C1 S1 125.42(17) . . ? C1 C2 C3 117.28(19) . . ? C1 C2 S5 120.08(17) . . ? C3 C2 S5 122.63(18) . . ? C4 C3 C2 120.4(2) . . ? C4 C3 S2 113.95(17) . . ? C2 C3 S2 124.87(17) . . ? C5 C4 C3 122.0(2) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C6 C5 C4 117.1(2) . . ? C6 C5 C13 122.8(2) . . ? C4 C5 C13 120.0(2) . . ? C5 C6 C1 122.0(2) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C2 S5 C7 101.42(11) . . ? C8 C7 S5 112.73(17) . . ? C8 C7 H7A 109.0 . . ? S5 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? S5 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C12 C8 C9 117.6(2) . . ? C12 C8 C7 121.7(2) . . ? C9 C8 C7 120.7(2) . . ? N1 C9 C8 124.1(2) . . ? N1 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C9 N1 C10 117.2(2) . . ? C9 N1 Fe1 120.65(15) . . ? C10 N1 Fe1 122.14(17) . . ? N1 C10 C11 122.9(2) . . ? N1 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C8 C12 C11 119.4(2) . . ? C8 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C15 C13 C5 109.6(2) . . ? C15 C13 C14 108.4(3) . . ? C5 C13 C14 112.4(2) . . ? C15 C13 C16 108.8(3) . . ? C5 C13 C16 109.4(2) . . ? C14 C13 C16 108.2(2) . . ? C3 S2 C17 107.90(11) . . ? C22 C17 C18 120.9(2) . . ? C22 C17 S2 114.68(17) . . ? C18 C17 S2 124.10(18) . . ? C17 C18 C19 117.1(2) . . ? C17 C18 S6 122.81(18) . . ? C19 C18 S6 120.08(16) . . ? C20 C19 C18 120.7(2) . . ? C20 C19 S3 115.85(18) . . ? C18 C19 S3 123.10(17) . . ? C19 C20 C21 122.0(2) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 117.2(2) . . ? C22 C21 C29 121.7(2) . . ? C20 C21 C29 121.0(2) . . ? C21 C22 C17 121.9(2) . . ? C21 C22 H22 119.1 . . ? C17 C22 H22 119.1 . . ? C18 S6 C23 100.41(14) . . ? C24 C23 S6 113.0(2) . . ? C24 C23 H23A 109.0 . . ? S6 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? S6 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C28 117.8(2) . . ? C25 C24 C23 121.9(3) . . ? C28 C24 C23 120.2(3) . . ? N2 C25 C24 123.5(2) . . ? N2 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C25 N2 C26 117.7(2) . . ? C25 N2 Fe2 122.56(18) . . ? C26 N2 Fe2 119.78(17) . . ? N2 C26 C27 122.8(2) . . ? N2 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C27 C28 C24 119.2(3) . . ? C27 C28 H28 120.4 . . ? C24 C28 H28 120.4 . . ? C30A C29 C32A 116.9(8) . . ? C30 C29 C32 111.4(6) . . ? C30A C29 C21 115.1(4) . . ? C30 C29 C21 110.0(4) . . ? C32A C29 C21 112.1(7) . . ? C32 C29 C21 114.1(5) . . ? C30 C29 C31 109.9(5) . . ? C32A C29 C31 89.4(7) . . ? C32 C29 C31 105.4(6) . . ? C21 C29 C31 105.8(4) . . ? C30A C29 C31A 103.2(7) . . ? C32A C29 C31A 104.7(7) . . ? C21 C29 C31A 102.5(4) . . ? C31 C29 C31A 140.5(5) . . ? C19 S3 C33 105.83(11) . . ? C38 C33 C34 120.7(2) . . ? C38 C33 S3 115.84(17) . . ? C34 C33 S3 123.15(17) . . ? C35 C34 C33 117.6(2) . . ? C35 C34 S7 120.23(17) . . ? C33 C34 S7 122.21(18) . . ? C34 C35 C36 120.8(2) . . ? C34 C35 S4 123.25(17) . . ? C36 C35 S4 115.86(19) . . ? C37 C36 C35 121.7(2) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 117.3(2) . . ? C36 C37 C45 122.4(2) . . ? C38 C37 C45 120.1(2) . . ? C33 C38 C37 121.7(2) . . ? C33 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C34 S7 C39 99.14(13) . . ? C40 C39 S7 108.6(2) . . ? C40 C39 H39A 110.0 . . ? S7 C39 H39A 110.0 . . ? C40 C39 H39B 110.0 . . ? S7 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? C44 C40 C41 118.5(3) . . ? C44 C40 C39 119.5(3) . . ? C41 C40 C39 122.0(3) . . ? N3 C41 C40 122.9(3) . . ? N3 C41 H41 118.5 . . ? C40 C41 H41 118.5 . . ? C42 N3 C41 117.3(2) . . ? C42 N3 Fe2 117.56(18) . 1_645 ? C41 N3 Fe2 124.7(2) . 1_645 ? N3 C42 C43 123.1(3) . . ? N3 C42 H42 118.5 . . ? C43 C42 H42 118.5 . . ? C44 C43 C42 118.9(3) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C40 C44 C43 119.3(3) . . ? C40 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C37 109.9(2) . . ? C46 C45 C47 108.3(3) . . ? C37 C45 C47 112.2(2) . . ? C46 C45 C48 109.3(3) . . ? C37 C45 C48 108.1(2) . . ? C47 C45 C48 109.1(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C35 S4 C49 106.92(11) . . ? C50 C49 C54 120.4(2) . . ? C50 C49 S4 124.48(16) . . ? C54 C49 S4 114.72(18) . . ? C49 C50 C51 117.80(19) . . ? C49 C50 S8 121.01(17) . . ? C51 C50 S8 121.03(18) . . ? C52 C51 C50 120.6(2) . . ? C52 C51 S1 114.74(18) . . ? C50 C51 S1 124.47(17) . . ? C53 C52 C51 121.8(2) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 117.4(2) . . ? C52 C53 C61 118.6(2) . . ? C54 C53 C61 123.9(2) . . ? C53 C54 C49 121.8(2) . . ? C53 C54 H54 119.1 . . ? C49 C54 H54 119.1 . . ? C50 S8 C55 102.09(11) . . ? C56 C55 S8 108.33(18) . . ? C56 C55 H55A 110.0 . . ? S8 C55 H55A 110.0 . . ? C56 C55 H55B 110.0 . . ? S8 C55 H55B 110.0 . . ? H55A C55 H55B 108.4 . . ? C60 C56 C57 117.6(2) . . ? C60 C56 C55 121.4(2) . . ? C57 C56 C55 121.1(2) . . ? N4 C57 C56 123.6(2) . . ? N4 C57 H57 118.2 . . ? C56 C57 H57 118.2 . . ? C58 N4 C57 117.6(2) . . ? C58 N4 Fe1 119.02(16) . 1_565 ? C57 N4 Fe1 123.14(16) . 1_565 ? N4 C58 C59 122.7(2) . . ? N4 C58 H58 118.7 . . ? C59 C58 H58 118.7 . . ? C58 C59 C60 119.5(3) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C59 C60 C56 119.0(2) . . ? C59 C60 H60 120.5 . . ? C56 C60 H60 120.5 . . ? C63 C61 C53 112.3(2) . . ? C63 C61 C62 108.5(3) . . ? C53 C61 C62 107.9(2) . . ? C63 C61 C64 109.7(3) . . ? C53 C61 C64 109.1(2) . . ? C62 C61 C64 109.4(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O1 C65 H65A 109.5 . . ? O1 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O1 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C65 O1 O1 123.2(6) . 2_666 ? C65 O1 H1 109.5 . . ? O1 O1 H1 119.2 2_666 . ? H30D C30A H30E 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? H32D C32A H32E 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? H31D C31A H31E 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.91 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.092 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.087 _database_code_depnum_ccdc_archive 'CCDC 970403'