# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound1at153K _audit_creation_date 2013-09-26 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C62 H64 Cl4 Fe N6 O5 S2' _chemical_formula_sum 'C62 H64 Cl4 Fe N6 O5 S2' _chemical_formula_weight 1234.96 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z' 3 'x, -y+1/2, -z+1/2' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y, -z' 7 '-x, y-1/2, z-1/2' 8 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9124(7) _cell_length_b 40.300(4) _cell_length_c 35.5336(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 24218(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_temperature 153(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 2.348 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 0.677 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 5152 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_unetI/netI 0.1439 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 51639 _diffrn_reflns_theta_full 58.01 _diffrn_reflns_theta_max 58.01 _diffrn_reflns_theta_min 3.52 _diffrn_ambient_temperature 153(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4908 _reflns_number_total 16637 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 0.347 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 566 _refine_ls_number_reflns 16637 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1833 _refine_ls_R_factor_gt 0.0938 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2032 _refine_ls_wR_factor_ref 0.2304 _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. During the refinement, the restraint command 'dfix' was used to refine the distances of C-C bond, C-N bond and C-S bonds in the disorder of S1, S2, C23 and C54 atom. These restraint commands led to a restraint value (5), but it cannot be totally avoided in order to get a reasonable refinement. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.13471(8) 0.2500 0.2500 0.0986(5) Uani 1 2 d S . . Fe2 Fe 0.7500 0.0000 0.74209(4) 0.1995(14) Uani 1 2 d S . . S1 S 0.1113(3) 0.36540(10) 0.25041(9) 0.2612(19) Uani 1 1 d D . . S2 S 0.4810(7) -0.0301(3) 0.75078(19) 0.2624(11) Uani 1 1 d D . . N1 N 0.2182(2) 0.25048(14) 0.28984(9) 0.0922(15) Uani 1 1 d . . . N2 N 0.7303(5) 0.46277(15) 0.71473(18) 0.266(6) Uani 1 1 d G . . N3 N 1.0535(3) 0.25075(13) 0.29018(10) 0.0927(15) Uani 1 1 d . . . N4 N 0.7310(7) 0.03715(18) 0.69949(16) 0.194(4) Uani 1 1 d . . . N5 N 0.1293(5) 0.2970(3) 0.2484(3) 0.169(7) Uani 1 1 d . . . N6 N 0.6419(7) -0.0096(3) 0.7424(3) 0.195(5) Uani 1 1 d D . . C1 C 0.2754(3) 0.27360(18) 0.28988(11) 0.102(2) Uani 1 1 d . . . H1 H 0.2777 0.2878 0.2692 0.122 Uiso 1 1 calc R . . C2 C 0.3316(3) 0.27829(17) 0.31808(11) 0.110(2) Uani 1 1 d . . . H2 H 0.3695 0.2950 0.3172 0.132 Uiso 1 1 calc R . . C3 C 0.3257(3) 0.25454(18) 0.34926(11) 0.110(2) Uani 1 1 d . . . C4 C 0.2669(3) 0.23101(16) 0.34960(12) 0.0962(19) Uani 1 1 d . . . H4 H 0.2620 0.2163 0.3696 0.115 Uiso 1 1 calc R . . C5 C 0.2146(3) 0.22979(16) 0.31911(12) 0.096(2) Uani 1 1 d . . . H5 H 0.1752 0.2137 0.3193 0.116 Uiso 1 1 calc R . . C6 C 0.3850(3) 0.26096(15) 0.38068(12) 0.0969(19) Uani 1 1 d . . . H6 H 0.4238 0.2769 0.3767 0.116 Uiso 1 1 calc R . . C7 C 0.3843(2) 0.24515(15) 0.41316(11) 0.0870(18) Uani 1 1 d . . . H7 H 0.3433 0.2301 0.4169 0.104 Uiso 1 1 calc R . . C8 C 0.4413(3) 0.24872(17) 0.44395(12) 0.0819(16) Uani 1 1 d . . . C9 C 0.4918(3) 0.27540(15) 0.44474(10) 0.0856(16) Uani 1 1 d . . . H9 H 0.4862 0.2924 0.4273 0.103 Uiso 1 1 calc R . . C10 C 0.5523(3) 0.27694(14) 0.47224(12) 0.0849(16) Uani 1 1 d . . . H10 H 0.5876 0.2946 0.4713 0.102 Uiso 1 1 calc R . . C11 C 0.5613(3) 0.25385(12) 0.50001(10) 0.0595(12) Uani 1 1 d . . . C12 C 0.5040(3) 0.22853(14) 0.49995(10) 0.0750(15) Uani 1 1 d . . . H12 H 0.5055 0.2128 0.5191 0.090 Uiso 1 1 calc R . . C13 C 0.4455(3) 0.22582(14) 0.47277(11) 0.0754(14) Uani 1 1 d . . . H13 H 0.4091 0.2086 0.4740 0.091 Uiso 1 1 calc R . . C14 C 0.6324(3) 0.25539(12) 0.52537(10) 0.0640(12) Uani 1 1 d . . . C15 C 0.6318(3) 0.28507(15) 0.55214(11) 0.0726(15) Uani 1 1 d . . . C16 C 0.5773(3) 0.31027(17) 0.55142(12) 0.0891(18) Uani 1 1 d . . . H16 H 0.5356 0.3094 0.5344 0.107 Uiso 1 1 calc R . . C17 C 0.5838(4) 0.33754(16) 0.57641(15) 0.1034(19) Uani 1 1 d . . . H17 H 0.5479 0.3550 0.5752 0.124 Uiso 1 1 calc R . . C18 C 0.6430(4) 0.33790(18) 0.60219(13) 0.100(2) Uani 1 1 d . . . C19 C 0.6942(4) 0.31272(19) 0.60488(14) 0.102(2) Uani 1 1 d . . . H19 H 0.7331 0.3130 0.6234 0.123 Uiso 1 1 calc R . . C20 C 0.6894(3) 0.28654(16) 0.58047(12) 0.0889(17) Uani 1 1 d . . . H20 H 0.7254 0.2692 0.5827 0.107 Uiso 1 1 calc R . . C21 C 0.6456(4) 0.3711(3) 0.62477(17) 0.197(5) Uani 1 1 d . . . H21 H 0.6065 0.3871 0.6224 0.236 Uiso 1 1 calc R . . C22 C 0.6962(6) 0.3743(2) 0.6436(3) 0.200(4) Uiso 1 1 d D . . H22 H 0.7319 0.3568 0.6446 0.240 Uiso 1 1 calc R . . C23 C 0.7168(5) 0.40625(16) 0.6703(2) 0.231(5) Uani 1 1 d GD . . C24 C 0.6643(4) 0.4325(2) 0.66552(14) 0.243(6) Uani 1 1 d G . . H24 H 0.6247 0.4311 0.6475 0.291 Uiso 1 1 calc R . . C25 C 0.6710(5) 0.46068(16) 0.6877(2) 0.259(7) Uani 1 1 d G . . H25 H 0.6359 0.4782 0.6845 0.325 Uiso 1 1 calc R . . C26 C 0.7761(5) 0.40834(19) 0.6973(2) 0.263(8) Uani 1 1 d G . . H26 H 0.8113 0.3908 0.7005 0.322 Uiso 1 1 calc R . . C27 C 0.7828(4) 0.4366(2) 0.71953(15) 0.293(9) Uani 1 1 d G . . H27 H 0.8225 0.4380 0.7376 0.351 Uiso 1 1 calc R . . C28 C 1.0576(3) 0.27171(16) 0.31939(13) 0.0990(19) Uani 1 1 d . . . H28 H 1.0990 0.2869 0.3197 0.119 Uiso 1 1 calc R . . C29 C 1.0040(3) 0.27249(17) 0.34968(11) 0.096(2) Uani 1 1 d . . . H29 H 1.0099 0.2878 0.3690 0.115 Uiso 1 1 calc R . . C30 C 0.9438(3) 0.25050(16) 0.35009(12) 0.0904(17) Uani 1 1 d . . . C31 C 0.9356(3) 0.22729(18) 0.31920(11) 0.110(2) Uani 1 1 d . . . H31 H 0.8950 0.2118 0.3180 0.132 Uiso 1 1 calc R . . C32 C 0.9957(4) 0.23022(17) 0.29045(11) 0.100(2) Uani 1 1 d . . . H32 H 0.9920 0.2157 0.2701 0.120 Uiso 1 1 calc R . . C33 C 0.8842(2) 0.24773(15) 0.38080(11) 0.0857(17) Uani 1 1 d . . . H33 H 0.8438 0.2324 0.3773 0.103 Uiso 1 1 calc R . . C34 C 0.8830(3) 0.26487(14) 0.41240(12) 0.0909(17) Uani 1 1 d . . . H34 H 0.9230 0.2803 0.4163 0.109 Uiso 1 1 calc R . . C35 C 0.8222(3) 0.26117(14) 0.44222(11) 0.0757(16) Uani 1 1 d . . . C36 C 0.8222(3) 0.28269(14) 0.47189(12) 0.0787(15) Uani 1 1 d . . . H36 H 0.8616 0.2987 0.4740 0.094 Uiso 1 1 calc R . . C37 C 0.7617(3) 0.28054(14) 0.49956(10) 0.0781(15) Uani 1 1 d . . . H37 H 0.7616 0.2954 0.5196 0.094 Uiso 1 1 calc R . . C38 C 0.7043(3) 0.25720(13) 0.49730(11) 0.0666(14) Uani 1 1 d . . . C39 C 0.7064(3) 0.23476(14) 0.46745(12) 0.0811(16) Uani 1 1 d . . . H39 H 0.6679 0.2184 0.4657 0.097 Uiso 1 1 calc R . . C40 C 0.7654(3) 0.23666(14) 0.44036(12) 0.0832(16) Uani 1 1 d . . . H40 H 0.7667 0.2213 0.4208 0.100 Uiso 1 1 calc R . . C41 C 0.6379(3) 0.22376(14) 0.55013(11) 0.0698(14) Uani 1 1 d . . . C42 C 0.6980(3) 0.20099(17) 0.54568(12) 0.0934(18) Uani 1 1 d . . . H42 H 0.7357 0.2041 0.5270 0.112 Uiso 1 1 calc R . . C43 C 0.7025(3) 0.17386(16) 0.56864(14) 0.0957(18) Uani 1 1 d . . . H43 H 0.7424 0.1583 0.5647 0.115 Uiso 1 1 calc R . . C44 C 0.6491(4) 0.16893(17) 0.59775(14) 0.0975(19) Uani 1 1 d . . . C45 C 0.5896(4) 0.19158(19) 0.60163(14) 0.0971(19) Uani 1 1 d . . . H45 H 0.5515 0.1884 0.6201 0.116 Uiso 1 1 calc R . . C46 C 0.5849(3) 0.21906(15) 0.57877(11) 0.0801(16) Uani 1 1 d . . . H46 H 0.5453 0.2346 0.5828 0.096 Uiso 1 1 calc R . . C47 C 0.6520(5) 0.14137(19) 0.62325(17) 0.123(3) Uani 1 1 d . . . H47 H 0.6148 0.1407 0.6425 0.147 Uiso 1 1 calc R . . C48 C 0.7023(5) 0.1176(2) 0.62136(15) 0.132(3) Uani 1 1 d . . . H48 H 0.7368 0.1184 0.6010 0.158 Uiso 1 1 calc R . . C49 C 0.7132(7) 0.0884(2) 0.64764(19) 0.164(4) Uani 1 1 d . . . C50 C 0.7788(7) 0.0671(2) 0.6449(2) 0.180(4) Uani 1 1 d . . . H50 H 0.8157 0.0693 0.6257 0.216 Uiso 1 1 calc R . . C51 C 0.7857(6) 0.0429(2) 0.6719(2) 0.164(4) Uani 1 1 d . . . H51 H 0.8305 0.0295 0.6713 0.197 Uiso 1 1 calc R . . C52 C 0.6545(7) 0.0844(2) 0.6750(2) 0.204(5) Uani 1 1 d . . . H52 H 0.6106 0.0982 0.6763 0.245 Uiso 1 1 calc R . . C53 C 0.6665(8) 0.0575(3) 0.7009(2) 0.206(5) Uani 1 1 d . . . H53 H 0.6286 0.0537 0.7194 0.248 Uiso 1 1 calc R . . C54 C 0.5860(9) -0.0132(6) 0.7454(5) 0.265(9) Uani 1 1 d D . . C55 C 0.1324(9) 0.3217(5) 0.2508(6) 0.173(8) Uani 1 1 d D . . 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 0.0624(8) 0.2052(16) 0.0285(5) 0.0057(10) 0.000 0.000 Fe2 0.400(5) 0.1321(16) 0.0665(9) 0.000 0.000 0.058(3) S1 0.307(5) 0.240(4) 0.236(3) 0.042(3) -0.074(3) -0.067(3) S2 0.306(5) 0.250(3) 0.21(4) 0.040(3) -0.073(4) -0.068(3) N1 0.046(3) 0.209(5) 0.0217(19) 0.019(2) 0.0031(16) -0.011(3) N2 0.52(2) 0.101(6) 0.178(8) -0.020(5) 0.067(10) -0.080(8) N3 0.042(3) 0.197(5) 0.039(2) -0.014(3) -0.0095(19) -0.020(3) N4 0.371(14) 0.150(6) 0.061(4) 0.007(4) 0.036(5) 0.070(7) N5 0.038(3) 0.45(2) 0.024(3) -0.023(10) 0.003(2) -0.054(8) N6 0.309(16) 0.171(8) 0.101(5) -0.008(5) 0.068(8) 0.005(13) C1 0.065(4) 0.216(7) 0.024(2) 0.007(3) 0.005(2) -0.003(4) C2 0.073(4) 0.219(7) 0.037(3) 0.013(3) -0.002(2) -0.040(4) C3 0.068(4) 0.236(7) 0.024(2) 0.019(3) 0.009(2) 0.006(5) C4 0.059(4) 0.187(6) 0.042(3) 0.007(3) 0.015(3) -0.036(4) C5 0.052(3) 0.207(6) 0.031(2) -0.008(3) 0.005(2) -0.009(4) C6 0.067(4) 0.179(6) 0.044(3) 0.012(3) -0.003(2) -0.013(4) C7 0.026(3) 0.202(6) 0.034(2) 0.000(3) 0.0004(18) 0.002(3) C8 0.046(3) 0.155(5) 0.046(3) -0.009(3) 0.008(2) -0.001(4) C9 0.096(4) 0.129(5) 0.032(2) 0.014(3) -0.012(3) -0.007(4) C10 0.079(4) 0.129(5) 0.046(3) -0.006(3) 0.004(3) -0.014(3) C11 0.048(3) 0.109(4) 0.0206(19) 0.013(2) 0.0068(19) 0.005(3) C12 0.048(3) 0.144(5) 0.033(2) 0.007(3) -0.001(2) -0.009(3) C13 0.056(3) 0.131(4) 0.039(2) 0.010(3) 0.011(2) -0.004(3) C14 0.048(3) 0.105(4) 0.039(2) -0.009(3) 0.001(2) 0.002(3) C15 0.049(3) 0.133(5) 0.035(2) 0.000(3) 0.012(2) -0.001(3) C16 0.071(4) 0.150(6) 0.046(3) 0.006(3) 0.005(3) -0.024(4) C17 0.121(6) 0.124(5) 0.066(3) -0.018(4) 0.017(4) 0.002(4) C18 0.108(5) 0.161(6) 0.032(3) -0.044(4) -0.002(3) -0.021(5) C19 0.081(4) 0.175(6) 0.050(3) -0.030(4) -0.011(3) 0.015(5) C20 0.060(3) 0.161(5) 0.046(3) -0.010(3) -0.012(2) 0.002(4) C21 0.111(6) 0.405(16) 0.073(4) 0.055(7) -0.042(4) -0.080(8) C22 0.122(6) 0.395(16) 0.067(4) 0.065(7) -0.035(4) -0.086(8) C23 0.381(14) 0.235(13) 0.095(6) -0.094(8) 0.020(5) -0.071(10) C24 0.390(17) 0.239(11) 0.098(5) -0.091(6) 0.019(7) -0.068(12) C25 0.399(16) 0.257(15) 0.099(7) -0.111(9) 0.032(6) -0.075(14) C26 0.410(18) 0.270(14) 0.101(8) -0.121(8) 0.029(7) -0.079(12) C27 0.57(3) 0.202(12) 0.108(6) -0.068(7) 0.021(9) -0.138(14) C28 0.076(4) 0.174(6) 0.048(3) 0.013(4) -0.019(3) -0.013(4) C29 0.048(3) 0.207(6) 0.033(2) -0.007(3) 0.006(2) -0.017(4) C30 0.047(3) 0.176(5) 0.048(3) 0.003(3) -0.009(2) 0.009(4) C31 0.068(4) 0.228(7) 0.034(2) -0.015(3) -0.002(2) 0.002(4) C32 0.073(4) 0.197(6) 0.032(2) -0.012(3) -0.012(3) 0.015(5) C33 0.027(3) 0.192(6) 0.038(2) 0.004(3) 0.0075(18) -0.015(3) C34 0.086(4) 0.147(5) 0.041(3) 0.002(3) 0.010(2) -0.018(4) C35 0.046(3) 0.148(5) 0.033(2) -0.006(3) 0.001(2) -0.005(3) C36 0.052(3) 0.133(5) 0.051(3) -0.012(3) -0.007(2) -0.014(3) C37 0.058(3) 0.145(5) 0.032(2) -0.013(3) 0.002(2) -0.003(4) C38 0.040(3) 0.116(4) 0.043(2) 0.003(3) -0.003(2) -0.015(3) C39 0.059(3) 0.135(5) 0.049(3) -0.012(3) 0.005(2) -0.010(3) C40 0.055(3) 0.141(5) 0.053(3) -0.016(3) 0.005(3) -0.012(3) C41 0.041(3) 0.132(4) 0.036(2) -0.001(3) -0.008(2) 0.009(3) C42 0.076(4) 0.169(6) 0.035(2) 0.003(3) -0.010(3) -0.001(4) C43 0.102(5) 0.143(5) 0.042(3) -0.002(3) -0.004(3) 0.006(4) C44 0.122(6) 0.125(5) 0.045(3) 0.018(4) -0.029(3) 0.004(5) C45 0.081(5) 0.163(6) 0.048(3) 0.006(4) -0.001(3) -0.009(4) C46 0.065(4) 0.147(5) 0.028(2) 0.002(3) 0.002(2) -0.008(3) C47 0.161(8) 0.132(6) 0.075(4) -0.005(4) 0.003(4) 0.037(5) C48 0.186(9) 0.165(7) 0.045(3) 0.012(4) 0.002(4) 0.005(6) C49 0.260(13) 0.178(9) 0.056(4) 0.016(5) -0.008(6) 0.021(8) C50 0.277(14) 0.158(8) 0.104(6) 0.055(6) 0.020(7) 0.038(8) C51 0.236(11) 0.156(7) 0.101(5) -0.001(6) -0.015(6) 0.066(7) C52 0.358(16) 0.184(8) 0.069(4) 0.047(5) 0.035(7) 0.044(9) C53 0.334(17) 0.199(10) 0.084(6) -0.016(7) 0.046(7) 0.059(10) C54 0.34(2) 0.275(18) 0.184(11) 0.045(10) 0.142(14) 0.084(19) C55 0.106(7) 0.37(2) 0.046(5) 0.003(10) -0.012(4) -0.103(11) _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 N1 2.000(4) 3 ? Fe1 N1 2.000(4) . ? Fe1 N3 1.981(4) 3_455 ? Fe1 N3 1.981(4) 1_455 ? Fe1 N5 1.899(14) . ? Fe1 N5 1.899(14) 3 ? Fe2 N2 2.173(4) 3_556 ? Fe2 N2 2.173(4) 4_646 ? Fe2 N4 2.153(6) . ? Fe2 N4 2.153(6) 2_655 ? Fe2 N6 1.870(12) . ? Fe2 N6 1.870(12) 2_655 ? S1 C55 1.79(2) . ? S2 C54 1.916(14) . ? N1 C5 1.334(6) . ? N1 C1 1.343(7) . ? N2 C27 1.3900 . ? N2 C25 1.3900 . ? N2 Fe2 2.173(4) 3_556 ? N3 C32 1.281(7) . ? N3 C28 1.340(7) . ? N3 Fe1 1.981(4) 1_655 ? N4 C53 1.365(12) . ? N4 C51 1.369(11) . ? N5 C55 1.00(2) . ? N6 C54 0.960(15) . ? C1 C2 1.394(7) . ? C2 C3 1.467(8) . ? C3 C4 1.374(7) . ? C3 C6 1.523(7) . ? C4 C5 1.400(6) . ? C6 C7 1.318(6) . ? C7 C8 1.465(6) . ? C8 C9 1.373(7) . ? C8 C13 1.381(7) . ? C9 C10 1.416(6) . ? C10 C11 1.365(6) . ? C11 C12 1.407(6) . ? C11 C14 1.503(6) . ? C12 C13 1.388(6) . ? C14 C15 1.528(7) . ? C14 C41 1.552(7) . ? C14 C38 1.575(6) . ? C15 C16 1.372(7) . ? C15 C20 1.402(6) . ? C16 C17 1.417(7) . ? C17 C18 1.358(8) . ? C18 C19 1.337(8) . ? C18 C21 1.559(12) . ? C19 C20 1.368(7) . ? C21 C22 1.095(10) . ? C23 C24 1.3900 . ? C23 C22 1.636(9) . ? C24 C25 1.3900 . ? C26 C23 1.3900 . ? C27 C26 1.3900 . ? C28 C29 1.408(6) . ? C29 C30 1.350(7) . ? C30 C31 1.449(8) . ? C30 C33 1.490(6) . ? C31 C32 1.446(7) . ? C33 C34 1.318(6) . ? C34 C35 1.483(6) . ? C35 C36 1.365(6) . ? C35 C40 1.380(7) . ? C36 C37 1.421(6) . ? C37 C38 1.354(6) . ? C38 C39 1.394(6) . ? C39 C40 1.389(6) . ? C41 C46 1.368(6) . ? C41 C42 1.379(7) . ? C42 C43 1.365(8) . ? C43 C44 1.388(8) . ? C44 C45 1.364(7) . ? C44 C47 1.434(8) . ? C45 C46 1.376(7) . ? C47 C48 1.284(8) . ? C48 C49 1.513(11) . ? C49 C52 1.400(12) . ? C49 C50 1.407(11) . ? C50 C51 1.372(10) . ? C52 C53 1.440(11) . ? 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 N5 Fe1 N5 174.5(5) . 3 ? N5 Fe1 N3 87.7(3) . 3_455 ? N5 Fe1 N3 88.5(3) 3 3_455 ? N5 Fe1 N3 88.5(3) . 1_455 ? N5 Fe1 N3 87.7(3) 3 1_455 ? N3 Fe1 N3 92.2(2) 3_455 1_455 ? N5 Fe1 N1 91.2(3) . 3 ? N5 Fe1 N1 92.7(3) 3 3 ? N3 Fe1 N1 88.82(15) 3_455 3 ? N3 Fe1 N1 178.91(19) 1_455 3 ? N5 Fe1 N1 92.7(3) . . ? N5 Fe1 N1 91.2(3) 3 . ? N3 Fe1 N1 178.91(19) 3_455 . ? N3 Fe1 N1 88.82(15) 1_455 . ? N1 Fe1 N1 90.2(2) 3 . ? N6 Fe2 N6 179.3(6) . 2_655 ? N6 Fe2 N4 89.9(5) . . ? N6 Fe2 N4 90.4(5) 2_655 . ? N6 Fe2 N4 90.4(5) . 2_655 ? N6 Fe2 N4 89.9(5) 2_655 2_655 ? N4 Fe2 N4 90.7(4) . 2_655 ? N6 Fe2 N2 89.3(4) . 3_556 ? N6 Fe2 N2 90.2(5) 2_655 3_556 ? N4 Fe2 N2 89.6(3) . 3_556 ? N4 Fe2 N2 179.6(4) 2_655 3_556 ? N6 Fe2 N2 90.2(5) . 4_646 ? N6 Fe2 N2 89.3(4) 2_655 4_646 ? N4 Fe2 N2 179.6(4) . 4_646 ? N4 Fe2 N2 89.6(3) 2_655 4_646 ? N2 Fe2 N2 90.1(4) 3_556 4_646 ? C5 N1 C1 117.7(4) . . ? C5 N1 Fe1 120.9(4) . . ? C1 N1 Fe1 121.1(4) . . ? C27 N2 C25 120.0 . . ? C27 N2 Fe2 109.8(6) . 3_556 ? C25 N2 Fe2 129.8(6) . 3_556 ? C32 N3 C28 116.2(5) . . ? C32 N3 Fe1 121.6(4) . 1_655 ? C28 N3 Fe1 122.1(4) . 1_655 ? C53 N4 C51 117.8(8) . . ? C53 N4 Fe2 120.7(8) . . ? C51 N4 Fe2 121.3(8) . . ? C55 N5 Fe1 172.3(19) . . ? C54 N6 Fe2 173.9(18) . . ? N1 C1 C2 125.9(5) . . ? C1 C2 C3 114.1(5) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 C6 125.9(5) . . ? C2 C3 C6 113.5(6) . . ? C3 C4 C5 118.3(5) . . ? N1 C5 C4 123.6(5) . . ? C7 C6 C3 123.7(5) . . ? C6 C7 C8 126.9(5) . . ? C9 C8 C13 118.5(4) . . ? C9 C8 C7 120.1(5) . . ? C13 C8 C7 121.5(6) . . ? C8 C9 C10 119.8(5) . . ? C11 C10 C9 123.4(5) . . ? C10 C11 C12 114.6(4) . . ? C10 C11 C14 119.7(5) . . ? C12 C11 C14 125.5(4) . . ? C13 C12 C11 123.3(4) . . ? C8 C13 C12 120.1(5) . . ? C11 C14 C15 113.6(4) . . ? C11 C14 C41 110.7(4) . . ? C15 C14 C41 106.9(3) . . ? C11 C14 C38 103.9(3) . . ? C15 C14 C38 111.3(4) . . ? C41 C14 C38 110.5(4) . . ? C16 C15 C20 116.7(5) . . ? C16 C15 C14 124.9(4) . . ? C20 C15 C14 118.4(5) . . ? C15 C16 C17 120.7(5) . . ? C18 C17 C16 119.2(6) . . ? C19 C18 C17 121.2(6) . . ? C19 C18 C21 126.5(6) . . ? C17 C18 C21 112.2(7) . . ? C18 C19 C20 120.1(6) . . ? C19 C20 C15 121.9(6) . . ? C22 C21 C18 116.2(11) . . ? C21 C22 C23 128.1(12) . . ? C26 C23 C24 120.0 . . ? C26 C23 C22 127.0(8) . . ? C24 C23 C22 112.9(8) . . ? C25 C24 C23 120.0 . . ? C24 C25 N2 120.0 . . ? C23 C26 C27 120.0 . . ? C26 C27 N2 120.0 . . ? N3 C28 C29 125.0(5) . . ? C30 C29 C28 118.7(5) . . ? C29 C30 C31 119.2(5) . . ? C29 C30 C33 124.6(5) . . ? C31 C30 C33 116.3(5) . . ? C32 C31 C30 114.6(6) . . ? N3 C32 C31 126.5(5) . . ? C34 C33 C30 126.5(5) . . ? C33 C34 C35 124.5(5) . . ? C36 C35 C40 119.5(4) . . ? C36 C35 C34 119.2(5) . . ? C40 C35 C34 121.3(4) . . ? C35 C36 C37 119.7(5) . . ? C38 C37 C36 121.1(4) . . ? C37 C38 C39 118.5(4) . . ? C37 C38 C14 123.3(4) . . ? C39 C38 C14 118.1(4) . . ? C40 C39 C38 120.6(5) . . ? C35 C40 C39 120.4(5) . . ? C46 C41 C42 118.5(5) . . ? C46 C41 C14 119.7(5) . . ? C42 C41 C14 121.7(4) . . ? C43 C42 C41 120.3(5) . . ? C42 C43 C44 121.5(6) . . ? C45 C44 C43 117.3(5) . . ? C45 C44 C47 118.7(7) . . ? C43 C44 C47 124.0(7) . . ? C44 C45 C46 121.4(5) . . ? C41 C46 C45 120.8(5) . . ? C48 C47 C44 124.6(7) . . ? C47 C48 C49 129.0(8) . . ? C52 C49 C50 122.4(9) . . ? C52 C49 C48 115.6(10) . . ? C50 C49 C48 122.0(9) . . ? C51 C50 C49 117.1(9) . . ? N4 C51 C50 124.2(9) . . ? C49 C52 C53 115.6(10) . . ? N4 C53 C52 122.8(10) . . ? N6 C54 S2 168(3) . . ? N5 C55 S1 164.9(19) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.003 -0.001 -0.015 16898.5 1574.9 _platon_squeeze_details ; Approximately 69.8% of the unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 1574.9 electrons per unit cell. According to the final formula which was calculated from TGA combined with elemental analysis data, these electrons were assigned to be 40 methanol and 16 dichloromethane molecules per unit cell. The F(000) value with sovent is 5152, Mu (mm^-1) value with sovent is 2.348,and crystal density with solvent is 0.677. ; _database_code_depnum_ccdc_archive 'CCDC 950638' ####################################################################### # # 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_compound1at200K _audit_creation_date 2013-09-26 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C62 H64 Cl4 Fe N6 O5 S2' _chemical_formula_sum 'C62 H64 Cl4 Fe N6 O5 S2' _chemical_formula_weight 1234.96 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 50 _space_group_name_H-M_alt 'P b a n' _space_group_name_Hall '-P 2ab 2b' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y+1/2, z' 3 'x, -y+1/2, -z' 4 '-x+1/2, y, -z' 5 '-x, -y, -z' 6 'x-1/2, y-1/2, -z' 7 '-x, y-1/2, z' 8 'x-1/2, -y, z' _cell_length_a 17.2737(11) _cell_length_b 35.4221(17) _cell_length_c 20.8250(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12742.2(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_temperature 200(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 0.644 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 2576 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_unetI/netI 0.1481 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 27965 _diffrn_reflns_theta_full 65.69 _diffrn_reflns_theta_max 65.69 _diffrn_reflns_theta_min 3.55 _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3092 _reflns_number_total 10446 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.373 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.042 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 10446 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2040 _refine_ls_R_factor_gt 0.1110 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2554 _refine_ls_wR_factor_ref 0.2977 _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. During the refinement, the restraint command 'dfix' was used to refine the distances of N-C in the disorder of C29 atom. This restraint command led to a restraint value (1), but it cannot be totally avoided in order to get a reasonable refinement. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.2500 0.2500 0.5000 0.0990(7) Uani 1 4 d S . . Fe2 Fe 0.7500 0.7500 1.0000 0.303(3) Uani 1 4 d S . . S1 S 0.2950(8) 0.2413(4) 0.7188(8) 0.254(8) Uani 0.50 1 d P . . S2 S 0.4846(9) 0.7524(3) 0.9517(6) 0.255(5) Uani 0.50 1 d P . . N1 N 0.3377(2) 0.29214(8) 0.5008(2) 0.1085(15) Uani 1 1 d . . . N2 N 0.7477(5) 0.70591(12) 0.9242(2) 0.304(3) Uani 1 1 d G . . N3 N 0.2500 0.2500 0.5962(7) 0.164(5) Uani 1 2 d S . . N4 N 0.6357(8) 0.7500 1.0000 0.264(7) Uani 1 2 d SD . . C1 C 0.3334(2) 0.32170(11) 0.4594(3) 0.1003(16) Uani 1 1 d . . . H1 H 0.2943 0.3219 0.4286 0.120 Uiso 1 1 calc R . . C2 C 0.3850(3) 0.35146(10) 0.4615(2) 0.0906(14) Uani 1 1 d . . . H2 H 0.3800 0.3712 0.4324 0.109 Uiso 1 1 calc R . . C3 C 0.4414(3) 0.35215(10) 0.5044(3) 0.0948(16) Uani 1 1 d . . . C4 C 0.4475(2) 0.32175(11) 0.5488(3) 0.125(2) Uani 1 1 d . . . H4 H 0.4860 0.3214 0.5800 0.150 Uiso 1 1 calc R . . C5 C 0.3940(3) 0.29274(12) 0.5441(3) 0.116(2) Uani 1 1 d . . . H5 H 0.3978 0.2727 0.5727 0.139 Uiso 1 1 calc R . . C6 C 0.5018(3) 0.38235(12) 0.5133(2) 0.1017(16) Uani 1 1 d . . . H6 H 0.5419 0.3775 0.5419 0.122 Uiso 1 1 calc R . . C7 C 0.5021(3) 0.41491(11) 0.4837(2) 0.0927(14) Uani 1 1 d . . . H7 H 0.4610 0.4199 0.4560 0.111 Uiso 1 1 calc R . . C8 C 0.5616(2) 0.44440(10) 0.4902(2) 0.0770(12) Uani 1 1 d . . . C9 C 0.5640(2) 0.47349(10) 0.4463(2) 0.0887(14) Uani 1 1 d . . . H9 H 0.5273 0.4751 0.4137 0.106 Uiso 1 1 calc R . . C10 C 0.6236(2) 0.50099(10) 0.4515(2) 0.0785(12) Uani 1 1 d . . . H10 H 0.6242 0.5209 0.4225 0.094 Uiso 1 1 calc R . . C11 C 0.6796(2) 0.49941(9) 0.4972(2) 0.0627(10) Uani 1 1 d . . . C12 C 0.6753(2) 0.47018(10) 0.5403(2) 0.0876(14) Uani 1 1 d . . . H12 H 0.7131 0.4678 0.5719 0.105 Uiso 1 1 calc R . . C13 C 0.6147(3) 0.44374(10) 0.5377(2) 0.0796(12) Uani 1 1 d . . . H13 H 0.6111 0.4254 0.5695 0.095 Uiso 1 1 calc R . . C14 C 0.7500 0.52592(13) 0.5000 0.0673(15) Uani 1 2 d S . . C15 C 0.7451(2) 0.55140(9) 0.5589(2) 0.0664(11) Uani 1 1 d . . . C16 C 0.8011(3) 0.58057(10) 0.5638(2) 0.0813(12) Uani 1 1 d . . . H16 H 0.8378 0.5837 0.5316 0.098 Uiso 1 1 calc R . . C17 C 0.8010(3) 0.60452(13) 0.6166(3) 0.0955(15) Uani 1 1 d . . . H17 H 0.8385 0.6233 0.6194 0.114 Uiso 1 1 calc R . . C18 C 0.7502(3) 0.60160(12) 0.6622(3) 0.0991(15) Uani 1 1 d . . . C19 C 0.6914(3) 0.57315(14) 0.6582(3) 0.1051(16) Uani 1 1 d . . . H19 H 0.6538 0.5712 0.6900 0.126 Uiso 1 1 calc R . . C20 C 0.6917(3) 0.54893(11) 0.6070(2) 0.0826(12) Uani 1 1 d . . . H20 H 0.6541 0.5302 0.6049 0.099 Uiso 1 1 calc R . . C21 C 0.7580(5) 0.6286(2) 0.7210(4) 0.156(3) Uani 1 1 d . . . H21 H 0.7946 0.6478 0.7194 0.188 Uiso 1 1 calc R . . C22 C 0.7203(5) 0.6258(2) 0.7665(4) 0.176(3) Uani 1 1 d . . . H22 H 0.6817 0.6076 0.7705 0.211 Uiso 1 1 calc R . . C23 C 0.7392(5) 0.65564(15) 0.8220(3) 0.319(9) Uani 1 1 d G . . C24 C 0.7983(4) 0.6822(2) 0.8243(3) 0.317(6) Uani 1 1 d G . . H24 H 0.8351 0.6832 0.7917 0.380 Uiso 1 1 calc R . . C25 C 0.8025(4) 0.70736(15) 0.8754(3) 0.324(8) Uani 1 1 d G . . H25 H 0.8421 0.7251 0.8771 0.388 Uiso 1 1 calc R . . C26 C 0.6886(4) 0.67930(17) 0.9218(3) 0.316(6) Uani 1 1 d G . . H26 H 0.6518 0.6784 0.9544 0.380 Uiso 1 1 calc R . . C27 C 0.6843(4) 0.65418(15) 0.8707(4) 0.355(10) Uani 1 1 d G . . H27 H 0.6448 0.6364 0.8691 0.426 Uiso 1 1 calc R . . C28 C 0.2500 0.2500 0.6397(10) 0.227(10) Uani 1 2 d S . . C29 C 0.5711(12) 0.7500 1.0000 0.240(6) Uani 1 2 d SD . . 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 0.0663(9) 0.0409(7) 0.189(2) 0.000 0.000 0.000 Fe2 0.764(10) 0.0753(11) 0.0753(12) 0.000 0.000 0.000 S1 0.33(2) 0.325(15) 0.103(5) -0.001(8) -0.019(8) -0.058(15) S2 0.34(3) 0.321(3) 0.126(3) -0.01(3) -0.04(2) 0.01(2) N1 0.079(3) 0.0394(17) 0.207(5) 0.026(2) -0.009(3) 0.0069(17) N2 0.766(10) 0.0751(11) 0.0755(12) 0.000 0.000 0.000 N3 0.075(4) 0.016(2) 0.40(2) 0.000 0.000 0.003(2) N4 0.54(3) 0.127(7) 0.154(10) -0.020(5) 0.000 0.000 C1 0.055(2) 0.063(3) 0.183(5) -0.011(3) -0.024(3) -0.004(2) C2 0.069(3) 0.061(2) 0.143(4) 0.002(2) -0.023(3) -0.001(2) C3 0.053(2) 0.051(2) 0.181(5) 0.015(3) 0.012(3) -0.0054(19) C4 0.059(3) 0.060(3) 0.258(7) 0.019(3) -0.010(4) -0.010(2) C5 0.064(3) 0.076(3) 0.209(6) 0.033(3) -0.021(4) 0.007(3) C6 0.068(3) 0.068(3) 0.169(5) 0.004(3) -0.007(3) -0.001(2) C7 0.075(3) 0.067(3) 0.136(4) 0.005(2) -0.001(3) 0.004(2) C8 0.056(2) 0.059(2) 0.117(4) -0.001(2) -0.010(3) -0.0121(19) C9 0.057(3) 0.065(2) 0.145(4) 0.019(3) -0.016(3) 0.000(2) C10 0.068(3) 0.062(2) 0.108(3) 0.015(2) -0.011(3) -0.003(2) C11 0.070(3) 0.0448(18) 0.074(3) 0.0006(19) -0.005(3) 0.0035(16) C12 0.072(3) 0.065(2) 0.126(4) 0.009(3) -0.008(3) 0.002(2) C13 0.083(3) 0.065(2) 0.091(3) 0.011(2) 0.003(3) -0.015(2) C14 0.048(3) 0.058(3) 0.097(4) 0.000 -0.014(3) 0.000 C15 0.048(2) 0.059(2) 0.094(3) -0.013(2) 0.010(3) 0.0130(19) C16 0.092(3) 0.065(2) 0.088(3) -0.022(2) -0.010(3) 0.008(2) C17 0.096(4) 0.089(3) 0.101(4) -0.005(3) 0.030(3) -0.003(2) C18 0.123(4) 0.069(3) 0.105(4) -0.034(3) -0.013(4) 0.008(3) C19 0.109(4) 0.099(3) 0.107(4) -0.022(3) 0.003(3) 0.021(3) C20 0.086(3) 0.070(2) 0.093(3) -0.011(2) -0.001(3) 0.003(2) C21 0.179(8) 0.151(6) 0.140(6) 0.021(5) 0.056(6) 0.024(5) C22 0.224(10) 0.117(5) 0.187(9) -0.005(6) -0.009(7) -0.028(5) C23 0.71(3) 0.125(6) 0.104(6) -0.012(5) -0.054(10) 0.050(9) C24 0.674(19) 0.115(4) 0.163(6) -0.018(4) -0.053(8) 0.007(7) C25 0.69(3) 0.174(7) 0.103(6) -0.042(6) 0.023(10) 0.008(11) C26 0.674(19) 0.112(4) 0.165(6) -0.015(4) -0.050(8) 0.006(7) C27 0.75(3) 0.148(7) 0.173(9) -0.064(7) -0.171(14) 0.086(11) C28 0.27(2) 0.207(15) 0.208(17) 0.000 0.000 -0.038(11) C29 0.29(3) 0.227(12) 0.218(14) 0.000 0.000 -0.029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.127(3) . ? Fe1 N1 2.127(3) 4_556 ? Fe1 N1 2.127(3) 2 ? Fe1 N1 2.127(3) 3_556 ? Fe2 N2 2.220(4) 3_567 ? Fe2 N2 2.220(4) 2_665 ? Fe2 N2 2.220(4) . ? Fe2 N2 2.220(4) 4_657 ? Fe1 N3 2.004(16) . ? Fe1 N3 2.004(16) 3_556 ? Fe2 N4 1.972(14) . ? Fe2 N4 1.972(14) 2_665 ? S1 S1 1.68(3) 2 ? S1 C28 1.85(3) . ? S2 C29 1.802(18) . ? S2 S2 2.01(3) 3_567 ? N1 C1 1.357(6) . ? N1 C5 1.326(6) . ? N2 C26 1.3900 . ? N3 C28 0.93(2) . ? N4 C29 1.13(2) . ? C1 C2 1.383(6) . ? C2 C3 1.323(6) . ? C4 C3 1.425(6) . ? C5 C4 1.385(6) . ? C6 C3 1.505(6) . ? C6 C7 1.307(6) . ? C7 C8 1.474(6) . ? C8 C13 1.349(5) . ? C8 C9 1.379(5) . ? C10 C9 1.420(5) . ? C10 C11 1.359(5) . ? C11 C12 1.373(5) . ? C12 C13 1.405(5) . ? C14 C11 1.537(5) . ? C14 C11 1.537(5) 4_656 ? C14 C15 1.526(5) 4_656 ? C14 C15 1.526(5) . ? C15 C20 1.366(5) . ? C15 C16 1.418(5) . ? C16 C17 1.388(6) . ? C17 C18 1.296(6) . ? C19 C20 1.369(6) . ? C19 C18 1.434(7) . ? C21 C22 1.152(9) . ? C21 C18 1.562(9) . ? C22 C23 1.600(8) . ? C23 C24 1.3900 . ? C25 N2 1.3900 . ? C25 C24 1.3900 . ? C26 C27 1.3900 . ? C27 C23 1.3900 . ? C28 S1 1.83(2) 2 ? C29 S2 1.80(18) 3_567 ? 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 N3 Fe1 N3 180.0 . 3_556 ? N3 Fe1 N1 89.55(13) . . ? N3 Fe1 N1 90.46(13) 3_556 . ? N3 Fe1 N1 90.46(13) . 4_556 ? N3 Fe1 N1 89.55(13) 3_556 4_556 ? N1 Fe1 N1 90.88(18) . 4_556 ? N3 Fe1 N1 89.55(13) . 2 ? N3 Fe1 N1 90.46(13) 3_556 2 ? N1 Fe1 N1 179.1(3) . 2 ? N1 Fe1 N1 89.12(18) 4_556 2 ? N3 Fe1 N1 90.46(13) . 3_556 ? N3 Fe1 N1 89.55(13) 3_556 3_556 ? N1 Fe1 N1 89.12(18) . 3_556 ? N1 Fe1 N1 179.1(3) 4_556 3_556 ? N1 Fe1 N1 90.88(18) 2 3_556 ? N4 Fe2 N4 180.0 . 2_665 ? N4 Fe2 N2 88.9(7) . 3_567 ? N4 Fe2 N2 91.0(7) 2_665 3_567 ? N4 Fe2 N2 91.0(5) . 2_665 ? N4 Fe2 N2 88.9(5) 2_665 2_665 ? N2 Fe2 N2 90.5(8) 3_567 2_665 ? N4 Fe2 N2 88.9(2) . . ? N4 Fe2 N2 91.0(2) 2_665 . ? N2 Fe2 N2 177.8(9) 3_567 . ? N2 Fe2 N2 89.5(4) 2_665 . ? N4 Fe2 N2 91.0(5) . 4_657 ? N4 Fe2 N2 88.9(5) 2_665 4_657 ? N2 Fe2 N2 89.5(8) 3_567 4_657 ? N2 Fe2 N2 177.8(9) 2_665 4_657 ? N2 Fe2 N2 90.5(4) . 4_657 ? S1 S1 C28 63.0(5) 2 . ? C29 S2 S2 56.2(6) . 3_567 ? C5 N1 C1 117.4(4) . . ? C5 N1 Fe1 122.6(3) . . ? C1 N1 Fe1 119.7(3) . . ? C25 N2 C26 120.0 . . ? C25 N2 Fe2 118.7(4) . . ? C26 N2 Fe2 121.0(4) . . ? C28 N3 Fe1 180.0 . . ? C29 N4 Fe2 180.0 . . ? N1 C1 C2 122.1(5) . . ? C3 C2 C1 120.8(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 C6 127.4(4) . . ? C4 C3 C6 114.0(5) . . ? C5 C4 C3 117.8(5) . . ? N1 C5 C4 123.3(5) . . ? C7 C6 C3 124.8(5) . . ? C6 C7 C8 125.7(5) . . ? C13 C8 C9 118.6(3) . . ? C13 C8 C7 122.1(4) . . ? C9 C8 C7 119.3(4) . . ? C8 C9 C10 118.9(4) . . ? C11 C10 C9 122.8(4) . . ? C10 C11 C12 116.7(3) . . ? C10 C11 C14 124.4(3) . . ? C12 C11 C14 118.6(4) . . ? C11 C12 C13 121.2(4) . . ? C8 C13 C12 121.5(4) . . ? C15 C14 C15 107.5(4) 4_656 . ? C15 C14 C11 112.0(2) 4_656 . ? C15 C14 C11 110.4(2) . . ? C15 C14 C11 110.4(2) 4_656 4_656 ? C15 C14 C11 112.0(2) . 4_656 ? C11 C14 C11 104.7(4) . 4_656 ? C20 C15 C16 117.1(4) . . ? C20 C15 C14 126.1(3) . . ? C16 C15 C14 116.8(4) . . ? C17 C16 C15 120.0(4) . . ? C18 C17 C16 122.2(5) . . ? C17 C18 C19 119.5(5) . . ? C17 C18 C21 117.9(5) . . ? C19 C18 C21 122.5(6) . . ? C20 C19 C18 118.9(5) . . ? C15 C20 C19 122.2(4) . . ? C22 C21 C18 122.9(9) . . ? C21 C22 C23 114.8(9) . . ? C24 C23 C27 120.0 . . ? C24 C23 C22 128.6(7) . . ? C27 C23 C22 111.3(7) . . ? C23 C24 C25 120.0 . . ? N2 C25 C24 120.0 . . ? C27 C26 N2 120.0 . . ? C26 C27 C23 120.0 . . ? N3 C28 S1 153.0(5) . . ? N3 C28 S1 153.0(5) . 2 ? S1 C28 S1 54.0(10) . 2 ? N4 C29 S2 146.2(6) . . ? N4 C29 S2 146.2(6) . 3_567 ? S2 C29 S2 67.7(11) . 3_567 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 0.002 -0.001 8464 748 ' ' _platon_squeeze_details ; Approximately 66.4% of the unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 748 electrons per unit cell. According to the final formula which was calculated from TGA combined with elemental analysis data, these electrons were assigned to be 20 methanol and 8 dichloromethane molecules per unit cell. The F(000) value with solvent is 2576, Mu (mm^-1) value with solvent is 2.231,and crystal density with solvent is 0.644. ; #_eof #End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 950639'