# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 #TrackingRef 'complex_1.cif' _audit_creation_date 10-09-12 _publ_contact_author_name 'Richard Welter' _publ_contact_author_address ; Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE ; _publ_contact_author_phone 0383681593 _publ_contact_author_fax 0383681232 _publ_contact_author_email welter@unistra.fr _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Manganese and Iron Mononuclear and Dinuclear Complexes Supported by 2-Salicyloylhydrazono-1,3-dithiane Ligand: Synthesis, Characterization and Magnetic Properties ; loop_ _publ_author_address ; Laboratoire DECOMET, UMR-CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; _publ_author_name 'Richard WELTER' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 844919' #TrackingRef 'complex_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H29 Mn N4 O6 S4' _chemical_formula_sum 'C27 H29 Mn N4 O6 S4' _chemical_formula_weight 688.72 _chemical_absolute_configuration ? 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.712(5) _cell_length_b 12.670(5) _cell_length_c 20.965(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.49(1) _cell_angle_gamma 90.00 _cell_volume 3076.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19821 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23981 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8992 _reflns_number_gt 5256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0701P)^2^+1.0720P] 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 8992 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Mn Mn 0.16802(3) 0.05032(3) 0.808873(18) 0.03571(12) Uani 1 1 d . . . S1 S -0.11184(7) -0.09999(8) 0.93398(4) 0.0617(3) Uani 1 1 d . . . S2 S -0.15735(6) 0.00023(8) 0.80214(4) 0.0585(2) Uani 1 1 d . . . S3 S 0.47485(8) 0.28396(7) 0.75513(4) 0.0652(3) Uani 1 1 d . . . S4 S 0.41165(9) 0.05972(7) 0.71100(5) 0.0742(3) Uani 1 1 d . . . O1 O 0.15582(16) -0.22765(18) 1.00797(9) 0.0522(5) Uani 1 1 d . . . H1O H 0.1159 -0.1909 0.9797 0.078 Uiso 1 1 calc . . . O2 O 0.27346(15) -0.02602(15) 0.87127(8) 0.0410(4) Uani 1 1 d . . . O3 O 0.3425(2) 0.44643(17) 0.87068(11) 0.0614(6) Uani 1 1 d . . . H3O H 0.3481 0.3930 0.8476 0.092 Uiso 1 1 calc . . . O4 O 0.15706(15) 0.16200(15) 0.86964(8) 0.0428(4) Uani 1 1 d . . . O5 O 0.17168(16) -0.06507(14) 0.75042(8) 0.0396(4) Uani 1 1 d . . . O6 O 0.06253(16) 0.12553(14) 0.74705(9) 0.0429(4) Uani 1 1 d . . . N1 N 0.11820(17) -0.09136(18) 0.91605(10) 0.0359(5) Uani 1 1 d . . . N2 N 0.05029(17) -0.04120(16) 0.86501(10) 0.0342(5) Uani 1 1 d . . . C18 C 0.2218(2) 0.2446(2) 0.86780(12) 0.0358(5) Uani 1 1 d . . . N3 N 0.29919(18) 0.25640(17) 0.82899(10) 0.0373(5) Uani 1 1 d . . . C1 C 0.2686(2) -0.2074(2) 1.00746(12) 0.0430(6) Uani 1 1 d . . . C2 C 0.3481(3) -0.2585(3) 1.05256(14) 0.0528(7) Uani 1 1 d . . . H2 H 0.3217 -0.3076 1.0814 0.063 Uiso 1 1 calc . . . C3 C 0.4645(3) -0.2396(3) 1.05646(16) 0.0625(9) Uani 1 1 d . . . H3 H 0.5177 -0.2769 1.0869 0.075 Uiso 1 1 calc . . . C4 C 0.5044(3) -0.1657(3) 1.01569(16) 0.0629(9) Uani 1 1 d . . . H4 H 0.5844 -0.1498 1.0196 0.075 Uiso 1 1 calc . . . C5 C 0.4273(2) -0.1162(3) 0.97000(14) 0.0509(7) Uani 1 1 d . . . H5 H 0.4552 -0.0678 0.9413 0.061 Uiso 1 1 calc . . . C6 C 0.3083(2) -0.1348(2) 0.96435(12) 0.0390(6) Uani 1 1 d . . . C7 C 0.2293(2) -0.0804(2) 0.91427(12) 0.0361(6) Uani 1 1 d . . . C8 C -0.0595(2) -0.0459(2) 0.86731(12) 0.0371(6) Uani 1 1 d . . . C9 C -0.2606(3) -0.1235(3) 0.90007(19) 0.0701(10) Uani 1 1 d . . . H9A H -0.2621 -0.1701 0.8620 0.084 Uiso 1 1 calc . . . H9B H -0.2986 -0.1619 0.9323 0.084 Uiso 1 1 calc . . . C10 C -0.3301(3) -0.0255(3) 0.87979(17) 0.0613(9) Uani 1 1 d . . . H10A H -0.3551 0.0070 0.9184 0.074 Uiso 1 1 calc . . . H10B H -0.4003 -0.0460 0.8501 0.074 Uiso 1 1 calc . . . C11 C -0.2640(3) 0.0558(3) 0.84677(19) 0.0680(10) Uani 1 1 d . . . H11A H -0.2248 0.1047 0.8798 0.082 Uiso 1 1 calc . . . H11B H -0.3197 0.0977 0.8168 0.082 Uiso 1 1 calc . . . C12 C 0.2727(3) 0.4245(2) 0.91459(14) 0.0482(7) Uani 1 1 d . . . C13 C 0.2609(3) 0.5004(3) 0.96088(16) 0.0609(9) Uani 1 1 d . . . H13 H 0.3036 0.5643 0.9617 0.073 Uiso 1 1 calc . . . C14 C 0.1874(4) 0.4836(3) 1.00604(16) 0.0690(10) Uani 1 1 d . . . H14 H 0.1797 0.5362 1.0374 0.083 Uiso 1 1 calc . . . C15 C 0.1255(3) 0.3915(3) 1.00580(15) 0.0613(9) Uani 1 1 d . . . H15 H 0.0751 0.3805 1.0368 0.074 Uiso 1 1 calc . . . C16 C 0.1368(3) 0.3149(2) 0.96044(12) 0.0458(7) Uani 1 1 d . . . H16 H 0.0940 0.2513 0.9606 0.055 Uiso 1 1 calc . . . C17 C 0.2100(2) 0.3290(2) 0.91429(12) 0.0392(6) Uani 1 1 d . . . N4 N 0.30692(18) 0.16759(18) 0.79017(10) 0.0384(5) Uani 1 1 d . . . C19 C 0.3871(2) 0.1724(2) 0.75451(12) 0.0401(6) Uani 1 1 d . . . C20 C 0.5712(4) 0.2584(4) 0.6995(2) 0.1002(16) Uani 1 1 d . . . H20A H 0.5755 0.3251 0.6753 0.120 Uiso 1 1 calc . . . H20B H 0.6479 0.2493 0.7259 0.120 Uiso 1 1 calc . . . C21 C 0.5635(6) 0.1822(4) 0.6554(3) 0.137(3) Uani 1 1 d . . . H21A H 0.6293 0.1339 0.6684 0.164 Uiso 1 1 calc . . . H21B H 0.5770 0.2158 0.6145 0.164 Uiso 1 1 calc . . . C22 C 0.4584(4) 0.1145(3) 0.63972(17) 0.0749(11) Uani 1 1 d . . . H22A H 0.4753 0.0562 0.6111 0.090 Uiso 1 1 calc . . . H22B H 0.3950 0.1572 0.6161 0.090 Uiso 1 1 calc . . . C23 C 0.1185(3) -0.1852(3) 0.66615(15) 0.0543(8) Uani 1 1 d . . . H23A H 0.1992 -0.2084 0.6749 0.081 Uiso 1 1 calc . . . H23B H 0.0943 -0.1804 0.6195 0.081 Uiso 1 1 calc . . . H23C H 0.0695 -0.2362 0.6845 0.081 Uiso 1 1 calc . . . C24 C 0.1072(2) -0.0790(2) 0.69621(13) 0.0401(6) Uani 1 1 d . . . C25 C 0.0299(3) -0.0051(2) 0.66648(13) 0.0454(7) Uani 1 1 d . . . H25 H -0.0130 -0.0227 0.6258 0.055 Uiso 1 1 calc . . . C26 C 0.0115(2) 0.0929(2) 0.69229(13) 0.0422(6) Uani 1 1 d . . . C27 C -0.0721(3) 0.1705(3) 0.65731(15) 0.0630(9) Uani 1 1 d . . . H27A H -0.1361 0.1817 0.6818 0.094 Uiso 1 1 calc . . . H27B H -0.1021 0.1427 0.6145 0.094 Uiso 1 1 calc . . . H27C H -0.0326 0.2376 0.6528 0.094 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0375(2) 0.0317(2) 0.0399(2) -0.00271(17) 0.01215(16) -0.00264(17) S1 0.0409(4) 0.0851(7) 0.0608(5) 0.0281(5) 0.0134(3) -0.0090(4) S2 0.0381(4) 0.0868(7) 0.0513(4) 0.0147(4) 0.0087(3) 0.0031(4) S3 0.0764(6) 0.0579(5) 0.0698(5) -0.0077(4) 0.0388(4) -0.0280(5) S4 0.0892(7) 0.0477(5) 0.1009(7) -0.0131(5) 0.0646(6) -0.0084(5) O1 0.0432(11) 0.0582(14) 0.0537(11) 0.0167(10) 0.0022(9) -0.0106(10) O2 0.0349(9) 0.0465(11) 0.0433(10) 0.0029(9) 0.0112(8) -0.0048(8) O3 0.0702(15) 0.0419(12) 0.0769(15) -0.0122(11) 0.0267(12) -0.0160(11) O4 0.0455(10) 0.0388(11) 0.0479(10) -0.0090(9) 0.0194(8) -0.0087(9) O5 0.0431(10) 0.0349(10) 0.0417(10) -0.0035(8) 0.0096(8) 0.0016(8) O6 0.0493(11) 0.0320(10) 0.0482(11) -0.0004(8) 0.0100(8) 0.0020(9) N1 0.0329(11) 0.0354(12) 0.0400(11) -0.0006(10) 0.0073(9) -0.0044(9) N2 0.0323(11) 0.0336(12) 0.0370(11) -0.0015(9) 0.0062(8) -0.0034(9) C18 0.0374(13) 0.0326(14) 0.0368(13) 0.0022(11) 0.0031(10) 0.0019(11) N3 0.0414(12) 0.0332(12) 0.0375(11) -0.0003(9) 0.0071(9) -0.0023(10) C1 0.0436(15) 0.0439(16) 0.0408(14) -0.0030(12) 0.0041(11) -0.0058(13) C2 0.0530(18) 0.0526(19) 0.0511(16) 0.0073(15) 0.0019(13) 0.0005(15) C3 0.0516(19) 0.072(2) 0.0600(19) 0.0069(18) -0.0036(15) 0.0100(17) C4 0.0391(16) 0.083(3) 0.065(2) 0.0061(19) 0.0046(15) 0.0041(17) C5 0.0405(15) 0.061(2) 0.0522(16) 0.0006(15) 0.0107(13) -0.0030(14) C6 0.0359(13) 0.0420(15) 0.0395(13) -0.0066(12) 0.0064(11) -0.0034(12) C7 0.0375(13) 0.0338(14) 0.0381(13) -0.0073(11) 0.0088(10) -0.0046(11) C8 0.0365(13) 0.0351(14) 0.0411(13) -0.0015(11) 0.0102(10) -0.0066(11) C9 0.0429(17) 0.074(3) 0.096(3) 0.016(2) 0.0200(17) -0.0163(17) C10 0.0397(16) 0.072(2) 0.074(2) -0.0020(18) 0.0148(15) -0.0103(16) C11 0.0458(18) 0.074(3) 0.087(2) 0.008(2) 0.0163(17) 0.0088(17) C12 0.0531(17) 0.0389(16) 0.0532(17) -0.0026(13) 0.0102(13) -0.0037(14) C13 0.076(2) 0.0390(18) 0.068(2) -0.0126(16) 0.0121(17) -0.0080(16) C14 0.098(3) 0.052(2) 0.060(2) -0.0205(17) 0.0242(19) -0.003(2) C15 0.084(2) 0.054(2) 0.0501(17) -0.0086(16) 0.0254(16) 0.0019(19) C16 0.0591(18) 0.0402(16) 0.0397(14) 0.0029(12) 0.0127(12) 0.0006(14) C17 0.0450(15) 0.0331(14) 0.0383(13) 0.0007(11) 0.0022(11) 0.0026(12) N4 0.0397(12) 0.0329(12) 0.0447(12) -0.0001(10) 0.0134(9) -0.0025(10) C19 0.0381(14) 0.0385(15) 0.0451(14) 0.0018(12) 0.0109(11) -0.0013(12) C20 0.064(2) 0.127(4) 0.121(4) -0.020(3) 0.052(2) -0.025(3) C21 0.190(6) 0.079(3) 0.181(5) -0.042(4) 0.156(5) -0.051(4) C22 0.093(3) 0.075(3) 0.060(2) 0.0001(19) 0.0258(19) 0.025(2) C23 0.065(2) 0.0435(17) 0.0548(17) -0.0117(14) 0.0102(14) 0.0053(15) C24 0.0441(15) 0.0368(15) 0.0431(14) -0.0025(12) 0.0193(12) -0.0049(12) C25 0.0541(17) 0.0410(16) 0.0414(14) -0.0021(13) 0.0078(12) 0.0003(13) C26 0.0456(15) 0.0404(15) 0.0422(14) 0.0064(13) 0.0116(12) -0.0012(13) C27 0.077(2) 0.052(2) 0.0568(18) 0.0109(16) 0.0003(16) 0.0147(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O6 1.9082(19) . ? Mn O5 1.9123(19) . ? Mn O4 1.9209(19) . ? Mn O2 1.9221(19) . ? Mn N2 2.261(2) . ? Mn N4 2.280(2) . ? S1 C8 1.747(3) . ? S1 C9 1.806(3) . ? S2 C8 1.749(3) . ? S2 C11 1.810(4) . ? S3 C19 1.746(3) . ? S3 C20 1.769(4) . ? S4 C19 1.741(3) . ? S4 C22 1.804(4) . ? O1 C1 1.347(3) . ? O1 H1O 0.8400 . ? O2 C7 1.301(3) . ? O3 C12 1.348(4) . ? O3 H3O 0.8400 . ? O4 C18 1.296(3) . ? O5 C24 1.280(3) . ? O6 C26 1.282(3) . ? N1 C7 1.314(3) . ? N1 N2 1.389(3) . ? N2 C8 1.295(3) . ? C18 N3 1.313(3) . ? C18 C17 1.468(4) . ? N3 N4 1.400(3) . ? C1 C2 1.386(4) . ? C1 C6 1.415(4) . ? C2 C3 1.374(5) . ? C2 H2 0.9500 . ? C3 C4 1.395(5) . ? C3 H3 0.9500 . ? C4 C5 1.368(4) . ? C4 H4 0.9500 . ? C5 C6 1.401(4) . ? C5 H5 0.9500 . ? C6 C7 1.466(4) . ? C9 C10 1.511(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.516(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.387(4) . ? C12 C17 1.415(4) . ? C13 C14 1.387(5) . ? C13 H13 0.9500 . ? C14 C15 1.373(5) . ? C14 H14 0.9500 . ? C15 C16 1.378(4) . ? C15 H15 0.9500 . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? N4 C19 1.285(3) . ? C20 C21 1.331(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.497(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.500(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.385(4) . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 C27 1.500(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 O6 Mn O5 91.15(8) . . ? O6 Mn O4 89.00(8) . . ? O5 Mn O4 176.59(8) . . ? O6 Mn O2 179.63(8) . . ? O5 Mn O2 88.76(8) . . ? O4 Mn O2 91.06(8) . . ? O6 Mn N2 103.08(8) . . ? O5 Mn N2 90.84(8) . . ? O4 Mn N2 85.81(8) . . ? O2 Mn N2 76.56(8) . . ? O6 Mn N4 87.97(8) . . ? O5 Mn N4 107.69(8) . . ? O4 Mn N4 75.72(8) . . ? O2 Mn N4 92.41(8) . . ? N2 Mn N4 158.37(8) . . ? C8 S1 C9 100.49(15) . . ? C8 S2 C11 98.56(15) . . ? C19 S3 C20 106.22(19) . . ? C19 S4 C22 102.25(16) . . ? C1 O1 H1O 109.5 . . ? C7 O2 Mn 117.16(16) . . ? C12 O3 H3O 109.5 . . ? C18 O4 Mn 118.58(16) . . ? C24 O5 Mn 127.44(18) . . ? C26 O6 Mn 128.08(18) . . ? C7 N1 N2 112.7(2) . . ? C8 N2 N1 114.1(2) . . ? C8 N2 Mn 136.74(18) . . ? N1 N2 Mn 108.16(14) . . ? O4 C18 N3 124.8(2) . . ? O4 C18 C17 117.2(2) . . ? N3 C18 C17 118.0(2) . . ? C18 N3 N4 112.2(2) . . ? O1 C1 C2 117.8(3) . . ? O1 C1 C6 123.0(2) . . ? C2 C1 C6 119.2(3) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 118.2(3) . . ? C5 C6 C7 119.8(2) . . ? C1 C6 C7 122.0(2) . . ? O2 C7 N1 124.9(2) . . ? O2 C7 C6 118.1(2) . . ? N1 C7 C6 117.0(2) . . ? N2 C8 S1 121.0(2) . . ? N2 C8 S2 119.67(19) . . ? S1 C8 S2 119.27(15) . . ? C10 C9 S1 115.0(3) . . ? C10 C9 H9A 108.5 . . ? S1 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? S1 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 113.4(3) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 S2 114.2(3) . . ? C10 C11 H11A 108.7 . . ? S2 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? S2 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O3 C12 C13 117.9(3) . . ? O3 C12 C17 122.7(3) . . ? C13 C12 C17 119.4(3) . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 121.3(3) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 118.6(3) . . ? C16 C17 C18 119.6(3) . . ? C12 C17 C18 121.8(2) . . ? C19 N4 N3 114.6(2) . . ? C19 N4 Mn 137.09(19) . . ? N3 N4 Mn 108.36(14) . . ? N4 C19 S4 117.2(2) . . ? N4 C19 S3 120.9(2) . . ? S4 C19 S3 121.67(15) . . ? C21 C20 S3 127.4(3) . . ? C21 C20 H20A 105.5 . . ? S3 C20 H20A 105.5 . . ? C21 C20 H20B 105.5 . . ? S3 C20 H20B 105.5 . . ? H20A C20 H20B 106.0 . . ? C20 C21 C22 122.5(4) . . ? C20 C21 H21A 106.7 . . ? C22 C21 H21A 106.7 . . ? C20 C21 H21B 106.7 . . ? C22 C21 H21B 106.7 . . ? H21A C21 H21B 106.6 . . ? C21 C22 S4 112.3(3) . . ? C21 C22 H22A 109.2 . . ? S4 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? S4 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 124.5(3) . . ? O5 C24 C23 114.8(3) . . ? C25 C24 C23 120.7(3) . . ? C26 C25 C24 124.1(3) . . ? C26 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? O6 C26 C25 124.1(3) . . ? O6 C26 C27 114.3(3) . . ? C25 C26 C27 121.7(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Mn O2 C7 -20(14) . . . . ? O5 Mn O2 C7 -96.32(18) . . . . ? O4 Mn O2 C7 80.28(18) . . . . ? N2 Mn O2 C7 -5.16(17) . . . . ? N4 Mn O2 C7 156.02(18) . . . . ? O6 Mn O4 C18 -83.97(19) . . . . ? O5 Mn O4 C18 -176.6(13) . . . . ? O2 Mn O4 C18 96.40(19) . . . . ? N2 Mn O4 C18 172.84(19) . . . . ? N4 Mn O4 C18 4.19(18) . . . . ? O6 Mn O5 C24 -9.0(2) . . . . ? O4 Mn O5 C24 83.6(15) . . . . ? O2 Mn O5 C24 170.7(2) . . . . ? N2 Mn O5 C24 94.1(2) . . . . ? N4 Mn O5 C24 -97.2(2) . . . . ? O5 Mn O6 C26 7.0(2) . . . . ? O4 Mn O6 C26 -169.6(2) . . . . ? O2 Mn O6 C26 -70(14) . . . . ? N2 Mn O6 C26 -84.1(2) . . . . ? N4 Mn O6 C26 114.7(2) . . . . ? C7 N1 N2 C8 -176.5(2) . . . . ? C7 N1 N2 Mn -5.9(2) . . . . ? O6 Mn N2 C8 -6.6(3) . . . . ? O5 Mn N2 C8 -97.9(3) . . . . ? O4 Mn N2 C8 81.4(3) . . . . ? O2 Mn N2 C8 173.5(3) . . . . ? N4 Mn N2 C8 112.6(3) . . . . ? O6 Mn N2 N1 -174.11(14) . . . . ? O5 Mn N2 N1 94.52(15) . . . . ? O4 Mn N2 N1 -86.11(15) . . . . ? O2 Mn N2 N1 5.99(14) . . . . ? N4 Mn N2 N1 -55.0(3) . . . . ? Mn O4 C18 N3 -3.2(3) . . . . ? Mn O4 C18 C17 179.14(17) . . . . ? O4 C18 N3 N4 -1.6(3) . . . . ? C17 C18 N3 N4 176.0(2) . . . . ? O1 C1 C2 C3 -178.0(3) . . . . ? C6 C1 C2 C3 0.4(5) . . . . ? C1 C2 C3 C4 1.7(5) . . . . ? C2 C3 C4 C5 -3.1(6) . . . . ? C3 C4 C5 C6 2.3(5) . . . . ? C4 C5 C6 C1 -0.1(5) . . . . ? C4 C5 C6 C7 -179.5(3) . . . . ? O1 C1 C6 C5 177.1(3) . . . . ? C2 C1 C6 C5 -1.2(4) . . . . ? O1 C1 C6 C7 -3.5(4) . . . . ? C2 C1 C6 C7 178.2(3) . . . . ? Mn O2 C7 N1 3.8(3) . . . . ? Mn O2 C7 C6 -176.90(17) . . . . ? N2 N1 C7 O2 2.2(4) . . . . ? N2 N1 C7 C6 -177.1(2) . . . . ? C5 C6 C7 O2 8.4(4) . . . . ? C1 C6 C7 O2 -171.0(2) . . . . ? C5 C6 C7 N1 -172.2(3) . . . . ? C1 C6 C7 N1 8.4(4) . . . . ? N1 N2 C8 S1 6.0(3) . . . . ? Mn N2 C8 S1 -161.05(14) . . . . ? N1 N2 C8 S2 -172.79(17) . . . . ? Mn N2 C8 S2 20.2(4) . . . . ? C9 S1 C8 N2 -162.6(2) . . . . ? C9 S1 C8 S2 16.2(2) . . . . ? C11 S2 C8 N2 -143.7(2) . . . . ? C11 S2 C8 S1 37.5(2) . . . . ? C8 S1 C9 C10 -64.3(3) . . . . ? S1 C9 C10 C11 40.9(4) . . . . ? C9 C10 C11 S2 30.6(4) . . . . ? C8 S2 C11 C10 -68.9(3) . . . . ? O3 C12 C13 C14 178.0(3) . . . . ? C17 C12 C13 C14 -0.8(5) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? C13 C14 C15 C16 0.2(6) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C15 C16 C17 C12 -0.3(4) . . . . ? C15 C16 C17 C18 178.5(3) . . . . ? O3 C12 C17 C16 -177.9(3) . . . . ? C13 C12 C17 C16 0.8(4) . . . . ? O3 C12 C17 C18 3.3(4) . . . . ? C13 C12 C17 C18 -178.0(3) . . . . ? O4 C18 C17 C16 4.0(4) . . . . ? N3 C18 C17 C16 -173.8(2) . . . . ? O4 C18 C17 C12 -177.1(2) . . . . ? N3 C18 C17 C12 5.0(4) . . . . ? C18 N3 N4 C19 -175.4(2) . . . . ? C18 N3 N4 Mn 4.5(2) . . . . ? O6 Mn N4 C19 -95.3(3) . . . . ? O5 Mn N4 C19 -4.7(3) . . . . ? O4 Mn N4 C19 175.2(3) . . . . ? O2 Mn N4 C19 84.8(3) . . . . ? N2 Mn N4 C19 143.1(3) . . . . ? O6 Mn N4 N3 84.78(16) . . . . ? O5 Mn N4 N3 175.34(14) . . . . ? O4 Mn N4 N3 -4.71(15) . . . . ? O2 Mn N4 N3 -95.19(16) . . . . ? N2 Mn N4 N3 -36.9(3) . . . . ? N3 N4 C19 S4 173.67(18) . . . . ? Mn N4 C19 S4 -6.3(4) . . . . ? N3 N4 C19 S3 -1.3(3) . . . . ? Mn N4 C19 S3 178.78(14) . . . . ? C22 S4 C19 N4 148.4(2) . . . . ? C22 S4 C19 S3 -36.7(2) . . . . ? C20 S3 C19 N4 -179.5(3) . . . . ? C20 S3 C19 S4 5.8(3) . . . . ? C19 S3 C20 C21 13.9(7) . . . . ? S3 C20 C21 C22 9.6(10) . . . . ? C20 C21 C22 S4 -49.9(8) . . . . ? C19 S4 C22 C21 58.6(3) . . . . ? Mn O5 C24 C25 7.6(4) . . . . ? Mn O5 C24 C23 -171.00(18) . . . . ? O5 C24 C25 C26 -1.1(4) . . . . ? C23 C24 C25 C26 177.5(3) . . . . ? Mn O6 C26 C25 -3.6(4) . . . . ? Mn O6 C26 C27 176.3(2) . . . . ? C24 C25 C26 O6 -1.1(4) . . . . ? C24 C25 C26 C27 179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.603 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.067 # Attachment 'complex_2.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 844920' #TrackingRef 'complex_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 Mn N6 O6 S6, C H2 Cl2' _chemical_formula_sum 'C34 H35 Cl2 Mn N6 O6 S6' _chemical_formula_weight 941.88 _chemical_absolute_configuration ? 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' Mn Mn 0.3368 0.7283 '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 10.429(2) _cell_length_b 11.778(2) _cell_length_c 17.263(3) _cell_angle_alpha 105.39(5) _cell_angle_beta 91.37(5) _cell_angle_gamma 90.35(5) _cell_volume 2043.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42705 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24068 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 30.04 _reflns_number_total 11916 _reflns_number_gt 8810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0694P)^2^+5.4212P] 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 11916 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.2064 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Mn1 Mn 0.18172(5) -0.60715(5) 0.70735(3) 0.02935(14) Uani 1 1 d . A . Cl1 Cl 0.12262(15) -0.87739(12) 1.00208(12) 0.0824(5) Uani 1 1 d . . . Cl2 Cl 0.35629(14) -0.98247(15) 1.04269(13) 0.0866(6) Uani 1 1 d . . . S1 S 0.47269(10) -0.29794(9) 0.87460(7) 0.0399(2) Uani 1 1 d . . . S2 S 0.50308(10) -0.56267(9) 0.82767(8) 0.0447(3) Uani 1 1 d . . . S3 S 0.48715(11) -0.90211(11) 0.63477(9) 0.0534(3) Uani 1 1 d . . . S4 S 0.31025(12) -0.84149(11) 0.78077(8) 0.0512(3) Uani 1 1 d . . . S5 S -0.18412(15) -0.8581(2) 0.58664(9) 0.0887(6) Uani 1 1 d . . . S6 S 0.03549(17) -0.7672(2) 0.50519(8) 0.0980(7) Uani 1 1 d . . . O1 O 0.2063(3) -0.1269(3) 0.8210(2) 0.0517(8) Uani 1 1 d . . . H1O H 0.2458 -0.1899 0.8180 0.077 Uiso 1 1 calc . . . O2 O 0.0698(2) -0.4740(2) 0.72703(16) 0.0353(6) Uani 1 1 d . . . O3 O 0.5208(4) -0.7645(4) 0.4714(2) 0.0743(12) Uani 1 1 d . . . H3O H 0.4877 -0.7775 0.5121 0.111 Uiso 1 1 calc . . . O4 O 0.2346(3) -0.5687(3) 0.61320(17) 0.0417(6) Uani 1 1 d . . . O5 O -0.2515(3) -0.7888(3) 0.79885(19) 0.0469(7) Uani 1 1 d . . . H5O H -0.2064 -0.7891 0.7591 0.070 Uiso 1 1 calc . . . O6 O 0.1215(3) -0.6483(2) 0.79910(16) 0.0361(6) Uani 1 1 d . A . N1 N 0.2373(3) -0.3506(3) 0.78892(18) 0.0299(6) Uani 1 1 d . . . N2 N 0.3042(3) -0.4548(3) 0.78501(18) 0.0297(6) Uani 1 1 d . . . N4 N 0.3194(3) -0.7357(3) 0.6665(2) 0.0378(7) Uani 1 1 d . . . N3 N 0.3655(3) -0.7266(3) 0.59264(19) 0.0373(7) Uani 1 1 d . . . N6 N 0.0130(3) -0.7286(3) 0.65914(19) 0.0379(7) Uani 1 1 d . . . N5 N -0.0547(3) -0.7417(3) 0.72523(19) 0.0338(7) Uani 1 1 d . A . C1 C -0.0896(4) -0.2855(4) 0.7348(3) 0.0512(11) Uani 1 1 d . . . H1 H -0.1228 -0.3633 0.7146 0.061 Uiso 1 1 calc . . . C2 C -0.1681(5) -0.1909(6) 0.7368(4) 0.0736(18) Uani 1 1 d . . . H2 H -0.2550 -0.2039 0.7185 0.088 Uiso 1 1 calc . . . C3 C -0.1211(6) -0.0785(5) 0.7651(4) 0.0699(16) Uani 1 1 d . . . H3A H -0.1756 -0.0139 0.7659 0.084 Uiso 1 1 calc . . . C4 C 0.0043(5) -0.0578(4) 0.7924(3) 0.0577(13) Uani 1 1 d . . . H4A H 0.0357 0.0208 0.8114 0.069 Uiso 1 1 calc . . . C5 C 0.0856(4) -0.1521(4) 0.7923(2) 0.0375(8) Uani 1 1 d . . . C6 C 0.0385(4) -0.2685(3) 0.7622(2) 0.0337(7) Uani 1 1 d . . . C7 C 0.1199(3) -0.3713(3) 0.7585(2) 0.0292(7) Uani 1 1 d . . . C8 C 0.4128(3) -0.4388(3) 0.8247(2) 0.0308(7) Uani 1 1 d . . . C9 C 0.6622(4) -0.4964(5) 0.8340(4) 0.0602(14) Uani 1 1 d . . . H9A H 0.7267 -0.5596 0.8243 0.072 Uiso 1 1 calc . . . H9B H 0.6694 -0.4558 0.7908 0.072 Uiso 1 1 calc . . . C10 C 0.6933(5) -0.4092(5) 0.9139(4) 0.0672(16) Uani 1 1 d . . . H10A H 0.7631 -0.3557 0.9069 0.081 Uiso 1 1 calc . . . H10B H 0.7249 -0.4525 0.9523 0.081 Uiso 1 1 calc . . . C11 C 0.5789(5) -0.3362(5) 0.9491(3) 0.0573(13) Uani 1 1 d . . . H11A H 0.6105 -0.2627 0.9876 0.069 Uiso 1 1 calc . . . H11B H 0.5287 -0.3805 0.9797 0.069 Uiso 1 1 calc . . . C12 C 0.2964(6) -0.5276(5) 0.4682(3) 0.0561(12) Uani 1 1 d . . . H12 H 0.2293 -0.4852 0.4990 0.067 Uiso 1 1 calc . . . C13 C 0.3355(6) -0.4990(5) 0.4008(3) 0.0647(15) Uani 1 1 d . . . H13 H 0.2919 -0.4399 0.3826 0.078 Uiso 1 1 calc . . . C14 C 0.4370(7) -0.5550(7) 0.3595(3) 0.0765(19) Uani 1 1 d . . . H14 H 0.4658 -0.5319 0.3141 0.092 Uiso 1 1 calc . . . C15 C 0.4991(6) -0.6454(6) 0.3826(3) 0.0704(17) Uani 1 1 d . . . H15 H 0.5686 -0.6850 0.3529 0.085 Uiso 1 1 calc . . . C16 C 0.4573(5) -0.6768(5) 0.4506(3) 0.0561(12) Uani 1 1 d . . . C17 C 0.3551(4) -0.6186(4) 0.4912(3) 0.0464(10) Uani 1 1 d . . . C18 C 0.3166(4) -0.6387(4) 0.5709(2) 0.0391(8) Uani 1 1 d . . . C19 C 0.3707(4) -0.8171(4) 0.6932(3) 0.0395(9) Uani 1 1 d . . . C20 C 0.5512(6) -1.0035(5) 0.6876(4) 0.0657(15) Uani 1 1 d . . . H20A H 0.5759 -1.0761 0.6470 0.079 Uiso 1 1 calc . . . H20B H 0.6307 -0.9680 0.7168 0.079 Uiso 1 1 calc . . . C21 C 0.4687(6) -1.0374(5) 0.7446(4) 0.0684(16) Uani 1 1 d . . . H21A H 0.5143 -1.0943 0.7681 0.082 Uiso 1 1 calc . . . H21B H 0.3908 -1.0772 0.7157 0.082 Uiso 1 1 calc . . . C22 C 0.4289(5) -0.9320(5) 0.8123(4) 0.0645(15) Uani 1 1 d . . . H22A H 0.5058 -0.8830 0.8338 0.077 Uiso 1 1 calc . . . H22B H 0.3940 -0.9611 0.8565 0.077 Uiso 1 1 calc . . . C23 C -0.1827(4) -0.7420(3) 0.8676(2) 0.0356(8) Uani 1 1 d . . . C24 C -0.2414(4) -0.7338(4) 0.9402(3) 0.0460(10) Uani 1 1 d . . . H24 H -0.3272 -0.7615 0.9402 0.055 Uiso 1 1 calc . . . C25 C -0.1773(5) -0.6864(4) 1.0118(3) 0.0468(10) Uani 1 1 d . . . H25 H -0.2186 -0.6822 1.0608 0.056 Uiso 1 1 calc . . . C26 C -0.0537(5) -0.6448(4) 1.0132(2) 0.0435(9) Uani 1 1 d . . . H26 H -0.0098 -0.6119 1.0631 0.052 Uiso 1 1 calc . . . C27 C 0.0069(4) -0.6510(4) 0.9412(2) 0.0375(8) Uani 1 1 d . . . H27 H 0.0925 -0.6224 0.9423 0.045 Uiso 1 1 calc . . . C28 C -0.0558(4) -0.6985(3) 0.8679(2) 0.0311(7) Uani 1 1 d . A . C29 C 0.0082(3) -0.6965(3) 0.7934(2) 0.0307(7) Uani 1 1 d . . . C30 C -0.0416(4) -0.7804(4) 0.5904(2) 0.0430(10) Uani 1 1 d . A . C31A C -0.1027(16) -0.7866(15) 0.4361(10) 0.091(3) Uiso 0.50 1 d P A 1 H31A H -0.1487 -0.7111 0.4524 0.109 Uiso 0.50 1 calc P B 1 H31B H -0.0659 -0.7892 0.3834 0.109 Uiso 0.50 1 calc P C 1 C32A C -0.1822(14) -0.8572(14) 0.4219(9) 0.079(3) Uiso 0.50 1 d P A 1 H32A H -0.1684 -0.9072 0.3669 0.094 Uiso 0.50 1 calc P D 1 H32B H -0.2645 -0.8164 0.4202 0.094 Uiso 0.50 1 calc P E 1 C33A C -0.2033(14) -0.9565(12) 0.4874(9) 0.072(2) Uiso 0.50 1 d P A 1 H33A H -0.2896 -0.9941 0.4792 0.086 Uiso 0.50 1 calc P F 1 H33B H -0.1375 -1.0185 0.4776 0.086 Uiso 0.50 1 calc P G 1 C31B C -0.0432(16) -0.8515(15) 0.4202(10) 0.091(3) Uiso 0.50 1 d P A 2 H31C H -0.0665 -0.7975 0.3871 0.109 Uiso 0.50 1 calc P H 2 H31D H 0.0209 -0.9062 0.3898 0.109 Uiso 0.50 1 calc P I 2 C32B C -0.1579(14) -0.9224(14) 0.4226(9) 0.079(3) Uiso 0.50 1 d P A 2 H32C H -0.2156 -0.9128 0.3785 0.094 Uiso 0.50 1 calc P J 2 H32D H -0.1303 -1.0055 0.4074 0.094 Uiso 0.50 1 calc P K 2 C333 C -0.2249(14) -0.9116(13) 0.4811(9) 0.072(2) Uiso 0.50 1 d P A 2 H33C H -0.2626 -0.9909 0.4750 0.086 Uiso 0.50 1 calc P L 2 H33D H -0.2968 -0.8617 0.4721 0.086 Uiso 0.50 1 calc P M 2 C34 C 0.1930(5) -1.0047(4) 1.0172(3) 0.0560(12) Uani 1 1 d . . . H34A H 0.1486 -1.0282 1.0607 0.067 Uiso 1 1 calc . . . H34B H 0.1825 -1.0697 0.9675 0.067 Uiso 1 1 calc . . . 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 Mn1 0.0313(3) 0.0320(3) 0.0245(3) 0.0071(2) 0.0002(2) -0.0030(2) Cl1 0.0692(9) 0.0464(7) 0.1306(15) 0.0257(8) -0.0405(9) -0.0052(6) Cl2 0.0536(8) 0.0706(9) 0.1471(17) 0.0518(10) -0.0281(9) -0.0102(7) S1 0.0330(5) 0.0360(5) 0.0490(6) 0.0094(4) -0.0097(4) -0.0062(4) S2 0.0387(5) 0.0360(5) 0.0619(7) 0.0191(5) -0.0168(5) -0.0033(4) S3 0.0404(6) 0.0515(7) 0.0697(8) 0.0186(6) 0.0025(5) 0.0046(5) S4 0.0527(6) 0.0541(7) 0.0550(7) 0.0287(6) 0.0020(5) 0.0033(5) S5 0.0538(8) 0.1454(17) 0.0445(7) -0.0128(9) -0.0027(6) -0.0448(9) S6 0.0808(11) 0.176(2) 0.0257(6) 0.0094(8) -0.0052(6) -0.0566(12) O1 0.0428(16) 0.0340(15) 0.074(2) 0.0088(15) -0.0154(15) -0.0015(13) O2 0.0271(12) 0.0376(14) 0.0385(14) 0.0054(11) -0.0028(10) -0.0013(10) O3 0.076(3) 0.088(3) 0.058(2) 0.016(2) 0.027(2) 0.023(2) O4 0.0483(16) 0.0460(16) 0.0321(14) 0.0122(12) 0.0072(12) 0.0004(13) O5 0.0408(16) 0.0539(18) 0.0442(17) 0.0105(14) -0.0016(13) -0.0155(14) O6 0.0344(13) 0.0455(15) 0.0294(13) 0.0125(11) -0.0046(10) -0.0138(11) N1 0.0256(14) 0.0343(15) 0.0298(15) 0.0086(12) -0.0008(11) -0.0018(12) N2 0.0288(14) 0.0343(15) 0.0268(14) 0.0094(12) 0.0011(11) 0.0000(12) N4 0.0384(17) 0.0403(18) 0.0376(17) 0.0156(14) -0.0030(14) -0.0066(14) N3 0.0385(17) 0.0421(18) 0.0309(16) 0.0090(14) 0.0056(13) -0.0006(14) N6 0.0419(18) 0.0427(18) 0.0273(15) 0.0067(14) -0.0048(13) -0.0091(14) N5 0.0343(16) 0.0359(16) 0.0290(15) 0.0048(13) -0.0017(12) -0.0054(13) C1 0.032(2) 0.050(3) 0.065(3) 0.007(2) -0.012(2) 0.0041(18) C2 0.043(3) 0.071(4) 0.096(5) 0.005(3) -0.024(3) 0.018(3) C3 0.060(3) 0.059(3) 0.085(4) 0.011(3) -0.018(3) 0.023(3) C4 0.062(3) 0.040(2) 0.067(3) 0.009(2) -0.013(3) 0.012(2) C5 0.038(2) 0.039(2) 0.0347(19) 0.0091(16) -0.0021(15) 0.0027(16) C6 0.0312(17) 0.0397(19) 0.0294(17) 0.0077(15) -0.0005(14) 0.0012(15) C7 0.0272(16) 0.0375(18) 0.0218(15) 0.0063(14) 0.0022(12) -0.0032(14) C8 0.0281(16) 0.0348(18) 0.0312(17) 0.0119(15) -0.0015(13) -0.0034(14) C9 0.033(2) 0.054(3) 0.097(4) 0.026(3) -0.013(2) 0.003(2) C10 0.046(3) 0.055(3) 0.102(4) 0.027(3) -0.040(3) -0.012(2) C11 0.059(3) 0.057(3) 0.056(3) 0.018(2) -0.029(2) -0.018(2) C12 0.074(3) 0.060(3) 0.037(2) 0.018(2) 0.004(2) -0.009(3) C13 0.079(4) 0.077(4) 0.043(3) 0.025(3) 0.002(3) -0.019(3) C14 0.086(4) 0.108(5) 0.039(3) 0.026(3) 0.003(3) -0.037(4) C15 0.064(3) 0.103(5) 0.041(3) 0.012(3) 0.013(2) -0.016(3) C16 0.055(3) 0.073(3) 0.037(2) 0.008(2) 0.007(2) -0.011(3) C17 0.040(2) 0.050(2) 0.058(3) 0.029(2) 0.0146(19) -0.0017(19) C18 0.041(2) 0.040(2) 0.0335(19) 0.0058(16) 0.0009(16) -0.0056(17) C19 0.0357(19) 0.040(2) 0.042(2) 0.0105(17) -0.0077(16) -0.0102(16) C20 0.061(3) 0.051(3) 0.082(4) 0.015(3) -0.023(3) 0.008(2) C21 0.058(3) 0.048(3) 0.100(5) 0.022(3) -0.015(3) 0.004(2) C22 0.060(3) 0.073(4) 0.071(4) 0.040(3) -0.016(3) -0.004(3) C23 0.0385(19) 0.0315(18) 0.0376(19) 0.0108(15) -0.0005(16) -0.0032(15) C24 0.042(2) 0.045(2) 0.053(3) 0.016(2) 0.0115(19) -0.0032(18) C25 0.056(3) 0.051(2) 0.036(2) 0.0157(19) 0.0114(19) 0.002(2) C26 0.056(3) 0.047(2) 0.0284(18) 0.0105(17) 0.0017(17) -0.0003(19) C27 0.039(2) 0.041(2) 0.0340(19) 0.0129(16) 0.0021(15) -0.0021(16) C28 0.0347(18) 0.0273(16) 0.0329(18) 0.0111(14) -0.0008(14) -0.0034(14) C29 0.0337(18) 0.0288(17) 0.0294(17) 0.0077(14) -0.0020(14) -0.0028(14) C30 0.037(2) 0.057(3) 0.0289(18) 0.0005(18) -0.0055(15) -0.0037(18) C34 0.051(3) 0.045(3) 0.072(3) 0.017(2) -0.008(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.892(3) . ? Mn1 O6 1.894(3) . ? Mn1 O2 1.922(3) . ? Mn1 N4 2.088(4) . ? Mn1 N6 2.259(3) . ? Mn1 N2 2.294(3) . ? Cl1 C34 1.752(5) . ? Cl2 C34 1.749(5) . ? S1 C8 1.757(4) . ? S1 C11 1.825(5) . ? S2 C8 1.753(4) . ? S2 C9 1.819(5) . ? S3 C19 1.741(5) . ? S3 C20 1.806(6) . ? S4 C19 1.744(4) . ? S4 C22 1.804(5) . ? S5 C30 1.731(5) . ? S5 C33A 1.801(15) . ? S5 C333 1.802(15) . ? S6 C31B 1.724(16) . ? S6 C30 1.736(5) . ? S6 C31A 1.822(17) . ? O1 C5 1.344(5) . ? O1 H1O 0.8400 . ? O2 C7 1.289(4) . ? O3 C16 1.353(7) . ? O3 H3O 0.8400 . ? O4 C18 1.290(5) . ? O5 C23 1.355(5) . ? O5 H5O 0.8400 . ? O6 C29 1.299(4) . ? N1 C7 1.316(4) . ? N1 N2 1.403(4) . ? N2 C8 1.295(4) . ? N4 C19 1.283(5) . ? N4 N3 1.403(5) . ? N3 C18 1.295(5) . ? N6 C30 1.297(5) . ? N6 N5 1.398(5) . ? N5 C29 1.313(5) . ? C1 C2 1.381(7) . ? C1 C6 1.401(5) . ? C1 H1 0.9500 . ? C2 C3 1.367(9) . ? C2 H2 0.9500 . ? C3 C4 1.378(8) . ? C3 H3A 0.9500 . ? C4 C5 1.401(6) . ? C4 H4A 0.9500 . ? C5 C6 1.412(6) . ? C6 C7 1.472(5) . ? C9 C10 1.512(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.517(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.365(7) . ? C12 C17 1.381(7) . ? C12 H12 0.9500 . ? C13 C14 1.363(9) . ? C13 H13 0.9500 . ? C14 C15 1.391(10) . ? C14 H14 0.9500 . ? C15 C16 1.398(7) . ? C15 H15 0.9500 . ? C16 C17 1.374(7) . ? C17 C18 1.519(6) . ? C20 C21 1.454(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.530(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.389(6) . ? C23 C28 1.416(5) . ? C24 C25 1.370(7) . ? C24 H24 0.9500 . ? C25 C26 1.373(7) . ? C25 H25 0.9500 . ? C26 C27 1.393(6) . ? C26 H26 0.9500 . ? C27 C28 1.386(5) . ? C27 H27 0.9500 . ? C28 C29 1.469(5) . ? C31A C32A 1.145(19) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A C33A 1.85(2) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C31B C32B 1.46(2) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B C333 1.221(19) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C333 H33C 0.9900 . ? C333 H33D 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O6 177.34(12) . . ? O4 Mn1 O2 88.45(13) . . ? O6 Mn1 O2 90.82(13) . . ? O4 Mn1 N4 79.05(14) . . ? O6 Mn1 N4 101.76(13) . . ? O2 Mn1 N4 167.30(12) . . ? O4 Mn1 N6 101.19(13) . . ? O6 Mn1 N6 76.25(12) . . ? O2 Mn1 N6 89.97(12) . . ? N4 Mn1 N6 94.64(13) . . ? O4 Mn1 N2 90.36(13) . . ? O6 Mn1 N2 91.94(11) . . ? O2 Mn1 N2 75.76(11) . . ? N4 Mn1 N2 101.81(12) . . ? N6 Mn1 N2 161.47(12) . . ? C8 S1 C11 99.7(2) . . ? C8 S2 C9 98.4(2) . . ? C19 S3 C20 108.8(3) . . ? C19 S4 C22 104.4(3) . . ? C30 S5 C33A 108.0(5) . . ? C30 S5 C333 104.9(5) . . ? C33A S5 C333 19.5(6) . . ? C31B S6 C30 109.9(6) . . ? C31B S6 C31A 31.7(6) . . ? C30 S6 C31A 99.0(5) . . ? C5 O1 H1O 109.5 . . ? C7 O2 Mn1 117.7(2) . . ? C16 O3 H3O 109.5 . . ? C18 O4 Mn1 115.7(3) . . ? C23 O5 H5O 109.5 . . ? C29 O6 Mn1 117.2(2) . . ? C7 N1 N2 112.2(3) . . ? C8 N2 N1 113.9(3) . . ? C8 N2 Mn1 138.9(3) . . ? N1 N2 Mn1 107.2(2) . . ? C19 N4 N3 114.9(4) . . ? C19 N4 Mn1 135.4(3) . . ? N3 N4 Mn1 109.8(2) . . ? C18 N3 N4 112.3(3) . . ? C30 N6 N5 113.7(3) . . ? C30 N6 Mn1 138.8(3) . . ? N5 N6 Mn1 107.3(2) . . ? C29 N5 N6 112.1(3) . . ? C2 C1 C6 121.0(5) . . ? C2 C1 H1 119.5 . . ? C6 C1 H1 119.5 . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? O1 C5 C4 117.9(4) . . ? O1 C5 C6 122.8(4) . . ? C4 C5 C6 119.2(4) . . ? C1 C6 C5 118.5(4) . . ? C1 C6 C7 119.5(4) . . ? C5 C6 C7 122.0(3) . . ? O2 C7 N1 125.4(3) . . ? O2 C7 C6 117.5(3) . . ? N1 C7 C6 117.1(3) . . ? N2 C8 S2 118.4(3) . . ? N2 C8 S1 122.4(3) . . ? S2 C8 S1 119.2(2) . . ? C10 C9 S2 113.7(4) . . ? C10 C9 H9A 108.8 . . ? S2 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? S2 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 113.0(4) . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 S1 114.2(4) . . ? C10 C11 H11A 108.7 . . ? S1 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? S1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C17 119.5(5) . . ? C13 C12 H12 120.3 . . ? C17 C12 H12 120.3 . . ? C14 C13 C12 120.1(6) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 118.8(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? O3 C16 C17 124.3(4) . . ? O3 C16 C15 116.9(5) . . ? C17 C16 C15 118.8(6) . . ? C16 C17 C12 121.5(4) . . ? C16 C17 C18 120.8(4) . . ? C12 C17 C18 117.0(4) . . ? O4 C18 N3 122.9(4) . . ? O4 C18 C17 118.4(4) . . ? N3 C18 C17 118.6(4) . . ? N4 C19 S3 117.2(3) . . ? N4 C19 S4 117.7(3) . . ? S3 C19 S4 124.9(3) . . ? C21 C20 S3 117.3(4) . . ? C21 C20 H20A 108.0 . . ? S3 C20 H20A 108.0 . . ? C21 C20 H20B 108.0 . . ? S3 C20 H20B 108.0 . . ? H20A C20 H20B 107.2 . . ? C20 C21 C22 112.6(5) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 S4 113.2(4) . . ? C21 C22 H22A 108.9 . . ? S4 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? S4 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? O5 C23 C24 118.0(4) . . ? O5 C23 C28 122.6(4) . . ? C24 C23 C28 119.3(4) . . ? C25 C24 C23 120.8(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 119.6(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.9(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C23 118.6(4) . . ? C27 C28 C29 119.3(3) . . ? C23 C28 C29 121.9(3) . . ? O6 C29 N5 124.3(3) . . ? O6 C29 C28 118.2(3) . . ? N5 C29 C28 117.5(3) . . ? N6 C30 S5 120.3(3) . . ? N6 C30 S6 116.6(3) . . ? S5 C30 S6 123.1(2) . . ? C32A C31A S6 130.6(15) . . ? C32A C31A H31A 104.6 . . ? S6 C31A H31A 104.6 . . ? C32A C31A H31B 104.6 . . ? S6 C31A H31B 104.6 . . ? H31A C31A H31B 105.7 . . ? C31A C32A C33A 120.2(14) . . ? C31A C32A H32A 107.3 . . ? C33A C32A H32A 107.3 . . ? C31A C32A H32B 107.3 . . ? C33A C32A H32B 107.3 . . ? H32A C32A H32B 106.9 . . ? S5 C33A C32A 102.7(9) . . ? S5 C33A H33A 111.2 . . ? C32A C33A H33A 111.2 . . ? S5 C33A H33B 111.2 . . ? C32A C33A H33B 111.2 . . ? H33A C33A H33B 109.1 . . ? C32B C31B S6 123.3(12) . . ? C32B C31B H31C 106.5 . . ? S6 C31B H31C 106.5 . . ? C32B C31B H31D 106.5 . . ? S6 C31B H31D 106.5 . . ? H31C C31B H31D 106.5 . . ? C333 C32B C31B 124.9(15) . . ? C333 C32B H32C 106.1 . . ? C31B C32B H32C 106.1 . . ? C333 C32B H32D 106.1 . . ? C31B C32B H32D 106.1 . . ? H32C C32B H32D 106.3 . . ? C32B C333 S5 130.0(13) . . ? C32B C333 H33C 104.8 . . ? S5 C333 H33C 104.8 . . ? C32B C333 H33D 104.8 . . ? S5 C333 H33D 104.8 . . ? H33C C333 H33D 105.8 . . ? Cl2 C34 Cl1 111.5(3) . . ? Cl2 C34 H34A 109.3 . . ? Cl1 C34 H34A 109.3 . . ? Cl2 C34 H34B 109.3 . . ? Cl1 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mn1 O2 C7 -79.7(3) . . . . ? O6 Mn1 O2 C7 102.9(3) . . . . ? N4 Mn1 O2 C7 -69.4(6) . . . . ? N6 Mn1 O2 C7 179.1(3) . . . . ? N2 Mn1 O2 C7 11.1(2) . . . . ? O6 Mn1 O4 C18 -104(3) . . . . ? O2 Mn1 O4 C18 -178.5(3) . . . . ? N4 Mn1 O4 C18 3.8(3) . . . . ? N6 Mn1 O4 C18 -88.8(3) . . . . ? N2 Mn1 O4 C18 105.7(3) . . . . ? O4 Mn1 O6 C29 1(3) . . . . ? O2 Mn1 O6 C29 74.9(3) . . . . ? N4 Mn1 O6 C29 -106.8(3) . . . . ? N6 Mn1 O6 C29 -14.9(3) . . . . ? N2 Mn1 O6 C29 150.7(3) . . . . ? C7 N1 N2 C8 -170.5(3) . . . . ? C7 N1 N2 Mn1 9.3(3) . . . . ? O4 Mn1 N2 C8 -103.0(4) . . . . ? O6 Mn1 N2 C8 78.4(4) . . . . ? O2 Mn1 N2 C8 168.7(4) . . . . ? N4 Mn1 N2 C8 -24.1(4) . . . . ? N6 Mn1 N2 C8 128.1(4) . . . . ? O4 Mn1 N2 N1 77.3(2) . . . . ? O6 Mn1 N2 N1 -101.4(2) . . . . ? O2 Mn1 N2 N1 -11.0(2) . . . . ? N4 Mn1 N2 N1 156.2(2) . . . . ? N6 Mn1 N2 N1 -51.7(5) . . . . ? O4 Mn1 N4 C19 175.2(4) . . . . ? O6 Mn1 N4 C19 -7.4(4) . . . . ? O2 Mn1 N4 C19 164.7(5) . . . . ? N6 Mn1 N4 C19 -84.3(4) . . . . ? N2 Mn1 N4 C19 87.1(4) . . . . ? O4 Mn1 N4 N3 -3.7(2) . . . . ? O6 Mn1 N4 N3 173.7(2) . . . . ? O2 Mn1 N4 N3 -14.2(7) . . . . ? N6 Mn1 N4 N3 96.8(2) . . . . ? N2 Mn1 N4 N3 -91.8(2) . . . . ? C19 N4 N3 C18 -176.0(4) . . . . ? Mn1 N4 N3 C18 3.2(4) . . . . ? O4 Mn1 N6 C30 7.7(5) . . . . ? O6 Mn1 N6 C30 -173.1(5) . . . . ? O2 Mn1 N6 C30 96.1(5) . . . . ? N4 Mn1 N6 C30 -72.1(5) . . . . ? N2 Mn1 N6 C30 135.3(5) . . . . ? O4 Mn1 N6 N5 -166.0(2) . . . . ? O6 Mn1 N6 N5 13.2(2) . . . . ? O2 Mn1 N6 N5 -77.6(3) . . . . ? N4 Mn1 N6 N5 114.2(3) . . . . ? N2 Mn1 N6 N5 -38.4(5) . . . . ? C30 N6 N5 C29 174.9(4) . . . . ? Mn1 N6 N5 C29 -9.7(4) . . . . ? C6 C1 C2 C3 0.6(10) . . . . ? C1 C2 C3 C4 -0.5(11) . . . . ? C2 C3 C4 C5 -0.6(10) . . . . ? C3 C4 C5 O1 -178.8(5) . . . . ? C3 C4 C5 C6 1.5(8) . . . . ? C2 C1 C6 C5 0.3(8) . . . . ? C2 C1 C6 C7 -179.4(5) . . . . ? O1 C5 C6 C1 178.9(4) . . . . ? C4 C5 C6 C1 -1.3(6) . . . . ? O1 C5 C6 C7 -1.3(6) . . . . ? C4 C5 C6 C7 178.4(4) . . . . ? Mn1 O2 C7 N1 -10.3(5) . . . . ? Mn1 O2 C7 C6 171.0(2) . . . . ? N2 N1 C7 O2 -1.1(5) . . . . ? N2 N1 C7 C6 177.7(3) . . . . ? C1 C6 C7 O2 2.5(5) . . . . ? C5 C6 C7 O2 -177.3(3) . . . . ? C1 C6 C7 N1 -176.4(4) . . . . ? C5 C6 C7 N1 3.9(5) . . . . ? N1 N2 C8 S2 177.6(2) . . . . ? Mn1 N2 C8 S2 -2.1(5) . . . . ? N1 N2 C8 S1 -2.8(4) . . . . ? Mn1 N2 C8 S1 177.47(19) . . . . ? C9 S2 C8 N2 148.8(3) . . . . ? C9 S2 C8 S1 -30.8(3) . . . . ? C11 S1 C8 N2 156.4(3) . . . . ? C11 S1 C8 S2 -24.0(3) . . . . ? C8 S2 C9 C10 70.7(4) . . . . ? S2 C9 C10 C11 -37.3(6) . . . . ? C9 C10 C11 S1 -36.0(6) . . . . ? C8 S1 C11 C10 66.7(4) . . . . ? C17 C12 C13 C14 -4.1(9) . . . . ? C12 C13 C14 C15 2.8(9) . . . . ? C13 C14 C15 C16 -1.3(9) . . . . ? C14 C15 C16 O3 -179.6(5) . . . . ? C14 C15 C16 C17 1.0(8) . . . . ? O3 C16 C17 C12 178.3(5) . . . . ? C15 C16 C17 C12 -2.4(8) . . . . ? O3 C16 C17 C18 8.3(8) . . . . ? C15 C16 C17 C18 -172.3(5) . . . . ? C13 C12 C17 C16 3.9(8) . . . . ? C13 C12 C17 C18 174.2(5) . . . . ? Mn1 O4 C18 N3 -3.3(5) . . . . ? Mn1 O4 C18 C17 175.2(3) . . . . ? N4 N3 C18 O4 -0.2(6) . . . . ? N4 N3 C18 C17 -178.8(3) . . . . ? C16 C17 C18 O4 168.7(4) . . . . ? C12 C17 C18 O4 -1.7(6) . . . . ? C16 C17 C18 N3 -12.7(7) . . . . ? C12 C17 C18 N3 176.9(4) . . . . ? N3 N4 C19 S3 0.0(5) . . . . ? Mn1 N4 C19 S3 -178.9(2) . . . . ? N3 N4 C19 S4 -175.3(3) . . . . ? Mn1 N4 C19 S4 5.8(5) . . . . ? C20 S3 C19 N4 176.5(3) . . . . ? C20 S3 C19 S4 -8.6(4) . . . . ? C22 S4 C19 N4 -165.9(3) . . . . ? C22 S4 C19 S3 19.2(3) . . . . ? C19 S3 C20 C21 26.2(5) . . . . ? S3 C20 C21 C22 -60.2(6) . . . . ? C20 C21 C22 S4 74.1(5) . . . . ? C19 S4 C22 C21 -48.8(5) . . . . ? O5 C23 C24 C25 -179.4(4) . . . . ? C28 C23 C24 C25 -1.3(6) . . . . ? C23 C24 C25 C26 0.7(7) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C25 C26 C27 C28 0.2(7) . . . . ? C26 C27 C28 C23 -0.7(6) . . . . ? C26 C27 C28 C29 176.0(4) . . . . ? O5 C23 C28 C27 179.3(4) . . . . ? C24 C23 C28 C27 1.3(6) . . . . ? O5 C23 C28 C29 2.7(6) . . . . ? C24 C23 C28 C29 -175.4(4) . . . . ? Mn1 O6 C29 N5 15.6(5) . . . . ? Mn1 O6 C29 C28 -162.9(3) . . . . ? N6 N5 C29 O6 -1.9(5) . . . . ? N6 N5 C29 C28 176.6(3) . . . . ? C27 C28 C29 O6 -1.0(5) . . . . ? C23 C28 C29 O6 175.6(3) . . . . ? C27 C28 C29 N5 -179.6(4) . . . . ? C23 C28 C29 N5 -3.0(5) . . . . ? N5 N6 C30 S5 -0.7(5) . . . . ? Mn1 N6 C30 S5 -174.1(3) . . . . ? N5 N6 C30 S6 179.4(3) . . . . ? Mn1 N6 C30 S6 6.0(7) . . . . ? C33A S5 C30 N6 -160.9(6) . . . . ? C333 S5 C30 N6 179.0(6) . . . . ? C33A S5 C30 S6 19.0(6) . . . . ? C333 S5 C30 S6 -1.1(6) . . . . ? C31B S6 C30 N6 174.9(7) . . . . ? C31A S6 C30 N6 -154.3(6) . . . . ? C31B S6 C30 S5 -5.0(7) . . . . ? C31A S6 C30 S5 25.8(6) . . . . ? C31B S6 C31A C32A 64(2) . . . . ? C30 S6 C31A C32A -49(2) . . . . ? S6 C31A C32A C33A 13(3) . . . . ? C30 S5 C33A C32A -52.1(8) . . . . ? C333 S5 C33A C32A 31.8(19) . . . . ? C31A C32A C33A S5 42.5(18) . . . . ? C30 S6 C31B C32B 0.0(16) . . . . ? C31A S6 C31B C32B -74.3(18) . . . . ? S6 C31B C32B C333 16(3) . . . . ? C31B C32B C333 S5 -27(3) . . . . ? C30 S5 C333 C32B 18.4(17) . . . . ? C33A S5 C333 C32B -83(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.169 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.093 # Attachment 'complex_3.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 844921' #TrackingRef 'complex_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 Fe N6 O6 S6, 2(C H Cl3)' _chemical_formula_sum 'C35 H35 Cl6 Fe N6 O6 S6' _chemical_formula_weight 1096.60 _chemical_absolute_configuration ? 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.227(3) _cell_length_b 13.922(7) _cell_length_c 15.914(6) _cell_angle_alpha 69.021(2) _cell_angle_beta 89.488(2) _cell_angle_gamma 77.920(2) _cell_volume 2265.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14676 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19566 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10304 _reflns_number_gt 7683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0428P)^2^+4.5133P] 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 10304 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.58434(4) 0.18220(4) 0.18928(3) 0.02133(12) Uani 1 1 d . . . Cl1 Cl 0.92502(16) 0.67859(12) 0.18636(10) 0.0788(4) Uani 1 1 d . . . Cl2 Cl 0.9127(2) 0.84607(15) 0.25096(12) 0.1055(7) Uani 1 1 d . . . Cl3 Cl 0.82812(17) 0.66279(13) 0.35775(10) 0.0864(5) Uani 1 1 d . . . Cl4 Cl 0.99688(10) 0.38489(10) 0.28695(8) 0.0521(3) Uani 1 1 d . . . Cl5 Cl 0.80137(13) 0.28740(12) 0.36794(10) 0.0698(4) Uani 1 1 d . . . Cl6 Cl 0.95411(12) 0.35257(14) 0.47342(9) 0.0732(4) Uani 1 1 d . . . S1 S 0.35196(7) 0.49273(7) -0.03097(6) 0.02621(19) Uani 1 1 d . . . S2 S 0.47357(8) 0.28376(7) -0.04375(6) 0.02773(19) Uani 1 1 d . . . S3 S 0.60626(9) 0.00217(8) 0.42164(7) 0.0373(2) Uani 1 1 d . . . S4 S 0.88193(9) -0.05002(9) 0.42695(6) 0.0393(2) Uani 1 1 d . . . S5 S 0.78673(8) 0.13638(8) 0.00364(6) 0.0302(2) Uani 1 1 d . . . S6 S 0.70130(9) -0.06328(8) 0.03033(7) 0.0354(2) Uani 1 1 d . . . O1 O 0.2206(2) 0.5091(2) 0.19267(19) 0.0434(7) Uani 1 1 d . . . H1O H 0.2579 0.4766 0.1614 0.065 Uiso 1 1 calc . . . O2 O 0.5306(2) 0.25716(18) 0.27285(15) 0.0262(5) Uani 1 1 d . . . O3 O 1.0748(2) 0.1101(2) 0.26979(17) 0.0391(7) Uani 1 1 d . . . H3O H 1.0104 0.0883 0.2843 0.059 Uiso 1 1 calc . . . O4 O 0.72261(19) 0.24380(18) 0.13910(15) 0.0238(5) Uani 1 1 d . . . O5 O 0.5397(3) -0.2088(2) 0.21419(19) 0.0415(7) Uani 1 1 d . . . H5O H 0.5674 -0.1560 0.1842 0.062 Uiso 1 1 calc . . . O6 O 0.4652(2) 0.09389(18) 0.22757(17) 0.0282(5) Uani 1 1 d . . . N1 N 0.3979(2) 0.3795(2) 0.15603(18) 0.0234(6) Uani 1 1 d . . . N2 N 0.4549(2) 0.3182(2) 0.10740(18) 0.0212(6) Uani 1 1 d . . . N3 N 0.8456(2) 0.1094(2) 0.25506(19) 0.0248(6) Uani 1 1 d . . . N4 N 0.7333(2) 0.0888(2) 0.28735(18) 0.0238(6) Uani 1 1 d . . . N5 N 0.5728(2) -0.0203(2) 0.16601(19) 0.0256(6) Uani 1 1 d . . . N6 N 0.6295(2) 0.0636(2) 0.12213(19) 0.0243(6) Uani 1 1 d . . . C1 C 0.2803(3) 0.4735(3) 0.2753(3) 0.0321(8) Uani 1 1 d . . . C2 C 0.2308(4) 0.5188(3) 0.3366(3) 0.0421(10) Uani 1 1 d . . . H2 H 0.1579 0.5723 0.3196 0.051 Uiso 1 1 calc . . . C3 C 0.2870(4) 0.4864(3) 0.4217(3) 0.0441(10) Uani 1 1 d . . . H3 H 0.2512 0.5167 0.4633 0.053 Uiso 1 1 calc . . . C4 C 0.3947(4) 0.4105(3) 0.4474(3) 0.0412(10) Uani 1 1 d . . . H4 H 0.4345 0.3906 0.5055 0.049 Uiso 1 1 calc . . . C5 C 0.4440(3) 0.3638(3) 0.3879(2) 0.0320(8) Uani 1 1 d . . . H5 H 0.5173 0.3107 0.4058 0.038 Uiso 1 1 calc . . . C6 C 0.3874(3) 0.3937(3) 0.3015(2) 0.0261(7) Uani 1 1 d . . . C7 C 0.4421(3) 0.3393(3) 0.2409(2) 0.0229(7) Uani 1 1 d . . . C8 C 0.4291(3) 0.3612(3) 0.0206(2) 0.0221(7) Uani 1 1 d . . . C9 C 0.2899(3) 0.4890(3) -0.1346(3) 0.0340(8) Uani 1 1 d . . . H9A H 0.2379 0.4366 -0.1186 0.041 Uiso 1 1 calc . . . H9B H 0.2368 0.5588 -0.1686 0.041 Uiso 1 1 calc . . . C10 C 0.3850(3) 0.4614(3) -0.1963(2) 0.0333(8) Uani 1 1 d . . . H10A H 0.3493 0.4287 -0.2330 0.040 Uiso 1 1 calc . . . H10B H 0.4049 0.5273 -0.2382 0.040 Uiso 1 1 calc . . . C11 C 0.5021(3) 0.3868(3) -0.1456(2) 0.0303(8) Uani 1 1 d . . . H11A H 0.5542 0.4276 -0.1292 0.036 Uiso 1 1 calc . . . H11B H 0.5473 0.3539 -0.1857 0.036 Uiso 1 1 calc . . . C12 C 1.0530(3) 0.1918(3) 0.1896(2) 0.0290(8) Uani 1 1 d . . . C13 C 1.1503(3) 0.2385(4) 0.1542(3) 0.0398(10) Uani 1 1 d . . . H13 H 1.2283 0.2128 0.1864 0.048 Uiso 1 1 calc . . . C14 C 1.1332(4) 0.3213(4) 0.0731(3) 0.0427(10) Uani 1 1 d . . . H14 H 1.1993 0.3535 0.0502 0.051 Uiso 1 1 calc . . . C15 C 1.0209(3) 0.3589(3) 0.0239(3) 0.0356(9) Uani 1 1 d . . . H15 H 1.0107 0.4149 -0.0331 0.043 Uiso 1 1 calc . . . C16 C 0.9244(3) 0.3141(3) 0.0588(2) 0.0273(7) Uani 1 1 d . . . H16 H 0.8472 0.3401 0.0256 0.033 Uiso 1 1 calc . . . C17 C 0.9380(3) 0.2314(3) 0.1419(2) 0.0239(7) Uani 1 1 d . . . C18 C 0.8296(3) 0.1920(3) 0.1800(2) 0.0211(6) Uani 1 1 d . . . C19 C 0.7408(3) 0.0199(3) 0.3692(2) 0.0257(7) Uani 1 1 d . . . C20 C 0.6473(4) -0.1394(3) 0.4807(3) 0.0446(10) Uani 1 1 d . . . H20A H 0.5740 -0.1637 0.5075 0.054 Uiso 1 1 calc . . . H20B H 0.6728 -0.1733 0.4364 0.054 Uiso 1 1 calc . . . C21 C 0.7487(5) -0.1764(4) 0.5547(3) 0.0573(13) Uani 1 1 d . . . H21A H 0.7949 -0.2473 0.5598 0.069 Uiso 1 1 calc . . . H21B H 0.7116 -0.1832 0.6127 0.069 Uiso 1 1 calc . . . C22 C 0.8373(4) -0.1044(4) 0.5404(3) 0.0459(10) Uani 1 1 d . . . H22A H 0.9120 -0.1444 0.5806 0.055 Uiso 1 1 calc . . . H22B H 0.8001 -0.0453 0.5596 0.055 Uiso 1 1 calc . . . C23 C 0.4592(3) -0.1828(3) 0.2712(2) 0.0284(7) Uani 1 1 d . . . C24 C 0.4036(4) -0.2605(3) 0.3265(3) 0.0379(9) Uani 1 1 d . . . H24 H 0.4248 -0.3299 0.3257 0.046 Uiso 1 1 calc . . . C25 C 0.3176(4) -0.2371(3) 0.3827(3) 0.0467(11) Uani 1 1 d . . . H25 H 0.2789 -0.2902 0.4198 0.056 Uiso 1 1 calc . . . C26 C 0.2874(5) -0.1367(4) 0.3854(3) 0.0561(13) Uani 1 1 d . . . H26 H 0.2281 -0.1209 0.4242 0.067 Uiso 1 1 calc . . . C27 C 0.3438(4) -0.0599(3) 0.3315(3) 0.0452(11) Uani 1 1 d . . . H27 H 0.3230 0.0088 0.3338 0.054 Uiso 1 1 calc . . . C28 C 0.4308(3) -0.0811(3) 0.2736(2) 0.0277(7) Uani 1 1 d . . . C29 C 0.4913(3) 0.0029(3) 0.2194(2) 0.0251(7) Uani 1 1 d . . . C30 C 0.6976(3) 0.0471(3) 0.0597(2) 0.0235(7) Uani 1 1 d . . . C31 C 0.7844(4) 0.1232(3) -0.1059(2) 0.0371(9) Uani 1 1 d . . . H31A H 0.6983 0.1357 -0.1280 0.045 Uiso 1 1 calc . . . H31B H 0.8206 0.1789 -0.1488 0.045 Uiso 1 1 calc . . . C32 C 0.8523(4) 0.0168(3) -0.1066(3) 0.0389(9) Uani 1 1 d . . . H32A H 0.8161 0.0033 -0.1567 0.047 Uiso 1 1 calc . . . H32B H 0.9386 0.0192 -0.1180 0.047 Uiso 1 1 calc . . . C33 C 0.8478(4) -0.0730(3) -0.0192(3) 0.0381(9) Uani 1 1 d . . . H33A H 0.9115 -0.0759 0.0249 0.046 Uiso 1 1 calc . . . H33B H 0.8680 -0.1400 -0.0302 0.046 Uiso 1 1 calc . . . C34 C 0.8458(4) 0.7473(4) 0.2488(3) 0.0491(11) Uani 1 1 d . . . H34 H 0.7623 0.7811 0.2179 0.059 Uiso 1 1 calc . . . C35 C 0.8862(4) 0.3811(4) 0.3652(3) 0.0473(11) Uani 1 1 d . . . H35 H 0.8293 0.4520 0.3459 0.057 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0171(2) 0.0207(2) 0.0252(3) -0.0072(2) 0.00504(17) -0.00440(17) Cl1 0.1084(12) 0.0655(9) 0.0696(9) -0.0446(8) -0.0018(8) 0.0019(8) Cl2 0.183(2) 0.0953(13) 0.0885(12) -0.0638(11) 0.0576(12) -0.0846(13) Cl3 0.1306(14) 0.0817(11) 0.0460(8) -0.0083(7) 0.0053(8) -0.0483(10) Cl4 0.0467(6) 0.0624(8) 0.0426(6) -0.0140(5) 0.0008(5) -0.0112(5) Cl5 0.0699(8) 0.0799(10) 0.0644(8) -0.0214(7) 0.0107(6) -0.0360(7) Cl6 0.0575(7) 0.1142(12) 0.0524(7) -0.0507(8) -0.0066(6) 0.0081(7) S1 0.0244(4) 0.0233(4) 0.0280(4) -0.0081(4) -0.0024(3) -0.0012(3) S2 0.0331(5) 0.0238(4) 0.0269(4) -0.0103(4) 0.0034(3) -0.0057(3) S3 0.0334(5) 0.0356(5) 0.0329(5) -0.0029(4) 0.0140(4) -0.0039(4) S4 0.0321(5) 0.0494(6) 0.0242(5) -0.0038(4) -0.0005(4) -0.0007(4) S5 0.0306(5) 0.0362(5) 0.0315(5) -0.0171(4) 0.0137(4) -0.0156(4) S6 0.0407(5) 0.0365(5) 0.0399(5) -0.0232(5) 0.0137(4) -0.0158(4) O1 0.0336(14) 0.0487(18) 0.0436(17) -0.0226(14) 0.0002(12) 0.0103(12) O2 0.0228(12) 0.0272(13) 0.0260(12) -0.0103(10) 0.0012(9) 0.0009(9) O3 0.0231(13) 0.0608(19) 0.0308(14) -0.0148(14) -0.0019(10) -0.0070(12) O4 0.0185(11) 0.0231(12) 0.0270(12) -0.0056(10) 0.0038(9) -0.0050(9) O5 0.0569(18) 0.0325(15) 0.0462(17) -0.0216(13) 0.0250(13) -0.0212(13) O6 0.0218(12) 0.0233(13) 0.0394(14) -0.0112(11) 0.0112(10) -0.0055(9) N1 0.0217(14) 0.0245(15) 0.0243(15) -0.0106(12) 0.0044(11) -0.0026(11) N2 0.0184(13) 0.0204(14) 0.0242(14) -0.0073(12) 0.0028(10) -0.0041(10) N3 0.0191(13) 0.0298(16) 0.0258(15) -0.0104(13) 0.0054(11) -0.0055(11) N4 0.0241(14) 0.0238(15) 0.0234(14) -0.0088(12) 0.0066(11) -0.0046(11) N5 0.0272(15) 0.0235(15) 0.0283(15) -0.0092(12) 0.0071(12) -0.0107(12) N6 0.0201(14) 0.0256(15) 0.0281(15) -0.0096(12) 0.0067(11) -0.0076(11) C1 0.0316(19) 0.031(2) 0.034(2) -0.0134(17) 0.0085(15) -0.0051(15) C2 0.040(2) 0.037(2) 0.050(3) -0.022(2) 0.0154(18) 0.0003(17) C3 0.056(3) 0.040(2) 0.045(2) -0.026(2) 0.023(2) -0.012(2) C4 0.058(3) 0.042(2) 0.029(2) -0.0162(18) 0.0113(18) -0.017(2) C5 0.036(2) 0.032(2) 0.0305(19) -0.0137(16) 0.0083(15) -0.0094(16) C6 0.0274(17) 0.0245(18) 0.0284(18) -0.0105(15) 0.0097(14) -0.0086(14) C7 0.0197(16) 0.0214(17) 0.0304(18) -0.0110(14) 0.0066(13) -0.0079(13) C8 0.0172(15) 0.0232(17) 0.0277(17) -0.0101(14) 0.0022(12) -0.0067(12) C9 0.033(2) 0.037(2) 0.031(2) -0.0111(17) -0.0077(15) -0.0052(16) C10 0.041(2) 0.035(2) 0.0242(18) -0.0081(16) -0.0003(15) -0.0126(16) C11 0.0319(19) 0.034(2) 0.0294(19) -0.0142(16) 0.0100(14) -0.0120(15) C12 0.0210(16) 0.043(2) 0.0310(19) -0.0226(17) 0.0053(14) -0.0088(15) C13 0.0204(18) 0.063(3) 0.049(2) -0.031(2) 0.0063(16) -0.0171(17) C14 0.031(2) 0.052(3) 0.057(3) -0.027(2) 0.0175(18) -0.0244(19) C15 0.036(2) 0.032(2) 0.045(2) -0.0172(18) 0.0183(17) -0.0152(16) C16 0.0253(17) 0.0238(18) 0.037(2) -0.0149(16) 0.0095(14) -0.0067(13) C17 0.0217(16) 0.0285(18) 0.0279(18) -0.0155(15) 0.0076(13) -0.0100(13) C18 0.0212(16) 0.0215(17) 0.0227(16) -0.0111(14) 0.0031(12) -0.0038(12) C19 0.0264(17) 0.0268(18) 0.0246(17) -0.0112(15) 0.0051(13) -0.0044(14) C20 0.049(2) 0.030(2) 0.047(3) -0.0034(19) 0.0107(19) -0.0105(18) C21 0.062(3) 0.046(3) 0.046(3) 0.003(2) 0.004(2) -0.008(2) C22 0.059(3) 0.052(3) 0.0207(19) -0.0060(19) -0.0022(17) -0.012(2) C23 0.0325(19) 0.0304(19) 0.0265(18) -0.0120(15) 0.0033(14) -0.0129(15) C24 0.057(3) 0.031(2) 0.032(2) -0.0140(17) 0.0102(18) -0.0209(18) C25 0.059(3) 0.037(2) 0.048(3) -0.011(2) 0.023(2) -0.029(2) C26 0.065(3) 0.042(3) 0.070(3) -0.024(2) 0.044(3) -0.024(2) C27 0.045(2) 0.034(2) 0.060(3) -0.018(2) 0.028(2) -0.0168(18) C28 0.0232(17) 0.0311(19) 0.0289(18) -0.0096(15) 0.0045(13) -0.0091(14) C29 0.0210(16) 0.0250(18) 0.0280(18) -0.0079(15) 0.0023(13) -0.0056(13) C30 0.0209(16) 0.0264(18) 0.0233(17) -0.0093(14) 0.0017(12) -0.0053(13) C31 0.040(2) 0.049(3) 0.0211(18) -0.0106(17) 0.0056(15) -0.0106(18) C32 0.042(2) 0.051(3) 0.032(2) -0.0246(19) 0.0101(16) -0.0120(19) C33 0.040(2) 0.041(2) 0.041(2) -0.0262(19) 0.0128(17) -0.0059(17) C34 0.056(3) 0.046(3) 0.041(2) -0.015(2) 0.004(2) -0.005(2) C35 0.041(2) 0.051(3) 0.048(3) -0.023(2) -0.0046(19) 0.0018(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O6 1.952(2) . ? Fe O4 1.957(2) . ? Fe O2 1.984(2) . ? Fe N2 2.123(3) . ? Fe N4 2.146(3) . ? Fe N6 2.243(3) . ? Cl1 C34 1.732(5) . ? Cl2 C34 1.710(5) . ? Cl3 C34 1.750(5) . ? Cl4 C35 1.747(5) . ? Cl5 C35 1.758(5) . ? Cl6 C35 1.764(5) . ? S1 C8 1.746(3) . ? S1 C9 1.818(4) . ? S2 C8 1.736(3) . ? S2 C11 1.818(4) . ? S3 C19 1.739(3) . ? S3 C20 1.812(4) . ? S4 C19 1.745(3) . ? S4 C22 1.803(4) . ? S5 C30 1.747(3) . ? S5 C31 1.818(4) . ? S6 C30 1.752(4) . ? S6 C33 1.818(4) . ? O1 C1 1.354(5) . ? O1 H1O 0.8400 . ? O2 C7 1.293(4) . ? O3 C12 1.353(5) . ? O3 H3O 0.8400 . ? O4 C18 1.304(4) . ? O5 C23 1.361(4) . ? O5 H5O 0.8400 . ? O6 C29 1.292(4) . ? N1 C7 1.318(4) . ? N1 N2 1.404(4) . ? N2 C8 1.301(4) . ? N3 C18 1.310(4) . ? N3 N4 1.403(4) . ? N4 C19 1.303(4) . ? N5 C29 1.312(4) . ? N5 N6 1.406(4) . ? N6 C30 1.304(4) . ? C1 C2 1.394(5) . ? C1 C6 1.404(5) . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.401(5) . ? C5 H5 0.9500 . ? C6 C7 1.483(5) . ? C9 C10 1.527(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.519(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.399(5) . ? C12 C17 1.403(5) . ? C13 C14 1.370(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(5) . ? C16 H16 0.9500 . ? C17 C18 1.476(4) . ? C20 C21 1.513(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.515(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.388(5) . ? C23 C28 1.400(5) . ? C24 C25 1.378(6) . ? C24 H24 0.9500 . ? C25 C26 1.383(6) . ? C25 H25 0.9500 . ? C26 C27 1.377(6) . ? C26 H26 0.9500 . ? C27 C28 1.395(5) . ? C27 H27 0.9500 . ? C28 C29 1.475(5) . ? C31 C32 1.522(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.510(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34 1.0000 . ? C35 H35 1.0000 . ? 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 O6 Fe O4 165.71(10) . . ? O6 Fe O2 92.67(10) . . ? O4 Fe O2 100.98(10) . . ? O6 Fe N2 94.71(10) . . ? O4 Fe N2 92.56(10) . . ? O2 Fe N2 76.73(10) . . ? O6 Fe N4 100.11(11) . . ? O4 Fe N4 76.59(10) . . ? O2 Fe N4 87.10(10) . . ? N2 Fe N4 158.55(11) . . ? O6 Fe N6 74.65(10) . . ? O4 Fe N6 91.26(10) . . ? O2 Fe N6 165.32(10) . . ? N2 Fe N6 111.09(11) . . ? N4 Fe N6 87.90(11) . . ? C8 S1 C9 100.08(17) . . ? C8 S2 C11 98.01(17) . . ? C19 S3 C20 99.01(18) . . ? C19 S4 C22 100.95(18) . . ? C30 S5 C31 99.50(17) . . ? C30 S6 C33 100.20(17) . . ? C1 O1 H1O 109.5 . . ? C7 O2 Fe 115.4(2) . . ? C12 O3 H3O 109.5 . . ? C18 O4 Fe 115.9(2) . . ? C23 O5 H5O 109.5 . . ? C29 O6 Fe 117.1(2) . . ? C7 N1 N2 111.1(3) . . ? C8 N2 N1 114.4(3) . . ? C8 N2 Fe 132.4(2) . . ? N1 N2 Fe 112.64(19) . . ? C18 N3 N4 111.1(3) . . ? C19 N4 N3 114.6(3) . . ? C19 N4 Fe 133.9(2) . . ? N3 N4 Fe 111.44(19) . . ? C29 N5 N6 112.0(3) . . ? C30 N6 N5 112.5(3) . . ? C30 N6 Fe 138.9(2) . . ? N5 N6 Fe 108.48(19) . . ? O1 C1 C2 117.4(3) . . ? O1 C1 C6 123.3(3) . . ? C2 C1 C6 119.3(4) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C7 118.8(3) . . ? C1 C6 C7 122.1(3) . . ? O2 C7 N1 123.7(3) . . ? O2 C7 C6 119.1(3) . . ? N1 C7 C6 117.2(3) . . ? N2 C8 S2 118.1(2) . . ? N2 C8 S1 121.6(3) . . ? S2 C8 S1 120.30(19) . . ? C10 C9 S1 115.0(3) . . ? C10 C9 H9A 108.5 . . ? S1 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? S1 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 113.5(3) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 S2 112.4(2) . . ? C10 C11 H11A 109.1 . . ? S2 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? S2 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? O3 C12 C13 117.7(3) . . ? O3 C12 C17 122.9(3) . . ? C13 C12 C17 119.4(3) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 119.1(3) . . ? C16 C17 C18 119.2(3) . . ? C12 C17 C18 121.6(3) . . ? O4 C18 N3 123.5(3) . . ? O4 C18 C17 118.2(3) . . ? N3 C18 C17 118.2(3) . . ? N4 C19 S3 118.4(3) . . ? N4 C19 S4 121.2(2) . . ? S3 C19 S4 120.3(2) . . ? C21 C20 S3 114.5(3) . . ? C21 C20 H20A 108.6 . . ? S3 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? S3 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 114.6(4) . . ? C20 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? C20 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C21 C22 S4 116.2(3) . . ? C21 C22 H22A 108.2 . . ? S4 C22 H22A 108.2 . . ? C21 C22 H22B 108.2 . . ? S4 C22 H22B 108.2 . . ? H22A C22 H22B 107.4 . . ? O5 C23 C24 117.8(3) . . ? O5 C23 C28 121.8(3) . . ? C24 C23 C28 120.4(3) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.6(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 121.3(4) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C23 118.2(3) . . ? C27 C28 C29 119.2(3) . . ? C23 C28 C29 122.6(3) . . ? O6 C29 N5 123.1(3) . . ? O6 C29 C28 119.7(3) . . ? N5 C29 C28 117.2(3) . . ? N6 C30 S5 119.8(3) . . ? N6 C30 S6 121.2(3) . . ? S5 C30 S6 119.00(19) . . ? C32 C31 S5 114.9(3) . . ? C32 C31 H31A 108.6 . . ? S5 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? S5 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C31 112.8(3) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C32 C33 S6 114.3(3) . . ? C32 C33 H33A 108.7 . . ? S6 C33 H33A 108.7 . . ? C32 C33 H33B 108.7 . . ? S6 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? Cl2 C34 Cl1 111.5(3) . . ? Cl2 C34 Cl3 111.5(3) . . ? Cl1 C34 Cl3 111.6(3) . . ? Cl2 C34 H34 107.3 . . ? Cl1 C34 H34 107.3 . . ? Cl3 C34 H34 107.3 . . ? Cl4 C35 Cl5 110.2(3) . . ? Cl4 C35 Cl6 110.8(2) . . ? Cl5 C35 Cl6 110.5(3) . . ? Cl4 C35 H35 108.4 . . ? Cl5 C35 H35 108.4 . . ? Cl6 C35 H35 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Fe O2 C7 -88.2(2) . . . . ? O4 Fe O2 C7 96.1(2) . . . . ? N2 Fe O2 C7 6.0(2) . . . . ? N4 Fe O2 C7 171.8(2) . . . . ? N6 Fe O2 C7 -117.9(4) . . . . ? O6 Fe O4 C18 -69.2(5) . . . . ? O2 Fe O4 C18 93.3(2) . . . . ? N2 Fe O4 C18 170.3(2) . . . . ? N4 Fe O4 C18 9.0(2) . . . . ? N6 Fe O4 C18 -78.6(2) . . . . ? O4 Fe O6 C29 9.2(6) . . . . ? O2 Fe O6 C29 -153.6(2) . . . . ? N2 Fe O6 C29 129.5(2) . . . . ? N4 Fe O6 C29 -66.0(3) . . . . ? N6 Fe O6 C29 18.9(2) . . . . ? C7 N1 N2 C8 -170.3(3) . . . . ? C7 N1 N2 Fe 2.2(3) . . . . ? O6 Fe N2 C8 -102.0(3) . . . . ? O4 Fe N2 C8 65.7(3) . . . . ? O2 Fe N2 C8 166.3(3) . . . . ? N4 Fe N2 C8 124.3(3) . . . . ? N6 Fe N2 C8 -26.7(3) . . . . ? O6 Fe N2 N1 87.2(2) . . . . ? O4 Fe N2 N1 -105.1(2) . . . . ? O2 Fe N2 N1 -4.45(19) . . . . ? N4 Fe N2 N1 -46.5(4) . . . . ? N6 Fe N2 N1 162.54(18) . . . . ? C18 N3 N4 C19 -168.5(3) . . . . ? C18 N3 N4 Fe 10.5(3) . . . . ? O6 Fe N4 C19 -26.0(3) . . . . ? O4 Fe N4 C19 168.2(3) . . . . ? O2 Fe N4 C19 66.2(3) . . . . ? N2 Fe N4 C19 106.9(4) . . . . ? N6 Fe N4 C19 -100.0(3) . . . . ? O6 Fe N4 N3 155.2(2) . . . . ? O4 Fe N4 N3 -10.6(2) . . . . ? O2 Fe N4 N3 -112.6(2) . . . . ? N2 Fe N4 N3 -71.8(3) . . . . ? N6 Fe N4 N3 81.2(2) . . . . ? C29 N5 N6 C30 -171.0(3) . . . . ? C29 N5 N6 Fe 13.1(3) . . . . ? O6 Fe N6 C30 168.7(4) . . . . ? O4 Fe N6 C30 -13.7(4) . . . . ? O2 Fe N6 C30 -160.4(4) . . . . ? N2 Fe N6 C30 79.5(4) . . . . ? N4 Fe N6 C30 -90.2(4) . . . . ? O6 Fe N6 N5 -17.02(19) . . . . ? O4 Fe N6 N5 160.6(2) . . . . ? O2 Fe N6 N5 13.9(5) . . . . ? N2 Fe N6 N5 -106.2(2) . . . . ? N4 Fe N6 N5 84.1(2) . . . . ? O1 C1 C2 C3 -179.9(4) . . . . ? C6 C1 C2 C3 0.7(6) . . . . ? C1 C2 C3 C4 1.5(7) . . . . ? C2 C3 C4 C5 -2.4(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C4 C5 C6 C1 1.1(5) . . . . ? C4 C5 C6 C7 -178.5(3) . . . . ? O1 C1 C6 C5 178.7(3) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? O1 C1 C6 C7 -1.8(5) . . . . ? C2 C1 C6 C7 177.6(3) . . . . ? Fe O2 C7 N1 -7.4(4) . . . . ? Fe O2 C7 C6 173.6(2) . . . . ? N2 N1 C7 O2 3.2(4) . . . . ? N2 N1 C7 C6 -177.9(3) . . . . ? C5 C6 C7 O2 8.9(5) . . . . ? C1 C6 C7 O2 -170.6(3) . . . . ? C5 C6 C7 N1 -170.0(3) . . . . ? C1 C6 C7 N1 10.4(5) . . . . ? N1 N2 C8 S2 -169.4(2) . . . . ? Fe N2 C8 S2 19.9(4) . . . . ? N1 N2 C8 S1 10.5(4) . . . . ? Fe N2 C8 S1 -160.18(17) . . . . ? C11 S2 C8 N2 -147.7(3) . . . . ? C11 S2 C8 S1 32.5(2) . . . . ? C9 S1 C8 N2 -157.6(3) . . . . ? C9 S1 C8 S2 22.3(2) . . . . ? C8 S1 C9 C10 -63.2(3) . . . . ? S1 C9 C10 C11 32.0(4) . . . . ? C9 C10 C11 S2 40.2(4) . . . . ? C8 S2 C11 C10 -72.0(3) . . . . ? O3 C12 C13 C14 179.8(4) . . . . ? C17 C12 C13 C14 -0.7(6) . . . . ? C12 C13 C14 C15 -1.4(6) . . . . ? C13 C14 C15 C16 2.0(6) . . . . ? C14 C15 C16 C17 -0.6(6) . . . . ? C15 C16 C17 C12 -1.4(5) . . . . ? C15 C16 C17 C18 174.8(3) . . . . ? O3 C12 C17 C16 -178.5(3) . . . . ? C13 C12 C17 C16 2.0(5) . . . . ? O3 C12 C17 C18 5.5(5) . . . . ? C13 C12 C17 C18 -174.1(3) . . . . ? Fe O4 C18 N3 -6.3(4) . . . . ? Fe O4 C18 C17 176.4(2) . . . . ? N4 N3 C18 O4 -3.6(4) . . . . ? N4 N3 C18 C17 173.7(3) . . . . ? C16 C17 C18 O4 -7.3(5) . . . . ? C12 C17 C18 O4 168.7(3) . . . . ? C16 C17 C18 N3 175.2(3) . . . . ? C12 C17 C18 N3 -8.7(5) . . . . ? N3 N4 C19 S3 171.1(2) . . . . ? Fe N4 C19 S3 -7.6(5) . . . . ? N3 N4 C19 S4 -6.6(4) . . . . ? Fe N4 C19 S4 174.63(17) . . . . ? C20 S3 C19 N4 142.0(3) . . . . ? C20 S3 C19 S4 -40.2(3) . . . . ? C22 S4 C19 N4 166.2(3) . . . . ? C22 S4 C19 S3 -11.5(3) . . . . ? C19 S3 C20 C21 66.6(4) . . . . ? S3 C20 C21 C22 -27.7(5) . . . . ? C20 C21 C22 S4 -41.0(5) . . . . ? C19 S4 C22 C21 60.2(4) . . . . ? O5 C23 C24 C25 -177.3(4) . . . . ? C28 C23 C24 C25 1.6(6) . . . . ? C23 C24 C25 C26 -1.0(7) . . . . ? C24 C25 C26 C27 0.0(8) . . . . ? C25 C26 C27 C28 0.3(8) . . . . ? C26 C27 C28 C23 0.4(7) . . . . ? C26 C27 C28 C29 -178.1(4) . . . . ? O5 C23 C28 C27 177.6(4) . . . . ? C24 C23 C28 C27 -1.3(6) . . . . ? O5 C23 C28 C29 -4.0(5) . . . . ? C24 C23 C28 C29 177.1(4) . . . . ? Fe O6 C29 N5 -19.3(4) . . . . ? Fe O6 C29 C28 158.9(2) . . . . ? N6 N5 C29 O6 1.9(5) . . . . ? N6 N5 C29 C28 -176.3(3) . . . . ? C27 C28 C29 O6 1.5(5) . . . . ? C23 C28 C29 O6 -176.9(3) . . . . ? C27 C28 C29 N5 179.8(4) . . . . ? C23 C28 C29 N5 1.4(5) . . . . ? N5 N6 C30 S5 -174.5(2) . . . . ? Fe N6 C30 S5 -0.3(5) . . . . ? N5 N6 C30 S6 5.8(4) . . . . ? Fe N6 C30 S6 179.93(18) . . . . ? C31 S5 C30 N6 -148.4(3) . . . . ? C31 S5 C30 S6 31.3(2) . . . . ? C33 S6 C30 N6 -157.7(3) . . . . ? C33 S6 C30 S5 22.6(2) . . . . ? C30 S5 C31 C32 -67.7(3) . . . . ? S5 C31 C32 C33 32.1(4) . . . . ? C31 C32 C33 S6 39.7(4) . . . . ? C30 S6 C33 C32 -67.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.787 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.107 # Attachment 'complex_4.cif' data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 844922' #TrackingRef 'complex_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Cl2 Fe N4 O4 S4, 2(C H4 0)' _chemical_formula_sum 'C24 H32 Cl2 Fe N4 O6 S4' _chemical_formula_weight 727.53 _chemical_absolute_configuration ? 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.394(4) _cell_length_b 9.405(4) _cell_length_c 17.332(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.676(19) _cell_angle_gamma 90.00 _cell_volume 1539.58(95) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7911 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14463 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 30.01 _reflns_number_total 4496 _reflns_number_gt 3713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0552P)^2^+0.1653P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4496 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Fe Fe 1.0000 0.0000 1.0000 0.01693(9) Uani 1 2 d S . . Cl Cl 1.04321(5) 0.24851(5) 1.03149(3) 0.02766(11) Uani 1 1 d . . . S1 S 0.96516(4) 0.05937(6) 0.78953(2) 0.02572(12) Uani 1 1 d . . . S2 S 1.24583(4) -0.09893(5) 0.82131(2) 0.02631(11) Uani 1 1 d . . . O1 O 1.52313(12) -0.19909(17) 1.03121(7) 0.0306(3) Uani 1 1 d . . . O2 O 1.20305(12) -0.05431(15) 1.09608(6) 0.0234(3) Uani 1 1 d . . . O3 O 1.29207(14) -0.65219(17) 0.99742(9) 0.0385(3) Uani 1 1 d . . . H3O H 1.2238 -0.6868 1.0051 0.058 Uiso 1 1 calc . . . N1 N 1.27620(14) -0.07966(17) 0.99122(8) 0.0207(3) Uani 1 1 d . . . H1N H 1.337(2) -0.107(2) 0.9753(11) 0.019(5) Uiso 1 1 d . . . N2 N 1.15134(14) -0.01603(15) 0.93486(8) 0.0193(3) Uani 1 1 d . . . C1 C 1.53381(16) -0.2171(2) 1.11153(9) 0.0221(3) Uani 1 1 d . . . C2 C 1.64878(18) -0.2895(2) 1.17257(10) 0.0267(4) Uani 1 1 d . . . H2 H 1.7209 -0.3263 1.1580 0.032 Uiso 1 1 calc . . . C3 C 1.65831(18) -0.3079(2) 1.25379(11) 0.0293(4) Uani 1 1 d . . . H3 H 1.7359 -0.3589 1.2945 0.035 Uiso 1 1 calc . . . C4 C 1.55510(19) -0.2524(2) 1.27631(10) 0.0287(4) Uani 1 1 d . . . H4 H 1.5625 -0.2640 1.3325 0.034 Uiso 1 1 calc . . . C5 C 1.44136(17) -0.1800(2) 1.21645(9) 0.0235(3) Uani 1 1 d . . . H5 H 1.3715 -0.1410 1.2323 0.028 Uiso 1 1 calc . . . C6 C 1.42717(15) -0.16306(18) 1.13295(9) 0.0195(3) Uani 1 1 d . . . C7 C 1.29548(16) -0.09395(19) 1.07252(9) 0.0191(3) Uani 1 1 d . . . C8 C 1.12835(16) -0.01536(17) 0.85534(9) 0.0180(3) Uani 1 1 d . . . C9 C 0.9754(2) 0.0870(2) 0.68857(10) 0.0301(4) Uani 1 1 d . . . H9A H 0.8797 0.1102 0.6450 0.036 Uiso 1 1 calc . . . H9B H 1.0372 0.1699 0.6938 0.036 Uiso 1 1 calc . . . C10 C 1.0315(2) -0.0390(2) 0.65871(10) 0.0284(4) Uani 1 1 d . . . H10A H 1.0108 -0.0267 0.5979 0.034 Uiso 1 1 calc . . . H10B H 0.9826 -0.1261 0.6643 0.034 Uiso 1 1 calc . . . C11 C 1.1891(2) -0.0567(2) 0.70908(11) 0.0307(4) Uani 1 1 d . . . H11A H 1.2363 0.0324 0.7047 0.037 Uiso 1 1 calc . . . H11B H 1.2222 -0.1333 0.6826 0.037 Uiso 1 1 calc . . . C12 C 1.3210(2) -0.5125(3) 1.03217(14) 0.0422(5) Uani 1 1 d . . . H12A H 1.3804 -0.5182 1.0933 0.063 Uiso 1 1 calc . . . H12B H 1.2319 -0.4647 1.0225 0.063 Uiso 1 1 calc . . . H12C H 1.3708 -0.4585 1.0046 0.063 Uiso 1 1 calc . . . H1 H 1.5931 -0.2402 1.0184 0.050 Uiso 1 1 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 Fe 0.01481(16) 0.02182(19) 0.01254(15) -0.00089(11) 0.00409(12) 0.00100(12) Cl 0.0350(2) 0.0235(2) 0.0289(2) -0.00434(15) 0.01778(18) -0.00362(17) S1 0.0231(2) 0.0384(3) 0.01482(18) 0.00432(16) 0.00709(15) 0.00777(17) S2 0.0250(2) 0.0369(3) 0.01897(19) 0.00116(16) 0.01107(16) 0.00674(18) O1 0.0248(6) 0.0490(9) 0.0202(5) 0.0071(5) 0.0116(5) 0.0126(6) O2 0.0175(5) 0.0368(7) 0.0143(5) -0.0005(5) 0.0052(4) 0.0045(5) O3 0.0310(7) 0.0439(9) 0.0492(8) -0.0122(7) 0.0251(6) -0.0029(6) N1 0.0162(6) 0.0315(9) 0.0147(6) 0.0043(5) 0.0066(5) 0.0051(6) N2 0.0166(6) 0.0255(8) 0.0137(6) 0.0026(5) 0.0043(5) 0.0024(5) C1 0.0190(7) 0.0272(9) 0.0179(7) 0.0015(6) 0.0056(6) 0.0004(7) C2 0.0204(8) 0.0294(10) 0.0267(8) 0.0017(7) 0.0061(6) 0.0051(7) C3 0.0245(8) 0.0305(10) 0.0232(7) 0.0040(7) 0.0002(6) 0.0027(7) C4 0.0292(9) 0.0347(11) 0.0159(7) 0.0056(6) 0.0032(6) 0.0001(7) C5 0.0225(7) 0.0289(10) 0.0172(7) 0.0004(6) 0.0063(6) -0.0015(7) C6 0.0163(7) 0.0233(8) 0.0154(6) 0.0009(6) 0.0032(5) -0.0007(6) C7 0.0171(7) 0.0239(8) 0.0138(6) 0.0000(5) 0.0041(5) -0.0010(6) C8 0.0184(7) 0.0202(8) 0.0149(7) 0.0013(5) 0.0064(5) -0.0010(6) C9 0.0426(10) 0.0325(10) 0.0164(7) 0.0060(6) 0.0134(7) 0.0108(8) C10 0.0399(10) 0.0294(10) 0.0152(7) -0.0003(6) 0.0108(7) 0.0024(8) C11 0.0375(10) 0.0387(11) 0.0220(8) 0.0041(7) 0.0185(7) 0.0061(8) C12 0.0428(12) 0.0443(14) 0.0405(11) -0.0056(9) 0.0182(10) -0.0066(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2 2.1340(11) 3_757 ? Fe O2 2.1340(11) . ? Fe N2 2.2924(13) 3_757 ? Fe N2 2.2924(13) . ? Fe Cl 2.3995(5) 3_757 ? Fe Cl 2.3995(5) . ? S1 C8 1.7484(16) . ? S1 C9 1.8156(16) . ? S2 C8 1.7487(17) . ? S2 C11 1.8252(17) . ? O1 C1 1.3601(19) . ? O1 H1 0.9288 . ? O2 C7 1.2474(19) . ? O3 C12 1.424(3) . ? O3 H3O 0.8400 . ? N1 C7 1.345(2) . ? N1 N2 1.3922(18) . ? N1 H1N 0.829(19) . ? N2 C8 1.2967(19) . ? C1 C2 1.398(2) . ? C1 C6 1.403(2) . ? C2 C3 1.380(2) . ? C2 H2 0.9500 . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(2) . ? C4 H4 0.9500 . ? C5 C6 1.401(2) . ? C5 H5 0.9500 . ? C6 C7 1.482(2) . ? C9 C10 1.505(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.509(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 O2 Fe O2 180.000(1) 3_757 . ? O2 Fe N2 73.15(4) 3_757 3_757 ? O2 Fe N2 106.85(4) . 3_757 ? O2 Fe N2 106.85(4) 3_757 . ? O2 Fe N2 73.15(4) . . ? N2 Fe N2 180.0 3_757 . ? O2 Fe Cl 91.46(4) 3_757 3_757 ? O2 Fe Cl 88.54(4) . 3_757 ? N2 Fe Cl 94.26(4) 3_757 3_757 ? N2 Fe Cl 85.74(4) . 3_757 ? O2 Fe Cl 88.54(4) 3_757 . ? O2 Fe Cl 91.46(4) . . ? N2 Fe Cl 85.74(4) 3_757 . ? N2 Fe Cl 94.26(4) . . ? Cl Fe Cl 180.0 3_757 . ? C8 S1 C9 104.77(8) . . ? C8 S2 C11 107.53(8) . . ? C1 O1 H1 117.1 . . ? C7 O2 Fe 117.52(9) . . ? C12 O3 H3O 109.5 . . ? C7 N1 N2 117.76(13) . . ? C7 N1 H1N 121.2(13) . . ? N2 N1 H1N 121.0(13) . . ? C8 N2 N1 116.88(13) . . ? C8 N2 Fe 131.55(11) . . ? N1 N2 Fe 108.24(9) . . ? O1 C1 C2 120.91(15) . . ? O1 C1 C6 119.34(14) . . ? C2 C1 C6 119.76(14) . . ? C3 C2 C1 120.50(16) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.32(16) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.56(15) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.28(16) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.55(14) . . ? C5 C6 C7 116.60(14) . . ? C1 C6 C7 124.79(13) . . ? O2 C7 N1 120.99(14) . . ? O2 C7 C6 120.67(13) . . ? N1 C7 C6 118.30(14) . . ? N2 C8 S1 113.17(12) . . ? N2 C8 S2 120.76(12) . . ? S1 C8 S2 125.77(9) . . ? C10 C9 S1 113.95(12) . . ? C10 C9 H9A 108.8 . . ? S1 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? S1 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 111.76(16) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 S2 115.48(12) . . ? C10 C11 H11A 108.4 . . ? S2 C11 H11A 108.4 . . ? C10 C11 H11B 108.4 . . ? S2 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? O3 C12 H12A 109.5 . . ? O3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe O2 C7 71(100) 3_757 . . . ? N2 Fe O2 C7 167.15(13) 3_757 . . . ? N2 Fe O2 C7 -12.85(13) . . . . ? Cl Fe O2 C7 73.14(13) 3_757 . . . ? Cl Fe O2 C7 -106.86(13) . . . . ? C7 N1 N2 C8 -173.60(15) . . . . ? C7 N1 N2 Fe -11.81(18) . . . . ? O2 Fe N2 C8 -9.62(17) 3_757 . . . ? O2 Fe N2 C8 170.38(17) . . . . ? N2 Fe N2 C8 2(100) 3_757 . . . ? Cl Fe N2 C8 80.62(16) 3_757 . . . ? Cl Fe N2 C8 -99.38(16) . . . . ? O2 Fe N2 N1 -167.75(10) 3_757 . . . ? O2 Fe N2 N1 12.25(10) . . . . ? N2 Fe N2 N1 -156(100) 3_757 . . . ? Cl Fe N2 N1 -77.52(10) 3_757 . . . ? Cl Fe N2 N1 102.48(10) . . . . ? O1 C1 C2 C3 -179.63(17) . . . . ? C6 C1 C2 C3 -0.2(3) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C3 C4 C5 C6 0.8(3) . . . . ? C4 C5 C6 C1 -2.2(3) . . . . ? C4 C5 C6 C7 175.21(16) . . . . ? O1 C1 C6 C5 -178.71(17) . . . . ? C2 C1 C6 C5 1.8(3) . . . . ? O1 C1 C6 C7 4.2(3) . . . . ? C2 C1 C6 C7 -175.31(17) . . . . ? Fe O2 C7 N1 11.2(2) . . . . ? Fe O2 C7 C6 -166.47(12) . . . . ? N2 N1 C7 O2 1.6(2) . . . . ? N2 N1 C7 C6 179.28(14) . . . . ? C5 C6 C7 O2 -0.3(3) . . . . ? C1 C6 C7 O2 176.86(17) . . . . ? C5 C6 C7 N1 -178.06(16) . . . . ? C1 C6 C7 N1 -0.9(3) . . . . ? N1 N2 C8 S1 177.14(11) . . . . ? Fe N2 C8 S1 20.5(2) . . . . ? N1 N2 C8 S2 3.1(2) . . . . ? Fe N2 C8 S2 -153.56(9) . . . . ? C9 S1 C8 N2 166.88(13) . . . . ? C9 S1 C8 S2 -19.40(14) . . . . ? C11 S2 C8 N2 -173.33(14) . . . . ? C11 S2 C8 S1 13.40(14) . . . . ? C8 S1 C9 C10 46.75(17) . . . . ? S1 C9 C10 C11 -73.75(19) . . . . ? C9 C10 C11 S2 64.9(2) . . . . ? C8 S2 C11 C10 -32.51(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.573 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.111 # Attachment 'complex_5.cif' data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 844923' #TrackingRef 'complex_5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H50 Fe2 N8 O10 S8, 1/2(C H3 O)' _chemical_formula_sum 'C46.50 H51.50 Fe2 N8 O10.50 S8' _chemical_formula_weight 1258.64 _chemical_absolute_configuration ? 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' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall ? 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' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 23.038(2) _cell_length_b 10.461(6) _cell_length_c 22.989(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5540(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20723 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2602 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25825 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7431 _reflns_number_gt 5424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ; # start Validation Reply Form _vrf_PLAT413_I ; PROBLEM: Short Inter XH3 .. XHn H11B .. H24B .. 1.88 Ang. RESPONSE: due to the disorder occurring within this solvent molecule ; # end Validation Reply Form _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^)+(0.0736P)^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 -0.013(18) _refine_ls_number_reflns 7431 _refine_ls_number_parameters 350 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.34927(2) 0.02607(14) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.48384(3) 0.02771(14) Uani 1 2 d S . . S1 S 0.56389(5) 0.31279(8) 0.45393(5) 0.0479(2) Uani 1 1 d . . . S2 S 0.60432(4) -0.15587(9) 0.24551(5) 0.0425(2) Uani 1 1 d . . . S3 S 0.67584(5) 0.23567(11) 0.51246(5) 0.0534(3) Uani 1 1 d . . . S4 S 0.50747(4) -0.32487(11) 0.20122(5) 0.0506(3) Uani 1 1 d . . . O1 O 0.36337(12) -0.3758(3) 0.25548(14) 0.0592(8) Uani 1 1 d . . . H1 H 0.3956 -0.3383 0.2537 0.089 Uiso 1 1 calc . . . O2 O 0.41717(10) -0.0465(2) 0.34486(11) 0.0336(5) Uani 1 1 d . . . O3 O 0.28420(14) 0.0778(4) 0.57808(17) 0.0753(10) Uani 1 1 d . . . H3A H 0.3051 0.0286 0.5582 0.113 Uiso 1 1 calc . . . O4 O 0.46246(10) 0.1171(2) 0.53988(11) 0.0352(5) Uani 1 1 d . . . O5 O 0.47771(9) 0.10819(18) 0.41603(11) 0.0301(4) Uani 1 1 d . . . O6 O 0.5000 0.5000 0.3428(5) 0.210(16) Uani 0.50 2 d SP . . N1 N 0.44086(12) -0.2079(2) 0.28215(13) 0.0323(6) Uani 1 1 d . . . N2 N 0.49667(11) -0.1549(2) 0.28484(12) 0.0284(6) Uani 1 1 d . . . N4 N 0.58354(11) 0.0853(2) 0.49990(12) 0.0306(6) Uani 1 1 d . . . N3 N 0.37926(13) -0.0013(2) 0.52904(13) 0.0354(6) Uani 1 1 d . . . C1 C 0.32690(16) -0.3085(3) 0.28974(17) 0.0403(8) Uani 1 1 d . . . C2 C 0.27077(17) -0.3562(4) 0.2977(2) 0.0500(9) Uani 1 1 d . . . H2 H 0.2594 -0.4335 0.2792 0.060 Uiso 1 1 calc . . . C3 C 0.23218(17) -0.2920(4) 0.3322(2) 0.0516(10) Uani 1 1 d . . . H3 H 0.1939 -0.3244 0.3368 0.062 Uiso 1 1 calc . . . C4 C 0.24805(17) -0.1803(4) 0.3605(2) 0.0521(10) Uani 1 1 d . . . H4 H 0.2208 -0.1358 0.3840 0.063 Uiso 1 1 calc . . . C5 C 0.30392(15) -0.1344(3) 0.35398(19) 0.0426(8) Uani 1 1 d . . . H5 H 0.3151 -0.0587 0.3738 0.051 Uiso 1 1 calc . . . C6 C 0.34403(15) -0.1966(3) 0.31916(15) 0.0342(7) Uani 1 1 d . . . C7 C 0.40400(14) -0.1466(3) 0.31571(13) 0.0277(6) Uani 1 1 d . . . C8 C 0.53250(13) -0.2053(3) 0.24784(14) 0.0291(6) Uani 1 1 d . . . C9 C 0.5641(2) -0.3278(6) 0.1466(2) 0.0698(14) Uani 1 1 d . . . H9A H 0.5529 -0.3890 0.1158 0.084 Uiso 1 1 calc . . . H9B H 0.5667 -0.2420 0.1286 0.084 Uiso 1 1 calc . . . C10 C 0.62268(19) -0.3640(4) 0.1692(2) 0.0553(10) Uani 1 1 d . . . H10A H 0.6249 -0.4584 0.1713 0.066 Uiso 1 1 calc . . . H10B H 0.6523 -0.3353 0.1408 0.066 Uiso 1 1 calc . . . C11 C 0.6380(2) -0.3109(5) 0.2274(2) 0.0623(12) Uani 1 1 d . . . H11A H 0.6807 -0.3011 0.2294 0.075 Uiso 1 1 calc . . . H11B H 0.6266 -0.3739 0.2574 0.075 Uiso 1 1 calc . . . C12 C 0.3162(2) 0.1790(5) 0.59624(19) 0.0580(11) Uani 1 1 d . . . C13 C 0.2875(3) 0.2701(6) 0.6302(3) 0.0839(17) Uani 1 1 d . . . H13 H 0.2475 0.2601 0.6391 0.101 Uiso 1 1 calc . . . C14 C 0.3176(3) 0.3741(7) 0.6504(3) 0.090(2) Uani 1 1 d . . . H14 H 0.2982 0.4354 0.6738 0.108 Uiso 1 1 calc . . . C15 C 0.3750(3) 0.3914(4) 0.6374(2) 0.0738(16) Uani 1 1 d . . . H15 H 0.3949 0.4648 0.6514 0.089 Uiso 1 1 calc . . . C16 C 0.4043(2) 0.3014(4) 0.60392(18) 0.0566(11) Uani 1 1 d . . . H16 H 0.4443 0.3130 0.5954 0.068 Uiso 1 1 calc . . . C17 C 0.37488(18) 0.1935(4) 0.58273(15) 0.0413(8) Uani 1 1 d . . . C18 C 0.40724(16) 0.0987(3) 0.54820(15) 0.0349(7) Uani 1 1 d . . . C19 C 0.60584(16) 0.1975(3) 0.48944(15) 0.0372(7) Uani 1 1 d . . . C20 C 0.68892(18) 0.3781(4) 0.46948(19) 0.0553(10) Uani 1 1 d . . . H20A H 0.7300 0.4037 0.4744 0.066 Uiso 1 1 calc . . . H20B H 0.6831 0.3569 0.4279 0.066 Uiso 1 1 calc . . . C21 C 0.6504(2) 0.4919(4) 0.4847(2) 0.0652(13) Uani 1 1 d . . . H21A H 0.6657 0.5341 0.5201 0.078 Uiso 1 1 calc . . . H21B H 0.6517 0.5548 0.4526 0.078 Uiso 1 1 calc . . . C22 C 0.5875(2) 0.4518(4) 0.4953(2) 0.0565(11) Uani 1 1 d . . . H22A H 0.5619 0.5247 0.4856 0.068 Uiso 1 1 calc . . . H22B H 0.5826 0.4334 0.5373 0.068 Uiso 1 1 calc . . . C23 C 0.43078(15) 0.1961(3) 0.41427(17) 0.0386(7) Uani 1 1 d . . . H23A H 0.4274 0.2391 0.4520 0.058 Uiso 1 1 calc . . . H23B H 0.3947 0.1500 0.4058 0.058 Uiso 1 1 calc . . . H23C H 0.4379 0.2597 0.3838 0.058 Uiso 1 1 calc . . . C24 C 0.4227(10) 0.4721(13) 0.3472(8) 0.058(5) Uani 0.25 1 d P . . H24A H 0.4155 0.3819 0.3562 0.086 Uiso 0.25 1 calc P . . H24B H 0.4046 0.4935 0.3098 0.086 Uiso 0.25 1 calc P . . H24C H 0.4060 0.5258 0.3779 0.086 Uiso 0.25 1 calc 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 Fe1 0.0301(3) 0.0235(3) 0.0246(3) 0.000 0.000 -0.0025(2) Fe2 0.0332(3) 0.0257(3) 0.0242(3) 0.000 0.000 0.0010(2) S1 0.0620(6) 0.0334(4) 0.0484(5) 0.0052(4) -0.0091(5) -0.0096(4) S2 0.0332(4) 0.0487(5) 0.0456(5) -0.0056(4) 0.0063(4) -0.0058(4) S3 0.0485(6) 0.0663(7) 0.0455(5) 0.0063(5) -0.0051(5) -0.0210(5) S4 0.0417(5) 0.0599(6) 0.0502(6) -0.0288(5) 0.0087(5) -0.0079(4) O1 0.0482(16) 0.0570(16) 0.072(2) -0.0307(15) 0.0108(16) -0.0182(13) O2 0.0357(12) 0.0268(10) 0.0384(13) -0.0050(10) 0.0049(11) -0.0020(9) O3 0.0422(17) 0.094(2) 0.090(3) -0.008(2) 0.0066(18) 0.0165(17) O4 0.0374(12) 0.0359(12) 0.0322(12) -0.0066(10) 0.0018(11) 0.0011(10) O5 0.0400(11) 0.0229(9) 0.0275(10) -0.0023(9) -0.0004(11) 0.0046(8) O6 0.54(5) 0.063(7) 0.031(6) 0.000 0.000 0.103(15) N1 0.0301(13) 0.0306(13) 0.0363(15) -0.0044(11) 0.0015(12) -0.0027(11) N2 0.0288(13) 0.0263(12) 0.0300(14) 0.0005(11) 0.0015(11) -0.0034(10) N4 0.0341(13) 0.0291(13) 0.0286(14) -0.0002(10) -0.0002(11) -0.0014(11) N3 0.0345(15) 0.0395(15) 0.0321(15) 0.0025(11) 0.0006(12) 0.0049(11) C1 0.040(2) 0.0389(18) 0.0423(19) -0.0047(15) -0.0046(16) -0.0081(14) C2 0.041(2) 0.051(2) 0.058(2) 0.0019(19) -0.0105(19) -0.0141(17) C3 0.0308(18) 0.063(2) 0.061(3) 0.010(2) -0.0054(18) -0.0138(17) C4 0.0330(18) 0.055(2) 0.068(3) 0.005(2) 0.005(2) -0.0018(17) C5 0.0316(17) 0.0409(18) 0.055(2) 0.0007(16) -0.0008(17) 0.0017(14) C6 0.0357(18) 0.0333(16) 0.0335(16) 0.0053(13) -0.0021(15) -0.0006(13) C7 0.0308(16) 0.0264(14) 0.0258(15) 0.0044(12) 0.0002(13) -0.0020(12) C8 0.0311(15) 0.0311(15) 0.0250(14) -0.0001(12) -0.0020(13) 0.0003(12) C9 0.057(3) 0.106(4) 0.046(3) -0.031(3) 0.006(2) -0.003(3) C10 0.052(2) 0.061(2) 0.052(3) -0.009(2) 0.015(2) 0.008(2) C11 0.047(2) 0.087(3) 0.053(3) -0.011(2) -0.003(2) 0.012(2) C12 0.056(3) 0.074(3) 0.044(2) -0.001(2) 0.002(2) 0.030(2) C13 0.074(4) 0.112(4) 0.065(3) -0.006(3) 0.012(3) 0.056(3) C14 0.110(5) 0.106(5) 0.055(3) -0.017(3) 0.005(3) 0.066(4) C15 0.123(5) 0.055(3) 0.044(2) -0.009(2) -0.005(3) 0.035(3) C16 0.084(3) 0.050(2) 0.036(2) -0.0040(17) 0.001(2) 0.017(2) C17 0.053(2) 0.0445(19) 0.0267(17) 0.0001(15) -0.0035(16) 0.0153(17) C18 0.0415(19) 0.0382(17) 0.0251(15) -0.0009(13) -0.0005(14) 0.0067(15) C19 0.0457(18) 0.0377(17) 0.0282(16) -0.0024(14) 0.0017(15) -0.0062(14) C20 0.055(2) 0.063(2) 0.048(2) 0.0048(19) 0.006(2) -0.022(2) C21 0.080(3) 0.047(2) 0.069(3) -0.012(2) 0.021(3) -0.027(2) C22 0.071(3) 0.0359(19) 0.063(3) -0.0057(19) 0.003(2) -0.0103(19) C23 0.052(2) 0.0304(15) 0.0331(16) -0.0040(15) -0.0015(17) 0.0155(14) C24 0.102(15) 0.017(6) 0.054(10) 0.007(7) -0.015(11) 0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.972(2) . ? Fe1 O2 1.972(2) 2_655 ? Fe1 O5 1.975(2) . ? Fe1 O5 1.975(2) 2_655 ? Fe1 N2 2.196(3) . ? Fe1 N2 2.196(3) 2_655 ? Fe2 O4 1.977(2) . ? Fe2 O4 1.977(2) 2_655 ? Fe2 O5 1.994(2) 2_655 ? Fe2 O5 1.994(2) . ? Fe2 N4 2.154(3) . ? Fe2 N4 2.154(3) 2_655 ? S1 C19 1.748(4) . ? S1 C22 1.822(4) . ? S2 C8 1.734(3) . ? S2 C11 1.846(5) . ? S3 C19 1.744(4) . ? S3 C20 1.813(4) . ? S4 C8 1.745(3) . ? S4 C9 1.810(5) . ? O1 C1 1.350(5) . ? O1 H1 0.8400 . ? O2 C7 1.280(4) . ? O3 C12 1.356(6) . ? O3 H3A 0.8400 . ? O4 C18 1.301(4) . ? O5 C23 1.420(4) . ? O6 C24 1.81(2) 2_665 ? O6 C24 1.81(2) . ? N1 C7 1.314(4) . ? N1 N2 1.402(4) . ? N2 C8 1.297(4) . ? N4 C19 1.303(4) . ? N4 N3 1.398(4) 2_655 ? N3 C18 1.306(4) . ? N3 N4 1.398(4) 2_655 ? C1 C2 1.398(5) . ? C1 C6 1.409(5) . ? C2 C3 1.367(6) . ? C2 H2 0.9500 . ? C3 C4 1.387(6) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.479(4) . ? C9 C10 1.496(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.491(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.395(6) . ? C12 C13 1.398(7) . ? C13 C14 1.371(9) . ? C13 H13 0.9500 . ? C14 C15 1.368(9) . ? C14 H14 0.9500 . ? C15 C16 1.391(6) . ? C15 H15 0.9500 . ? C16 C17 1.403(6) . ? C16 H16 0.9500 . ? C17 C18 1.473(5) . ? C20 C21 1.526(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.528(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 O2 Fe1 O2 174.12(15) . 2_655 ? O2 Fe1 O5 85.95(9) . . ? O2 Fe1 O5 98.64(10) 2_655 . ? O2 Fe1 O5 98.64(10) . 2_655 ? O2 Fe1 O5 85.95(9) 2_655 2_655 ? O5 Fe1 O5 78.00(13) . 2_655 ? O2 Fe1 N2 75.51(9) . . ? O2 Fe1 N2 100.43(10) 2_655 . ? O5 Fe1 N2 159.66(9) . . ? O5 Fe1 N2 96.34(10) 2_655 . ? O2 Fe1 N2 100.43(10) . 2_655 ? O2 Fe1 N2 75.51(9) 2_655 2_655 ? O5 Fe1 N2 96.34(10) . 2_655 ? O5 Fe1 N2 159.66(9) 2_655 2_655 ? N2 Fe1 N2 95.20(15) . 2_655 ? O4 Fe2 O4 98.67(15) . 2_655 ? O4 Fe2 O5 166.90(9) . 2_655 ? O4 Fe2 O5 92.58(10) 2_655 2_655 ? O4 Fe2 O5 92.58(10) . . ? O4 Fe2 O5 166.90(9) 2_655 . ? O5 Fe2 O5 77.13(12) 2_655 . ? O4 Fe2 N4 91.28(10) . . ? O4 Fe2 N4 75.77(10) 2_655 . ? O5 Fe2 N4 98.00(10) 2_655 . ? O5 Fe2 N4 97.41(10) . . ? O4 Fe2 N4 75.77(10) . 2_655 ? O4 Fe2 N4 91.28(10) 2_655 2_655 ? O5 Fe2 N4 97.41(10) 2_655 2_655 ? O5 Fe2 N4 98.00(10) . 2_655 ? N4 Fe2 N4 160.26(15) . 2_655 ? C19 S1 C22 98.15(19) . . ? C8 S2 C11 98.40(19) . . ? C19 S3 C20 100.18(19) . . ? C8 S4 C9 101.53(19) . . ? C1 O1 H1 109.5 . . ? C7 O2 Fe1 117.3(2) . . ? C12 O3 H3A 109.5 . . ? C18 O4 Fe2 115.6(2) . . ? C23 O5 Fe1 123.2(2) . . ? C23 O5 Fe2 125.9(2) . . ? Fe1 O5 Fe2 102.44(9) . . ? C24 O6 C24 173.6(15) 2_665 . ? C7 N1 N2 111.9(3) . . ? C8 N2 N1 113.2(3) . . ? C8 N2 Fe1 136.0(2) . . ? N1 N2 Fe1 110.72(19) . . ? C19 N4 N3 114.4(3) . 2_655 ? C19 N4 Fe2 133.9(2) . . ? N3 N4 Fe2 111.67(19) 2_655 . ? C18 N3 N4 111.3(3) . 2_655 ? O1 C1 C2 117.8(3) . . ? O1 C1 C6 122.6(3) . . ? C2 C1 C6 119.5(4) . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C7 119.2(3) . . ? C1 C6 C7 122.0(3) . . ? O2 C7 N1 123.6(3) . . ? O2 C7 C6 118.8(3) . . ? N1 C7 C6 117.5(3) . . ? N2 C8 S2 120.4(2) . . ? N2 C8 S4 118.9(2) . . ? S2 C8 S4 120.66(19) . . ? C10 C9 S4 114.4(4) . . ? C10 C9 H9A 108.6 . . ? S4 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S4 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 115.5(4) . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? C9 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C10 C11 S2 115.5(3) . . ? C10 C11 H11A 108.4 . . ? S2 C11 H11A 108.4 . . ? C10 C11 H11B 108.4 . . ? S2 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? O3 C12 C17 122.9(4) . . ? O3 C12 C13 116.5(5) . . ? C17 C12 C13 120.5(5) . . ? C14 C13 C12 119.4(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.4(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.2(5) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 118.6(4) . . ? C12 C17 C18 122.4(4) . . ? C16 C17 C18 119.0(4) . . ? O4 C18 N3 123.5(3) . . ? O4 C18 C17 118.3(3) . . ? N3 C18 C17 118.2(3) . . ? N4 C19 S1 119.3(3) . . ? N4 C19 S3 121.0(3) . . ? S1 C19 S3 119.65(19) . . ? C21 C20 S3 114.8(3) . . ? C21 C20 H20A 108.6 . . ? S3 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? S3 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 111.9(3) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 S1 114.8(3) . . ? C21 C22 H22A 108.6 . . ? S1 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? S1 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C24 H24A 109.5 . . ? O6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O2 C7 55.7(2) 2_655 . . . ? O5 Fe1 O2 C7 -162.7(2) . . . . ? O5 Fe1 O2 C7 -85.5(2) 2_655 . . . ? N2 Fe1 O2 C7 8.9(2) . . . . ? N2 Fe1 O2 C7 101.6(2) 2_655 . . . ? O4 Fe2 O4 C18 -101.3(2) 2_655 . . . ? O5 Fe2 O4 C18 47.6(5) 2_655 . . . ? O5 Fe2 O4 C18 85.4(2) . . . . ? N4 Fe2 O4 C18 -177.1(2) . . . . ? N4 Fe2 O4 C18 -12.2(2) 2_655 . . . ? O2 Fe1 O5 C23 -49.7(2) . . . . ? O2 Fe1 O5 C23 126.6(2) 2_655 . . . ? O5 Fe1 O5 C23 -149.4(3) 2_655 . . . ? N2 Fe1 O5 C23 -73.8(4) . . . . ? N2 Fe1 O5 C23 50.4(2) 2_655 . . . ? O2 Fe1 O5 Fe2 99.74(10) . . . . ? O2 Fe1 O5 Fe2 -83.96(10) 2_655 . . . ? O5 Fe1 O5 Fe2 0.0 2_655 . . . ? N2 Fe1 O5 Fe2 75.6(3) . . . . ? N2 Fe1 O5 Fe2 -160.20(10) 2_655 . . . ? O4 Fe2 O5 C23 -23.5(2) . . . . ? O4 Fe2 O5 C23 -172.8(4) 2_655 . . . ? O5 Fe2 O5 C23 148.3(3) 2_655 . . . ? N4 Fe2 O5 C23 -115.1(2) . . . . ? N4 Fe2 O5 C23 52.5(2) 2_655 . . . ? O4 Fe2 O5 Fe1 -171.81(10) . . . . ? O4 Fe2 O5 Fe1 38.9(5) 2_655 . . . ? O5 Fe2 O5 Fe1 0.0 2_655 . . . ? N4 Fe2 O5 Fe1 96.56(11) . . . . ? N4 Fe2 O5 Fe1 -95.82(11) 2_655 . . . ? C7 N1 N2 C8 -173.5(3) . . . . ? C7 N1 N2 Fe1 4.2(3) . . . . ? O2 Fe1 N2 C8 170.0(3) . . . . ? O2 Fe1 N2 C8 -5.6(3) 2_655 . . . ? O5 Fe1 N2 C8 -165.0(3) . . . . ? O5 Fe1 N2 C8 -92.6(3) 2_655 . . . ? N2 Fe1 N2 C8 70.6(3) 2_655 . . . ? O2 Fe1 N2 N1 -6.89(19) . . . . ? O2 Fe1 N2 N1 177.5(2) 2_655 . . . ? O5 Fe1 N2 N1 18.0(4) . . . . ? O5 Fe1 N2 N1 90.4(2) 2_655 . . . ? N2 Fe1 N2 N1 -106.3(2) 2_655 . . . ? O4 Fe2 N4 C19 -67.1(3) . . . . ? O4 Fe2 N4 C19 -165.7(3) 2_655 . . . ? O5 Fe2 N4 C19 103.7(3) 2_655 . . . ? O5 Fe2 N4 C19 25.7(3) . . . . ? N4 Fe2 N4 C19 -115.3(3) 2_655 . . . ? O4 Fe2 N4 N3 111.3(2) . . . 2_655 ? O4 Fe2 N4 N3 12.6(2) 2_655 . . 2_655 ? O5 Fe2 N4 N3 -78.0(2) 2_655 . . 2_655 ? O5 Fe2 N4 N3 -156.0(2) . . . 2_655 ? N4 Fe2 N4 N3 62.99(19) 2_655 . . 2_655 ? O1 C1 C2 C3 179.8(4) . . . . ? C6 C1 C2 C3 2.4(6) . . . . ? C1 C2 C3 C4 -1.1(6) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 1.0(6) . . . . ? C4 C5 C6 C1 0.3(6) . . . . ? C4 C5 C6 C7 -177.4(3) . . . . ? O1 C1 C6 C5 -179.2(4) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? O1 C1 C6 C7 -1.6(5) . . . . ? C2 C1 C6 C7 175.6(3) . . . . ? Fe1 O2 C7 N1 -10.3(4) . . . . ? Fe1 O2 C7 C6 170.2(2) . . . . ? N2 N1 C7 O2 3.4(4) . . . . ? N2 N1 C7 C6 -177.1(3) . . . . ? C5 C6 C7 O2 -0.4(5) . . . . ? C1 C6 C7 O2 -178.0(3) . . . . ? C5 C6 C7 N1 -179.9(3) . . . . ? C1 C6 C7 N1 2.5(5) . . . . ? N1 N2 C8 S2 -178.3(2) . . . . ? Fe1 N2 C8 S2 4.8(4) . . . . ? N1 N2 C8 S4 0.9(4) . . . . ? Fe1 N2 C8 S4 -176.02(18) . . . . ? C11 S2 C8 N2 145.0(3) . . . . ? C11 S2 C8 S4 -34.2(3) . . . . ? C9 S4 C8 N2 163.7(3) . . . . ? C9 S4 C8 S2 -17.1(3) . . . . ? C8 S4 C9 C10 62.5(4) . . . . ? S4 C9 C10 C11 -39.2(6) . . . . ? C9 C10 C11 S2 -29.4(6) . . . . ? C8 S2 C11 C10 65.4(4) . . . . ? O3 C12 C13 C14 179.4(5) . . . . ? C17 C12 C13 C14 -0.3(8) . . . . ? C12 C13 C14 C15 0.8(9) . . . . ? C13 C14 C15 C16 -1.0(8) . . . . ? C14 C15 C16 C17 0.7(7) . . . . ? O3 C12 C17 C16 -179.6(4) . . . . ? C13 C12 C17 C16 0.0(6) . . . . ? O3 C12 C17 C18 -1.0(6) . . . . ? C13 C12 C17 C18 178.7(4) . . . . ? C15 C16 C17 C12 -0.3(6) . . . . ? C15 C16 C17 C18 -178.9(4) . . . . ? Fe2 O4 C18 N3 10.8(4) . . . . ? Fe2 O4 C18 C17 -171.3(2) . . . . ? N4 N3 C18 O4 1.1(5) 2_655 . . . ? N4 N3 C18 C17 -176.8(3) 2_655 . . . ? C12 C17 C18 O4 -176.9(4) . . . . ? C16 C17 C18 O4 1.7(5) . . . . ? C12 C17 C18 N3 1.1(5) . . . . ? C16 C17 C18 N3 179.7(3) . . . . ? N3 N4 C19 S1 -179.3(2) 2_655 . . . ? Fe2 N4 C19 S1 -1.0(5) . . . . ? N3 N4 C19 S3 -1.5(4) 2_655 . . . ? Fe2 N4 C19 S3 176.81(17) . . . . ? C22 S1 C19 N4 141.0(3) . . . . ? C22 S1 C19 S3 -36.9(3) . . . . ? C20 S3 C19 N4 165.0(3) . . . . ? C20 S3 C19 S1 -17.2(3) . . . . ? C19 S3 C20 C21 66.0(4) . . . . ? S3 C20 C21 C22 -41.9(5) . . . . ? C20 C21 C22 S1 -30.4(5) . . . . ? C19 S1 C22 C21 69.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.588 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.072 # Attachment 'complex_6.cif' data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 844924' #TrackingRef 'complex_6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Fe2 N8 O9 S8, 3 (C H2 Cl2)' _chemical_formula_sum 'C47 H50 Cl6 Fe2 N8 O9 S8' _chemical_formula_weight 1451.83 _chemical_absolute_configuration ? 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' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8070(2) _cell_length_b 32.3360(8) _cell_length_c 15.2010(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.1750(11) _cell_angle_gamma 90.00 _cell_volume 6075.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35095 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37050 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13388 _reflns_number_gt 8532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1152P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13388 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.74586(4) 0.139546(19) 0.20908(4) 0.02866(16) Uani 1 1 d . . . Fe2 Fe 0.74994(5) 0.088744(19) 0.41138(4) 0.02884(16) Uani 1 1 d . . . Cl1 Cl 0.32223(12) 0.06618(7) 0.15521(11) 0.0871(6) Uani 1 1 d . . . Cl2 Cl 0.44851(13) -0.00376(7) 0.12123(14) 0.0965(6) Uani 1 1 d . . . Cl3 Cl 0.72624(14) 0.10173(6) -0.09015(12) 0.0856(5) Uani 1 1 d . . . Cl4 Cl 0.87442(18) 0.05108(6) -0.15912(11) 0.0919(6) Uani 1 1 d . . . Cl5 Cl 1.06413(12) 0.29532(7) -0.10497(11) 0.0932(7) Uani 1 1 d . . . Cl6 Cl 1.14268(9) 0.34721(4) 0.05292(8) 0.0497(3) Uani 1 1 d . . . S1 S 0.92584(9) 0.03204(4) 0.09251(7) 0.0384(3) Uani 1 1 d . . . S2 S 0.70480(9) 0.03564(4) 0.13076(9) 0.0473(3) Uani 1 1 d . . . S3 S 0.55457(9) 0.26007(4) 0.25514(8) 0.0398(3) Uani 1 1 d . . . S4 S 0.75889(9) 0.21644(4) 0.37317(7) 0.0415(3) Uani 1 1 d . . . S5 S 1.00831(12) 0.07839(5) 0.38457(14) 0.0778(5) Uani 1 1 d . . . S6 S 0.99020(9) -0.01587(4) 0.36923(9) 0.0450(3) Uani 1 1 d . . . S7 S 0.50677(8) 0.18466(4) 0.48562(7) 0.0365(3) Uani 1 1 d . . . S8 S 0.47182(9) 0.11633(4) 0.34491(8) 0.0420(3) Uani 1 1 d . . . O1 O 1.1012(3) 0.12300(12) 0.0761(2) 0.0507(9) Uani 1 1 d . . . H1O H 1.0444 0.1117 0.0821 0.076 Uiso 1 1 calc . . . O2 O 0.8616(2) 0.17440(9) 0.18916(19) 0.0372(7) Uani 1 1 d . . . O3 O 0.4044(2) 0.22955(11) 0.0193(2) 0.0433(8) Uani 1 1 d . . . H3O H 0.4495 0.2267 0.0701 0.065 Uiso 1 1 calc . . . O4 O 0.6179(2) 0.13014(10) 0.10894(19) 0.0366(7) Uani 1 1 d . . . O5 O 0.7341(2) -0.07823(10) 0.3472(2) 0.0435(8) Uani 1 1 d . . . H5O H 0.7772 -0.0586 0.3662 0.065 Uiso 1 1 calc . . . O6 O 0.6474(2) 0.04294(9) 0.40254(19) 0.0354(7) Uani 1 1 d . . . O7 O 0.7646(2) 0.20629(11) 0.6702(2) 0.0462(8) Uani 1 1 d . . . H7O H 0.7173 0.1909 0.6374 0.069 Uiso 1 1 calc . . . O8 O 0.8462(2) 0.10342(9) 0.52972(17) 0.0320(6) Uani 1 1 d . . . O9 O 0.7599(3) 0.11771(11) 0.3167(2) 0.0487(9) Uani 1 1 d . . . N1 N 0.9308(3) 0.11639(12) 0.1364(2) 0.0333(8) Uani 1 1 d . . . N2 N 0.8384(3) 0.09779(12) 0.1509(2) 0.0310(8) Uani 1 1 d . . . N3 N 0.5575(2) 0.19425(11) 0.1391(2) 0.0293(7) Uani 1 1 d . . . N4 N 0.6478(2) 0.19199(11) 0.2166(2) 0.0290(7) Uani 1 1 d . . . N5 N 0.7813(3) -0.00065(11) 0.3834(2) 0.0284(7) Uani 1 1 d . . . N6 N 0.8415(2) 0.03617(11) 0.3927(2) 0.0275(7) Uani 1 1 d . . . N7 N 0.7144(2) 0.14905(11) 0.5470(2) 0.0282(7) Uani 1 1 d . . . N8 N 0.6544(2) 0.12933(11) 0.4676(2) 0.0283(7) Uani 1 1 d . . . C1 C 1.1032(3) 0.16299(17) 0.1025(3) 0.0405(11) Uani 1 1 d . . . C2 C 1.1864(4) 0.1879(2) 0.0891(3) 0.0511(14) Uani 1 1 d . . . H2 H 1.2384 0.1767 0.0612 0.061 Uiso 1 1 calc . . . C3 C 1.1937(4) 0.22865(19) 0.1162(3) 0.0534(14) Uani 1 1 d . . . H3 H 1.2509 0.2452 0.1066 0.064 Uiso 1 1 calc . . . C4 C 1.1191(4) 0.24608(17) 0.1573(3) 0.0481(12) Uani 1 1 d . . . H4 H 1.1257 0.2741 0.1768 0.058 Uiso 1 1 calc . . . C5 C 1.0348(4) 0.22162(15) 0.1691(3) 0.0387(10) Uani 1 1 d . . . H5 H 0.9822 0.2334 0.1955 0.046 Uiso 1 1 calc . . . C6 C 1.0256(3) 0.18023(15) 0.1430(3) 0.0350(10) Uani 1 1 d . . . C7 C 0.9347(3) 0.15566(14) 0.1572(3) 0.0319(9) Uani 1 1 d . . . C8 C 0.8260(3) 0.05882(14) 0.1288(2) 0.0304(9) Uani 1 1 d . . . C9 C 0.8467(4) -0.01079(17) 0.0326(3) 0.0532(13) Uani 1 1 d . . . H9A H 0.7871 0.0005 -0.0168 0.064 Uiso 1 1 calc . . . H9B H 0.8933 -0.0276 0.0039 0.064 Uiso 1 1 calc . . . C10 C 0.7989(5) -0.03876(17) 0.0918(4) 0.0599(14) Uani 1 1 d . . . H10A H 0.7455 -0.0573 0.0517 0.072 Uiso 1 1 calc . . . H10B H 0.8573 -0.0563 0.1289 0.072 Uiso 1 1 calc . . . C11 C 0.7447(5) -0.01678(18) 0.1541(4) 0.0613(15) Uani 1 1 d . . . H11A H 0.7941 -0.0178 0.2163 0.074 Uiso 1 1 calc . . . H11B H 0.6793 -0.0328 0.1556 0.074 Uiso 1 1 calc . . . C12 C 0.4009(3) 0.19438(16) -0.0303(3) 0.0383(11) Uani 1 1 d . . . C13 C 0.3297(4) 0.19289(19) -0.1169(3) 0.0513(14) Uani 1 1 d . . . H13 H 0.2847 0.2160 -0.1389 0.062 Uiso 1 1 calc . . . C14 C 0.3237(4) 0.1585(2) -0.1709(3) 0.0576(16) Uani 1 1 d . . . H14 H 0.2755 0.1583 -0.2302 0.069 Uiso 1 1 calc . . . C15 C 0.3872(4) 0.12397(19) -0.1400(3) 0.0518(14) Uani 1 1 d . . . H15 H 0.3821 0.1001 -0.1774 0.062 Uiso 1 1 calc . . . C16 C 0.4579(3) 0.12482(16) -0.0539(3) 0.0406(11) Uani 1 1 d . . . H16 H 0.5008 0.1012 -0.0320 0.049 Uiso 1 1 calc . . . C17 C 0.4673(3) 0.16014(15) 0.0020(3) 0.0348(10) Uani 1 1 d . . . C18 C 0.5508(3) 0.16104(13) 0.0882(3) 0.0292(9) Uani 1 1 d . . . C19 C 0.6544(3) 0.22227(13) 0.2742(3) 0.0295(9) Uani 1 1 d . . . C20 C 0.6112(4) 0.30021(16) 0.3354(3) 0.0476(12) Uani 1 1 d . . . H20A H 0.6673 0.3150 0.3135 0.057 Uiso 1 1 calc . . . H20B H 0.5535 0.3204 0.3369 0.057 Uiso 1 1 calc . . . C21 C 0.6615(4) 0.28509(17) 0.4321(3) 0.0484(12) Uani 1 1 d . . . H21A H 0.6752 0.3091 0.4741 0.058 Uiso 1 1 calc . . . H21B H 0.6099 0.2665 0.4510 0.058 Uiso 1 1 calc . . . C22 C 0.7640(4) 0.26284(18) 0.4396(3) 0.0544(14) Uani 1 1 d . . . H22A H 0.7948 0.2556 0.5045 0.065 Uiso 1 1 calc . . . H22B H 0.8151 0.2822 0.4223 0.065 Uiso 1 1 calc . . . C23 C 0.6359(3) -0.06890(14) 0.3599(2) 0.0337(10) Uani 1 1 d . . . C24 C 0.5619(4) -0.10096(15) 0.3520(3) 0.0421(11) Uani 1 1 d . . . H24 H 0.5812 -0.1282 0.3388 0.050 Uiso 1 1 calc . . . C25 C 0.4604(4) -0.09329(17) 0.3634(3) 0.0506(13) Uani 1 1 d . . . H25 H 0.4099 -0.1153 0.3575 0.061 Uiso 1 1 calc . . . C26 C 0.4315(4) -0.05441(19) 0.3831(3) 0.0533(13) Uani 1 1 d . . . H26 H 0.3613 -0.0495 0.3909 0.064 Uiso 1 1 calc . . . C27 C 0.5046(4) -0.02214(16) 0.3919(3) 0.0432(11) Uani 1 1 d . . . H27 H 0.4841 0.0048 0.4060 0.052 Uiso 1 1 calc . . . C28 C 0.6070(3) -0.02846(14) 0.3802(2) 0.0316(9) Uani 1 1 d . . . C29 C 0.6830(3) 0.00671(13) 0.3891(2) 0.0279(8) Uani 1 1 d . . . C30 C 0.9403(3) 0.03239(13) 0.3853(2) 0.0296(9) Uani 1 1 d . . . C31 C 1.1395(5) 0.0679(2) 0.3836(6) 0.103(3) Uani 1 1 d . . . H31A H 1.1662 0.0919 0.3553 0.123 Uiso 1 1 calc . . . H31B H 1.1830 0.0667 0.4479 0.123 Uiso 1 1 calc . . . C32 C 1.1644(4) 0.0301(2) 0.3375(4) 0.0608(15) Uani 1 1 d . . . H32A H 1.1271 0.0318 0.2717 0.073 Uiso 1 1 calc . . . H32B H 1.2432 0.0290 0.3435 0.073 Uiso 1 1 calc . . . C33 C 1.1309(4) -0.00836(18) 0.3754(3) 0.0504(13) Uani 1 1 d . . . H33A H 1.1714 -0.0100 0.4404 0.061 Uiso 1 1 calc . . . H33B H 1.1547 -0.0320 0.3440 0.061 Uiso 1 1 calc . . . C34 C 0.8575(3) 0.18433(14) 0.7028(3) 0.0338(10) Uani 1 1 d . . . C35 C 0.9281(4) 0.19864(17) 0.7825(3) 0.0442(12) Uani 1 1 d . . . H35 H 0.9114 0.2230 0.8109 0.053 Uiso 1 1 calc . . . C36 C 1.0228(4) 0.17728(18) 0.8206(3) 0.0486(13) Uani 1 1 d . . . H36 H 1.0705 0.1871 0.8755 0.058 Uiso 1 1 calc . . . C37 C 1.0493(4) 0.14204(17) 0.7801(3) 0.0455(12) Uani 1 1 d . . . H37 H 1.1139 0.1274 0.8075 0.055 Uiso 1 1 calc . . . C38 C 0.9806(3) 0.12820(15) 0.6988(3) 0.0365(10) Uani 1 1 d . . . H38 H 0.9995 0.1044 0.6699 0.044 Uiso 1 1 calc . . . C39 C 0.8834(3) 0.14904(13) 0.6589(2) 0.0293(9) Uani 1 1 d . . . C40 C 0.8117(3) 0.13290(13) 0.5738(3) 0.0279(9) Uani 1 1 d . . . C41 C 0.5556(3) 0.14261(13) 0.4373(3) 0.0306(9) Uani 1 1 d . . . C42 C 0.3622(3) 0.17582(16) 0.4419(3) 0.0422(11) Uani 1 1 d . . . H42A H 0.3452 0.1477 0.4600 0.051 Uiso 1 1 calc . . . H42B H 0.3231 0.1958 0.4710 0.051 Uiso 1 1 calc . . . C43 C 0.3206(4) 0.17977(18) 0.3397(3) 0.0523(13) Uani 1 1 d . . . H43A H 0.3115 0.2095 0.3237 0.063 Uiso 1 1 calc . . . H43B H 0.2484 0.1666 0.3202 0.063 Uiso 1 1 calc . . . C44 C 0.3943(4) 0.16021(17) 0.2876(3) 0.0449(12) Uani 1 1 d . . . H44A H 0.4452 0.1815 0.2770 0.054 Uiso 1 1 calc . . . H44B H 0.3497 0.1511 0.2273 0.054 Uiso 1 1 calc . . . C45 C 0.4502(5) 0.0425(3) 0.1758(4) 0.085(2) Uani 1 1 d . . . H45A H 0.5003 0.0615 0.1561 0.102 Uiso 1 1 calc . . . H45B H 0.4787 0.0380 0.2422 0.102 Uiso 1 1 calc . . . C46 C 0.8476(5) 0.09990(19) -0.1193(4) 0.0667(16) Uani 1 1 d . . . H46A H 0.9068 0.1073 -0.0653 0.080 Uiso 1 1 calc . . . H46B H 0.8465 0.1208 -0.1672 0.080 Uiso 1 1 calc . . . C47 C 1.0313(3) 0.31963(17) -0.0138(3) 0.0440(11) Uani 1 1 d . . . H47A H 1.0079 0.2986 0.0245 0.053 Uiso 1 1 calc . . . H47B H 0.9702 0.3389 -0.0371 0.053 Uiso 1 1 calc . . . 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 0.0330(3) 0.0280(4) 0.0287(3) 0.0009(2) 0.0148(2) 0.0052(3) Fe2 0.0371(3) 0.0222(3) 0.0297(3) -0.0020(2) 0.0132(2) 0.0028(3) Cl1 0.0611(9) 0.1080(16) 0.0839(10) -0.0460(11) 0.0043(8) 0.0085(9) Cl2 0.0627(9) 0.0897(15) 0.1318(15) -0.0489(12) 0.0159(9) -0.0038(9) Cl3 0.0910(11) 0.0754(13) 0.1053(12) 0.0367(10) 0.0523(10) 0.0288(10) Cl4 0.1631(18) 0.0600(11) 0.0676(9) 0.0036(8) 0.0571(10) 0.0297(12) Cl5 0.0598(9) 0.146(2) 0.0763(10) -0.0625(11) 0.0232(7) -0.0292(10) Cl6 0.0507(7) 0.0483(8) 0.0515(7) -0.0082(6) 0.0161(5) -0.0133(6) S1 0.0424(6) 0.0328(7) 0.0450(6) -0.0061(5) 0.0202(5) 0.0061(5) S2 0.0447(6) 0.0336(7) 0.0714(8) -0.0051(6) 0.0289(6) -0.0023(5) S3 0.0372(6) 0.0280(6) 0.0563(7) -0.0029(5) 0.0163(5) 0.0075(5) S4 0.0449(6) 0.0357(7) 0.0403(6) -0.0072(5) 0.0049(5) 0.0082(5) S5 0.0586(8) 0.0346(8) 0.1578(16) -0.0238(10) 0.0599(10) -0.0125(7) S6 0.0374(6) 0.0306(7) 0.0677(8) -0.0110(6) 0.0152(5) 0.0052(5) S7 0.0317(5) 0.0296(6) 0.0506(6) -0.0067(5) 0.0152(5) 0.0028(5) S8 0.0422(6) 0.0373(7) 0.0415(6) -0.0079(5) 0.0018(5) 0.0055(5) O1 0.0463(18) 0.050(2) 0.066(2) -0.0040(18) 0.0324(16) 0.0048(17) O2 0.0421(16) 0.0274(18) 0.0494(16) 0.0005(14) 0.0250(13) 0.0026(14) O3 0.0398(16) 0.047(2) 0.0440(17) 0.0084(16) 0.0120(13) 0.0070(15) O4 0.0413(16) 0.0299(18) 0.0393(16) -0.0041(13) 0.0116(13) 0.0042(14) O5 0.0460(17) 0.0239(18) 0.062(2) -0.0027(15) 0.0170(15) 0.0009(14) O6 0.0414(16) 0.0253(17) 0.0439(16) -0.0047(13) 0.0192(13) 0.0018(13) O7 0.0422(17) 0.039(2) 0.0590(19) -0.0154(16) 0.0159(15) 0.0054(15) O8 0.0365(14) 0.0290(17) 0.0332(14) -0.0041(13) 0.0140(12) 0.0067(13) O9 0.079(2) 0.036(2) 0.0385(16) 0.0088(15) 0.0290(16) 0.0211(18) N1 0.0336(17) 0.035(2) 0.0366(18) -0.0023(16) 0.0180(14) 0.0008(16) N2 0.0346(17) 0.029(2) 0.0329(17) -0.0004(15) 0.0157(14) 0.0002(16) N3 0.0312(17) 0.026(2) 0.0323(17) 0.0034(15) 0.0115(14) 0.0023(15) N4 0.0308(16) 0.026(2) 0.0323(17) 0.0033(15) 0.0119(14) 0.0034(15) N5 0.0346(18) 0.0228(19) 0.0291(16) -0.0020(14) 0.0104(13) -0.0022(14) N6 0.0313(17) 0.0230(19) 0.0288(16) -0.0016(14) 0.0089(13) 0.0003(14) N7 0.0300(17) 0.028(2) 0.0289(16) -0.0031(14) 0.0125(13) -0.0001(15) N8 0.0318(17) 0.027(2) 0.0281(16) -0.0043(14) 0.0108(13) -0.0008(15) C1 0.038(2) 0.045(3) 0.041(2) 0.006(2) 0.0141(19) 0.004(2) C2 0.035(2) 0.077(5) 0.045(3) 0.004(3) 0.015(2) -0.005(3) C3 0.044(3) 0.060(4) 0.056(3) 0.016(3) 0.012(2) -0.014(3) C4 0.054(3) 0.047(3) 0.043(2) 0.008(2) 0.012(2) -0.010(2) C5 0.046(2) 0.037(3) 0.036(2) 0.004(2) 0.0161(19) 0.000(2) C6 0.033(2) 0.041(3) 0.035(2) 0.008(2) 0.0161(17) 0.003(2) C7 0.036(2) 0.030(3) 0.031(2) 0.0016(18) 0.0115(17) 0.0030(19) C8 0.036(2) 0.032(3) 0.0252(18) -0.0010(18) 0.0118(16) 0.0013(19) C9 0.076(3) 0.041(3) 0.054(3) -0.014(2) 0.037(3) -0.008(3) C10 0.092(4) 0.028(3) 0.070(3) -0.001(3) 0.039(3) 0.008(3) C11 0.078(4) 0.042(3) 0.078(4) 0.015(3) 0.044(3) 0.004(3) C12 0.031(2) 0.045(3) 0.043(2) 0.009(2) 0.0162(18) -0.004(2) C13 0.034(2) 0.071(4) 0.045(3) 0.014(3) 0.002(2) -0.007(2) C14 0.047(3) 0.083(5) 0.038(3) 0.009(3) 0.003(2) -0.024(3) C15 0.059(3) 0.057(4) 0.040(3) -0.007(3) 0.013(2) -0.025(3) C16 0.045(2) 0.040(3) 0.038(2) 0.000(2) 0.0127(19) -0.012(2) C17 0.032(2) 0.039(3) 0.037(2) 0.003(2) 0.0161(17) -0.007(2) C18 0.0288(19) 0.030(2) 0.034(2) 0.0028(18) 0.0171(16) 0.0000(18) C19 0.031(2) 0.026(2) 0.036(2) 0.0035(18) 0.0173(16) 0.0009(17) C20 0.062(3) 0.031(3) 0.055(3) -0.009(2) 0.024(2) 0.005(2) C21 0.061(3) 0.042(3) 0.049(3) -0.010(2) 0.028(2) 0.004(3) C22 0.056(3) 0.063(4) 0.045(3) -0.022(3) 0.014(2) 0.000(3) C23 0.044(2) 0.032(3) 0.0260(19) 0.0011(18) 0.0111(17) -0.003(2) C24 0.060(3) 0.027(3) 0.042(2) 0.000(2) 0.019(2) -0.008(2) C25 0.060(3) 0.048(3) 0.049(3) -0.005(2) 0.024(2) -0.023(3) C26 0.050(3) 0.056(4) 0.062(3) -0.006(3) 0.029(2) -0.016(3) C27 0.049(3) 0.041(3) 0.046(2) -0.005(2) 0.022(2) -0.005(2) C28 0.043(2) 0.027(2) 0.0273(19) -0.0024(17) 0.0141(17) -0.0053(19) C29 0.037(2) 0.024(2) 0.0217(17) 0.0007(16) 0.0068(15) 0.0016(18) C30 0.036(2) 0.029(2) 0.0236(18) -0.0015(17) 0.0069(16) 0.0012(18) C31 0.072(4) 0.062(5) 0.199(8) -0.037(5) 0.081(5) -0.016(4) C32 0.065(3) 0.059(4) 0.072(3) 0.004(3) 0.043(3) 0.008(3) C33 0.040(2) 0.059(4) 0.057(3) -0.001(3) 0.020(2) 0.009(2) C34 0.036(2) 0.036(3) 0.033(2) 0.0009(19) 0.0169(17) -0.0023(19) C35 0.049(3) 0.050(3) 0.038(2) -0.017(2) 0.021(2) -0.015(2) C36 0.054(3) 0.059(4) 0.032(2) -0.005(2) 0.010(2) -0.019(3) C37 0.042(2) 0.045(3) 0.047(3) 0.009(2) 0.006(2) -0.007(2) C38 0.036(2) 0.032(3) 0.042(2) 0.002(2) 0.0109(18) -0.0020(19) C39 0.037(2) 0.027(2) 0.0286(19) 0.0015(17) 0.0159(16) -0.0027(18) C40 0.032(2) 0.023(2) 0.033(2) 0.0006(17) 0.0164(16) -0.0018(17) C41 0.033(2) 0.027(2) 0.035(2) 0.0056(18) 0.0135(17) 0.0020(18) C42 0.032(2) 0.042(3) 0.057(3) -0.003(2) 0.020(2) 0.001(2) C43 0.034(2) 0.061(4) 0.062(3) 0.007(3) 0.012(2) 0.017(2) C44 0.042(2) 0.049(3) 0.042(2) 0.009(2) 0.0063(19) 0.006(2) C45 0.060(4) 0.105(7) 0.084(4) -0.030(4) 0.010(3) -0.001(4) C46 0.087(4) 0.047(4) 0.073(4) 0.014(3) 0.034(3) 0.001(3) C47 0.036(2) 0.049(3) 0.047(3) -0.001(2) 0.0109(19) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O9 1.747(3) . ? Fe1 O4 1.946(3) . ? Fe1 O2 1.948(3) . ? Fe1 N4 2.131(3) . ? Fe1 N2 2.135(3) . ? Fe2 O9 1.750(3) . ? Fe2 O8 1.954(3) . ? Fe2 O6 1.960(3) . ? Fe2 N8 2.120(3) . ? Fe2 N6 2.126(3) . ? Cl1 C45 1.762(6) . ? Cl2 C45 1.707(7) . ? Cl3 C46 1.725(6) . ? Cl4 C46 1.757(7) . ? Cl5 C47 1.738(5) . ? Cl6 C47 1.761(5) . ? S1 C8 1.748(4) . ? S1 C9 1.814(5) . ? S2 C8 1.731(4) . ? S2 C11 1.779(6) . ? S3 C19 1.737(4) . ? S3 C20 1.799(5) . ? S4 C19 1.742(4) . ? S4 C22 1.800(5) . ? S5 C31 1.718(6) . ? S5 C30 1.725(4) . ? S6 C30 1.728(4) . ? S6 C33 1.796(5) . ? S7 C41 1.738(4) . ? S7 C42 1.819(4) . ? S8 C41 1.748(4) . ? S8 C44 1.818(5) . ? O1 C1 1.352(6) . ? O1 H1O 0.8400 . ? O2 C7 1.311(5) . ? O3 C12 1.358(6) . ? O3 H3O 0.8400 . ? O4 C18 1.302(5) . ? O5 C23 1.355(5) . ? O5 H5O 0.8400 . ? O6 C29 1.292(5) . ? O7 C34 1.363(5) . ? O7 H7O 0.8400 . ? O8 C40 1.307(5) . ? N1 C7 1.306(6) . ? N1 N2 1.395(5) . ? N2 C8 1.303(5) . ? N3 C18 1.314(5) . ? N3 N4 1.419(4) . ? N4 C19 1.302(5) . ? N5 C29 1.307(5) . ? N5 N6 1.405(5) . ? N6 C30 1.306(5) . ? N7 C40 1.314(5) . ? N7 N8 1.403(4) . ? N8 C41 1.301(5) . ? C1 C2 1.392(7) . ? C1 C6 1.413(6) . ? C2 C3 1.376(8) . ? C2 H2 0.9500 . ? C3 C4 1.390(7) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(6) . ? C5 H5 0.9500 . ? C6 C7 1.471(6) . ? C9 C10 1.513(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.493(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.392(6) . ? C12 C17 1.404(6) . ? C13 C14 1.373(8) . ? C13 H13 0.9500 . ? C14 C15 1.388(8) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 C17 1.409(6) . ? C16 H16 0.9500 . ? C17 C18 1.459(6) . ? C20 C21 1.523(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.475(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.389(6) . ? C23 C28 1.415(6) . ? C24 C25 1.378(7) . ? C24 H24 0.9500 . ? C25 C26 1.366(8) . ? C25 H25 0.9500 . ? C26 C27 1.385(7) . ? C26 H26 0.9500 . ? C27 C28 1.384(6) . ? C27 H27 0.9500 . ? C28 C29 1.479(6) . ? C31 C32 1.486(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.481(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.388(6) . ? C34 C39 1.405(6) . ? C35 C36 1.385(7) . ? C35 H35 0.9500 . ? C36 C37 1.379(7) . ? C36 H36 0.9500 . ? C37 C38 1.390(6) . ? C37 H37 0.9500 . ? C38 C39 1.405(6) . ? C38 H38 0.9500 . ? C39 C40 1.471(5) . ? C42 C43 1.510(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.521(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Fe1 O4 121.88(15) . . ? O9 Fe1 O2 118.91(15) . . ? O4 Fe1 O2 119.21(12) . . ? O9 Fe1 N4 100.89(13) . . ? O4 Fe1 N4 77.22(12) . . ? O2 Fe1 N4 91.78(12) . . ? O9 Fe1 N2 101.55(14) . . ? O4 Fe1 N2 91.28(12) . . ? O2 Fe1 N2 76.93(13) . . ? N4 Fe1 N2 157.55(13) . . ? O9 Fe2 O8 117.58(15) . . ? O9 Fe2 O6 122.66(15) . . ? O8 Fe2 O6 119.75(12) . . ? O9 Fe2 N8 100.01(14) . . ? O8 Fe2 N8 76.73(11) . . ? O6 Fe2 N8 92.78(12) . . ? O9 Fe2 N6 99.02(13) . . ? O8 Fe2 N6 94.61(11) . . ? O6 Fe2 N6 76.67(12) . . ? N8 Fe2 N6 160.97(13) . . ? C8 S1 C9 100.2(2) . . ? C8 S2 C11 101.7(2) . . ? C19 S3 C20 104.2(2) . . ? C19 S4 C22 107.5(2) . . ? C31 S5 C30 109.1(3) . . ? C30 S6 C33 105.9(2) . . ? C41 S7 C42 99.6(2) . . ? C41 S8 C44 98.6(2) . . ? C1 O1 H1O 109.5 . . ? C7 O2 Fe1 115.9(3) . . ? C12 O3 H3O 109.5 . . ? C18 O4 Fe1 115.9(3) . . ? C23 O5 H5O 109.5 . . ? C29 O6 Fe2 116.0(3) . . ? C34 O7 H7O 109.5 . . ? C40 O8 Fe2 115.7(2) . . ? Fe1 O9 Fe2 167.1(2) . . ? C7 N1 N2 111.2(3) . . ? C8 N2 N1 115.3(3) . . ? C8 N2 Fe1 132.4(3) . . ? N1 N2 Fe1 112.2(3) . . ? C18 N3 N4 111.1(3) . . ? C19 N4 N3 114.5(3) . . ? C19 N4 Fe1 134.3(3) . . ? N3 N4 Fe1 111.1(2) . . ? C29 N5 N6 110.6(3) . . ? C30 N6 N5 115.5(3) . . ? C30 N6 Fe2 131.9(3) . . ? N5 N6 Fe2 112.6(2) . . ? C40 N7 N8 110.4(3) . . ? C41 N8 N7 114.7(3) . . ? C41 N8 Fe2 132.2(3) . . ? N7 N8 Fe2 112.6(2) . . ? O1 C1 C2 117.8(4) . . ? O1 C1 C6 123.1(4) . . ? C2 C1 C6 119.2(5) . . ? C3 C2 C1 120.3(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.5(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 118.4(5) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.1(4) . . ? C5 C6 C7 119.3(4) . . ? C1 C6 C7 121.6(4) . . ? N1 C7 O2 123.6(4) . . ? N1 C7 C6 118.2(4) . . ? O2 C7 C6 118.3(4) . . ? N2 C8 S2 117.6(3) . . ? N2 C8 S1 120.7(3) . . ? S2 C8 S1 121.6(3) . . ? C10 C9 S1 114.7(4) . . ? C10 C9 H9A 108.6 . . ? S1 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S1 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 114.9(5) . . ? C11 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C10 C11 S2 118.9(4) . . ? C10 C11 H11A 107.6 . . ? S2 C11 H11A 107.6 . . ? C10 C11 H11B 107.6 . . ? S2 C11 H11B 107.6 . . ? H11A C11 H11B 107.0 . . ? O3 C12 C13 118.2(4) . . ? O3 C12 C17 122.5(4) . . ? C13 C12 C17 119.3(5) . . ? C14 C13 C12 121.0(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.8(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.0(5) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 121.2(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C12 C17 C16 118.7(4) . . ? C12 C17 C18 122.2(4) . . ? C16 C17 C18 119.0(4) . . ? O4 C18 N3 123.2(4) . . ? O4 C18 C17 119.0(4) . . ? N3 C18 C17 117.7(4) . . ? N4 C19 S3 120.1(3) . . ? N4 C19 S4 113.6(3) . . ? S3 C19 S4 125.8(2) . . ? C21 C20 S3 114.6(4) . . ? C21 C20 H20A 108.6 . . ? S3 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? S3 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 112.0(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 S4 117.6(4) . . ? C21 C22 H22A 107.9 . . ? S4 C22 H22A 107.9 . . ? C21 C22 H22B 107.9 . . ? S4 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? O5 C23 C24 117.4(4) . . ? O5 C23 C28 122.8(4) . . ? C24 C23 C28 119.8(4) . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.9(5) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 121.1(5) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C23 118.4(4) . . ? C27 C28 C29 119.8(4) . . ? C23 C28 C29 121.8(4) . . ? O6 C29 N5 124.1(4) . . ? O6 C29 C28 117.4(4) . . ? N5 C29 C28 118.4(4) . . ? N6 C30 S5 115.0(3) . . ? N6 C30 S6 119.9(3) . . ? S5 C30 S6 124.9(2) . . ? C32 C31 S5 119.8(5) . . ? C32 C31 H31A 107.4 . . ? S5 C31 H31A 107.4 . . ? C32 C31 H31B 107.4 . . ? S5 C31 H31B 107.4 . . ? H31A C31 H31B 106.9 . . ? C33 C32 C31 112.8(5) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C32 C33 S6 118.8(4) . . ? C32 C33 H33A 107.6 . . ? S6 C33 H33A 107.6 . . ? C32 C33 H33B 107.6 . . ? S6 C33 H33B 107.6 . . ? H33A C33 H33B 107.0 . . ? O7 C34 C35 116.8(4) . . ? O7 C34 C39 122.9(4) . . ? C35 C34 C39 120.3(4) . . ? C36 C35 C34 119.8(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C37 C38 C39 120.9(4) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 118.5(4) . . ? C38 C39 C40 119.2(4) . . ? C34 C39 C40 122.3(4) . . ? O8 C40 N7 123.4(4) . . ? O8 C40 C39 119.5(4) . . ? N7 C40 C39 117.1(4) . . ? N8 C41 S7 122.2(3) . . ? N8 C41 S8 117.3(3) . . ? S7 C41 S8 120.5(2) . . ? C43 C42 S7 114.5(3) . . ? C43 C42 H42A 108.6 . . ? S7 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? S7 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 113.6(4) . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? C44 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C43 C44 S8 114.2(3) . . ? C43 C44 H44A 108.7 . . ? S8 C44 H44A 108.7 . . ? C43 C44 H44B 108.7 . . ? S8 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? Cl2 C45 Cl1 113.7(3) . . ? Cl2 C45 H45A 108.8 . . ? Cl1 C45 H45A 108.8 . . ? Cl2 C45 H45B 108.8 . . ? Cl1 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? Cl3 C46 Cl4 113.0(4) . . ? Cl3 C46 H46A 109.0 . . ? Cl4 C46 H46A 109.0 . . ? Cl3 C46 H46B 109.0 . . ? Cl4 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? Cl5 C47 Cl6 111.1(2) . . ? Cl5 C47 H47A 109.4 . . ? Cl6 C47 H47A 109.4 . . ? Cl5 C47 H47B 109.4 . . ? Cl6 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Fe1 O2 C7 93.0(3) . . . . ? O4 Fe1 O2 C7 -87.2(3) . . . . ? N4 Fe1 O2 C7 -163.5(3) . . . . ? N2 Fe1 O2 C7 -3.1(3) . . . . ? O9 Fe1 O4 C18 105.6(3) . . . . ? O2 Fe1 O4 C18 -74.2(3) . . . . ? N4 Fe1 O4 C18 10.6(3) . . . . ? N2 Fe1 O4 C18 -149.9(3) . . . . ? O9 Fe2 O6 C29 91.1(3) . . . . ? O8 Fe2 O6 C29 -88.9(3) . . . . ? N8 Fe2 O6 C29 -165.2(3) . . . . ? N6 Fe2 O6 C29 -1.2(3) . . . . ? O9 Fe2 O8 C40 85.5(3) . . . . ? O6 Fe2 O8 C40 -94.5(3) . . . . ? N8 Fe2 O8 C40 -8.9(3) . . . . ? N6 Fe2 O8 C40 -171.8(3) . . . . ? O4 Fe1 O9 Fe2 15.5(10) . . . . ? O2 Fe1 O9 Fe2 -164.7(9) . . . . ? N4 Fe1 O9 Fe2 97.1(9) . . . . ? N2 Fe1 O9 Fe2 -83.4(9) . . . . ? O8 Fe2 O9 Fe1 -177.7(9) . . . . ? O6 Fe2 O9 Fe1 2.3(10) . . . . ? N8 Fe2 O9 Fe1 -97.6(9) . . . . ? N6 Fe2 O9 Fe1 82.2(9) . . . . ? C7 N1 N2 C8 177.6(3) . . . . ? C7 N1 N2 Fe1 -3.7(4) . . . . ? O9 Fe1 N2 C8 64.7(4) . . . . ? O4 Fe1 N2 C8 -58.2(4) . . . . ? O2 Fe1 N2 C8 -177.9(4) . . . . ? N4 Fe1 N2 C8 -116.5(4) . . . . ? O9 Fe1 N2 N1 -113.6(3) . . . . ? O4 Fe1 N2 N1 123.5(2) . . . . ? O2 Fe1 N2 N1 3.8(2) . . . . ? N4 Fe1 N2 N1 65.2(4) . . . . ? C18 N3 N4 C19 -174.5(3) . . . . ? C18 N3 N4 Fe1 7.3(4) . . . . ? O9 Fe1 N4 C19 52.1(4) . . . . ? O4 Fe1 N4 C19 172.7(4) . . . . ? O2 Fe1 N4 C19 -67.8(4) . . . . ? N2 Fe1 N4 C19 -126.6(4) . . . . ? O9 Fe1 N4 N3 -130.2(2) . . . . ? O4 Fe1 N4 N3 -9.6(2) . . . . ? O2 Fe1 N4 N3 109.9(2) . . . . ? N2 Fe1 N4 N3 51.1(5) . . . . ? C29 N5 N6 C30 -178.1(3) . . . . ? C29 N5 N6 Fe2 -0.3(3) . . . . ? O9 Fe2 N6 C30 56.5(4) . . . . ? O8 Fe2 N6 C30 -62.4(3) . . . . ? O6 Fe2 N6 C30 178.1(3) . . . . ? N8 Fe2 N6 C30 -124.2(4) . . . . ? O9 Fe2 N6 N5 -120.8(2) . . . . ? O8 Fe2 N6 N5 120.3(2) . . . . ? O6 Fe2 N6 N5 0.8(2) . . . . ? N8 Fe2 N6 N5 58.5(5) . . . . ? C40 N7 N8 C41 178.2(3) . . . . ? C40 N7 N8 Fe2 -9.0(4) . . . . ? O9 Fe2 N8 C41 64.7(4) . . . . ? O8 Fe2 N8 C41 -179.1(4) . . . . ? O6 Fe2 N8 C41 -59.1(4) . . . . ? N6 Fe2 N8 C41 -114.6(5) . . . . ? O9 Fe2 N8 N7 -106.4(3) . . . . ? O8 Fe2 N8 N7 9.8(2) . . . . ? O6 Fe2 N8 N7 129.8(3) . . . . ? N6 Fe2 N8 N7 74.3(5) . . . . ? O1 C1 C2 C3 -178.8(4) . . . . ? C6 C1 C2 C3 0.9(7) . . . . ? C1 C2 C3 C4 0.0(8) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? C3 C4 C5 C6 1.7(7) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C4 C5 C6 C7 179.9(4) . . . . ? O1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C5 -0.5(6) . . . . ? O1 C1 C6 C7 -1.5(6) . . . . ? C2 C1 C6 C7 178.7(4) . . . . ? N2 N1 C7 O2 1.3(5) . . . . ? N2 N1 C7 C6 -178.1(3) . . . . ? Fe1 O2 C7 N1 2.2(5) . . . . ? Fe1 O2 C7 C6 -178.5(3) . . . . ? C5 C6 C7 N1 -176.6(4) . . . . ? C1 C6 C7 N1 4.2(6) . . . . ? C5 C6 C7 O2 4.0(6) . . . . ? C1 C6 C7 O2 -175.2(4) . . . . ? N1 N2 C8 S2 -171.7(3) . . . . ? Fe1 N2 C8 S2 10.1(5) . . . . ? N1 N2 C8 S1 4.9(5) . . . . ? Fe1 N2 C8 S1 -173.37(19) . . . . ? C11 S2 C8 N2 -152.0(3) . . . . ? C11 S2 C8 S1 31.5(3) . . . . ? C9 S1 C8 N2 -159.2(3) . . . . ? C9 S1 C8 S2 17.2(3) . . . . ? C8 S1 C9 C10 -62.8(4) . . . . ? S1 C9 C10 C11 46.6(7) . . . . ? C9 C10 C11 S2 18.9(7) . . . . ? C8 S2 C11 C10 -56.7(5) . . . . ? O3 C12 C13 C14 178.9(4) . . . . ? C17 C12 C13 C14 0.0(7) . . . . ? C12 C13 C14 C15 1.1(7) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C17 -0.8(7) . . . . ? O3 C12 C17 C16 179.7(4) . . . . ? C13 C12 C17 C16 -1.5(6) . . . . ? O3 C12 C17 C18 -4.8(6) . . . . ? C13 C12 C17 C18 174.0(4) . . . . ? C15 C16 C17 C12 1.9(6) . . . . ? C15 C16 C17 C18 -173.7(4) . . . . ? Fe1 O4 C18 N3 -10.7(5) . . . . ? Fe1 O4 C18 C17 165.9(3) . . . . ? N4 N3 C18 O4 1.5(5) . . . . ? N4 N3 C18 C17 -175.1(3) . . . . ? C12 C17 C18 O4 -171.9(4) . . . . ? C16 C17 C18 O4 3.6(6) . . . . ? C12 C17 C18 N3 4.8(6) . . . . ? C16 C17 C18 N3 -179.7(4) . . . . ? N3 N4 C19 S3 2.4(5) . . . . ? Fe1 N4 C19 S3 -179.96(19) . . . . ? N3 N4 C19 S4 174.7(2) . . . . ? Fe1 N4 C19 S4 -7.7(5) . . . . ? C20 S3 C19 N4 -167.8(3) . . . . ? C20 S3 C19 S4 21.0(3) . . . . ? C22 S4 C19 N4 174.8(3) . . . . ? C22 S4 C19 S3 -13.4(3) . . . . ? C19 S3 C20 C21 -47.4(4) . . . . ? S3 C20 C21 C22 71.8(5) . . . . ? C20 C21 C22 S4 -61.6(6) . . . . ? C19 S4 C22 C21 30.9(5) . . . . ? O5 C23 C24 C25 -179.4(4) . . . . ? C28 C23 C24 C25 0.4(6) . . . . ? C23 C24 C25 C26 -0.5(7) . . . . ? C24 C25 C26 C27 0.0(8) . . . . ? C25 C26 C27 C28 0.5(7) . . . . ? C26 C27 C28 C23 -0.5(6) . . . . ? C26 C27 C28 C29 179.4(4) . . . . ? O5 C23 C28 C27 179.9(4) . . . . ? C24 C23 C28 C27 0.1(6) . . . . ? O5 C23 C28 C29 0.0(6) . . . . ? C24 C23 C28 C29 -179.9(4) . . . . ? Fe2 O6 C29 N5 1.5(5) . . . . ? Fe2 O6 C29 C28 -178.8(2) . . . . ? N6 N5 C29 O6 -0.7(5) . . . . ? N6 N5 C29 C28 179.6(3) . . . . ? C27 C28 C29 O6 -3.9(5) . . . . ? C23 C28 C29 O6 176.1(3) . . . . ? C27 C28 C29 N5 175.8(4) . . . . ? C23 C28 C29 N5 -4.2(5) . . . . ? N5 N6 C30 S5 173.3(2) . . . . ? Fe2 N6 C30 S5 -3.9(5) . . . . ? N5 N6 C30 S6 -2.2(4) . . . . ? Fe2 N6 C30 S6 -179.38(18) . . . . ? C31 S5 C30 N6 175.3(4) . . . . ? C31 S5 C30 S6 -9.5(5) . . . . ? C33 S6 C30 N6 -173.7(3) . . . . ? C33 S6 C30 S5 11.2(3) . . . . ? C30 S5 C31 C32 31.6(8) . . . . ? S5 C31 C32 C33 -58.8(8) . . . . ? C31 C32 C33 S6 61.3(7) . . . . ? C30 S6 C33 C32 -36.2(5) . . . . ? O7 C34 C35 C36 178.6(4) . . . . ? C39 C34 C35 C36 -2.1(7) . . . . ? C34 C35 C36 C37 0.6(7) . . . . ? C35 C36 C37 C38 1.2(7) . . . . ? C36 C37 C38 C39 -1.7(7) . . . . ? C37 C38 C39 C34 0.3(6) . . . . ? C37 C38 C39 C40 -178.7(4) . . . . ? O7 C34 C39 C38 -179.1(4) . . . . ? C35 C34 C39 C38 1.6(6) . . . . ? O7 C34 C39 C40 -0.1(6) . . . . ? C35 C34 C39 C40 -179.5(4) . . . . ? Fe2 O8 C40 N7 7.2(5) . . . . ? Fe2 O8 C40 C39 -173.6(3) . . . . ? N8 N7 C40 O8 1.7(5) . . . . ? N8 N7 C40 C39 -177.4(3) . . . . ? C38 C39 C40 O8 -10.1(6) . . . . ? C34 C39 C40 O8 171.0(4) . . . . ? C38 C39 C40 N7 169.1(4) . . . . ? C34 C39 C40 N7 -9.8(6) . . . . ? N7 N8 C41 S7 5.7(5) . . . . ? Fe2 N8 C41 S7 -165.2(2) . . . . ? N7 N8 C41 S8 -174.1(3) . . . . ? Fe2 N8 C41 S8 14.9(5) . . . . ? C42 S7 C41 N8 -161.5(4) . . . . ? C42 S7 C41 S8 18.4(3) . . . . ? C44 S8 C41 N8 -144.7(3) . . . . ? C44 S8 C41 S7 35.4(3) . . . . ? C41 S7 C42 C43 -65.7(4) . . . . ? S7 C42 C43 C44 41.7(6) . . . . ? C42 C43 C44 S8 29.8(6) . . . . ? C41 S8 C44 C43 -67.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.971 _refine_diff_density_min -2.018 _refine_diff_density_rms 0.167