# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Welter' _publ_contact_author_email WELTER@UNISTRA.FR _publ_section_title ; Novel CrIII dinuclear complexes supported by salicyloylhydrazono dithiolane and dithiane ligands: synthesis, stability, crystal structures and magnetic properties ; loop_ _publ_author_name 'Richard Welter' 'Lydia Brelot' 'Sylvie Choua' 'Nicolas Clement' 'Samuel Dagorne' 'Guylaine Freund' ; J.Kortus ; 'Claudia Loose' 'Guillaume Rogez' 'Clement Toussaint' 'Philippe Turek' # Attachment 'complex_1a.cif' data_complex_1a _database_code_depnum_ccdc_archive 'CCDC 712216' #TrackingRef 'complex_1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H27 Cr N6 O6 S6, C H4 O' _chemical_formula_sum 'C31 H31 Cr N6 O7 S6' _chemical_formula_weight 843.98 _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' Cr Cr 0.3209 0.6236 '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 9.932(2) _cell_length_b 12.037(4) _cell_length_c 16.021(5) _cell_angle_alpha 80.157(5) _cell_angle_beta 83.167(5) _cell_angle_gamma 69.42 _cell_volume 1763.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11190 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.737 _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 193(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 20821 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 29.71 _reflns_number_total 9883 _reflns_number_gt 7817 _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^)+(0.0836P)^2^+1.0686P] 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 9883 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr -0.03108(4) 0.25058(3) 0.73444(2) 0.01853(10) Uani 1 1 d . . . S1 S -0.46797(8) 0.38787(8) 0.60476(6) 0.0414(2) Uani 1 1 d . . . S2 S -0.19350(7) 0.20829(7) 0.55083(5) 0.03344(16) Uani 1 1 d . . . S3 S 0.13709(7) 0.56936(6) 0.63112(5) 0.03377(17) Uani 1 1 d . . . S4 S 0.00355(7) 0.51945(6) 0.80197(5) 0.03218(16) Uani 1 1 d . . . S5 S 0.32889(7) 0.26582(7) 0.77381(6) 0.03771(19) Uani 1 1 d . . . S6 S 0.37974(7) 0.03895(6) 0.89125(4) 0.02799(15) Uani 1 1 d . . . O1 O -0.5490(2) 0.5982(2) 0.75254(15) 0.0362(5) Uani 1 1 d . . . O2 O -0.14534(17) 0.34612(15) 0.82243(11) 0.0230(3) Uani 1 1 d . . . O3 O 0.2053(2) 0.42369(19) 0.44275(15) 0.0341(4) Uani 1 1 d . . . O4 O 0.07182(17) 0.18495(15) 0.63200(11) 0.0223(3) Uani 1 1 d . . . O5 O 0.13646(19) -0.12302(17) 0.98247(12) 0.0268(4) Uani 1 1 d . . . O6 O -0.08631(18) 0.10999(15) 0.77736(11) 0.0232(3) Uani 1 1 d . . . O7 O 0.1929(3) -0.0741(2) 0.66534(17) 0.0484(6) Uani 1 1 d . . . H7 H 0.1370 -0.0027 0.6614 0.073 Uiso 1 1 calc . . . N1 N -0.3214(2) 0.41919(19) 0.72694(14) 0.0242(4) Uani 1 1 d . . . N2 N -0.2245(2) 0.33145(18) 0.68033(13) 0.0210(4) Uani 1 1 d . . . N3 N 0.1011(2) 0.36825(18) 0.59387(14) 0.0243(4) Uani 1 1 d . . . N4 N 0.0461(2) 0.38397(18) 0.67761(13) 0.0219(4) Uani 1 1 d . . . N5 N 0.1122(2) 0.04791(17) 0.85660(13) 0.0215(4) Uani 1 1 d . . . N6 N 0.1383(2) 0.14962(17) 0.81017(13) 0.0205(4) Uani 1 1 d . . . C1 C -0.4947(3) 0.5940(2) 0.82711(19) 0.0287(5) Uani 1 1 d . . . C2 C -0.5769(3) 0.6778(3) 0.8801(2) 0.0359(6) Uani 1 1 d . . . H2 H -0.6657 0.7356 0.8625 0.043 Uiso 1 1 calc . . . C3 C -0.5298(3) 0.6769(3) 0.9577(2) 0.0362(6) Uani 1 1 d . . . H3 H -0.5876 0.7331 0.9938 0.043 Uiso 1 1 calc . . . C4 C -0.3989(3) 0.5951(3) 0.98378(19) 0.0332(6) Uani 1 1 d . . . H4 H -0.3665 0.5958 1.0371 0.040 Uiso 1 1 calc . . . C5 C -0.3157(3) 0.5123(2) 0.93156(18) 0.0287(5) Uani 1 1 d . . . H5 H -0.2260 0.4564 0.9496 0.034 Uiso 1 1 calc . . . C6 C -0.3610(2) 0.5092(2) 0.85294(17) 0.0241(5) Uani 1 1 d . . . C7 C -0.2706(2) 0.4194(2) 0.79877(16) 0.0219(5) Uani 1 1 d . . . C8 C -0.2847(2) 0.3116(2) 0.61955(16) 0.0235(5) Uani 1 1 d . . . C9 C -0.4839(4) 0.2944(5) 0.5345(3) 0.0697(9) Uani 1 1 d . . . H9A H -0.5114 0.2273 0.5673 0.084 Uiso 1 1 calc . . . H9B H -0.5601 0.3410 0.4951 0.084 Uiso 1 1 calc . . . C10 C -0.3465(4) 0.2473(5) 0.4862(3) 0.0697(9) Uani 1 1 d . . . H10A H -0.3385 0.3082 0.4376 0.084 Uiso 1 1 calc . . . H10B H -0.3441 0.1753 0.4633 0.084 Uiso 1 1 calc . . . C11 C 0.2191(3) 0.3126(2) 0.43032(17) 0.0272(5) Uani 1 1 d . . . C12 C 0.2810(3) 0.2775(3) 0.35196(18) 0.0362(6) Uani 1 1 d . . . H12 H 0.3124 0.3315 0.3107 0.043 Uiso 1 1 calc . . . C13 C 0.2972(4) 0.1658(3) 0.33367(19) 0.0426(7) Uani 1 1 d . . . H13 H 0.3405 0.1432 0.2802 0.051 Uiso 1 1 calc . . . C14 C 0.2511(4) 0.0859(3) 0.3924(2) 0.0450(8) Uani 1 1 d . . . H14 H 0.2607 0.0095 0.3790 0.054 Uiso 1 1 calc . . . C15 C 0.1906(3) 0.1185(3) 0.47120(18) 0.0351(6) Uani 1 1 d . . . H15 H 0.1597 0.0634 0.5117 0.042 Uiso 1 1 calc . . . C16 C 0.1743(3) 0.2311(2) 0.49192(16) 0.0257(5) Uani 1 1 d . . . C17 C 0.1127(2) 0.2621(2) 0.57688(15) 0.0221(5) Uani 1 1 d . . . C18 C 0.0579(2) 0.4786(2) 0.70090(17) 0.0243(5) Uani 1 1 d . . . C19 C 0.1019(3) 0.6814(3) 0.7011(3) 0.0442(8) Uani 1 1 d . . . H19A H 0.1745 0.7221 0.6889 0.053 Uiso 1 1 calc . . . H19B H 0.0051 0.7423 0.6931 0.053 Uiso 1 1 calc . . . C20 C 0.1101(3) 0.6169(3) 0.7908(2) 0.0405(7) Uani 1 1 d . . . H20A H 0.0719 0.6755 0.8317 0.049 Uiso 1 1 calc . . . H20B H 0.2114 0.5692 0.8025 0.049 Uiso 1 1 calc . . . C21 C 0.0257(2) -0.1397(2) 0.95087(15) 0.0220(5) Uani 1 1 d . . . C22 C -0.0219(3) -0.2317(2) 0.99434(16) 0.0268(5) Uani 1 1 d . . . H22 H 0.0236 -0.2790 1.0437 0.032 Uiso 1 1 calc . . . C23 C -0.1343(3) -0.2541(2) 0.96589(18) 0.0302(5) Uani 1 1 d . . . H23 H -0.1662 -0.3164 0.9960 0.036 Uiso 1 1 calc . . . C24 C -0.2016(3) -0.1860(2) 0.89327(18) 0.0293(5) Uani 1 1 d . . . H24 H -0.2779 -0.2025 0.8733 0.035 Uiso 1 1 calc . . . C25 C -0.1561(3) -0.0939(2) 0.85044(17) 0.0251(5) Uani 1 1 d . . . H25 H -0.2017 -0.0477 0.8009 0.030 Uiso 1 1 calc . . . C26 C -0.0440(2) -0.0676(2) 0.87904(15) 0.0205(4) Uani 1 1 d . . . C27 C -0.0047(2) 0.0361(2) 0.83462(15) 0.0195(4) Uani 1 1 d . . . C28 C 0.2630(3) 0.1529(2) 0.82366(16) 0.0227(5) Uani 1 1 d . . . C29 C 0.5113(3) 0.1907(3) 0.8077(2) 0.0421(7) Uani 1 1 d . . . H29A H 0.5694 0.1357 0.7673 0.051 Uiso 1 1 calc . . . H29B H 0.5582 0.2502 0.8102 0.051 Uiso 1 1 calc . . . C30 C 0.5001(3) 0.1211(3) 0.8948(2) 0.0343(6) Uani 1 1 d . . . H30A H 0.4620 0.1768 0.9376 0.041 Uiso 1 1 calc . . . H30B H 0.5964 0.0650 0.9105 0.041 Uiso 1 1 calc . . . C31 C 0.3314(4) -0.0792(3) 0.6817(2) 0.0539(9) Uani 1 1 d . . . H31A H 0.3641 -0.0251 0.6378 0.081 Uiso 1 1 calc . . . H31B H 0.3986 -0.1613 0.6813 0.081 Uiso 1 1 calc . . . H31C H 0.3279 -0.0547 0.7374 0.081 Uiso 1 1 calc . . . H3O H 0.169(4) 0.438(4) 0.486(3) 0.051(12) Uiso 1 1 d . . . H1O H -0.495(5) 0.551(4) 0.725(3) 0.061(13) Uiso 1 1 d . . . H5O H 0.152(4) -0.060(3) 0.951(2) 0.045(10) 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 Cr 0.01746(18) 0.01895(18) 0.01798(19) 0.00159(14) -0.00286(13) -0.00606(13) S1 0.0249(3) 0.0515(5) 0.0477(5) -0.0091(4) -0.0157(3) -0.0074(3) S2 0.0332(3) 0.0407(4) 0.0300(4) -0.0102(3) -0.0054(3) -0.0133(3) S3 0.0323(3) 0.0265(3) 0.0442(4) 0.0001(3) 0.0012(3) -0.0155(3) S4 0.0273(3) 0.0353(4) 0.0388(4) -0.0139(3) 0.0041(3) -0.0146(3) S5 0.0230(3) 0.0337(4) 0.0546(5) 0.0165(3) -0.0135(3) -0.0142(3) S6 0.0271(3) 0.0271(3) 0.0285(3) 0.0032(2) -0.0116(2) -0.0077(2) O1 0.0235(9) 0.0382(11) 0.0412(12) -0.0101(10) -0.0067(8) 0.0003(8) O2 0.0202(8) 0.0253(8) 0.0210(8) -0.0001(7) -0.0028(6) -0.0057(6) O3 0.0342(10) 0.0350(11) 0.0312(11) 0.0054(9) 0.0018(9) -0.0152(8) O4 0.0231(8) 0.0216(8) 0.0204(8) 0.0014(6) -0.0001(6) -0.0077(6) O5 0.0283(9) 0.0270(9) 0.0246(9) 0.0027(7) -0.0067(7) -0.0099(7) O6 0.0231(8) 0.0229(8) 0.0235(9) 0.0040(7) -0.0065(7) -0.0095(6) O7 0.0536(14) 0.0312(11) 0.0537(15) -0.0068(10) 0.0011(11) -0.0071(10) N1 0.0196(9) 0.0244(10) 0.0266(11) -0.0024(8) -0.0024(8) -0.0052(8) N2 0.0189(9) 0.0221(9) 0.0206(10) 0.0013(8) -0.0027(7) -0.0066(7) N3 0.0251(10) 0.0243(10) 0.0222(10) 0.0020(8) -0.0012(8) -0.0092(8) N4 0.0207(9) 0.0200(9) 0.0231(10) 0.0000(8) -0.0021(8) -0.0056(7) N5 0.0226(9) 0.0205(9) 0.0206(10) 0.0014(8) -0.0030(8) -0.0076(7) N6 0.0191(9) 0.0208(9) 0.0204(10) 0.0003(8) -0.0019(7) -0.0066(7) C1 0.0197(11) 0.0289(12) 0.0379(15) -0.0056(11) 0.0019(10) -0.0093(9) C2 0.0235(12) 0.0335(14) 0.0495(18) -0.0110(13) 0.0029(12) -0.0074(10) C3 0.0309(13) 0.0334(14) 0.0473(18) -0.0179(13) 0.0096(12) -0.0129(11) C4 0.0315(13) 0.0411(15) 0.0335(15) -0.0133(12) 0.0051(11) -0.0189(12) C5 0.0249(12) 0.0321(13) 0.0300(14) -0.0059(11) 0.0033(10) -0.0116(10) C6 0.0206(11) 0.0241(11) 0.0280(13) -0.0045(10) 0.0034(9) -0.0091(9) C7 0.0196(10) 0.0230(11) 0.0222(11) 0.0020(9) -0.0002(9) -0.0089(8) C8 0.0213(10) 0.0259(11) 0.0241(12) 0.0022(9) -0.0050(9) -0.0103(9) C9 0.0487(14) 0.106(3) 0.065(2) -0.0389(19) -0.0180(13) -0.0225(16) C10 0.0487(14) 0.106(3) 0.065(2) -0.0389(19) -0.0180(13) -0.0225(16) C11 0.0232(11) 0.0354(13) 0.0223(12) 0.0049(10) -0.0057(9) -0.0121(10) C12 0.0349(14) 0.0533(18) 0.0232(13) 0.0044(12) -0.0018(11) -0.0229(13) C13 0.0490(18) 0.065(2) 0.0213(14) -0.0078(14) 0.0031(12) -0.0287(16) C14 0.065(2) 0.0489(18) 0.0289(15) -0.0125(14) 0.0079(14) -0.0283(16) C15 0.0479(16) 0.0388(15) 0.0231(13) -0.0028(11) 0.0025(12) -0.0224(13) C16 0.0242(11) 0.0326(13) 0.0200(11) 0.0026(10) -0.0040(9) -0.0112(10) C17 0.0185(10) 0.0250(11) 0.0209(11) 0.0024(9) -0.0038(8) -0.0069(9) C18 0.0167(10) 0.0207(11) 0.0335(13) 0.0012(10) -0.0054(9) -0.0050(8) C19 0.0366(15) 0.0280(14) 0.073(2) -0.0170(15) 0.0090(15) -0.0169(12) C20 0.0297(13) 0.0437(16) 0.059(2) -0.0253(16) 0.0046(13) -0.0197(12) C21 0.0237(11) 0.0217(11) 0.0187(11) -0.0038(9) -0.0007(9) -0.0052(9) C22 0.0341(13) 0.0232(11) 0.0200(11) -0.0004(9) -0.0017(10) -0.0071(10) C23 0.0352(13) 0.0254(12) 0.0310(14) 0.0006(10) 0.0034(11) -0.0154(10) C24 0.0302(12) 0.0287(13) 0.0313(14) -0.0009(11) -0.0028(10) -0.0142(10) C25 0.0249(11) 0.0254(12) 0.0249(12) -0.0011(10) -0.0040(9) -0.0086(9) C26 0.0233(10) 0.0183(10) 0.0190(11) -0.0007(8) -0.0013(8) -0.0068(8) C27 0.0217(10) 0.0176(10) 0.0166(10) -0.0006(8) 0.0000(8) -0.0045(8) C28 0.0223(11) 0.0224(11) 0.0224(12) -0.0005(9) -0.0044(9) -0.0067(9) C29 0.0230(12) 0.0448(17) 0.057(2) 0.0102(15) -0.0142(13) -0.0136(12) C30 0.0265(12) 0.0365(14) 0.0422(16) -0.0026(12) -0.0145(12) -0.0109(11) C31 0.061(2) 0.050(2) 0.045(2) -0.0171(16) -0.0114(17) -0.0033(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr O6 1.9500(18) . ? Cr O4 1.9593(18) . ? Cr O2 1.9631(18) . ? Cr N2 2.045(2) . ? Cr N4 2.048(2) . ? Cr N6 2.079(2) . ? S1 C8 1.751(2) . ? S1 C9 1.777(4) . ? S2 C8 1.737(3) . ? S2 C10 1.819(4) . ? S3 C18 1.744(3) . ? S3 C19 1.814(3) . ? S4 C18 1.742(3) . ? S4 C20 1.812(3) . ? S5 C28 1.744(3) . ? S5 C29 1.819(3) . ? S6 C28 1.752(2) . ? S6 C30 1.810(3) . ? O1 C1 1.354(4) . ? O1 H1O 0.79(4) . ? O2 C7 1.303(3) . ? O3 C11 1.343(3) . ? O3 H3O 0.75(4) . ? O4 C17 1.307(3) . ? O5 C21 1.353(3) . ? O5 H5O 0.88(4) . ? O6 C27 1.297(3) . ? O7 C31 1.409(5) . ? O7 H7 0.8400 . ? N1 C7 1.311(3) . ? N1 N2 1.408(3) . ? N2 C8 1.297(3) . ? N3 C17 1.314(3) . ? N3 N4 1.405(3) . ? N4 C18 1.304(3) . ? N5 C27 1.312(3) . ? N5 N6 1.409(3) . ? N6 C28 1.298(3) . ? C1 C2 1.397(4) . ? C1 C6 1.417(3) . ? C2 C3 1.377(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.398(4) . ? C5 H5 0.9500 . ? C6 C7 1.477(3) . ? C9 C10 1.462(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.396(4) . ? C11 C16 1.415(4) . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? C14 C15 1.390(4) . ? C14 H14 0.9500 . ? C15 C16 1.401(4) . ? C15 H15 0.9500 . ? C16 C17 1.477(4) . ? C19 C20 1.509(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.400(4) . ? C21 C26 1.408(3) . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.403(3) . ? C25 H25 0.9500 . ? C26 C27 1.480(3) . ? C29 C30 1.513(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 Cr O4 93.53(7) . . ? O6 Cr O2 95.38(8) . . ? O4 Cr O2 168.85(7) . . ? O6 Cr N2 89.58(8) . . ? O4 Cr N2 94.47(8) . . ? O2 Cr N2 78.92(8) . . ? O6 Cr N4 172.05(8) . . ? O4 Cr N4 78.72(8) . . ? O2 Cr N4 92.53(8) . . ? N2 Cr N4 92.76(8) . . ? O6 Cr N6 79.11(7) . . ? O4 Cr N6 93.09(8) . . ? O2 Cr N6 95.17(8) . . ? N2 Cr N6 166.75(8) . . ? N4 Cr N6 99.38(8) . . ? C8 S1 C9 95.68(16) . . ? C8 S2 C10 93.87(16) . . ? C18 S3 C19 95.19(14) . . ? C18 S4 C20 93.69(14) . . ? C28 S5 C29 95.41(13) . . ? C28 S6 C30 94.48(13) . . ? C1 O1 H1O 111(3) . . ? C7 O2 Cr 113.46(15) . . ? C11 O3 H3O 112(3) . . ? C17 O4 Cr 113.55(15) . . ? C21 O5 H5O 108(2) . . ? C27 O6 Cr 113.73(15) . . ? C31 O7 H7 109.5 . . ? C7 N1 N2 111.72(19) . . ? C8 N2 N1 112.28(19) . . ? C8 N2 Cr 134.98(17) . . ? N1 N2 Cr 112.12(14) . . ? C17 N3 N4 111.7(2) . . ? C18 N4 N3 112.8(2) . . ? C18 N4 Cr 135.32(19) . . ? N3 N4 Cr 111.91(15) . . ? C27 N5 N6 111.93(19) . . ? C28 N6 N5 111.95(19) . . ? C28 N6 Cr 137.14(17) . . ? N5 N6 Cr 110.85(14) . . ? O1 C1 C2 117.2(2) . . ? O1 C1 C6 123.1(2) . . ? C2 C1 C6 119.7(3) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.3(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.3(2) . . ? C5 C6 C7 120.2(2) . . ? C1 C6 C7 121.4(2) . . ? O2 C7 N1 122.9(2) . . ? O2 C7 C6 120.1(2) . . ? N1 C7 C6 117.1(2) . . ? N2 C8 S2 123.36(18) . . ? N2 C8 S1 120.27(19) . . ? S2 C8 S1 116.35(14) . . ? C10 C9 S1 109.7(3) . . ? C10 C9 H9A 109.7 . . ? S1 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? S1 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 S2 112.1(3) . . ? C9 C10 H10A 109.2 . . ? S2 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? S2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O3 C11 C12 117.2(2) . . ? O3 C11 C16 123.5(2) . . ? C12 C11 C16 119.3(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 118.6(2) . . ? C15 C16 C17 119.9(2) . . ? C11 C16 C17 121.5(2) . . ? O4 C17 N3 122.4(2) . . ? O4 C17 C16 119.8(2) . . ? N3 C17 C16 117.8(2) . . ? N4 C18 S4 123.4(2) . . ? N4 C18 S3 120.4(2) . . ? S4 C18 S3 116.11(14) . . ? C20 C19 S3 107.1(2) . . ? C20 C19 H19A 110.3 . . ? S3 C19 H19A 110.3 . . ? C20 C19 H19B 110.3 . . ? S3 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 S4 108.0(2) . . ? C19 C20 H20A 110.1 . . ? S4 C20 H20A 110.1 . . ? C19 C20 H20B 110.1 . . ? S4 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O5 C21 C22 117.0(2) . . ? O5 C21 C26 123.1(2) . . ? C22 C21 C26 119.9(2) . . ? C23 C22 C21 120.3(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.5(2) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 121.2(2) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 118.6(2) . . ? C25 C26 C27 119.5(2) . . ? C21 C26 C27 121.9(2) . . ? O6 C27 N5 123.7(2) . . ? O6 C27 C26 119.2(2) . . ? N5 C27 C26 117.1(2) . . ? N6 C28 S5 123.11(18) . . ? N6 C28 S6 121.28(19) . . ? S5 C28 S6 115.57(13) . . ? C30 C29 S5 107.2(2) . . ? C30 C29 H29A 110.3 . . ? S5 C29 H29A 110.3 . . ? C30 C29 H29B 110.3 . . ? S5 C29 H29B 110.3 . . ? H29A C29 H29B 108.5 . . ? C29 C30 S6 108.02(19) . . ? C29 C30 H30A 110.1 . . ? S6 C30 H30A 110.1 . . ? C29 C30 H30B 110.1 . . ? S6 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? O7 C31 H31A 109.5 . . ? O7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.71 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.536 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.182 # Attachment 'complex_2a.cif' data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 712217' #TrackingRef 'complex_2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H42 Cr2 N8 O10 S8, C H4 O, C H2 CL2' _chemical_formula_sum 'C44 H48 Cl2 Cr2 N8 O11 S8' _chemical_formula_weight 1296.28 _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' Cr Cr 0.3209 0.6236 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.7350(3) _cell_length_b 15.7800(3) _cell_length_c 21.3140(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.4720(10) _cell_angle_gamma 90.00 _cell_volume 5424.59(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32140 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _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 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.872 _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 43151 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 30.03 _reflns_number_total 15835 _reflns_number_gt 12640 _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^)+(0.1142P)^2^+8.0156P] 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 15835 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.2125 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Cr1 Cr 0.63568(3) 0.09918(3) 0.85128(2) 0.01726(11) Uani 1 1 d . . . Cr2 Cr 0.53893(3) 0.00739(3) 0.73023(2) 0.01782(11) Uani 1 1 d . . . S1 S 0.92451(5) 0.11003(5) 0.94891(4) 0.02753(17) Uani 1 1 d . . . S2 S 0.70091(5) -0.14547(5) 0.81283(4) 0.02762(17) Uani 1 1 d . . . S3 S 0.56922(6) -0.27063(6) 0.81343(5) 0.0397(2) Uani 1 1 d . . . S4 S 0.61798(8) 0.10664(7) 1.02369(4) 0.0438(3) Uani 1 1 d . . . S6 S 0.58148(6) 0.29022(6) 1.00607(4) 0.03179(19) Uani 1 1 d . . . S7 S 0.82033(5) 0.22951(5) 0.85456(4) 0.02773(17) Uani 1 1 d . . . S8 S 0.45216(6) 0.23315(6) 0.58389(4) 0.03227(19) Uani 1 1 d . . . S9 S 0.41013(6) 0.20081(6) 0.70821(4) 0.0332(2) Uani 1 1 d . . . O1 O 0.5493(2) 0.42650(18) 0.86715(14) 0.0464(7) Uani 1 1 d . . . HO1 H 0.5542 0.3782 0.8844 0.070 Uiso 1 1 calc . . . O2 O 0.63445(13) 0.20174(13) 0.79958(10) 0.0204(4) Uani 1 1 d . . . O3 O 0.86000(17) -0.1267(2) 0.97044(18) 0.0509(8) Uani 1 1 d . . . HO3 H 0.8486 -0.0839 0.9463 0.076 Uiso 1 1 calc . . . O4 O 0.63705(13) 0.00367(14) 0.90936(10) 0.0207(4) Uani 1 1 d . . . O5 O 0.56307(17) 0.10667(19) 0.49215(12) 0.0375(6) Uani 1 1 d . . . H5O H 0.5465 0.1201 0.5247 0.056 Uiso 1 1 calc . . . O6 O 0.57959(14) -0.03875(14) 0.65886(10) 0.0225(4) Uani 1 1 d . . . O7 O 0.3490(2) -0.2662(2) 0.74805(16) 0.0508(8) Uani 1 1 d . . . H7 H 0.3972 -0.2461 0.7566 0.076 Uiso 1 1 calc . . . O8 O 0.42109(14) -0.02280(16) 0.69980(11) 0.0265(5) Uani 1 1 d . . . O9 O 0.65335(12) 0.03210(13) 0.77929(10) 0.0192(4) Uani 1 1 d . . . O10 O 0.52103(12) 0.07199(14) 0.80470(9) 0.0195(4) Uani 1 1 d . . . O11 O 0.5233(3) 0.5799(2) 0.92529(17) 0.0596(9) Uani 1 1 d . . . H11 H 0.5183 0.5362 0.9022 0.089 Uiso 1 1 calc . . . N1 N 0.76051(16) 0.09307(16) 0.90055(12) 0.0214(5) Uani 1 1 d . . . N2 N 0.77907(16) 0.01860(18) 0.93829(14) 0.0263(5) Uani 1 1 d . . . N3 N 0.60763(16) 0.19041(17) 0.91248(12) 0.0218(5) Uani 1 1 d . . . N4 N 0.59057(17) 0.26916(17) 0.88032(13) 0.0239(5) Uani 1 1 d . . . N5 N 0.51649(16) 0.10742(17) 0.66470(12) 0.0216(5) Uani 1 1 d . . . N6 N 0.55505(17) 0.09457(17) 0.61369(12) 0.0241(5) Uani 1 1 d . . . N7 N 0.53880(16) -0.11357(17) 0.76823(12) 0.0223(5) Uani 1 1 d . . . N8 N 0.45785(17) -0.14693(19) 0.75734(13) 0.0275(6) Uani 1 1 d . . . C1 C 0.5642(2) 0.4214(2) 0.80761(19) 0.0344(7) Uani 1 1 d . . . C2 C 0.5514(3) 0.4939(2) 0.7693(2) 0.0478(10) Uani 1 1 d . . . H2 H 0.5339 0.5450 0.7852 0.057 Uiso 1 1 calc . . . C3 C 0.5644(3) 0.4913(3) 0.7077(3) 0.0488(11) Uani 1 1 d . . . H3 H 0.5567 0.5414 0.6820 0.059 Uiso 1 1 calc . . . C4 C 0.5881(3) 0.4176(3) 0.6830(2) 0.0438(9) Uani 1 1 d . . . H4 H 0.5948 0.4165 0.6402 0.053 Uiso 1 1 calc . . . C5 C 0.6019(2) 0.3450(2) 0.72107(18) 0.0317(7) Uani 1 1 d . . . H5 H 0.6188 0.2943 0.7042 0.038 Uiso 1 1 calc . . . C6 C 0.59121(19) 0.3457(2) 0.78426(16) 0.0251(6) Uani 1 1 d . . . C7 C 0.60643(18) 0.26751(19) 0.82269(14) 0.0211(5) Uani 1 1 d . . . C8 C 0.60328(19) 0.1947(2) 0.97265(15) 0.0248(6) Uani 1 1 d . . . C9 C 0.5748(5) 0.2454(4) 1.0823(2) 0.077(2) Uani 1 1 d . . . H9A H 0.5991 0.2856 1.1180 0.092 Uiso 1 1 calc . . . H9B H 0.5158 0.2370 1.0811 0.092 Uiso 1 1 calc . . . C10 C 0.6175(4) 0.1659(3) 1.0955(2) 0.0622(15) Uani 1 1 d . . . H10A H 0.5910 0.1311 1.1230 0.075 Uiso 1 1 calc . . . H10B H 0.6755 0.1765 1.1206 0.075 Uiso 1 1 calc . . . C11 C 0.7914(2) -0.1511(2) 0.9890(2) 0.0355(8) Uani 1 1 d . . . C12 C 0.7942(2) -0.2295(3) 1.0203(2) 0.0402(9) Uani 1 1 d . . . H12 H 0.8423 -0.2640 1.0273 0.048 Uiso 1 1 calc . . . C13 C 0.7271(2) -0.2568(3) 1.04114(19) 0.0366(8) Uani 1 1 d . . . H13 H 0.7301 -0.3091 1.0638 0.044 Uiso 1 1 calc . . . C14 C 0.6551(2) -0.2082(2) 1.02917(17) 0.0323(7) Uani 1 1 d . . . H14 H 0.6093 -0.2272 1.0439 0.039 Uiso 1 1 calc . . . C15 C 0.6503(2) -0.1322(2) 0.99581(16) 0.0283(6) Uani 1 1 d . . . H15 H 0.6003 -0.1004 0.9861 0.034 Uiso 1 1 calc . . . C16 C 0.7186(2) -0.1021(2) 0.97629(16) 0.0267(6) Uani 1 1 d . . . C17 C 0.71045(18) -0.0220(2) 0.93929(15) 0.0232(6) Uani 1 1 d . . . C18 C 0.82583(18) 0.13796(19) 0.90137(14) 0.0215(5) Uani 1 1 d . . . C19 C 0.9230(2) 0.2671(2) 0.8995(2) 0.0375(8) Uani 1 1 d . . . H19A H 0.9454 0.3063 0.8721 0.045 Uiso 1 1 calc . . . H19B H 0.9193 0.2980 0.9391 0.045 Uiso 1 1 calc . . . C20 C 0.9782(2) 0.1929(3) 0.9178(2) 0.0393(9) Uani 1 1 d . . . H20A H 1.0290 0.2094 0.9515 0.047 Uiso 1 1 calc . . . H20B H 0.9947 0.1720 0.8793 0.047 Uiso 1 1 calc . . . C21 C 0.6152(2) 0.0402(2) 0.50732(15) 0.0267(6) Uani 1 1 d . . . C22 C 0.6546(2) 0.0136(3) 0.46059(16) 0.0344(8) Uani 1 1 d . . . H22 H 0.6427 0.0410 0.4194 0.041 Uiso 1 1 calc . . . C23 C 0.7110(2) -0.0525(3) 0.47409(19) 0.0383(8) Uani 1 1 d . . . H23 H 0.7376 -0.0700 0.4421 0.046 Uiso 1 1 calc . . . C24 C 0.7291(3) -0.0934(3) 0.53360(19) 0.0365(8) Uani 1 1 d . . . H24 H 0.7691 -0.1375 0.5431 0.044 Uiso 1 1 calc . . . C25 C 0.6879(2) -0.0692(2) 0.57921(16) 0.0297(7) Uani 1 1 d . . . H25 H 0.6995 -0.0978 0.6198 0.036 Uiso 1 1 calc . . . C26 C 0.62978(19) -0.0035(2) 0.56675(14) 0.0225(6) Uani 1 1 d . . . C27 C 0.58498(18) 0.0178(2) 0.61585(14) 0.0209(5) Uani 1 1 d . . . C28 C 0.4672(2) 0.1717(2) 0.65426(14) 0.0248(6) Uani 1 1 d . . . C29 C 0.3639(3) 0.2904(3) 0.5962(2) 0.0445(10) Uani 1 1 d . . . H29A H 0.3592 0.3463 0.5744 0.053 Uiso 1 1 calc . . . H29B H 0.3123 0.2583 0.5774 0.053 Uiso 1 1 calc . . . C30 C 0.3765(3) 0.3017(3) 0.66793(19) 0.0402(9) Uani 1 1 d . . . H30A H 0.3240 0.3200 0.6769 0.048 Uiso 1 1 calc . . . H30B H 0.4189 0.3458 0.6846 0.048 Uiso 1 1 calc . . . C31 C 0.2934(2) -0.2059(3) 0.71824(17) 0.0368(8) Uani 1 1 d . . . C32 C 0.2093(3) -0.2297(3) 0.6999(2) 0.0468(11) Uani 1 1 d . . . H32 H 0.1939 -0.2861 0.7069 0.056 Uiso 1 1 calc . . . C33 C 0.1495(2) -0.1712(4) 0.6717(2) 0.0515(13) Uani 1 1 d . . . H33 H 0.0929 -0.1877 0.6601 0.062 Uiso 1 1 calc . . . C34 C 0.1699(2) -0.0897(4) 0.6601(2) 0.0489(11) Uani 1 1 d . . . H34 H 0.1276 -0.0501 0.6412 0.059 Uiso 1 1 calc . . . C35 C 0.2533(2) -0.0652(3) 0.67621(17) 0.0401(9) Uani 1 1 d . . . H35 H 0.2677 -0.0091 0.6672 0.048 Uiso 1 1 calc . . . C36 C 0.3155(2) -0.1228(3) 0.70539(15) 0.0317(7) Uani 1 1 d . . . C37 C 0.4031(2) -0.0951(2) 0.72170(14) 0.0259(6) Uani 1 1 d . . . C38 C 0.5953(2) -0.1681(2) 0.79480(14) 0.0241(6) Uani 1 1 d . . . C39 C 0.6723(3) -0.2986(2) 0.8613(2) 0.0416(9) Uani 1 1 d . . . H39A H 0.6803 -0.2805 0.9070 0.050 Uiso 1 1 calc . . . H39B H 0.6800 -0.3608 0.8607 0.050 Uiso 1 1 calc . . . C40 C 0.7347(3) -0.2544(2) 0.8321(2) 0.0374(8) Uani 1 1 d . . . H40A H 0.7384 -0.2843 0.7921 0.045 Uiso 1 1 calc . . . H40B H 0.7902 -0.2551 0.8635 0.045 Uiso 1 1 calc . . . C41 C 0.7203(2) 0.0455(2) 0.75078(16) 0.0268(6) Uani 1 1 d . . . H41A H 0.7147 0.1014 0.7300 0.040 Uiso 1 1 calc . . . H41B H 0.7194 0.0016 0.7181 0.040 Uiso 1 1 calc . . . H41C H 0.7730 0.0427 0.7847 0.040 Uiso 1 1 calc . . . C42 C 0.4589(2) 0.0584(3) 0.83799(16) 0.0300(7) Uani 1 1 d . . . H42A H 0.4753 0.0109 0.8684 0.045 Uiso 1 1 calc . . . H42B H 0.4062 0.0451 0.8064 0.045 Uiso 1 1 calc . . . H42C H 0.4526 0.1096 0.8622 0.045 Uiso 1 1 calc . . . C43 C 0.5858(3) 0.5670(3) 0.9837(3) 0.0561(12) Uani 1 1 d . . . H43A H 0.6156 0.6203 0.9972 0.084 Uiso 1 1 calc . . . H43B H 0.6247 0.5238 0.9768 0.084 Uiso 1 1 calc . . . H43C H 0.5605 0.5479 1.0178 0.084 Uiso 1 1 calc . . . Cl1 Cl 0.75651(19) -0.00584(18) 1.17500(19) 0.1442(13) Uani 1 1 d . . . Cl2 Cl 0.87814(11) -0.01820(12) 1.10412(9) 0.0805(5) Uani 1 1 d . . . C44 C 0.8187(6) -0.0705(6) 1.1486(4) 0.100(2) Uiso 1 1 d . . . H44A H 0.7849 -0.1147 1.1209 0.120 Uiso 1 1 calc . . . H44B H 0.8564 -0.0990 1.1865 0.120 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 Cr1 0.0172(2) 0.0166(2) 0.0169(2) 0.00033(15) 0.00275(16) 0.00075(16) Cr2 0.0181(2) 0.0193(2) 0.0165(2) -0.00103(16) 0.00531(16) -0.00108(16) S1 0.0196(3) 0.0269(4) 0.0316(4) 0.0057(3) -0.0011(3) -0.0031(3) S2 0.0262(4) 0.0208(4) 0.0376(4) 0.0030(3) 0.0115(3) 0.0016(3) S3 0.0404(5) 0.0218(4) 0.0554(6) 0.0083(4) 0.0103(4) -0.0068(4) S4 0.0758(7) 0.0348(5) 0.0252(4) 0.0042(3) 0.0211(4) 0.0102(5) S6 0.0393(4) 0.0316(4) 0.0276(4) -0.0068(3) 0.0144(3) 0.0015(4) S7 0.0246(3) 0.0199(3) 0.0339(4) 0.0072(3) -0.0005(3) -0.0044(3) S8 0.0393(4) 0.0331(4) 0.0257(4) 0.0076(3) 0.0109(3) 0.0122(4) S9 0.0384(4) 0.0347(4) 0.0311(4) 0.0061(3) 0.0173(3) 0.0154(4) O1 0.074(2) 0.0251(13) 0.0394(14) -0.0046(11) 0.0138(14) 0.0144(14) O2 0.0233(10) 0.0180(9) 0.0202(9) 0.0008(7) 0.0062(7) 0.0021(8) O3 0.0245(12) 0.0462(17) 0.082(2) 0.0362(16) 0.0146(13) 0.0056(12) O4 0.0184(9) 0.0213(10) 0.0218(9) 0.0043(8) 0.0044(7) 0.0009(8) O5 0.0371(13) 0.0512(17) 0.0273(11) 0.0146(11) 0.0140(10) 0.0184(12) O6 0.0297(11) 0.0193(10) 0.0206(9) -0.0008(8) 0.0103(8) -0.0007(8) O7 0.0501(18) 0.0484(18) 0.0508(17) 0.0050(14) 0.0080(14) -0.0217(15) O8 0.0210(10) 0.0348(13) 0.0219(10) -0.0015(9) 0.0025(8) -0.0045(9) O9 0.0174(9) 0.0197(10) 0.0214(9) -0.0013(7) 0.0068(7) -0.0007(8) O10 0.0159(9) 0.0241(10) 0.0185(9) -0.0018(8) 0.0048(7) 0.0002(8) O11 0.082(3) 0.0374(17) 0.0536(19) -0.0081(14) 0.0087(18) 0.0172(17) N1 0.0193(11) 0.0189(11) 0.0239(11) 0.0037(9) 0.0023(9) -0.0019(9) N2 0.0206(12) 0.0241(13) 0.0312(13) 0.0120(11) 0.0018(10) -0.0012(10) N3 0.0239(11) 0.0209(12) 0.0196(11) -0.0012(9) 0.0039(9) 0.0016(10) N4 0.0273(12) 0.0202(12) 0.0233(11) -0.0012(9) 0.0053(10) 0.0041(10) N5 0.0231(11) 0.0235(12) 0.0194(11) -0.0001(9) 0.0077(9) 0.0029(10) N6 0.0291(13) 0.0252(13) 0.0211(11) 0.0029(9) 0.0116(10) 0.0041(10) N7 0.0233(11) 0.0231(12) 0.0217(11) -0.0014(9) 0.0081(9) -0.0079(10) N8 0.0238(12) 0.0317(14) 0.0276(12) -0.0010(11) 0.0081(10) -0.0108(11) C1 0.0396(19) 0.0209(15) 0.0397(18) -0.0014(13) 0.0053(15) 0.0026(14) C2 0.061(3) 0.0199(17) 0.059(3) 0.0054(16) 0.010(2) 0.0055(17) C3 0.051(2) 0.030(2) 0.064(3) 0.0238(19) 0.014(2) 0.0034(18) C4 0.044(2) 0.044(2) 0.048(2) 0.0212(18) 0.0194(18) 0.0051(18) C5 0.0295(16) 0.0300(17) 0.0387(17) 0.0101(14) 0.0144(13) 0.0048(13) C6 0.0221(13) 0.0207(14) 0.0312(15) 0.0026(12) 0.0046(11) 0.0006(11) C7 0.0178(12) 0.0204(13) 0.0239(13) 0.0002(10) 0.0035(10) 0.0005(10) C8 0.0248(14) 0.0272(15) 0.0224(13) -0.0034(11) 0.0061(11) -0.0015(12) C9 0.145(6) 0.064(3) 0.033(2) 0.005(2) 0.042(3) 0.038(4) C10 0.120(5) 0.046(3) 0.0255(18) -0.0006(17) 0.028(2) 0.000(3) C11 0.0227(15) 0.0319(18) 0.049(2) 0.0173(16) 0.0048(14) -0.0026(13) C12 0.0241(15) 0.0337(19) 0.058(2) 0.0229(17) 0.0025(15) 0.0037(14) C13 0.0317(17) 0.0331(18) 0.0402(18) 0.0184(15) 0.0015(14) -0.0050(15) C14 0.0266(15) 0.0348(18) 0.0350(16) 0.0104(14) 0.0073(13) -0.0070(14) C15 0.0230(14) 0.0306(16) 0.0304(15) 0.0059(13) 0.0054(12) -0.0029(12) C16 0.0226(13) 0.0258(15) 0.0293(15) 0.0103(12) 0.0024(11) -0.0009(12) C17 0.0207(13) 0.0237(14) 0.0237(13) 0.0055(11) 0.0035(10) -0.0001(11) C18 0.0216(13) 0.0183(13) 0.0230(13) -0.0009(10) 0.0031(10) -0.0019(11) C19 0.0290(16) 0.0277(17) 0.049(2) 0.0015(15) -0.0012(15) -0.0074(14) C20 0.0239(15) 0.036(2) 0.052(2) 0.0129(17) 0.0007(14) -0.0105(14) C21 0.0237(14) 0.0341(17) 0.0229(13) 0.0019(12) 0.0073(11) 0.0007(13) C22 0.0351(17) 0.047(2) 0.0246(15) 0.0040(14) 0.0143(13) 0.0030(16) C23 0.0375(19) 0.047(2) 0.0371(18) -0.0062(16) 0.0214(15) 0.0033(17) C24 0.0408(19) 0.0359(19) 0.0385(18) 0.0011(15) 0.0204(16) 0.0101(16) C25 0.0341(16) 0.0296(16) 0.0284(15) 0.0025(13) 0.0135(13) 0.0063(14) C26 0.0241(13) 0.0239(14) 0.0215(13) -0.0022(11) 0.0093(11) -0.0032(11) C27 0.0214(12) 0.0237(14) 0.0190(12) 0.0004(10) 0.0076(10) 0.0002(11) C28 0.0263(14) 0.0264(15) 0.0214(13) 0.0000(11) 0.0062(11) 0.0016(12) C29 0.047(2) 0.049(2) 0.041(2) 0.0122(18) 0.0169(17) 0.0223(19) C30 0.047(2) 0.038(2) 0.0382(19) 0.0040(16) 0.0154(16) 0.0194(18) C31 0.0334(17) 0.052(2) 0.0273(15) -0.0080(15) 0.0130(13) -0.0181(17) C32 0.036(2) 0.071(3) 0.0352(18) -0.0095(19) 0.0143(15) -0.028(2) C33 0.0273(18) 0.094(4) 0.0361(19) -0.009(2) 0.0132(15) -0.023(2) C34 0.0252(17) 0.083(4) 0.0366(19) -0.006(2) 0.0053(14) -0.004(2) C35 0.0275(16) 0.065(3) 0.0281(16) -0.0018(17) 0.0070(13) -0.0073(18) C36 0.0235(14) 0.051(2) 0.0208(13) -0.0065(14) 0.0068(11) -0.0119(15) C37 0.0259(14) 0.0347(17) 0.0179(12) -0.0049(11) 0.0074(11) -0.0093(13) C38 0.0304(15) 0.0197(13) 0.0237(13) -0.0007(11) 0.0100(11) -0.0044(12) C39 0.047(2) 0.0257(17) 0.050(2) 0.0126(16) 0.0087(17) 0.0024(16) C40 0.0408(19) 0.0256(17) 0.047(2) 0.0057(15) 0.0135(16) 0.0088(15) C41 0.0228(13) 0.0271(15) 0.0338(15) -0.0018(12) 0.0136(12) -0.0027(12) C42 0.0215(14) 0.044(2) 0.0273(14) -0.0014(14) 0.0122(11) -0.0015(14) C43 0.054(3) 0.043(2) 0.070(3) -0.011(2) 0.013(2) 0.002(2) Cl1 0.144(2) 0.1069(18) 0.230(3) -0.049(2) 0.134(2) -0.0261(16) Cl2 0.0721(9) 0.0833(11) 0.0890(11) -0.0258(9) 0.0267(8) -0.0153(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 Cr1 O4 1.947(2) . ? Cr1 O9 1.950(2) . ? Cr1 O2 1.955(2) . ? Cr1 O10 1.958(2) . ? Cr1 N1 2.075(3) . ? Cr1 N3 2.079(3) . ? Cr2 O9 1.961(2) . ? Cr2 O8 1.963(2) . ? Cr2 O6 1.964(2) . ? Cr2 O10 1.975(2) . ? Cr2 N7 2.074(3) . ? Cr2 N5 2.075(3) . ? S1 C18 1.748(3) . ? S1 C20 1.810(4) . ? S2 C38 1.743(3) . ? S2 C40 1.822(4) . ? S3 C38 1.749(3) . ? S3 C39 1.809(4) . ? S4 C8 1.742(3) . ? S4 C10 1.795(4) . ? S6 C8 1.746(3) . ? S6 C9 1.803(5) . ? S7 C18 1.744(3) . ? S7 C19 1.829(4) . ? S8 C28 1.747(3) . ? S8 C29 1.809(4) . ? S9 C28 1.741(3) . ? S9 C30 1.826(4) . ? O1 C1 1.359(5) . ? O1 HO1 0.8400 . ? O2 C7 1.290(4) . ? O3 C11 1.365(4) . ? O3 HO3 0.8400 . ? O4 C17 1.289(4) . ? O5 C21 1.348(4) . ? O5 H5O 0.8400 . ? O6 C27 1.300(4) . ? O7 C31 1.364(6) . ? O7 H7 0.8400 . ? O8 C37 1.298(4) . ? O9 C41 1.426(4) . ? O10 C42 1.422(4) . ? O11 C43 1.412(6) . ? O11 H11 0.8400 . ? N1 C18 1.299(4) . ? N1 N2 1.411(3) . ? N2 C17 1.320(4) . ? N3 C8 1.306(4) . ? N3 N4 1.411(4) . ? N4 C7 1.324(4) . ? N5 C28 1.289(4) . ? N5 N6 1.419(3) . ? N6 C27 1.307(4) . ? N7 C38 1.292(4) . ? N7 N8 1.414(4) . ? N8 C37 1.310(5) . ? C1 C2 1.389(5) . ? C1 C6 1.414(5) . ? C2 C3 1.387(7) . ? C2 H2 0.9500 . ? C3 C4 1.378(7) . ? C3 H3 0.9500 . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.405(5) . ? C5 H5 0.9500 . ? C6 C7 1.465(4) . ? C9 C10 1.434(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.402(5) . ? C11 C16 1.408(5) . ? C12 C13 1.382(5) . ? C12 H12 0.9500 . ? C13 C14 1.393(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(5) . ? C14 H14 0.9500 . ? C15 C16 1.400(4) . ? C15 H15 0.9500 . ? C16 C17 1.477(4) . ? C19 C20 1.478(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.398(5) . ? C21 C26 1.405(4) . ? C22 C23 1.384(6) . ? C22 H22 0.9500 . ? C23 C24 1.383(6) . ? C23 H23 0.9500 . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 C26 1.397(5) . ? C25 H25 0.9500 . ? C26 C27 1.480(4) . ? C29 C30 1.498(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.407(5) . ? C31 C36 1.409(6) . ? C32 C33 1.376(8) . ? C32 H32 0.9500 . ? C33 C34 1.370(8) . ? C33 H33 0.9500 . ? C34 C35 1.401(5) . ? C34 H34 0.9500 . ? C35 C36 1.397(6) . ? C35 H35 0.9500 . ? C36 C37 1.479(4) . ? C39 C40 1.521(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? Cl1 C44 1.659(9) . ? Cl2 C44 1.753(9) . ? C44 H44A 0.9900 . ? C44 H44B 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 Cr1 O9 95.83(9) . . ? O4 Cr1 O2 174.86(9) . . ? O9 Cr1 O2 89.25(9) . . ? O4 Cr1 O10 89.80(9) . . ? O9 Cr1 O10 79.39(8) . . ? O2 Cr1 O10 91.95(9) . . ? O4 Cr1 N1 78.62(9) . . ? O9 Cr1 N1 91.69(10) . . ? O2 Cr1 N1 100.46(10) . . ? O10 Cr1 N1 164.66(10) . . ? O4 Cr1 N3 95.94(10) . . ? O9 Cr1 N3 167.56(10) . . ? O2 Cr1 N3 79.06(9) . . ? O10 Cr1 N3 96.61(9) . . ? N1 Cr1 N3 94.59(10) . . ? O9 Cr2 O8 167.57(9) . . ? O9 Cr2 O6 89.77(9) . . ? O8 Cr2 O6 100.32(10) . . ? O9 Cr2 O10 78.74(8) . . ? O8 Cr2 O10 92.08(9) . . ? O6 Cr2 O10 166.30(9) . . ? O9 Cr2 N7 94.44(10) . . ? O8 Cr2 N7 78.47(10) . . ? O6 Cr2 N7 89.88(10) . . ? O10 Cr2 N7 98.34(10) . . ? O9 Cr2 N5 100.57(10) . . ? O8 Cr2 N5 88.67(10) . . ? O6 Cr2 N5 78.38(10) . . ? O10 Cr2 N5 96.27(9) . . ? N7 Cr2 N5 160.81(10) . . ? C18 S1 C20 95.17(16) . . ? C38 S2 C40 95.27(17) . . ? C38 S3 C39 95.51(17) . . ? C8 S4 C10 94.88(19) . . ? C8 S6 C9 95.7(2) . . ? C18 S7 C19 94.02(16) . . ? C28 S8 C29 95.12(17) . . ? C28 S9 C30 94.26(17) . . ? C1 O1 HO1 109.5 . . ? C7 O2 Cr1 113.64(18) . . ? C11 O3 HO3 109.5 . . ? C17 O4 Cr1 113.92(19) . . ? C21 O5 H5O 109.5 . . ? C27 O6 Cr2 113.27(19) . . ? C31 O7 H7 109.5 . . ? C37 O8 Cr2 113.8(2) . . ? C41 O9 Cr1 123.77(19) . . ? C41 O9 Cr2 124.69(18) . . ? Cr1 O9 Cr2 101.31(9) . . ? C42 O10 Cr1 121.84(18) . . ? C42 O10 Cr2 127.6(2) . . ? Cr1 O10 Cr2 100.51(9) . . ? C43 O11 H11 109.5 . . ? C18 N1 N2 113.0(2) . . ? C18 N1 Cr1 135.4(2) . . ? N2 N1 Cr1 111.47(18) . . ? C17 N2 N1 110.7(2) . . ? C8 N3 N4 112.0(3) . . ? C8 N3 Cr1 137.2(2) . . ? N4 N3 Cr1 110.81(18) . . ? C7 N4 N3 111.6(2) . . ? C28 N5 N6 112.4(2) . . ? C28 N5 Cr2 135.0(2) . . ? N6 N5 Cr2 111.67(18) . . ? C27 N6 N5 110.7(2) . . ? C38 N7 N8 112.4(3) . . ? C38 N7 Cr2 135.0(2) . . ? N8 N7 Cr2 112.3(2) . . ? C37 N8 N7 110.8(3) . . ? O1 C1 C2 117.5(4) . . ? O1 C1 C6 122.3(3) . . ? C2 C1 C6 120.2(4) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C7 118.8(3) . . ? C1 C6 C7 122.6(3) . . ? O2 C7 N4 123.6(3) . . ? O2 C7 C6 119.4(3) . . ? N4 C7 C6 117.0(3) . . ? N3 C8 S4 122.4(3) . . ? N3 C8 S6 121.2(3) . . ? S4 C8 S6 116.36(17) . . ? C10 C9 S6 111.8(3) . . ? C10 C9 H9A 109.2 . . ? S6 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? S6 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 S4 113.8(3) . . ? C9 C10 H10A 108.8 . . ? S4 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? S4 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O3 C11 C12 117.6(3) . . ? O3 C11 C16 122.8(3) . . ? C12 C11 C16 119.6(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 119.3(3) . . ? C15 C16 C17 118.9(3) . . ? C11 C16 C17 121.7(3) . . ? O4 C17 N2 124.0(3) . . ? O4 C17 C16 118.2(3) . . ? N2 C17 C16 117.8(3) . . ? N1 C18 S7 121.9(2) . . ? N1 C18 S1 122.1(2) . . ? S7 C18 S1 115.97(17) . . ? C20 C19 S7 108.3(3) . . ? C20 C19 H19A 110.0 . . ? S7 C19 H19A 110.0 . . ? C20 C19 H19B 110.0 . . ? S7 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 S1 109.4(3) . . ? C19 C20 H20A 109.8 . . ? S1 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? S1 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? O5 C21 C22 117.4(3) . . ? O5 C21 C26 122.9(3) . . ? C22 C21 C26 119.6(3) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 121.5(3) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C21 118.7(3) . . ? C25 C26 C27 119.5(3) . . ? C21 C26 C27 121.8(3) . . ? O6 C27 N6 124.3(3) . . ? O6 C27 C26 119.1(3) . . ? N6 C27 C26 116.6(3) . . ? N5 C28 S9 122.2(2) . . ? N5 C28 S8 121.6(2) . . ? S9 C28 S8 116.24(19) . . ? C30 C29 S8 108.1(3) . . ? C30 C29 H29A 110.1 . . ? S8 C29 H29A 110.1 . . ? C30 C29 H29B 110.1 . . ? S8 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? C29 C30 S9 108.5(3) . . ? C29 C30 H30A 110.0 . . ? S9 C30 H30A 110.0 . . ? C29 C30 H30B 110.0 . . ? S9 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? O7 C31 C32 116.8(4) . . ? O7 C31 C36 123.9(3) . . ? C32 C31 C36 119.3(4) . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 121.4(4) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 119.7(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.4(4) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 119.3(3) . . ? C35 C36 C37 119.1(4) . . ? C31 C36 C37 121.6(4) . . ? O8 C37 N8 124.3(3) . . ? O8 C37 C36 119.1(3) . . ? N8 C37 C36 116.6(3) . . ? N7 C38 S2 122.7(2) . . ? N7 C38 S3 121.2(2) . . ? S2 C38 S3 116.07(19) . . ? C40 C39 S3 108.2(3) . . ? C40 C39 H39A 110.1 . . ? S3 C39 H39A 110.1 . . ? C40 C39 H39B 110.1 . . ? S3 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? C39 C40 S2 108.6(3) . . ? C39 C40 H40A 110.0 . . ? S2 C40 H40A 110.0 . . ? C39 C40 H40B 110.0 . . ? S2 C40 H40B 110.0 . . ? H40A C40 H40B 108.3 . . ? O9 C41 H41A 109.5 . . ? O9 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O9 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O10 C42 H42A 109.5 . . ? O10 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O10 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O11 C43 H43A 109.5 . . ? O11 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O11 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Cl1 C44 Cl2 113.1(5) . . ? Cl1 C44 H44A 109.0 . . ? Cl2 C44 H44A 109.0 . . ? Cl1 C44 H44B 109.0 . . ? Cl2 C44 H44B 109.0 . . ? H44A C44 H44B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.406 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.225 # Attachment 'complex_2b.cif' data_complex_2b _database_code_depnum_ccdc_archive 'CCDC 760990' #TrackingRef 'complex_2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H50 Cr2 N8 O10 S8' _chemical_formula_sum 'C46 H50 Cr2 N8 O10 S8' _chemical_formula_weight 1235.42 _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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 23.3019(12) _cell_length_b 10.3977(6) _cell_length_c 22.5974(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5475.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14103 _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 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.764 _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 17872 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.1485 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5992 _reflns_number_gt 3248 _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^)+(0.0819P)^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 -0.09(4) _refine_ls_number_reflns 5992 _refine_ls_number_parameters 330 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1494 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.000 _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 Cr1 Cr -0.5000 1.0000 -0.34938(6) 0.0283(4) Uani 1 2 d S . . Cr2 Cr -0.5000 1.0000 -0.48308(6) 0.0310(4) Uani 1 2 d S . . S2 S -0.60639(8) 0.8536(2) -0.24930(9) 0.0461(5) Uani 1 1 d . . . S3 S -0.56018(9) 1.3168(2) -0.45225(9) 0.0470(5) Uani 1 1 d . . . S4 S -0.67041(9) 1.2346(2) -0.51148(9) 0.0520(6) Uani 1 1 d . . . O1 O -0.41979(19) 0.9503(5) -0.3491(2) 0.0342(11) Uani 1 1 d . . . O2 O -0.3687(3) 0.6211(6) -0.2549(3) 0.0686(19) Uani 1 1 d . . . H2 H -0.4013 0.6553 -0.2561 0.103 Uiso 1 1 calc . . . O3 O -0.51982(16) 0.8887(4) -0.4159(2) 0.0309(10) Uani 1 1 d . . . O4 O -0.5343(2) 0.8846(5) -0.5420(2) 0.0368(12) Uani 1 1 d . . . O5 O -0.7123(2) 0.9152(7) -0.5721(3) 0.0710(18) Uani 1 1 d . . . H5 H -0.6913 0.9652 -0.5527 0.106 Uiso 1 1 calc . . . N1 N -0.4997(2) 0.8521(5) -0.2858(2) 0.0307(13) Uani 1 1 d . . . N2 N -0.4444(2) 0.7936(6) -0.2822(2) 0.0324(14) Uani 1 1 d . . . N3 N -0.5798(2) 1.0836(6) -0.4957(2) 0.0343(14) Uani 1 1 d . . . N4 N -0.6174(2) 0.9981(6) -0.5259(2) 0.0368(14) Uani 1 1 d . . . C4 C -0.5362(3) 0.7985(7) -0.2498(3) 0.0352(17) Uani 1 1 d . A . C5 C -0.4072(3) 0.8516(7) -0.3161(3) 0.0314(17) Uani 1 1 d . . . C6 C -0.3480(3) 0.7999(8) -0.3179(3) 0.0388(18) Uani 1 1 d . . . C7 C -0.3074(3) 0.8633(7) -0.3530(4) 0.0454(19) Uani 1 1 d . . . H7 H -0.3178 0.9391 -0.3739 0.054 Uiso 1 1 calc R A . C8 C -0.2524(3) 0.8153(10) -0.3572(4) 0.059(2) Uani 1 1 d . . . H8 H -0.2241 0.8596 -0.3796 0.071 Uiso 1 1 calc R . . C9 C -0.2388(4) 0.7007(10) -0.3282(4) 0.065(3) Uani 1 1 d . . . H9 H -0.2014 0.6657 -0.3327 0.078 Uiso 1 1 calc R A . C10 C -0.2771(3) 0.6382(10) -0.2940(4) 0.060(3) Uani 1 1 d . . . H10 H -0.2666 0.5606 -0.2747 0.072 Uiso 1 1 calc R . . C11 C -0.3327(3) 0.6887(9) -0.2871(4) 0.052(2) Uani 1 1 d . . . C12 C -0.5676(3) 0.8018(7) -0.4141(3) 0.0398(17) Uani 1 1 d . . . H12A H -0.6030 0.8505 -0.4074 0.060 Uiso 1 1 calc R . . H12B H -0.5621 0.7400 -0.3818 0.060 Uiso 1 1 calc R . . H12C H -0.5702 0.7556 -0.4518 0.060 Uiso 1 1 calc R . . C13 C -0.5853(4) 1.4542(8) -0.4968(4) 0.060(2) Uani 1 1 d . . . H13A H -0.5605 1.5293 -0.4885 0.072 Uiso 1 1 calc R . . H13B H -0.5809 1.4327 -0.5393 0.072 Uiso 1 1 calc R . . C14 C -0.6471(4) 1.4914(9) -0.4854(4) 0.062(2) Uani 1 1 d . . . H14A H -0.6482 1.5548 -0.4527 0.074 Uiso 1 1 calc R . . H14B H -0.6627 1.5337 -0.5212 0.074 Uiso 1 1 calc R . . C15 C -0.6848(4) 1.3801(9) -0.4696(4) 0.058(2) Uani 1 1 d . . . H15A H -0.7253 1.4054 -0.4761 0.070 Uiso 1 1 calc R . . H15B H -0.6801 1.3612 -0.4270 0.070 Uiso 1 1 calc R . . C16 C -0.6015(3) 1.1968(8) -0.4874(3) 0.0351(17) Uani 1 1 d . . . C17 C -0.5883(3) 0.9019(7) -0.5479(3) 0.0335(17) Uani 1 1 d . . . C18 C -0.6214(3) 0.8041(9) -0.5831(3) 0.043(2) Uani 1 1 d . . . C19 C -0.5932(4) 0.7007(9) -0.6078(3) 0.052(2) Uani 1 1 d . . . H19 H -0.5532 0.6915 -0.6009 0.062 Uiso 1 1 calc R . . C20 C -0.6206(5) 0.6105(10) -0.6418(4) 0.074(3) Uani 1 1 d . . . H20 H -0.5998 0.5412 -0.6589 0.089 Uiso 1 1 calc R . . C21 C -0.6789(5) 0.6225(12) -0.6507(4) 0.079(3) Uani 1 1 d . . . H21 H -0.6985 0.5599 -0.6737 0.095 Uiso 1 1 calc R . . C22 C -0.7085(4) 0.7210(12) -0.6274(4) 0.079(3) Uani 1 1 d . . . H22 H -0.7487 0.7262 -0.6340 0.095 Uiso 1 1 calc R . . C23 C -0.6809(4) 0.8178(10) -0.5931(3) 0.055(2) Uani 1 1 d . . . S1 S -0.5152(7) 0.6566(16) -0.2115(7) 0.0508(17) Uani 0.50 1 d P A 1 C1 C -0.5726(8) 0.6201(18) -0.1606(8) 0.0508(17) Uani 0.50 1 d P A 1 H1A H -0.5659 0.5302 -0.1480 0.061 Uiso 0.50 1 calc PR A 1 H1B H -0.5652 0.6740 -0.1254 0.061 Uiso 0.50 1 calc PR A 1 C2 C -0.6275(9) 0.628(2) -0.1701(8) 0.0508(17) Uani 0.50 1 d PD A 1 H2A H -0.6454 0.6784 -0.1377 0.061 Uiso 0.50 1 calc PR A 1 H2B H -0.6443 0.5410 -0.1696 0.061 Uiso 0.50 1 calc PR A 1 C3 C -0.6410(7) 0.6917(16) -0.2283(6) 0.0508(17) Uani 0.50 1 d PD A 1 H3A H -0.6832 0.7038 -0.2299 0.061 Uiso 0.50 1 calc PR A 1 H3B H -0.6311 0.6295 -0.2599 0.061 Uiso 0.50 1 calc PR A 1 S1B S -0.5116(7) 0.6836(16) -0.2012(6) 0.0508(17) Uani 0.50 1 d P A 2 C1B C -0.5688(7) 0.6839(18) -0.1493(7) 0.0508(17) Uani 0.50 1 d PD A 2 H1B1 H -0.5613 0.6165 -0.1193 0.061 Uiso 0.50 1 calc PR A 2 H1B2 H -0.5691 0.7678 -0.1286 0.061 Uiso 0.50 1 calc PR A 2 C2B C -0.6300(8) 0.6602(18) -0.1766(9) 0.0508(17) Uani 0.50 1 d PD A 2 H2B1 H -0.6282 0.6039 -0.2118 0.061 Uiso 0.50 1 calc PR A 2 H2B2 H -0.6568 0.6232 -0.1473 0.061 Uiso 0.50 1 calc PR A 2 C3B C -0.6453(7) 0.7923(14) -0.1922(7) 0.0508(17) Uani 0.50 1 d PD A 2 H3B1 H -0.6398 0.8478 -0.1570 0.061 Uiso 0.50 1 calc PR A 2 H3B2 H -0.6865 0.7950 -0.2028 0.061 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0318(9) 0.0247(9) 0.0284(8) 0.000 0.000 0.0016(7) Cr2 0.0298(9) 0.0326(10) 0.0308(8) 0.000 0.000 0.0011(8) S2 0.0334(11) 0.0572(14) 0.0476(10) 0.0026(10) 0.0064(8) 0.0051(10) S3 0.0483(12) 0.0360(12) 0.0568(11) 0.0009(10) -0.0047(10) 0.0057(10) S4 0.0450(12) 0.0574(15) 0.0535(11) -0.0054(10) -0.0058(9) 0.0160(11) O1 0.036(3) 0.028(3) 0.039(3) 0.002(2) 0.003(2) 0.002(2) O2 0.059(4) 0.068(5) 0.079(4) 0.032(3) 0.015(3) 0.017(3) O3 0.036(2) 0.026(3) 0.031(2) -0.004(2) 0.001(2) -0.0044(19) O4 0.034(3) 0.040(3) 0.036(3) -0.004(2) 0.001(2) -0.003(2) O5 0.036(3) 0.088(5) 0.089(4) -0.013(4) -0.005(3) -0.016(4) N1 0.033(3) 0.028(4) 0.032(3) -0.001(3) 0.000(3) 0.003(3) N2 0.032(3) 0.032(4) 0.033(3) 0.007(3) 0.003(3) 0.001(3) N3 0.035(3) 0.035(4) 0.033(3) -0.001(3) -0.001(2) 0.003(3) N4 0.030(3) 0.041(4) 0.039(3) 0.000(3) -0.006(3) -0.003(3) C4 0.034(4) 0.038(5) 0.034(4) 0.004(3) -0.004(3) -0.001(3) C5 0.036(4) 0.034(4) 0.025(4) -0.006(3) -0.002(3) 0.000(4) C6 0.035(4) 0.040(5) 0.042(4) -0.002(4) -0.001(3) 0.004(4) C7 0.033(4) 0.035(5) 0.068(5) 0.001(4) -0.004(4) 0.001(4) C8 0.024(4) 0.072(7) 0.082(6) -0.016(6) 0.003(4) -0.010(4) C9 0.044(6) 0.067(7) 0.084(7) -0.005(6) -0.013(5) 0.030(5) C10 0.042(5) 0.078(7) 0.060(5) 0.016(5) 0.003(4) 0.014(5) C11 0.043(5) 0.050(6) 0.064(5) 0.010(4) -0.002(4) 0.004(4) C12 0.047(4) 0.033(4) 0.040(4) -0.007(4) 0.005(4) -0.009(3) C13 0.061(6) 0.030(5) 0.087(7) 0.012(4) 0.006(5) 0.011(4) C14 0.064(6) 0.048(6) 0.073(6) 0.016(5) 0.008(5) 0.020(5) C15 0.050(5) 0.059(7) 0.066(6) 0.001(4) 0.001(4) 0.028(5) C16 0.033(4) 0.045(5) 0.027(4) 0.001(3) 0.003(3) -0.002(4) C17 0.042(5) 0.036(5) 0.022(4) 0.003(3) 0.001(3) -0.009(4) C18 0.048(5) 0.051(6) 0.030(4) 0.007(4) -0.007(3) -0.012(4) C19 0.064(5) 0.056(6) 0.036(4) 0.001(4) 0.004(4) 0.007(5) C20 0.108(9) 0.055(7) 0.059(6) -0.019(5) -0.011(6) -0.022(6) C21 0.094(9) 0.082(9) 0.062(6) -0.024(6) -0.014(6) -0.034(7) C22 0.063(6) 0.112(10) 0.064(6) -0.007(6) -0.011(5) -0.043(7) C23 0.043(5) 0.072(7) 0.049(5) -0.009(5) -0.005(4) -0.016(5) S1 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C1 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C2 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C3 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) S1B 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C1B 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C2B 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) C3B 0.0492(18) 0.048(5) 0.055(4) 0.021(3) 0.010(2) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.939(4) 2_475 ? Cr1 O1 1.939(4) . ? Cr1 O3 1.952(4) . ? Cr1 O3 1.952(4) 2_475 ? Cr1 N1 2.104(5) 2_475 ? Cr1 N1 2.104(5) . ? Cr2 O4 1.962(5) . ? Cr2 O4 1.962(5) 2_475 ? Cr2 O3 1.964(4) 2_475 ? Cr2 O3 1.964(4) . ? Cr2 N3 2.071(6) . ? Cr2 N3 2.071(6) 2_475 ? S2 C3B 1.701(14) . ? S2 C4 1.732(7) . ? S2 C3 1.927(16) . ? S3 C16 1.764(7) . ? S3 C13 1.843(8) . ? S4 C16 1.741(7) . ? S4 C15 1.816(9) . ? O1 C5 1.302(8) . ? O2 C11 1.313(10) . ? O2 H2 0.8400 . ? O3 C12 1.434(7) . ? O4 C17 1.279(8) . ? O5 C23 1.337(10) . ? O5 H5 0.8400 . ? N1 C4 1.302(9) . ? N1 N2 1.427(7) . ? N2 C5 1.304(8) . ? N3 C16 1.295(9) . ? N3 N4 1.422(8) . ? N4 C17 1.307(9) . ? C4 S1B 1.72(2) . ? C4 S1 1.78(2) . ? C5 C6 1.481(10) . ? C6 C11 1.395(11) . ? C6 C7 1.400(10) . ? C7 C8 1.380(10) . ? C7 H7 0.9500 . ? C8 C9 1.396(13) . ? C8 H8 0.9500 . ? C9 C10 1.347(12) . ? C9 H9 0.9500 . ? C10 C11 1.407(10) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.514(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.496(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.503(10) . ? C18 C19 1.377(11) . ? C18 C23 1.412(11) . ? C19 C20 1.370(12) . ? C19 H19 0.9500 . ? C20 C21 1.379(14) . ? C20 H20 0.9500 . ? C21 C22 1.342(14) . ? C21 H21 0.9500 . ? C22 C23 1.425(12) . ? C22 H22 0.9500 . ? S1 C1 1.80(2) . ? C1 C2 1.30(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.504(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? S1B C1B 1.776(19) . ? C1B C2B 1.572(17) . ? C1B H1B1 0.9900 . ? C1B H1B2 0.9900 . ? C2B C3B 1.462(15) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B H3B1 0.9900 . ? C3B H3B2 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 O1 Cr1 O1 179.6(3) 2_475 . ? O1 Cr1 O3 86.13(18) 2_475 . ? O1 Cr1 O3 94.17(18) . . ? O1 Cr1 O3 94.17(18) 2_475 2_475 ? O1 Cr1 O3 86.13(18) . 2_475 ? O3 Cr1 O3 79.3(3) . 2_475 ? O1 Cr1 N1 78.5(2) 2_475 2_475 ? O1 Cr1 N1 101.3(2) . 2_475 ? O3 Cr1 N1 163.32(19) . 2_475 ? O3 Cr1 N1 95.33(19) 2_475 2_475 ? O1 Cr1 N1 101.3(2) 2_475 . ? O1 Cr1 N1 78.5(2) . . ? O3 Cr1 N1 95.33(19) . . ? O3 Cr1 N1 163.32(19) 2_475 . ? N1 Cr1 N1 93.9(3) 2_475 . ? O4 Cr2 O4 94.5(3) . 2_475 ? O4 Cr2 O3 168.69(17) . 2_475 ? O4 Cr2 O3 93.94(18) 2_475 2_475 ? O4 Cr2 O3 93.94(18) . . ? O4 Cr2 O3 168.69(17) 2_475 . ? O3 Cr2 O3 78.7(2) 2_475 . ? O4 Cr2 N3 78.3(2) . . ? O4 Cr2 N3 90.8(2) 2_475 . ? O3 Cr2 N3 94.0(2) 2_475 . ? O3 Cr2 N3 98.21(19) . . ? O4 Cr2 N3 90.8(2) . 2_475 ? O4 Cr2 N3 78.3(2) 2_475 2_475 ? O3 Cr2 N3 98.21(19) 2_475 2_475 ? O3 Cr2 N3 94.0(2) . 2_475 ? N3 Cr2 N3 164.1(3) . 2_475 ? C3B S2 C4 112.6(6) . . ? C3B S2 C3 42.5(7) . . ? C4 S2 C3 96.2(5) . . ? C16 S3 C13 97.4(4) . . ? C16 S4 C15 101.3(4) . . ? C5 O1 Cr1 115.4(4) . . ? C11 O2 H2 109.5 . . ? C12 O3 Cr1 122.3(4) . . ? C12 O3 Cr2 125.2(4) . . ? Cr1 O3 Cr2 100.98(19) . . ? C17 O4 Cr2 112.7(4) . . ? C23 O5 H5 109.5 . . ? C4 N1 N2 111.8(5) . . ? C4 N1 Cr1 137.5(5) . . ? N2 N1 Cr1 110.7(4) . . ? C5 N2 N1 111.7(5) . . ? C16 N3 N4 113.4(6) . . ? C16 N3 Cr2 135.4(5) . . ? N4 N3 Cr2 110.9(4) . . ? C17 N4 N3 110.0(5) . . ? N1 C4 S1B 118.6(8) . . ? N1 C4 S2 118.6(5) . . ? S1B C4 S2 122.7(7) . . ? N1 C4 S1 118.6(7) . . ? S1B C4 S1 12.1(7) . . ? S2 C4 S1 122.1(7) . . ? O1 C5 N2 123.5(6) . . ? O1 C5 C6 118.7(6) . . ? N2 C5 C6 117.9(6) . . ? C11 C6 C7 120.0(7) . . ? C11 C6 C5 121.7(7) . . ? C7 C6 C5 118.3(7) . . ? C8 C7 C6 119.8(8) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.1(8) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 122.1(8) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 119.6(9) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? O2 C11 C6 123.8(7) . . ? O2 C11 C10 116.7(8) . . ? C6 C11 C10 119.3(8) . . ? 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 . . ? C14 C13 S3 114.0(6) . . ? C14 C13 H13A 108.8 . . ? S3 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? S3 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 113.7(7) . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 S4 114.3(6) . . ? C14 C15 H15A 108.7 . . ? S4 C15 H15A 108.7 . . ? C14 C15 H15B 108.7 . . ? S4 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? N3 C16 S4 121.3(5) . . ? N3 C16 S3 119.7(5) . . ? S4 C16 S3 119.0(5) . . ? O4 C17 N4 125.3(6) . . ? O4 C17 C18 117.7(7) . . ? N4 C17 C18 117.0(6) . . ? C19 C18 C23 118.8(8) . . ? C19 C18 C17 119.9(7) . . ? C23 C18 C17 121.3(8) . . ? C20 C19 C18 122.7(9) . . ? C20 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C19 C20 C21 118.5(10) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 121.2(9) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 121.4(9) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? O5 C23 C18 124.0(7) . . ? O5 C23 C22 118.7(8) . . ? C18 C23 C22 117.3(9) . . ? C4 S1 C1 106.3(10) . . ? C2 C1 S1 127.7(14) . . ? C2 C1 H1A 105.4 . . ? S1 C1 H1A 105.4 . . ? C2 C1 H1B 105.4 . . ? S1 C1 H1B 105.4 . . ? H1A C1 H1B 106.0 . . ? C1 C2 C3 112.3(16) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C2 C3 S2 120.6(14) . . ? C2 C3 H3A 107.2 . . ? S2 C3 H3A 107.2 . . ? C2 C3 H3B 107.2 . . ? S2 C3 H3B 107.2 . . ? H3A C3 H3B 106.8 . . ? C4 S1B C1B 99.8(10) . . ? C2B C1B S1B 114.9(12) . . ? C2B C1B H1B1 108.6 . . ? S1B C1B H1B1 108.6 . . ? C2B C1B H1B2 108.6 . . ? S1B C1B H1B2 108.6 . . ? H1B1 C1B H1B2 107.5 . . ? C3B C2B C1B 99.7(15) . . ? C3B C2B H2B1 111.8 . . ? C1B C2B H2B1 111.8 . . ? C3B C2B H2B2 111.8 . . ? C1B C2B H2B2 111.8 . . ? H2B1 C2B H2B2 109.5 . . ? C2B C3B S2 113.8(13) . . ? C2B C3B H3B1 108.8 . . ? S2 C3B H3B1 108.8 . . ? C2B C3B H3B2 108.8 . . ? S2 C3B H3B2 108.8 . . ? H3B1 C3B H3B2 107.7 . . ? 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 O1 Cr1 O1 C5 50.8(5) 2_475 . . . ? O3 Cr1 O1 C5 -89.8(5) . . . . ? O3 Cr1 O1 C5 -168.7(5) 2_475 . . . ? N1 Cr1 O1 C5 96.6(5) 2_475 . . . ? N1 Cr1 O1 C5 4.8(4) . . . . ? O1 Cr1 O3 C12 -49.8(5) 2_475 . . . ? O1 Cr1 O3 C12 129.9(5) . . . . ? O3 Cr1 O3 C12 -144.8(5) 2_475 . . . ? N1 Cr1 O3 C12 -72.3(9) 2_475 . . . ? N1 Cr1 O3 C12 51.1(5) . . . . ? O1 Cr1 O3 Cr2 95.0(2) 2_475 . . . ? O1 Cr1 O3 Cr2 -85.3(2) . . . . ? O3 Cr1 O3 Cr2 0.0 2_475 . . . ? N1 Cr1 O3 Cr2 72.5(7) 2_475 . . . ? N1 Cr1 O3 Cr2 -164.05(19) . . . . ? O4 Cr2 O3 C12 -27.9(5) . . . . ? O4 Cr2 O3 C12 -166.3(9) 2_475 . . . ? O3 Cr2 O3 C12 143.4(5) 2_475 . . . ? N3 Cr2 O3 C12 50.9(5) . . . . ? N3 Cr2 O3 C12 -119.0(5) 2_475 . . . ? O4 Cr2 O3 Cr1 -171.30(19) . . . . ? O4 Cr2 O3 Cr1 50.3(11) 2_475 . . . ? O3 Cr2 O3 Cr1 0.0 2_475 . . . ? N3 Cr2 O3 Cr1 -92.5(2) . . . . ? N3 Cr2 O3 Cr1 97.6(2) 2_475 . . . ? O4 Cr2 O4 C17 -103.4(5) 2_475 . . . ? O3 Cr2 O4 C17 35.0(12) 2_475 . . . ? O3 Cr2 O4 C17 84.1(5) . . . . ? N3 Cr2 O4 C17 -13.5(4) . . . . ? N3 Cr2 O4 C17 178.2(5) 2_475 . . . ? O1 Cr1 N1 C4 -3.3(7) 2_475 . . . ? O1 Cr1 N1 C4 176.4(8) . . . . ? O3 Cr1 N1 C4 -90.4(7) . . . . ? O3 Cr1 N1 C4 -160.6(7) 2_475 . . . ? N1 Cr1 N1 C4 75.7(7) 2_475 . . . ? O1 Cr1 N1 N2 175.4(4) 2_475 . . . ? O1 Cr1 N1 N2 -4.9(4) . . . . ? O3 Cr1 N1 N2 88.3(4) . . . . ? O3 Cr1 N1 N2 18.1(9) 2_475 . . . ? N1 Cr1 N1 N2 -105.6(4) 2_475 . . . ? C4 N1 N2 C5 -176.7(6) . . . . ? Cr1 N1 N2 C5 4.2(6) . . . . ? O4 Cr2 N3 C16 -158.4(7) . . . . ? O4 Cr2 N3 C16 -64.0(7) 2_475 . . . ? O3 Cr2 N3 C16 30.0(7) 2_475 . . . ? O3 Cr2 N3 C16 109.2(6) . . . . ? N3 Cr2 N3 C16 -110.5(7) 2_475 . . . ? O4 Cr2 N3 N4 14.4(4) . . . . ? O4 Cr2 N3 N4 108.9(4) 2_475 . . . ? O3 Cr2 N3 N4 -157.1(4) 2_475 . . . ? O3 Cr2 N3 N4 -78.0(4) . . . . ? N3 Cr2 N3 N4 62.3(4) 2_475 . . . ? C16 N3 N4 C17 161.6(6) . . . . ? Cr2 N3 N4 C17 -12.9(6) . . . . ? N2 N1 C4 S1B 6.1(9) . . . . ? Cr1 N1 C4 S1B -175.2(5) . . . . ? N2 N1 C4 S2 -178.3(4) . . . . ? Cr1 N1 C4 S2 0.4(10) . . . . ? N2 N1 C4 S1 -7.7(9) . . . . ? Cr1 N1 C4 S1 171.0(5) . . . . ? C3B S2 C4 N1 -170.1(8) . . . . ? C3 S2 C4 N1 149.2(7) . . . . ? C3B S2 C4 S1B 5.3(10) . . . . ? C3 S2 C4 S1B -35.4(8) . . . . ? C3B S2 C4 S1 19.7(9) . . . . ? C3 S2 C4 S1 -21.0(8) . . . . ? Cr1 O1 C5 N2 -4.3(8) . . . . ? Cr1 O1 C5 C6 174.2(5) . . . . ? N1 N2 C5 O1 -0.3(9) . . . . ? N1 N2 C5 C6 -178.8(5) . . . . ? O1 C5 C6 C11 -175.1(7) . . . . ? N2 C5 C6 C11 3.4(10) . . . . ? O1 C5 C6 C7 2.9(10) . . . . ? N2 C5 C6 C7 -178.5(6) . . . . ? C11 C6 C7 C8 0.2(11) . . . . ? C5 C6 C7 C8 -177.9(7) . . . . ? C6 C7 C8 C9 2.7(12) . . . . ? C7 C8 C9 C10 -3.0(14) . . . . ? C8 C9 C10 C11 0.2(14) . . . . ? C7 C6 C11 O2 -177.5(8) . . . . ? C5 C6 C11 O2 0.5(13) . . . . ? C7 C6 C11 C10 -2.9(12) . . . . ? C5 C6 C11 C10 175.1(7) . . . . ? C9 C10 C11 O2 177.7(9) . . . . ? C9 C10 C11 C6 2.7(13) . . . . ? C16 S3 C13 C14 69.7(7) . . . . ? S3 C13 C14 C15 -32.4(11) . . . . ? C13 C14 C15 S4 -39.5(10) . . . . ? C16 S4 C15 C14 65.2(7) . . . . ? N4 N3 C16 S4 0.3(8) . . . . ? Cr2 N3 C16 S4 173.0(3) . . . . ? N4 N3 C16 S3 -178.4(4) . . . . ? Cr2 N3 C16 S3 -5.7(9) . . . . ? C15 S4 C16 N3 163.7(6) . . . . ? C15 S4 C16 S3 -17.6(5) . . . . ? C13 S3 C16 N3 142.6(6) . . . . ? C13 S3 C16 S4 -36.1(5) . . . . ? Cr2 O4 C17 N4 11.2(8) . . . . ? Cr2 O4 C17 C18 -169.0(4) . . . . ? N3 N4 C17 O4 1.7(9) . . . . ? N3 N4 C17 C18 -178.1(5) . . . . ? O4 C17 C18 C19 -0.1(10) . . . . ? N4 C17 C18 C19 179.7(7) . . . . ? O4 C17 C18 C23 -178.3(7) . . . . ? N4 C17 C18 C23 1.5(10) . . . . ? C23 C18 C19 C20 0.2(12) . . . . ? C17 C18 C19 C20 -178.0(8) . . . . ? C18 C19 C20 C21 -1.3(14) . . . . ? C19 C20 C21 C22 0.9(16) . . . . ? C20 C21 C22 C23 0.7(16) . . . . ? C19 C18 C23 O5 -179.0(8) . . . . ? C17 C18 C23 O5 -0.8(12) . . . . ? C19 C18 C23 C22 1.3(12) . . . . ? C17 C18 C23 C22 179.5(7) . . . . ? C21 C22 C23 O5 178.5(9) . . . . ? C21 C22 C23 C18 -1.8(14) . . . . ? N1 C4 S1 C1 174.1(8) . . . . ? S1B C4 S1 C1 81(5) . . . . ? S2 C4 S1 C1 -15.7(10) . . . . ? C4 S1 C1 C2 41(2) . . . . ? S1 C1 C2 C3 -8(3) . . . . ? C1 C2 C3 S2 -50(3) . . . . ? C3B S2 C3 C2 -54.2(16) . . . . ? C4 S2 C3 C2 62.7(15) . . . . ? N1 C4 S1B C1B 161.5(8) . . . . ? S2 C4 S1B C1B -13.9(10) . . . . ? S1 C4 S1B C1B -105(5) . . . . ? C4 S1B C1B C2B 54.8(15) . . . . ? S1B C1B C2B C3B -87.1(19) . . . . ? C1B C2B C3B S2 69.8(18) . . . . ? C4 S2 C3B C2B -34.6(16) . . . . ? C3 S2 C3B C2B 39.1(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 N2 0.84 1.85 2.591(8) 146.2 . O5 H5 N4 0.84 1.86 2.595(7) 145.8 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.594 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.230