# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_10a\a _database_code_depnum_ccdc_archive 'CCDC 830653' #TrackingRef 'Weaver.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H10 Cr O3 S2' _chemical_formula_sum 'C11 H10 Cr O3 S2' _chemical_formula_weight 306.31 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' 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 6.3675(9) _cell_length_b 7.5155(11) _cell_length_c 13.1748(19) _cell_angle_alpha 105.757(2) _cell_angle_beta 94.059(2) _cell_angle_gamma 91.292(2) _cell_volume 604.69(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2961 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 28.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5042 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.82 _reflns_number_total 2727 _reflns_number_gt 2313 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0414P)^2^+0.2191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'all non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2727 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.01889(5) -0.01445(4) 0.74045(3) 0.01909(10) Uani 1 1 d . . . C1 C 0.0875(3) 0.2878(3) 0.74403(16) 0.0199(4) Uani 1 1 d . . . C2 C 0.0703(3) 0.2785(3) 0.84891(16) 0.0203(4) Uani 1 1 d . . . C3 C -0.1136(3) 0.1913(3) 0.87329(18) 0.0247(4) Uani 1 1 d . . . H3 H -0.1253 0.1830 0.9434 0.030 Uiso 1 1 calc R . . C4 C -0.2766(3) 0.1180(3) 0.79536(19) 0.0287(5) Uani 1 1 d . . . H4 H -0.4002 0.0637 0.8129 0.034 Uiso 1 1 calc R . . C5 C -0.2571(3) 0.1248(3) 0.69031(19) 0.0280(5) Uani 1 1 d . . . H5 H -0.3670 0.0741 0.6370 0.034 Uiso 1 1 calc R . . C6 C -0.0762(3) 0.2062(3) 0.66504(18) 0.0250(4) Uani 1 1 d . . . H6 H -0.0623 0.2070 0.5939 0.030 Uiso 1 1 calc R . . S1 S 0.30945(8) 0.41000(7) 0.71956(4) 0.02478(13) Uani 1 1 d . . . C7 C 0.2854(4) 0.3682(4) 0.57802(19) 0.0371(6) Uani 1 1 d . . . H7A H 0.2775 0.2346 0.5444 0.056 Uiso 1 1 calc R . . H7B H 0.4084 0.4242 0.5559 0.056 Uiso 1 1 calc R . . H7C H 0.1572 0.4231 0.5567 0.056 Uiso 1 1 calc R . . S2 S 0.27454(8) 0.38767(7) 0.94430(4) 0.02501(13) Uani 1 1 d . . . C8 C 0.2204(4) 0.3162(3) 1.06016(17) 0.0281(5) Uani 1 1 d . . . H8A H 0.0818 0.3577 1.0823 0.042 Uiso 1 1 calc R . . H8B H 0.3287 0.3710 1.1175 0.042 Uiso 1 1 calc R . . H8C H 0.2212 0.1810 1.0437 0.042 Uiso 1 1 calc R . . C9 C -0.1234(3) -0.2425(3) 0.69869(17) 0.0245(4) Uani 1 1 d . . . O9 O -0.2133(3) -0.3843(2) 0.67132(14) 0.0349(4) Uani 1 1 d . . . C10 C 0.2019(3) -0.1023(3) 0.63911(17) 0.0240(4) Uani 1 1 d . . . O10 O 0.3184(3) -0.1590(2) 0.57478(13) 0.0354(4) Uani 1 1 d . . . C11 C 0.1953(3) -0.0941(3) 0.83473(17) 0.0225(4) Uani 1 1 d . . . O11 O 0.3087(3) -0.1363(2) 0.89548(13) 0.0310(4) Uani 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 Cr1 0.01657(17) 0.01710(17) 0.02276(18) 0.00433(13) 0.00020(12) 0.00143(12) C1 0.0182(9) 0.0154(9) 0.0260(10) 0.0058(8) 0.0004(8) 0.0037(7) C2 0.0179(9) 0.0171(9) 0.0248(10) 0.0035(8) 0.0020(8) 0.0028(7) C3 0.0240(10) 0.0202(10) 0.0286(11) 0.0031(8) 0.0074(8) 0.0028(8) C4 0.0174(10) 0.0249(11) 0.0414(13) 0.0043(10) 0.0055(9) 0.0023(8) C5 0.0172(10) 0.0249(11) 0.0385(13) 0.0056(9) -0.0090(9) 0.0024(8) C6 0.0249(11) 0.0211(10) 0.0287(11) 0.0076(8) -0.0049(9) 0.0051(8) S1 0.0246(3) 0.0245(3) 0.0259(3) 0.0085(2) 0.0017(2) -0.0021(2) C7 0.0443(14) 0.0422(14) 0.0261(12) 0.0105(10) 0.0086(10) -0.0039(11) S2 0.0247(3) 0.0265(3) 0.0219(3) 0.0046(2) -0.0015(2) -0.0044(2) C8 0.0312(12) 0.0303(11) 0.0233(11) 0.0084(9) -0.0001(9) 0.0038(9) C9 0.0231(10) 0.0264(11) 0.0240(11) 0.0073(9) 0.0005(8) 0.0017(8) O9 0.0382(9) 0.0240(8) 0.0406(10) 0.0081(7) -0.0046(8) -0.0079(7) C10 0.0236(10) 0.0216(10) 0.0258(11) 0.0060(8) -0.0032(9) 0.0000(8) O10 0.0294(9) 0.0427(10) 0.0313(9) 0.0038(7) 0.0078(7) 0.0057(7) C11 0.0229(10) 0.0189(10) 0.0240(10) 0.0024(8) 0.0044(8) 0.0015(8) O11 0.0303(8) 0.0315(9) 0.0320(9) 0.0110(7) -0.0031(7) 0.0069(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C10 1.831(2) . ? Cr1 C11 1.844(2) . ? Cr1 C9 1.846(2) . ? Cr1 C5 2.217(2) . ? Cr1 C4 2.223(2) . ? Cr1 C6 2.227(2) . ? Cr1 C3 2.228(2) . ? Cr1 C2 2.278(2) . ? Cr1 C1 2.291(2) . ? C1 C2 1.414(3) . ? C1 C6 1.420(3) . ? C1 S1 1.764(2) . ? C2 C3 1.427(3) . ? C2 S2 1.762(2) . ? C3 C4 1.397(3) . ? C4 C5 1.413(3) . ? C5 C6 1.394(3) . ? S1 C7 1.800(2) . ? S2 C8 1.802(2) . ? C9 O9 1.152(3) . ? C10 O10 1.165(3) . ? C11 O11 1.153(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Cr1 C11 88.52(9) . . ? C10 Cr1 C9 88.60(9) . . ? C11 Cr1 C9 90.54(9) . . ? C10 Cr1 C5 115.71(9) . . ? C11 Cr1 C5 155.68(9) . . ? C9 Cr1 C5 92.06(9) . . ? C10 Cr1 C4 152.70(9) . . ? C11 Cr1 C4 118.75(9) . . ? C9 Cr1 C4 89.91(9) . . ? C5 Cr1 C4 37.12(9) . . ? C10 Cr1 C6 91.11(9) . . ? C11 Cr1 C6 149.73(9) . . ? C9 Cr1 C6 119.72(9) . . ? C5 Cr1 C6 36.57(8) . . ? C4 Cr1 C6 66.20(9) . . ? C10 Cr1 C3 156.60(9) . . ? C11 Cr1 C3 90.72(9) . . ? C9 Cr1 C3 114.80(9) . . ? C5 Cr1 C3 66.31(9) . . ? C4 Cr1 C3 36.58(8) . . ? C6 Cr1 C3 77.97(8) . . ? C10 Cr1 C2 119.70(8) . . ? C11 Cr1 C2 88.35(8) . . ? C9 Cr1 C2 151.63(8) . . ? C5 Cr1 C2 78.03(8) . . ? C4 Cr1 C2 66.11(8) . . ? C6 Cr1 C2 65.72(8) . . ? C3 Cr1 C2 36.91(7) . . ? C10 Cr1 C1 93.25(8) . . ? C11 Cr1 C1 113.18(8) . . ? C9 Cr1 C1 156.24(9) . . ? C5 Cr1 C1 65.83(8) . . ? C4 Cr1 C1 77.70(8) . . ? C6 Cr1 C1 36.62(7) . . ? C3 Cr1 C1 65.66(8) . . ? C2 Cr1 C1 36.06(7) . . ? C2 C1 C6 119.19(18) . . ? C2 C1 S1 117.50(15) . . ? C6 C1 S1 123.26(16) . . ? C2 C1 Cr1 71.48(11) . . ? C6 C1 Cr1 69.24(11) . . ? S1 C1 Cr1 133.86(10) . . ? C1 C2 C3 119.17(19) . . ? C1 C2 S2 117.20(15) . . ? C3 C2 S2 123.54(16) . . ? C1 C2 Cr1 72.46(11) . . ? C3 C2 Cr1 69.65(11) . . ? S2 C2 Cr1 132.79(11) . . ? C4 C3 C2 120.8(2) . . ? C4 C3 Cr1 71.51(12) . . ? C2 C3 Cr1 73.44(12) . . ? C3 C4 C5 119.8(2) . . ? C3 C4 Cr1 71.91(12) . . ? C5 C4 Cr1 71.21(12) . . ? C6 C5 C4 119.9(2) . . ? C6 C5 Cr1 72.10(12) . . ? C4 C5 Cr1 71.67(12) . . ? C5 C6 C1 121.1(2) . . ? C5 C6 Cr1 71.34(12) . . ? C1 C6 Cr1 74.14(12) . . ? C1 S1 C7 103.30(11) . . ? C2 S2 C8 104.30(10) . . ? O9 C9 Cr1 179.0(2) . . ? O10 C10 Cr1 179.7(2) . . ? O11 C11 Cr1 177.13(18) . . ? 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 C10 Cr1 C1 C2 -139.90(13) . . . . ? C11 Cr1 C1 C2 -50.12(14) . . . . ? C9 Cr1 C1 C2 126.2(2) . . . . ? C5 Cr1 C1 C2 103.31(13) . . . . ? C4 Cr1 C1 C2 66.13(12) . . . . ? C6 Cr1 C1 C2 132.61(18) . . . . ? C3 Cr1 C1 C2 29.59(12) . . . . ? C10 Cr1 C1 C6 87.49(14) . . . . ? C11 Cr1 C1 C6 177.27(13) . . . . ? C9 Cr1 C1 C6 -6.4(3) . . . . ? C5 Cr1 C1 C6 -29.30(13) . . . . ? C4 Cr1 C1 C6 -66.48(13) . . . . ? C3 Cr1 C1 C6 -103.02(14) . . . . ? C2 Cr1 C1 C6 -132.61(18) . . . . ? C10 Cr1 C1 S1 -29.21(16) . . . . ? C11 Cr1 C1 S1 60.57(17) . . . . ? C9 Cr1 C1 S1 -123.1(2) . . . . ? C5 Cr1 C1 S1 -146.00(18) . . . . ? C4 Cr1 C1 S1 176.82(17) . . . . ? C6 Cr1 C1 S1 -116.7(2) . . . . ? C3 Cr1 C1 S1 140.28(17) . . . . ? C2 Cr1 C1 S1 110.7(2) . . . . ? C6 C1 C2 C3 -1.5(3) . . . . ? S1 C1 C2 C3 175.96(15) . . . . ? Cr1 C1 C2 C3 -53.55(17) . . . . ? C6 C1 C2 S2 -178.29(15) . . . . ? S1 C1 C2 S2 -0.8(2) . . . . ? Cr1 C1 C2 S2 129.69(14) . . . . ? C6 C1 C2 Cr1 52.03(16) . . . . ? S1 C1 C2 Cr1 -130.50(13) . . . . ? C10 Cr1 C2 C1 47.75(15) . . . . ? C11 Cr1 C2 C1 135.11(13) . . . . ? C9 Cr1 C2 C1 -136.81(18) . . . . ? C5 Cr1 C2 C1 -65.17(12) . . . . ? C4 Cr1 C2 C1 -102.27(13) . . . . ? C6 Cr1 C2 C1 -28.79(11) . . . . ? C3 Cr1 C2 C1 -131.49(18) . . . . ? C10 Cr1 C2 C3 179.24(13) . . . . ? C11 Cr1 C2 C3 -93.40(14) . . . . ? C9 Cr1 C2 C3 -5.3(2) . . . . ? C5 Cr1 C2 C3 66.32(13) . . . . ? C4 Cr1 C2 C3 29.22(13) . . . . ? C6 Cr1 C2 C3 102.70(14) . . . . ? C1 Cr1 C2 C3 131.49(18) . . . . ? C10 Cr1 C2 S2 -63.39(17) . . . . ? C11 Cr1 C2 S2 23.96(15) . . . . ? C9 Cr1 C2 S2 112.05(19) . . . . ? C5 Cr1 C2 S2 -176.32(16) . . . . ? C4 Cr1 C2 S2 146.58(17) . . . . ? C6 Cr1 C2 S2 -139.94(17) . . . . ? C3 Cr1 C2 S2 117.4(2) . . . . ? C1 Cr1 C2 S2 -111.15(19) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? S2 C2 C3 C4 175.66(16) . . . . ? Cr1 C2 C3 C4 -55.78(18) . . . . ? C1 C2 C3 Cr1 54.89(17) . . . . ? S2 C2 C3 Cr1 -128.57(15) . . . . ? C10 Cr1 C3 C4 129.8(2) . . . . ? C11 Cr1 C3 C4 -142.21(14) . . . . ? C9 Cr1 C3 C4 -51.28(16) . . . . ? C5 Cr1 C3 C4 29.55(13) . . . . ? C6 Cr1 C3 C4 66.10(14) . . . . ? C2 Cr1 C3 C4 131.5(2) . . . . ? C1 Cr1 C3 C4 102.56(15) . . . . ? C10 Cr1 C3 C2 -1.7(3) . . . . ? C11 Cr1 C3 C2 86.29(13) . . . . ? C9 Cr1 C3 C2 177.22(12) . . . . ? C5 Cr1 C3 C2 -101.95(14) . . . . ? C4 Cr1 C3 C2 -131.5(2) . . . . ? C6 Cr1 C3 C2 -65.40(13) . . . . ? C1 Cr1 C3 C2 -28.94(12) . . . . ? C2 C3 C4 C5 2.0(3) . . . . ? Cr1 C3 C4 C5 -54.73(18) . . . . ? C2 C3 C4 Cr1 56.69(18) . . . . ? C10 Cr1 C4 C3 -138.32(19) . . . . ? C11 Cr1 C4 C3 44.34(16) . . . . ? C9 Cr1 C4 C3 134.91(14) . . . . ? C5 Cr1 C4 C3 -131.6(2) . . . . ? C6 Cr1 C4 C3 -102.24(14) . . . . ? C2 Cr1 C4 C3 -29.47(12) . . . . ? C1 Cr1 C4 C3 -65.53(13) . . . . ? C10 Cr1 C4 C5 -6.8(3) . . . . ? C11 Cr1 C4 C5 175.89(13) . . . . ? C9 Cr1 C4 C5 -93.54(14) . . . . ? C6 Cr1 C4 C5 29.31(13) . . . . ? C3 Cr1 C4 C5 131.6(2) . . . . ? C2 Cr1 C4 C5 102.09(14) . . . . ? C1 Cr1 C4 C5 66.02(13) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? Cr1 C4 C5 C6 -55.65(18) . . . . ? C3 C4 C5 Cr1 55.06(18) . . . . ? C10 Cr1 C5 C6 -52.20(15) . . . . ? C11 Cr1 C5 C6 122.5(2) . . . . ? C9 Cr1 C5 C6 -141.64(14) . . . . ? C4 Cr1 C5 C6 131.24(19) . . . . ? C3 Cr1 C5 C6 102.10(14) . . . . ? C2 Cr1 C5 C6 65.19(13) . . . . ? C1 Cr1 C5 C6 29.34(12) . . . . ? C10 Cr1 C5 C4 176.56(13) . . . . ? C11 Cr1 C5 C4 -8.8(3) . . . . ? C9 Cr1 C5 C4 87.12(14) . . . . ? C6 Cr1 C5 C4 -131.24(19) . . . . ? C3 Cr1 C5 C4 -29.14(13) . . . . ? C2 Cr1 C5 C4 -66.05(13) . . . . ? C1 Cr1 C5 C4 -101.90(14) . . . . ? C4 C5 C6 C1 -1.9(3) . . . . ? Cr1 C5 C6 C1 -57.31(18) . . . . ? C4 C5 C6 Cr1 55.45(18) . . . . ? C2 C1 C6 C5 2.9(3) . . . . ? S1 C1 C6 C5 -174.41(16) . . . . ? Cr1 C1 C6 C5 55.99(18) . . . . ? C2 C1 C6 Cr1 -53.07(17) . . . . ? S1 C1 C6 Cr1 129.61(15) . . . . ? C10 Cr1 C6 C5 134.60(14) . . . . ? C11 Cr1 C6 C5 -136.44(17) . . . . ? C9 Cr1 C6 C5 45.57(16) . . . . ? C4 Cr1 C6 C5 -29.73(13) . . . . ? C3 Cr1 C6 C5 -66.28(14) . . . . ? C2 Cr1 C6 C5 -103.07(14) . . . . ? C1 Cr1 C6 C5 -131.45(19) . . . . ? C10 Cr1 C6 C1 -93.95(13) . . . . ? C11 Cr1 C6 C1 -5.0(2) . . . . ? C9 Cr1 C6 C1 177.02(12) . . . . ? C5 Cr1 C6 C1 131.45(19) . . . . ? C4 Cr1 C6 C1 101.72(14) . . . . ? C3 Cr1 C6 C1 65.17(13) . . . . ? C2 Cr1 C6 C1 28.38(11) . . . . ? C2 C1 S1 C7 174.22(17) . . . . ? C6 C1 S1 C7 -8.4(2) . . . . ? Cr1 C1 S1 C7 84.01(17) . . . . ? C1 C2 S2 C8 -171.21(16) . . . . ? C3 C2 S2 C8 12.2(2) . . . . ? Cr1 C2 S2 C8 -80.40(16) . . . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.430 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.075 data_10a\b _database_code_depnum_ccdc_archive 'CCDC 830654' #TrackingRef 'Weaver.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H10 Cr O3 S2' _chemical_formula_sum 'C11 H10 Cr O3 S2' _chemical_formula_weight 306.31 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' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.349(3) _cell_length_b 25.347(11) _cell_length_c 7.531(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.629(6) _cell_angle_gamma 90.00 _cell_volume 1211.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1017 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 23.39 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8036 _diffrn_reflns_av_R_equivalents 0.1360 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.00 _reflns_number_total 1899 _reflns_number_gt 1205 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0950P)^2^+16.9098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.041(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1899 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.2693 _refine_ls_wR_factor_gt 0.2398 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _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 Cr1 Cr 0.5543(3) 0.12938(8) 0.6122(3) 0.0256(8) Uani 1 1 d . . . C1 C 0.594(2) 0.0746(5) 0.8502(15) 0.022(3) Uani 1 1 d . . . C2 C 0.625(2) 0.1275(5) 0.9104(17) 0.027(3) Uani 1 1 d . . . C3 C 0.473(2) 0.1667(5) 0.8681(17) 0.028(3) Uani 1 1 d . . . H3 H 0.4984 0.2022 0.9035 0.034 Uiso 1 1 calc R . . C4 C 0.286(2) 0.1538(6) 0.774(2) 0.040(4) Uani 1 1 d . . . H4 H 0.1836 0.1803 0.7500 0.048 Uiso 1 1 calc R . . C5 C 0.249(2) 0.1022(6) 0.7155(19) 0.037(3) Uani 1 1 d . . . H5 H 0.1219 0.0936 0.6525 0.044 Uiso 1 1 calc R . . C6 C 0.4042(19) 0.0625(5) 0.7511(16) 0.025(3) Uani 1 1 d . . . H6 H 0.3812 0.0276 0.7086 0.029 Uiso 1 1 calc R . . S1 S 0.7849(5) 0.02809(12) 0.9134(5) 0.0296(9) Uani 1 1 d . . . C7 C 0.714(2) -0.0296(5) 0.7863(18) 0.033(3) Uani 1 1 d . . . H7A H 0.5703 -0.0402 0.8129 0.049 Uiso 1 1 calc R . . H7B H 0.8117 -0.0584 0.8174 0.049 Uiso 1 1 calc R . . H7C H 0.7230 -0.0217 0.6593 0.049 Uiso 1 1 calc R . . S2 S 0.8491(6) 0.14026(14) 1.0459(5) 0.0379(10) Uani 1 1 d . . . C8 C 0.851(3) 0.2111(6) 1.064(3) 0.061(5) Uani 1 1 d . . . H8A H 0.8808 0.2266 0.9480 0.091 Uiso 1 1 calc R . . H8B H 0.9608 0.2219 1.1509 0.091 Uiso 1 1 calc R . . H8C H 0.7137 0.2234 1.1028 0.091 Uiso 1 1 calc R . . C9 C 0.418(2) 0.1518(5) 0.4076(19) 0.031(3) Uani 1 1 d . . . O9 O 0.3316(17) 0.1655(4) 0.2764(15) 0.049(3) Uani 1 1 d . . . C10 C 0.715(2) 0.0830(5) 0.4875(18) 0.027(3) Uani 1 1 d . . . O10 O 0.8198(16) 0.0533(4) 0.4123(13) 0.039(2) Uani 1 1 d . . . C11 C 0.750(2) 0.1798(5) 0.5730(18) 0.029(3) Uani 1 1 d . . . O11 O 0.8757(16) 0.2126(4) 0.5399(14) 0.045(3) Uani 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 Cr1 0.0262(12) 0.0229(12) 0.0272(13) 0.0020(9) -0.0055(9) 0.0005(9) C1 0.031(7) 0.025(7) 0.010(6) 0.005(5) 0.003(5) 0.005(6) C2 0.031(7) 0.024(7) 0.027(7) -0.005(6) -0.001(6) -0.004(6) C3 0.032(8) 0.026(7) 0.027(7) 0.000(6) 0.006(6) 0.003(6) C4 0.025(8) 0.035(8) 0.060(10) 0.023(7) 0.002(7) 0.018(6) C5 0.027(8) 0.045(9) 0.038(9) -0.002(7) -0.004(6) -0.007(7) C6 0.022(7) 0.032(7) 0.019(7) 0.003(5) 0.008(5) 0.000(6) S1 0.0323(19) 0.0219(17) 0.034(2) 0.0011(15) -0.0085(15) 0.0026(15) C7 0.040(8) 0.029(7) 0.029(8) 0.000(6) -0.001(6) -0.002(6) S2 0.039(2) 0.029(2) 0.044(2) -0.0011(16) -0.0081(17) 0.0036(16) C8 0.065(12) 0.044(10) 0.071(13) -0.025(9) -0.022(10) -0.001(9) C9 0.026(7) 0.029(7) 0.038(9) 0.008(6) 0.012(7) -0.001(6) O9 0.047(7) 0.055(7) 0.043(7) 0.010(6) -0.010(5) 0.004(5) C10 0.024(7) 0.021(7) 0.035(8) 0.002(6) -0.015(6) 0.001(6) O10 0.041(6) 0.037(6) 0.039(6) 0.008(5) 0.007(5) 0.000(5) C11 0.033(8) 0.023(7) 0.031(8) 0.010(6) -0.003(6) 0.006(6) O11 0.044(6) 0.036(6) 0.056(7) -0.001(5) 0.007(5) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C11 1.814(14) . ? Cr1 C10 1.831(14) . ? Cr1 C9 1.836(15) . ? Cr1 C4 2.211(15) . ? Cr1 C5 2.218(14) . ? Cr1 C3 2.220(13) . ? Cr1 C6 2.222(12) . ? Cr1 C1 2.275(11) . ? Cr1 C2 2.278(13) . ? C1 C2 1.427(17) . ? C1 C6 1.434(18) . ? C1 S1 1.747(12) . ? C2 C3 1.412(18) . ? C2 S2 1.759(13) . ? C3 C4 1.41(2) . ? C4 C5 1.40(2) . ? C5 C6 1.428(19) . ? S1 C7 1.798(13) . ? S2 C8 1.801(16) . ? C9 O9 1.169(16) . ? C10 O10 1.164(16) . ? C11 O11 1.183(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Cr1 C10 88.6(6) . . ? C11 Cr1 C9 87.4(6) . . ? C10 Cr1 C9 91.4(6) . . ? C11 Cr1 C4 115.8(6) . . ? C10 Cr1 C4 155.5(6) . . ? C9 Cr1 C4 91.4(5) . . ? C11 Cr1 C5 152.4(6) . . ? C10 Cr1 C5 119.0(6) . . ? C9 Cr1 C5 89.7(5) . . ? C4 Cr1 C5 36.8(5) . . ? C11 Cr1 C3 91.0(6) . . ? C10 Cr1 C3 149.8(5) . . ? C9 Cr1 C3 118.8(5) . . ? C4 Cr1 C3 37.0(5) . . ? C5 Cr1 C3 66.5(5) . . ? C11 Cr1 C6 156.9(5) . . ? C10 Cr1 C6 90.2(5) . . ? C9 Cr1 C6 115.6(5) . . ? C4 Cr1 C6 66.8(5) . . ? C5 Cr1 C6 37.5(5) . . ? C3 Cr1 C6 78.7(5) . . ? C11 Cr1 C1 119.8(5) . . ? C10 Cr1 C1 87.8(5) . . ? C9 Cr1 C1 152.7(5) . . ? C4 Cr1 C1 78.8(5) . . ? C5 Cr1 C1 67.2(5) . . ? C3 Cr1 C1 66.4(4) . . ? C6 Cr1 C1 37.2(5) . . ? C11 Cr1 C2 93.3(5) . . ? C10 Cr1 C2 113.3(5) . . ? C9 Cr1 C2 155.3(5) . . ? C4 Cr1 C2 66.1(5) . . ? C5 Cr1 C2 78.3(5) . . ? C3 Cr1 C2 36.6(5) . . ? C6 Cr1 C2 66.1(5) . . ? C1 Cr1 C2 36.5(4) . . ? C2 C1 C6 118.2(11) . . ? C2 C1 S1 117.4(10) . . ? C6 C1 S1 124.3(9) . . ? C2 C1 Cr1 71.8(7) . . ? C6 C1 Cr1 69.4(7) . . ? S1 C1 Cr1 133.4(6) . . ? C3 C2 C1 120.2(12) . . ? C3 C2 S2 122.5(10) . . ? C1 C2 S2 117.2(10) . . ? C3 C2 Cr1 69.5(7) . . ? C1 C2 Cr1 71.6(7) . . ? S2 C2 Cr1 134.5(7) . . ? C4 C3 C2 120.7(12) . . ? C4 C3 Cr1 71.1(8) . . ? C2 C3 Cr1 74.0(7) . . ? C5 C4 C3 120.6(12) . . ? C5 C4 Cr1 71.9(8) . . ? C3 C4 Cr1 71.9(8) . . ? C4 C5 C6 119.4(12) . . ? C4 C5 Cr1 71.3(8) . . ? C6 C5 Cr1 71.4(7) . . ? C5 C6 C1 120.8(12) . . ? C5 C6 Cr1 71.1(8) . . ? C1 C6 Cr1 73.4(7) . . ? C1 S1 C7 104.1(6) . . ? C2 S2 C8 103.4(7) . . ? O9 C9 Cr1 179.3(13) . . ? O10 C10 Cr1 178.2(11) . . ? O11 C11 Cr1 177.2(12) . . ? 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 C11 Cr1 C1 C2 48.8(9) . . . . ? C10 Cr1 C1 C2 135.9(8) . . . . ? C9 Cr1 C1 C2 -135.4(12) . . . . ? C4 Cr1 C1 C2 -64.7(8) . . . . ? C5 Cr1 C1 C2 -101.3(8) . . . . ? C3 Cr1 C1 C2 -28.0(7) . . . . ? C6 Cr1 C1 C2 -130.9(11) . . . . ? C11 Cr1 C1 C6 179.7(8) . . . . ? C10 Cr1 C1 C6 -93.3(8) . . . . ? C9 Cr1 C1 C6 -4.6(14) . . . . ? C4 Cr1 C1 C6 66.2(8) . . . . ? C5 Cr1 C1 C6 29.5(7) . . . . ? C3 Cr1 C1 C6 102.8(8) . . . . ? C2 Cr1 C1 C6 130.9(11) . . . . ? C11 Cr1 C1 S1 -62.1(11) . . . . ? C10 Cr1 C1 S1 24.9(9) . . . . ? C9 Cr1 C1 S1 113.6(13) . . . . ? C4 Cr1 C1 S1 -175.6(10) . . . . ? C5 Cr1 C1 S1 147.7(11) . . . . ? C3 Cr1 C1 S1 -139.0(11) . . . . ? C6 Cr1 C1 S1 118.2(12) . . . . ? C2 Cr1 C1 S1 -110.9(13) . . . . ? C6 C1 C2 C3 -1.8(18) . . . . ? S1 C1 C2 C3 -178.3(10) . . . . ? Cr1 C1 C2 C3 51.6(11) . . . . ? C6 C1 C2 S2 175.3(9) . . . . ? S1 C1 C2 S2 -1.2(14) . . . . ? Cr1 C1 C2 S2 -131.3(9) . . . . ? C6 C1 C2 Cr1 -53.4(10) . . . . ? S1 C1 C2 Cr1 130.1(8) . . . . ? C11 Cr1 C2 C3 87.2(8) . . . . ? C10 Cr1 C2 C3 177.1(8) . . . . ? C9 Cr1 C2 C3 -4.0(16) . . . . ? C4 Cr1 C2 C3 -29.7(8) . . . . ? C5 Cr1 C2 C3 -66.3(8) . . . . ? C6 Cr1 C2 C3 -103.7(8) . . . . ? C1 Cr1 C2 C3 -133.7(11) . . . . ? C11 Cr1 C2 C1 -139.1(8) . . . . ? C10 Cr1 C2 C1 -49.2(9) . . . . ? C9 Cr1 C2 C1 129.7(12) . . . . ? C4 Cr1 C2 C1 104.0(8) . . . . ? C5 Cr1 C2 C1 67.4(8) . . . . ? C3 Cr1 C2 C1 133.7(11) . . . . ? C6 Cr1 C2 C1 30.0(7) . . . . ? C11 Cr1 C2 S2 -28.7(10) . . . . ? C10 Cr1 C2 S2 61.2(11) . . . . ? C9 Cr1 C2 S2 -119.8(13) . . . . ? C4 Cr1 C2 S2 -145.5(11) . . . . ? C5 Cr1 C2 S2 177.9(10) . . . . ? C3 Cr1 C2 S2 -115.9(13) . . . . ? C6 Cr1 C2 S2 140.4(11) . . . . ? C1 Cr1 C2 S2 110.4(13) . . . . ? C1 C2 C3 C4 3.2(19) . . . . ? S2 C2 C3 C4 -173.7(11) . . . . ? Cr1 C2 C3 C4 55.8(12) . . . . ? C1 C2 C3 Cr1 -52.6(11) . . . . ? S2 C2 C3 Cr1 130.5(10) . . . . ? C11 Cr1 C3 C4 134.5(8) . . . . ? C10 Cr1 C3 C4 -136.6(11) . . . . ? C9 Cr1 C3 C4 46.8(10) . . . . ? C5 Cr1 C3 C4 -29.0(8) . . . . ? C6 Cr1 C3 C4 -66.3(8) . . . . ? C1 Cr1 C3 C4 -103.2(8) . . . . ? C2 Cr1 C3 C4 -131.3(11) . . . . ? C11 Cr1 C3 C2 -94.2(8) . . . . ? C10 Cr1 C3 C2 -5.4(14) . . . . ? C9 Cr1 C3 C2 178.1(8) . . . . ? C4 Cr1 C3 C2 131.3(11) . . . . ? C5 Cr1 C3 C2 102.3(8) . . . . ? C6 Cr1 C3 C2 64.9(8) . . . . ? C1 Cr1 C3 C2 28.0(7) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? Cr1 C3 C4 C5 55.0(13) . . . . ? C2 C3 C4 Cr1 -57.1(11) . . . . ? C11 Cr1 C4 C5 175.5(8) . . . . ? C10 Cr1 C4 C5 -8.7(17) . . . . ? C9 Cr1 C4 C5 87.6(9) . . . . ? C3 Cr1 C4 C5 -132.1(12) . . . . ? C6 Cr1 C4 C5 -29.8(8) . . . . ? C1 Cr1 C4 C5 -66.7(8) . . . . ? C2 Cr1 C4 C5 -102.8(9) . . . . ? C11 Cr1 C4 C3 -52.4(9) . . . . ? C10 Cr1 C4 C3 123.4(13) . . . . ? C9 Cr1 C4 C3 -140.2(8) . . . . ? C5 Cr1 C4 C3 132.1(12) . . . . ? C6 Cr1 C4 C3 102.3(8) . . . . ? C1 Cr1 C4 C3 65.4(8) . . . . ? C2 Cr1 C4 C3 29.3(7) . . . . ? C3 C4 C5 C6 0(2) . . . . ? Cr1 C4 C5 C6 54.7(11) . . . . ? C3 C4 C5 Cr1 -55.0(12) . . . . ? C11 Cr1 C5 C4 -8.8(16) . . . . ? C10 Cr1 C5 C4 175.9(8) . . . . ? C9 Cr1 C5 C4 -92.7(9) . . . . ? C3 Cr1 C5 C4 29.1(8) . . . . ? C6 Cr1 C5 C4 131.4(12) . . . . ? C1 Cr1 C5 C4 102.2(9) . . . . ? C2 Cr1 C5 C4 65.6(8) . . . . ? C11 Cr1 C5 C6 -140.3(12) . . . . ? C10 Cr1 C5 C6 44.5(9) . . . . ? C9 Cr1 C5 C6 135.9(8) . . . . ? C4 Cr1 C5 C6 -131.4(12) . . . . ? C3 Cr1 C5 C6 -102.3(8) . . . . ? C1 Cr1 C5 C6 -29.3(7) . . . . ? C2 Cr1 C5 C6 -65.9(8) . . . . ? C4 C5 C6 C1 1.7(19) . . . . ? Cr1 C5 C6 C1 56.4(10) . . . . ? C4 C5 C6 Cr1 -54.6(12) . . . . ? C2 C1 C6 C5 -0.6(18) . . . . ? S1 C1 C6 C5 175.5(10) . . . . ? Cr1 C1 C6 C5 -55.3(11) . . . . ? C2 C1 C6 Cr1 54.6(10) . . . . ? S1 C1 C6 Cr1 -129.2(9) . . . . ? C11 Cr1 C6 C5 131.0(14) . . . . ? C10 Cr1 C6 C5 -142.2(8) . . . . ? C9 Cr1 C6 C5 -50.6(9) . . . . ? C4 Cr1 C6 C5 29.2(8) . . . . ? C3 Cr1 C6 C5 66.1(8) . . . . ? C1 Cr1 C6 C5 131.7(11) . . . . ? C2 Cr1 C6 C5 102.2(8) . . . . ? C11 Cr1 C6 C1 -0.7(17) . . . . ? C10 Cr1 C6 C1 86.1(8) . . . . ? C9 Cr1 C6 C1 177.7(7) . . . . ? C4 Cr1 C6 C1 -102.5(8) . . . . ? C5 Cr1 C6 C1 -131.7(11) . . . . ? C3 Cr1 C6 C1 -65.7(7) . . . . ? C2 Cr1 C6 C1 -29.5(7) . . . . ? C2 C1 S1 C7 -171.4(10) . . . . ? C6 C1 S1 C7 12.4(12) . . . . ? Cr1 C1 S1 C7 -80.9(10) . . . . ? C3 C2 S2 C8 -11.4(14) . . . . ? C1 C2 S2 C8 171.6(11) . . . . ? Cr1 C2 S2 C8 81.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.855 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.188 data_10b _database_code_depnum_ccdc_archive 'CCDC 830655' #TrackingRef 'Weaver.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H14 Cr O3 S2' _chemical_formula_sum 'C13 H14 Cr O3 S2' _chemical_formula_weight 334.36 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' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.6871(12) _cell_length_b 7.2672(8) _cell_length_c 18.787(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.4396(13) _cell_angle_gamma 90.00 _cell_volume 1446.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5388 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 31.04 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6719 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 16190 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 31.18 _reflns_number_total 4899 _reflns_number_gt 4581 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0568P)^2^+0.2541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.092(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4899 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Cr1 Cr 0.396921(15) 0.25981(2) 0.627108(9) 0.01775(9) Uani 1 1 d . . . C1 C 0.47281(9) 0.19870(15) 0.74016(5) 0.01959(18) Uani 1 1 d . . . C2 C 0.57888(9) 0.20644(15) 0.70102(5) 0.01878(18) Uani 1 1 d . . . C3 C 0.59414(10) 0.36182(15) 0.65781(6) 0.02177(19) Uani 1 1 d . . . H3 H 0.6619 0.3659 0.6297 0.026 Uiso 1 1 calc R . . C4 C 0.50923(12) 0.51115(15) 0.65614(7) 0.0246(2) Uani 1 1 d . . . H4 H 0.5209 0.6151 0.6270 0.030 Uiso 1 1 calc R . . C5 C 0.40797(12) 0.50839(15) 0.69680(7) 0.0253(2) Uani 1 1 d . . . H5 H 0.3535 0.6116 0.6971 0.030 Uiso 1 1 calc R . . C6 C 0.38852(10) 0.34989(16) 0.73716(6) 0.0227(2) Uani 1 1 d . . . H6 H 0.3176 0.3443 0.7628 0.027 Uiso 1 1 calc R . . S1 S 0.44444(3) -0.00030(4) 0.789759(15) 0.02400(9) Uani 1 1 d . . . C7 C 0.53220(13) 0.05525(19) 0.87705(7) 0.0303(2) Uani 1 1 d . . . H7A H 0.5512 -0.0605 0.9041 0.036 Uiso 1 1 calc R . . H7B H 0.6136 0.1121 0.8694 0.036 Uiso 1 1 calc R . . C8 C 0.46373(19) 0.1837(2) 0.92188(8) 0.0442(3) Uani 1 1 d . . . H8A H 0.3844 0.1267 0.9313 0.066 Uiso 1 1 calc R . . H8B H 0.4456 0.2996 0.8959 0.066 Uiso 1 1 calc R . . H8C H 0.5167 0.2081 0.9675 0.066 Uiso 1 1 calc R . . S2 S 0.68381(3) 0.01951(4) 0.710748(17) 0.02571(9) Uani 1 1 d . . . C9 C 0.81039(10) 0.08766(18) 0.66075(6) 0.0264(2) Uani 1 1 d . . . H9A H 0.8289 0.2196 0.6701 0.032 Uiso 1 1 calc R . . H9B H 0.8871 0.0173 0.6792 0.032 Uiso 1 1 calc R . . C10 C 0.78362(14) 0.0589(2) 0.58031(7) 0.0352(3) Uani 1 1 d . . . H10A H 0.7146 0.1400 0.5604 0.053 Uiso 1 1 calc R . . H10B H 0.7595 -0.0696 0.5703 0.053 Uiso 1 1 calc R . . H10C H 0.8595 0.0876 0.5582 0.053 Uiso 1 1 calc R . . C11 C 0.35851(12) 0.36008(17) 0.53671(6) 0.0272(2) Uani 1 1 d . . . O11 O 0.33087(12) 0.42292(18) 0.48048(6) 0.0444(3) Uani 1 1 d . . . C12 C 0.22972(11) 0.19587(17) 0.62126(6) 0.0258(2) Uani 1 1 d . . . O12 O 0.12464(10) 0.15337(16) 0.61592(7) 0.0420(3) Uani 1 1 d . . . C13 C 0.42455(13) 0.03369(17) 0.58686(7) 0.0288(2) Uani 1 1 d . . . O13 O 0.44045(13) -0.10896(15) 0.56297(6) 0.0473(3) Uani 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 Cr1 0.01732(12) 0.01759(11) 0.01733(11) 0.00090(5) -0.00157(7) 0.00156(5) C1 0.0180(4) 0.0224(4) 0.0177(4) 0.0014(3) -0.0003(3) -0.0013(3) C2 0.0159(4) 0.0206(4) 0.0188(4) 0.0028(3) -0.0013(3) -0.0006(3) C3 0.0190(4) 0.0221(4) 0.0233(4) 0.0040(3) -0.0006(3) -0.0017(3) C4 0.0260(5) 0.0188(4) 0.0277(5) 0.0023(4) -0.0018(4) -0.0014(3) C5 0.0266(5) 0.0206(5) 0.0273(5) -0.0039(4) -0.0019(4) 0.0033(4) C6 0.0206(4) 0.0262(5) 0.0209(4) -0.0026(4) 0.0006(3) 0.0011(4) S1 0.02376(15) 0.02599(15) 0.02185(15) 0.00434(9) 0.00146(10) -0.00516(9) C7 0.0332(6) 0.0347(6) 0.0217(5) 0.0046(4) -0.0016(4) -0.0014(5) C8 0.0601(10) 0.0446(8) 0.0284(6) -0.0034(6) 0.0075(6) 0.0013(7) S2 0.02025(14) 0.02775(15) 0.02886(16) 0.00952(10) 0.00213(10) 0.00622(9) C9 0.0182(4) 0.0340(6) 0.0266(5) 0.0009(4) 0.0014(4) 0.0025(4) C10 0.0360(6) 0.0422(7) 0.0273(6) -0.0027(5) 0.0045(5) 0.0024(5) C11 0.0288(5) 0.0278(5) 0.0236(5) 0.0038(4) -0.0021(4) -0.0008(4) O11 0.0549(7) 0.0477(6) 0.0276(5) 0.0142(4) -0.0059(4) -0.0028(5) C12 0.0244(5) 0.0261(5) 0.0262(5) -0.0030(4) 0.0004(4) -0.0015(4) O12 0.0254(4) 0.0449(6) 0.0552(7) -0.0125(5) 0.0038(4) -0.0091(4) C13 0.0323(6) 0.0257(5) 0.0254(5) -0.0015(4) -0.0079(4) 0.0066(4) O13 0.0672(8) 0.0303(5) 0.0390(6) -0.0096(4) -0.0139(5) 0.0175(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C12 1.8357(12) . ? Cr1 C11 1.8448(12) . ? Cr1 C13 1.8486(13) . ? Cr1 C6 2.1816(11) . ? Cr1 C4 2.2147(11) . ? Cr1 C1 2.2180(10) . ? Cr1 C5 2.2252(11) . ? Cr1 C3 2.2383(11) . ? Cr1 C2 2.2717(10) . ? C1 C6 1.4173(15) . ? C1 C2 1.4300(14) . ? C1 S1 1.7677(11) . ? C2 C3 1.4124(15) . ? C2 S2 1.7560(11) . ? C3 C4 1.4124(16) . ? C4 C5 1.4034(18) . ? C5 C6 1.4091(17) . ? S1 C7 1.8257(13) . ? C7 C8 1.509(2) . ? S2 C9 1.8128(12) . ? C9 C10 1.5159(18) . ? C11 O11 1.1536(15) . ? C12 O12 1.1565(15) . ? C13 O13 1.1509(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Cr1 C11 86.90(5) . . ? C12 Cr1 C13 87.50(6) . . ? C11 Cr1 C13 90.16(6) . . ? C12 Cr1 C6 88.48(5) . . ? C11 Cr1 C6 136.25(5) . . ? C13 Cr1 C6 133.06(5) . . ? C12 Cr1 C4 135.71(5) . . ? C11 Cr1 C4 87.12(5) . . ? C13 Cr1 C4 136.36(6) . . ? C6 Cr1 C4 66.84(5) . . ? C12 Cr1 C1 103.83(5) . . ? C11 Cr1 C1 166.12(5) . . ? C13 Cr1 C1 98.96(5) . . ? C6 Cr1 C1 37.57(4) . . ? C4 Cr1 C1 79.05(4) . . ? C12 Cr1 C5 102.58(5) . . ? C11 Cr1 C5 102.10(5) . . ? C13 Cr1 C5 164.42(5) . . ? C6 Cr1 C5 37.28(4) . . ? C4 Cr1 C5 36.85(5) . . ? C1 Cr1 C5 67.30(4) . . ? C12 Cr1 C3 167.44(5) . . ? C11 Cr1 C3 101.32(5) . . ? C13 Cr1 C3 101.82(5) . . ? C6 Cr1 C3 79.01(4) . . ? C4 Cr1 C3 36.98(4) . . ? C1 Cr1 C3 66.68(4) . . ? C5 Cr1 C3 66.61(4) . . ? C12 Cr1 C2 137.98(5) . . ? C11 Cr1 C2 134.50(5) . . ? C13 Cr1 C2 85.92(5) . . ? C6 Cr1 C2 66.98(4) . . ? C4 Cr1 C2 66.21(4) . . ? C1 Cr1 C2 37.12(4) . . ? C5 Cr1 C2 78.63(4) . . ? C3 Cr1 C2 36.49(4) . . ? C6 C1 C2 119.42(10) . . ? C6 C1 S1 120.24(8) . . ? C2 C1 S1 120.31(8) . . ? C6 C1 Cr1 69.82(6) . . ? C2 C1 Cr1 73.48(6) . . ? S1 C1 Cr1 127.02(6) . . ? C3 C2 C1 119.03(10) . . ? C3 C2 S2 123.96(8) . . ? C1 C2 S2 117.01(8) . . ? C3 C2 Cr1 70.47(6) . . ? C1 C2 Cr1 69.40(6) . . ? S2 C2 Cr1 132.87(6) . . ? C2 C3 C4 120.36(10) . . ? C2 C3 Cr1 73.04(6) . . ? C4 C3 Cr1 70.60(6) . . ? C5 C4 C3 121.02(10) . . ? C5 C4 Cr1 71.98(7) . . ? C3 C4 Cr1 72.42(6) . . ? C4 C5 C6 118.85(10) . . ? C4 C5 Cr1 71.17(7) . . ? C6 C5 Cr1 69.68(6) . . ? C5 C6 C1 121.18(10) . . ? C5 C6 Cr1 73.04(7) . . ? C1 C6 Cr1 72.61(6) . . ? C1 S1 C7 100.92(6) . . ? C8 C7 S1 114.11(11) . . ? C2 S2 C9 104.12(5) . . ? C10 C9 S2 114.94(9) . . ? O11 C11 Cr1 178.03(12) . . ? O12 C12 Cr1 178.25(12) . . ? O13 C13 Cr1 178.47(14) . . ? 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 C12 Cr1 C1 C6 -68.61(7) . . . . ? C11 Cr1 C1 C6 71.2(2) . . . . ? C13 Cr1 C1 C6 -158.22(7) . . . . ? C4 Cr1 C1 C6 66.08(7) . . . . ? C5 Cr1 C1 C6 29.45(7) . . . . ? C3 Cr1 C1 C6 102.69(7) . . . . ? C2 Cr1 C1 C6 130.91(9) . . . . ? C12 Cr1 C1 C2 160.49(7) . . . . ? C11 Cr1 C1 C2 -59.7(2) . . . . ? C13 Cr1 C1 C2 70.87(7) . . . . ? C6 Cr1 C1 C2 -130.91(9) . . . . ? C4 Cr1 C1 C2 -64.83(7) . . . . ? C5 Cr1 C1 C2 -101.46(7) . . . . ? C3 Cr1 C1 C2 -28.21(6) . . . . ? C12 Cr1 C1 S1 44.65(8) . . . . ? C11 Cr1 C1 S1 -175.50(18) . . . . ? C13 Cr1 C1 S1 -44.96(8) . . . . ? C6 Cr1 C1 S1 113.26(10) . . . . ? C4 Cr1 C1 S1 179.34(8) . . . . ? C5 Cr1 C1 S1 142.71(8) . . . . ? C3 Cr1 C1 S1 -144.05(8) . . . . ? C2 Cr1 C1 S1 -115.83(10) . . . . ? C6 C1 C2 C3 -2.63(15) . . . . ? S1 C1 C2 C3 175.55(8) . . . . ? Cr1 C1 C2 C3 51.90(9) . . . . ? C6 C1 C2 S2 176.85(8) . . . . ? S1 C1 C2 S2 -4.97(12) . . . . ? Cr1 C1 C2 S2 -128.62(7) . . . . ? C6 C1 C2 Cr1 -54.53(9) . . . . ? S1 C1 C2 Cr1 123.65(8) . . . . ? C12 Cr1 C2 C3 -162.09(8) . . . . ? C11 Cr1 C2 C3 30.01(10) . . . . ? C13 Cr1 C2 C3 116.22(8) . . . . ? C6 Cr1 C2 C3 -103.06(7) . . . . ? C4 Cr1 C2 C3 -29.31(7) . . . . ? C1 Cr1 C2 C3 -133.11(10) . . . . ? C5 Cr1 C2 C3 -65.85(7) . . . . ? C12 Cr1 C2 C1 -28.99(10) . . . . ? C11 Cr1 C2 C1 163.12(8) . . . . ? C13 Cr1 C2 C1 -110.67(8) . . . . ? C6 Cr1 C2 C1 30.05(6) . . . . ? C4 Cr1 C2 C1 103.80(7) . . . . ? C5 Cr1 C2 C1 67.26(7) . . . . ? C3 Cr1 C2 C1 133.11(10) . . . . ? C12 Cr1 C2 S2 79.26(10) . . . . ? C11 Cr1 C2 S2 -88.64(9) . . . . ? C13 Cr1 C2 S2 -2.43(8) . . . . ? C6 Cr1 C2 S2 138.29(9) . . . . ? C4 Cr1 C2 S2 -147.95(9) . . . . ? C1 Cr1 C2 S2 108.24(10) . . . . ? C5 Cr1 C2 S2 175.50(8) . . . . ? C3 Cr1 C2 S2 -118.65(11) . . . . ? C1 C2 C3 C4 3.08(16) . . . . ? S2 C2 C3 C4 -176.37(9) . . . . ? Cr1 C2 C3 C4 54.48(9) . . . . ? C1 C2 C3 Cr1 -51.40(9) . . . . ? S2 C2 C3 Cr1 129.15(8) . . . . ? C12 Cr1 C3 C2 71.2(2) . . . . ? C11 Cr1 C3 C2 -158.67(7) . . . . ? C13 Cr1 C3 C2 -66.10(8) . . . . ? C6 Cr1 C3 C2 65.97(7) . . . . ? C4 Cr1 C3 C2 131.88(10) . . . . ? C1 Cr1 C3 C2 28.67(6) . . . . ? C5 Cr1 C3 C2 102.92(7) . . . . ? C12 Cr1 C3 C4 -60.7(2) . . . . ? C11 Cr1 C3 C4 69.45(8) . . . . ? C13 Cr1 C3 C4 162.03(8) . . . . ? C6 Cr1 C3 C4 -65.91(7) . . . . ? C1 Cr1 C3 C4 -103.21(7) . . . . ? C5 Cr1 C3 C4 -28.95(7) . . . . ? C2 Cr1 C3 C4 -131.88(10) . . . . ? C2 C3 C4 C5 -0.32(17) . . . . ? Cr1 C3 C4 C5 55.30(10) . . . . ? C2 C3 C4 Cr1 -55.63(9) . . . . ? C12 Cr1 C4 C5 32.05(10) . . . . ? C11 Cr1 C4 C5 114.64(8) . . . . ? C13 Cr1 C4 C5 -158.15(8) . . . . ? C6 Cr1 C4 C5 -29.28(7) . . . . ? C1 Cr1 C4 C5 -66.60(7) . . . . ? C3 Cr1 C4 C5 -132.19(10) . . . . ? C2 Cr1 C4 C5 -103.25(8) . . . . ? C12 Cr1 C4 C3 164.24(7) . . . . ? C11 Cr1 C4 C3 -113.17(8) . . . . ? C13 Cr1 C4 C3 -25.95(10) . . . . ? C6 Cr1 C4 C3 102.91(7) . . . . ? C1 Cr1 C4 C3 65.59(7) . . . . ? C5 Cr1 C4 C3 132.19(10) . . . . ? C2 Cr1 C4 C3 28.94(6) . . . . ? C3 C4 C5 C6 -2.87(17) . . . . ? Cr1 C4 C5 C6 52.64(10) . . . . ? C3 C4 C5 Cr1 -55.51(10) . . . . ? C12 Cr1 C5 C4 -157.69(7) . . . . ? C11 Cr1 C5 C4 -68.19(8) . . . . ? C13 Cr1 C5 C4 73.0(2) . . . . ? C6 Cr1 C5 C4 132.07(10) . . . . ? C1 Cr1 C5 C4 102.40(7) . . . . ? C3 Cr1 C5 C4 29.05(7) . . . . ? C2 Cr1 C5 C4 65.29(7) . . . . ? C12 Cr1 C5 C6 70.25(8) . . . . ? C11 Cr1 C5 C6 159.74(7) . . . . ? C13 Cr1 C5 C6 -59.1(2) . . . . ? C4 Cr1 C5 C6 -132.07(10) . . . . ? C1 Cr1 C5 C6 -29.67(6) . . . . ? C3 Cr1 C5 C6 -103.02(7) . . . . ? C2 Cr1 C5 C6 -66.77(7) . . . . ? C4 C5 C6 C1 3.30(17) . . . . ? Cr1 C5 C6 C1 56.65(10) . . . . ? C4 C5 C6 Cr1 -53.34(10) . . . . ? C2 C1 C6 C5 -0.56(16) . . . . ? S1 C1 C6 C5 -178.74(8) . . . . ? Cr1 C1 C6 C5 -56.85(10) . . . . ? C2 C1 C6 Cr1 56.29(9) . . . . ? S1 C1 C6 Cr1 -121.89(8) . . . . ? C12 Cr1 C6 C5 -113.24(8) . . . . ? C11 Cr1 C6 C5 -29.31(10) . . . . ? C13 Cr1 C6 C5 161.62(8) . . . . ? C4 Cr1 C6 C5 28.96(7) . . . . ? C1 Cr1 C6 C5 131.51(10) . . . . ? C3 Cr1 C6 C5 65.64(7) . . . . ? C2 Cr1 C6 C5 101.80(7) . . . . ? C12 Cr1 C6 C1 115.26(7) . . . . ? C11 Cr1 C6 C1 -160.82(7) . . . . ? C13 Cr1 C6 C1 30.11(10) . . . . ? C4 Cr1 C6 C1 -102.55(7) . . . . ? C5 Cr1 C6 C1 -131.51(10) . . . . ? C3 Cr1 C6 C1 -65.87(6) . . . . ? C2 Cr1 C6 C1 -29.71(6) . . . . ? C6 C1 S1 C7 -91.27(10) . . . . ? C2 C1 S1 C7 90.57(9) . . . . ? Cr1 C1 S1 C7 -177.81(7) . . . . ? C1 S1 C7 C8 79.68(12) . . . . ? C3 C2 S2 C9 4.41(11) . . . . ? C1 C2 S2 C9 -175.04(8) . . . . ? Cr1 C2 S2 C9 98.72(8) . . . . ? C2 S2 C9 C10 -81.13(11) . . . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.426 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.071 data_10e _database_code_depnum_ccdc_archive 'CCDC 830656' #TrackingRef 'Weaver.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H18 Cr O3 S2' _chemical_formula_sum 'C23 H18 Cr O3 S2' _chemical_formula_weight 458.49 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' 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 9.0130(9) _cell_length_b 10.2094(10) _cell_length_c 12.8603(13) _cell_angle_alpha 106.7566(15) _cell_angle_beta 99.0147(16) _cell_angle_gamma 109.5597(15) _cell_volume 1024.82(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5322 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9059 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.92 _reflns_number_total 4714 _reflns_number_gt 3947 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0365P)^2^+0.4913P] 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 4714 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 -0.25394(3) 0.08699(3) 0.83026(2) 0.02338(9) Uani 1 1 d . . . C1 C -0.0594(2) 0.15815(19) 0.74359(14) 0.0228(3) Uani 1 1 d . . . C2 C -0.1804(2) 0.21516(19) 0.71956(14) 0.0235(3) Uani 1 1 d . . . C3 C -0.2192(2) 0.3023(2) 0.80908(16) 0.0287(4) Uani 1 1 d . . . H3 H -0.2975 0.3423 0.7931 0.034 Uiso 1 1 calc R . . C4 C -0.1424(2) 0.3307(2) 0.92252(16) 0.0324(4) Uani 1 1 d . . . H4 H -0.1704 0.3884 0.9824 0.039 Uiso 1 1 calc R . . C5 C -0.0254(2) 0.2741(2) 0.94688(15) 0.0306(4) Uani 1 1 d . . . H5 H 0.0272 0.2943 1.0232 0.037 Uiso 1 1 calc R . . C6 C 0.0144(2) 0.1864(2) 0.85712(15) 0.0264(4) Uani 1 1 d . . . H6 H 0.0921 0.1462 0.8739 0.032 Uiso 1 1 calc R . . S1 S -0.01580(5) 0.04786(5) 0.62843(4) 0.02509(10) Uani 1 1 d . . . C7 C 0.2005(2) 0.0869(2) 0.68438(16) 0.0287(4) Uani 1 1 d . . . H7A H 0.2145 0.0639 0.7541 0.034 Uiso 1 1 calc R . . H7B H 0.2326 0.0204 0.6283 0.034 Uiso 1 1 calc R . . C8 C 0.3124(2) 0.2463(2) 0.71091(15) 0.0259(4) Uani 1 1 d . . . C9 C 0.3831(2) 0.3479(2) 0.82192(16) 0.0337(4) Uani 1 1 d . . . H9 H 0.3623 0.3161 0.8826 0.040 Uiso 1 1 calc R . . C10 C 0.4839(3) 0.4955(2) 0.84449(18) 0.0418(5) Uani 1 1 d . . . H10 H 0.5303 0.5644 0.9204 0.050 Uiso 1 1 calc R . . C11 C 0.5167(3) 0.5423(2) 0.7572(2) 0.0443(5) Uani 1 1 d . . . H11 H 0.5861 0.6432 0.7729 0.053 Uiso 1 1 calc R . . C12 C 0.4487(3) 0.4424(3) 0.64706(19) 0.0447(5) Uani 1 1 d . . . H12 H 0.4713 0.4745 0.5867 0.054 Uiso 1 1 calc R . . C13 C 0.3474(2) 0.2954(2) 0.62421(16) 0.0348(4) Uani 1 1 d . . . H13 H 0.3013 0.2272 0.5480 0.042 Uiso 1 1 calc R . . S2 S -0.28617(5) 0.17692(5) 0.57816(4) 0.02689(11) Uani 1 1 d . . . C14 C -0.1241(2) 0.3070(2) 0.54161(15) 0.0283(4) Uani 1 1 d . . . H14A H -0.0333 0.2733 0.5393 0.034 Uiso 1 1 calc R . . H14B H -0.1689 0.3034 0.4650 0.034 Uiso 1 1 calc R . . C15 C -0.0569(2) 0.4659(2) 0.62337(15) 0.0269(4) Uani 1 1 d . . . C16 C 0.0921(3) 0.5254(2) 0.70570(17) 0.0348(4) Uani 1 1 d . . . H16 H 0.1521 0.4654 0.7098 0.042 Uiso 1 1 calc R . . C17 C 0.1544(3) 0.6717(3) 0.78214(19) 0.0480(6) Uani 1 1 d . . . H17 H 0.2572 0.7114 0.8373 0.058 Uiso 1 1 calc R . . C18 C 0.0683(4) 0.7592(3) 0.7783(2) 0.0523(7) Uani 1 1 d . . . H18 H 0.1104 0.8588 0.8312 0.063 Uiso 1 1 calc R . . C19 C -0.0796(4) 0.7020(3) 0.6973(3) 0.0552(7) Uani 1 1 d . . . H19 H -0.1395 0.7623 0.6944 0.066 Uiso 1 1 calc R . . C20 C -0.1417(3) 0.5562(2) 0.6197(2) 0.0420(5) Uani 1 1 d . . . H20 H -0.2433 0.5181 0.5636 0.050 Uiso 1 1 calc R . . C21 C -0.2235(2) -0.0350(2) 0.90531(15) 0.0264(4) Uani 1 1 d . . . O21 O -0.20261(17) -0.11176(15) 0.95133(12) 0.0351(3) Uani 1 1 d . . . C22 C -0.3844(2) -0.0843(2) 0.70494(16) 0.0314(4) Uani 1 1 d . . . O22 O -0.4645(2) -0.19237(17) 0.62860(12) 0.0466(4) Uani 1 1 d . . . C23 C -0.4375(2) 0.0784(2) 0.88001(17) 0.0326(4) Uani 1 1 d . . . O23 O -0.55027(19) 0.0743(2) 0.91265(14) 0.0483(4) Uani 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 Cr1 0.02407(15) 0.02382(15) 0.02054(15) 0.01104(12) 0.00507(11) 0.00567(11) C1 0.0224(8) 0.0212(8) 0.0210(8) 0.0088(7) 0.0050(7) 0.0037(7) C2 0.0245(8) 0.0224(8) 0.0240(8) 0.0127(7) 0.0071(7) 0.0059(7) C3 0.0313(10) 0.0244(9) 0.0345(10) 0.0145(8) 0.0142(8) 0.0108(8) C4 0.0393(11) 0.0224(9) 0.0294(10) 0.0067(8) 0.0151(8) 0.0053(8) C5 0.0317(10) 0.0289(9) 0.0211(9) 0.0086(7) 0.0052(7) 0.0016(8) C6 0.0238(9) 0.0256(9) 0.0245(9) 0.0113(7) 0.0033(7) 0.0034(7) S1 0.0236(2) 0.0251(2) 0.0225(2) 0.00679(17) 0.00378(17) 0.00787(17) C7 0.0264(9) 0.0270(9) 0.0326(10) 0.0102(8) 0.0045(8) 0.0128(7) C8 0.0204(8) 0.0277(9) 0.0272(9) 0.0078(7) 0.0048(7) 0.0095(7) C9 0.0328(10) 0.0356(11) 0.0252(9) 0.0109(8) 0.0053(8) 0.0063(8) C10 0.0404(12) 0.0339(11) 0.0282(10) 0.0010(9) 0.0015(9) 0.0002(9) C11 0.0384(12) 0.0309(11) 0.0460(13) 0.0135(10) 0.0053(10) -0.0034(9) C12 0.0373(11) 0.0506(13) 0.0356(11) 0.0220(10) 0.0091(9) 0.0003(10) C13 0.0286(10) 0.0415(11) 0.0242(9) 0.0082(8) 0.0065(8) 0.0057(8) S2 0.0245(2) 0.0293(2) 0.0267(2) 0.01534(19) 0.00397(17) 0.00765(18) C14 0.0328(10) 0.0297(9) 0.0253(9) 0.0160(8) 0.0109(8) 0.0101(8) C15 0.0341(10) 0.0277(9) 0.0279(9) 0.0177(8) 0.0161(8) 0.0134(8) C16 0.0408(11) 0.0324(10) 0.0338(11) 0.0164(9) 0.0102(9) 0.0143(9) C17 0.0602(15) 0.0371(12) 0.0328(12) 0.0126(10) 0.0088(11) 0.0053(11) C18 0.0829(19) 0.0290(11) 0.0488(14) 0.0164(10) 0.0413(14) 0.0149(12) C19 0.0717(18) 0.0364(13) 0.089(2) 0.0370(14) 0.0528(17) 0.0340(13) C20 0.0391(12) 0.0400(12) 0.0626(15) 0.0313(11) 0.0215(11) 0.0206(10) C21 0.0240(9) 0.0272(9) 0.0220(9) 0.0078(7) 0.0042(7) 0.0051(7) O21 0.0387(8) 0.0354(8) 0.0328(7) 0.0191(6) 0.0052(6) 0.0133(6) C22 0.0330(10) 0.0323(10) 0.0267(10) 0.0180(8) 0.0052(8) 0.0058(8) O22 0.0530(10) 0.0343(8) 0.0304(8) 0.0108(7) -0.0050(7) -0.0003(7) C23 0.0332(10) 0.0369(11) 0.0335(10) 0.0224(9) 0.0095(8) 0.0129(8) O23 0.0386(8) 0.0716(11) 0.0591(10) 0.0441(9) 0.0266(8) 0.0281(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 C21 1.8436(19) . ? Cr1 C23 1.850(2) . ? Cr1 C22 1.855(2) . ? Cr1 C4 2.2038(19) . ? Cr1 C5 2.2105(19) . ? Cr1 C6 2.2116(18) . ? Cr1 C3 2.2168(18) . ? Cr1 C2 2.2287(17) . ? Cr1 C1 2.2517(17) . ? C1 C6 1.408(2) . ? C1 C2 1.431(2) . ? C1 S1 1.7701(18) . ? C2 C3 1.408(3) . ? C2 S2 1.7792(18) . ? C3 C4 1.413(3) . ? C4 C5 1.397(3) . ? C5 C6 1.418(3) . ? S1 C7 1.8312(18) . ? C7 C8 1.502(3) . ? C8 C13 1.386(3) . ? C8 C9 1.392(3) . ? C9 C10 1.388(3) . ? C10 C11 1.377(3) . ? C11 C12 1.378(3) . ? C12 C13 1.385(3) . ? S2 C14 1.8422(18) . ? C14 C15 1.504(3) . ? C15 C20 1.387(3) . ? C15 C16 1.389(3) . ? C16 C17 1.390(3) . ? C17 C18 1.371(4) . ? C18 C19 1.377(4) . ? C19 C20 1.391(3) . ? C21 O21 1.153(2) . ? C22 O22 1.150(2) . ? C23 O23 1.152(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Cr1 C23 88.86(8) . . ? C21 Cr1 C22 87.90(8) . . ? C23 Cr1 C22 89.23(9) . . ? C21 Cr1 C4 118.79(8) . . ? C23 Cr1 C4 89.13(8) . . ? C22 Cr1 C4 153.21(8) . . ? C21 Cr1 C5 90.74(8) . . ? C23 Cr1 C5 113.49(8) . . ? C22 Cr1 C5 157.21(8) . . ? C4 Cr1 C5 36.89(8) . . ? C21 Cr1 C6 88.47(7) . . ? C23 Cr1 C6 150.71(8) . . ? C22 Cr1 C6 119.80(8) . . ? C4 Cr1 C6 66.90(7) . . ? C5 Cr1 C6 37.41(7) . . ? C21 Cr1 C3 155.94(8) . . ? C23 Cr1 C3 92.43(8) . . ? C22 Cr1 C3 116.12(8) . . ? C4 Cr1 C3 37.28(7) . . ? C5 Cr1 C3 66.76(7) . . ? C6 Cr1 C3 78.75(7) . . ? C21 Cr1 C2 150.64(7) . . ? C23 Cr1 C2 120.47(7) . . ? C22 Cr1 C2 91.02(7) . . ? C4 Cr1 C2 67.06(7) . . ? C5 Cr1 C2 79.18(7) . . ? C6 Cr1 C2 66.77(6) . . ? C3 Cr1 C2 36.92(7) . . ? C21 Cr1 C1 113.50(7) . . ? C23 Cr1 C1 157.60(8) . . ? C22 Cr1 C1 92.87(7) . . ? C4 Cr1 C1 79.04(7) . . ? C5 Cr1 C1 66.90(7) . . ? C6 Cr1 C1 36.75(6) . . ? C3 Cr1 C1 66.67(7) . . ? C2 Cr1 C1 37.24(6) . . ? C6 C1 C2 118.81(16) . . ? C6 C1 S1 122.84(14) . . ? C2 C1 S1 118.29(13) . . ? C6 C1 Cr1 70.07(10) . . ? C2 C1 Cr1 70.51(10) . . ? S1 C1 Cr1 129.05(9) . . ? C3 C2 C1 119.81(16) . . ? C3 C2 S2 118.66(14) . . ? C1 C2 S2 121.52(13) . . ? C3 C2 Cr1 71.08(10) . . ? C1 C2 Cr1 72.25(10) . . ? S2 C2 Cr1 128.21(9) . . ? C2 C3 C4 120.44(18) . . ? C2 C3 Cr1 72.00(10) . . ? C4 C3 Cr1 70.86(11) . . ? C5 C4 C3 120.20(17) . . ? C5 C4 Cr1 71.82(11) . . ? C3 C4 Cr1 71.86(11) . . ? C4 C5 C6 119.66(17) . . ? C4 C5 Cr1 71.29(11) . . ? C6 C5 Cr1 71.33(10) . . ? C1 C6 C5 121.04(17) . . ? C1 C6 Cr1 73.17(10) . . ? C5 C6 Cr1 71.25(11) . . ? C1 S1 C7 103.32(8) . . ? C8 C7 S1 112.85(12) . . ? C13 C8 C9 118.45(18) . . ? C13 C8 C7 120.15(17) . . ? C9 C8 C7 121.39(17) . . ? C10 C9 C8 120.47(19) . . ? C11 C10 C9 120.23(19) . . ? C10 C11 C12 119.8(2) . . ? C11 C12 C13 120.1(2) . . ? C12 C13 C8 120.92(18) . . ? C2 S2 C14 99.63(8) . . ? C15 C14 S2 113.47(13) . . ? C20 C15 C16 118.25(19) . . ? C20 C15 C14 121.31(19) . . ? C16 C15 C14 120.44(17) . . ? C15 C16 C17 120.8(2) . . ? C18 C17 C16 120.3(2) . . ? C17 C18 C19 119.7(2) . . ? C18 C19 C20 120.3(2) . . ? C15 C20 C19 120.7(2) . . ? O21 C21 Cr1 178.88(17) . . ? O22 C22 Cr1 178.44(17) . . ? O23 C23 Cr1 179.0(2) . . ? 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 C21 Cr1 C1 C6 -50.90(12) . . . . ? C23 Cr1 C1 C6 125.2(2) . . . . ? C22 Cr1 C1 C6 -139.86(12) . . . . ? C4 Cr1 C1 C6 65.89(11) . . . . ? C5 Cr1 C1 C6 29.30(11) . . . . ? C3 Cr1 C1 C6 102.85(12) . . . . ? C2 Cr1 C1 C6 132.23(15) . . . . ? C21 Cr1 C1 C2 176.87(10) . . . . ? C23 Cr1 C1 C2 -7.0(2) . . . . ? C22 Cr1 C1 C2 87.91(11) . . . . ? C4 Cr1 C1 C2 -66.34(11) . . . . ? C5 Cr1 C1 C2 -102.92(11) . . . . ? C6 Cr1 C1 C2 -132.23(15) . . . . ? C3 Cr1 C1 C2 -29.38(10) . . . . ? C21 Cr1 C1 S1 65.75(13) . . . . ? C23 Cr1 C1 S1 -118.2(2) . . . . ? C22 Cr1 C1 S1 -23.21(13) . . . . ? C4 Cr1 C1 S1 -177.46(13) . . . . ? C5 Cr1 C1 S1 145.96(14) . . . . ? C6 Cr1 C1 S1 116.66(17) . . . . ? C3 Cr1 C1 S1 -140.50(13) . . . . ? C2 Cr1 C1 S1 -111.12(16) . . . . ? C6 C1 C2 C3 2.2(2) . . . . ? S1 C1 C2 C3 179.49(13) . . . . ? Cr1 C1 C2 C3 54.84(14) . . . . ? C6 C1 C2 S2 -177.05(13) . . . . ? S1 C1 C2 S2 0.2(2) . . . . ? Cr1 C1 C2 S2 -124.44(12) . . . . ? C6 C1 C2 Cr1 -52.60(14) . . . . ? S1 C1 C2 Cr1 124.64(11) . . . . ? C21 Cr1 C2 C3 -137.28(15) . . . . ? C23 Cr1 C2 C3 45.47(14) . . . . ? C22 Cr1 C2 C3 135.18(12) . . . . ? C4 Cr1 C2 C3 -28.97(11) . . . . ? C5 Cr1 C2 C3 -65.52(11) . . . . ? C6 Cr1 C2 C3 -102.59(12) . . . . ? C1 Cr1 C2 C3 -131.42(15) . . . . ? C21 Cr1 C2 C1 -5.86(19) . . . . ? C23 Cr1 C2 C1 176.89(11) . . . . ? C22 Cr1 C2 C1 -93.40(11) . . . . ? C4 Cr1 C2 C1 102.45(11) . . . . ? C5 Cr1 C2 C1 65.89(11) . . . . ? C6 Cr1 C2 C1 28.83(10) . . . . ? C3 Cr1 C2 C1 131.42(15) . . . . ? C21 Cr1 C2 S2 110.66(16) . . . . ? C23 Cr1 C2 S2 -66.59(15) . . . . ? C22 Cr1 C2 S2 23.13(13) . . . . ? C4 Cr1 C2 S2 -141.02(14) . . . . ? C5 Cr1 C2 S2 -177.58(13) . . . . ? C6 Cr1 C2 S2 145.35(14) . . . . ? C3 Cr1 C2 S2 -112.06(17) . . . . ? C1 Cr1 C2 S2 116.52(16) . . . . ? C1 C2 C3 C4 -1.6(3) . . . . ? S2 C2 C3 C4 177.68(14) . . . . ? Cr1 C2 C3 C4 53.78(15) . . . . ? C1 C2 C3 Cr1 -55.40(14) . . . . ? S2 C2 C3 Cr1 123.90(12) . . . . ? C21 Cr1 C3 C2 125.31(18) . . . . ? C23 Cr1 C3 C2 -142.05(12) . . . . ? C22 Cr1 C3 C2 -51.71(13) . . . . ? C4 Cr1 C3 C2 132.59(17) . . . . ? C5 Cr1 C3 C2 103.37(12) . . . . ? C6 Cr1 C3 C2 66.12(11) . . . . ? C1 Cr1 C3 C2 29.62(10) . . . . ? C21 Cr1 C3 C4 -7.3(2) . . . . ? C23 Cr1 C3 C4 85.36(12) . . . . ? C22 Cr1 C3 C4 175.70(12) . . . . ? C5 Cr1 C3 C4 -29.22(11) . . . . ? C6 Cr1 C3 C4 -66.47(12) . . . . ? C2 Cr1 C3 C4 -132.59(17) . . . . ? C1 Cr1 C3 C4 -102.97(12) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? Cr1 C3 C4 C5 55.21(16) . . . . ? C2 C3 C4 Cr1 -54.31(15) . . . . ? C21 Cr1 C4 C5 44.96(13) . . . . ? C23 Cr1 C4 C5 133.18(12) . . . . ? C22 Cr1 C4 C5 -140.26(18) . . . . ? C6 Cr1 C4 C5 -29.53(11) . . . . ? C3 Cr1 C4 C5 -131.66(17) . . . . ? C2 Cr1 C4 C5 -102.96(12) . . . . ? C1 Cr1 C4 C5 -65.95(11) . . . . ? C21 Cr1 C4 C3 176.62(11) . . . . ? C23 Cr1 C4 C3 -95.16(12) . . . . ? C22 Cr1 C4 C3 -8.6(2) . . . . ? C5 Cr1 C4 C3 131.66(17) . . . . ? C6 Cr1 C4 C3 102.14(12) . . . . ? C2 Cr1 C4 C3 28.70(11) . . . . ? C1 Cr1 C4 C3 65.71(11) . . . . ? C3 C4 C5 C6 -0.8(3) . . . . ? Cr1 C4 C5 C6 54.43(15) . . . . ? C3 C4 C5 Cr1 -55.23(16) . . . . ? C21 Cr1 C5 C4 -141.73(12) . . . . ? C23 Cr1 C5 C4 -52.65(13) . . . . ? C22 Cr1 C5 C4 131.9(2) . . . . ? C6 Cr1 C5 C4 131.75(16) . . . . ? C3 Cr1 C5 C4 29.51(11) . . . . ? C2 Cr1 C5 C4 66.02(11) . . . . ? C1 Cr1 C5 C4 102.93(12) . . . . ? C21 Cr1 C5 C6 86.52(12) . . . . ? C23 Cr1 C5 C6 175.60(11) . . . . ? C22 Cr1 C5 C6 0.2(3) . . . . ? C4 Cr1 C5 C6 -131.75(16) . . . . ? C3 Cr1 C5 C6 -102.24(12) . . . . ? C2 Cr1 C5 C6 -65.73(11) . . . . ? C1 Cr1 C5 C6 -28.82(10) . . . . ? C2 C1 C6 C5 -2.2(3) . . . . ? S1 C1 C6 C5 -179.29(13) . . . . ? Cr1 C1 C6 C5 -54.98(15) . . . . ? C2 C1 C6 Cr1 52.81(14) . . . . ? S1 C1 C6 Cr1 -124.30(13) . . . . ? C4 C5 C6 C1 1.5(3) . . . . ? Cr1 C5 C6 C1 55.88(15) . . . . ? C4 C5 C6 Cr1 -54.41(16) . . . . ? C21 Cr1 C6 C1 134.60(11) . . . . ? C23 Cr1 C6 C1 -140.45(15) . . . . ? C22 Cr1 C6 C1 47.90(13) . . . . ? C4 Cr1 C6 C1 -103.04(12) . . . . ? C5 Cr1 C6 C1 -132.18(16) . . . . ? C3 Cr1 C6 C1 -65.90(11) . . . . ? C2 Cr1 C6 C1 -29.19(10) . . . . ? C21 Cr1 C6 C5 -93.22(12) . . . . ? C23 Cr1 C6 C5 -8.3(2) . . . . ? C22 Cr1 C6 C5 -179.92(11) . . . . ? C4 Cr1 C6 C5 29.14(11) . . . . ? C3 Cr1 C6 C5 66.28(11) . . . . ? C2 Cr1 C6 C5 102.99(12) . . . . ? C1 Cr1 C6 C5 132.18(16) . . . . ? C6 C1 S1 C7 -33.42(16) . . . . ? C2 C1 S1 C7 149.45(14) . . . . ? Cr1 C1 S1 C7 -123.49(11) . . . . ? C1 S1 C7 C8 -65.33(15) . . . . ? S1 C7 C8 C13 -75.0(2) . . . . ? S1 C7 C8 C9 104.98(18) . . . . ? C13 C8 C9 C10 1.2(3) . . . . ? C7 C8 C9 C10 -178.86(19) . . . . ? C8 C9 C10 C11 -0.9(3) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C11 C12 C13 C8 0.2(3) . . . . ? C9 C8 C13 C12 -0.8(3) . . . . ? C7 C8 C13 C12 179.21(19) . . . . ? C3 C2 S2 C14 104.22(15) . . . . ? C1 C2 S2 C14 -76.49(15) . . . . ? Cr1 C2 S2 C14 -168.07(11) . . . . ? C2 S2 C14 C15 -54.49(15) . . . . ? S2 C14 C15 C20 -78.1(2) . . . . ? S2 C14 C15 C16 101.21(18) . . . . ? C20 C15 C16 C17 -0.1(3) . . . . ? C14 C15 C16 C17 -179.46(18) . . . . ? C15 C16 C17 C18 0.9(3) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C17 C18 C19 C20 0.0(3) . . . . ? C16 C15 C20 C19 -0.6(3) . . . . ? C14 C15 C20 C19 178.69(19) . . . . ? C18 C19 C20 C15 0.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.347 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.057 data_11e _database_code_depnum_ccdc_archive 'CCDC 830657' #TrackingRef 'Weaver.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Cr O3 S3' _chemical_formula_sum 'C30 H24 Cr O3 S3' _chemical_formula_weight 580.67 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' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.7886(7) _cell_length_b 24.6453(15) _cell_length_c 10.2118(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.6251(9) _cell_angle_gamma 90.00 _cell_volume 2675.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11345 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.82 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23396 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.99 _reflns_number_total 6468 _reflns_number_gt 5276 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0544P)^2^+2.4095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'all non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6468 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Cr1 Cr 0.11720(3) 0.151036(13) 0.33628(4) 0.02312(10) Uani 1 1 d . . . C1 C 0.23919(19) 0.08153(8) 0.3383(2) 0.0237(4) Uani 1 1 d . . . C2 C 0.30272(19) 0.11404(8) 0.4663(2) 0.0227(4) Uani 1 1 d . . . C3 C 0.32418(19) 0.17018(9) 0.4524(2) 0.0242(4) Uani 1 1 d . . . C4 C 0.2734(2) 0.19469(9) 0.3132(2) 0.0257(4) Uani 1 1 d . . . H4 H 0.2845 0.2324 0.3034 0.031 Uiso 1 1 calc R . . C5 C 0.2065(2) 0.16264(9) 0.1902(2) 0.0260(4) Uani 1 1 d . . . H5 H 0.1700 0.1794 0.0972 0.031 Uiso 1 1 calc R . . C6 C 0.1919(2) 0.10638(9) 0.2006(2) 0.0256(4) Uani 1 1 d . . . H6 H 0.1504 0.0852 0.1152 0.031 Uiso 1 1 calc R . . S1 S 0.22278(5) 0.01158(2) 0.36389(6) 0.02847(13) Uani 1 1 d . . . C7 C 0.1078(2) -0.00849(9) 0.1829(2) 0.0302(5) Uani 1 1 d . . . H7A H 0.0369 0.0176 0.1460 0.036 Uiso 1 1 calc R . . H7B H 0.1474 -0.0089 0.1149 0.036 Uiso 1 1 calc R . . C8 C 0.0608(2) -0.06447(9) 0.1942(2) 0.0263(4) Uani 1 1 d . . . C9 C 0.1056(2) -0.11017(10) 0.1507(2) 0.0299(5) Uani 1 1 d . . . H9 H 0.1665 -0.1062 0.1137 0.036 Uiso 1 1 calc R . . C10 C 0.0614(2) -0.16129(9) 0.1614(2) 0.0314(5) Uani 1 1 d . . . H10 H 0.0926 -0.1923 0.1321 0.038 Uiso 1 1 calc R . . C11 C -0.0270(2) -0.16749(9) 0.2142(2) 0.0323(5) Uani 1 1 d . . . H11 H -0.0568 -0.2027 0.2215 0.039 Uiso 1 1 calc R . . C12 C -0.0726(2) -0.12244(10) 0.2565(3) 0.0354(5) Uani 1 1 d . . . H12 H -0.1348 -0.1266 0.2916 0.042 Uiso 1 1 calc R . . C13 C -0.0277(2) -0.07109(9) 0.2478(3) 0.0328(5) Uani 1 1 d . . . H13 H -0.0580 -0.0403 0.2788 0.039 Uiso 1 1 calc R . . S2 S 0.35506(5) 0.08508(2) 0.64124(5) 0.02424(12) Uani 1 1 d . . . C14 C 0.5174(2) 0.06748(10) 0.6781(2) 0.0316(5) Uani 1 1 d . . . H14A H 0.5182 0.0368 0.6160 0.038 Uiso 1 1 calc R . . H14B H 0.5597 0.0989 0.6577 0.038 Uiso 1 1 calc R . . C15 C 0.5840(2) 0.05196(9) 0.8359(2) 0.0270(4) Uani 1 1 d . . . C16 C 0.6005(2) -0.00255(10) 0.8780(3) 0.0332(5) Uani 1 1 d . . . H16 H 0.5708 -0.0303 0.8064 0.040 Uiso 1 1 calc R . . C17 C 0.6599(2) -0.01624(11) 1.0235(3) 0.0385(6) Uani 1 1 d . . . H17 H 0.6707 -0.0534 1.0514 0.046 Uiso 1 1 calc R . . C18 C 0.7035(2) 0.02379(11) 1.1285(3) 0.0359(5) Uani 1 1 d . . . H18 H 0.7440 0.0141 1.2283 0.043 Uiso 1 1 calc R . . C19 C 0.6883(2) 0.07784(10) 1.0885(3) 0.0329(5) Uani 1 1 d . . . H19 H 0.7189 0.1054 1.1606 0.039 Uiso 1 1 calc R . . C20 C 0.6283(2) 0.09180(10) 0.9425(2) 0.0297(5) Uani 1 1 d . . . H20 H 0.6174 0.1290 0.9153 0.036 Uiso 1 1 calc R . . S3 S 0.41293(5) 0.20652(2) 0.61420(6) 0.02908(13) Uani 1 1 d . . . C21 C 0.4611(2) 0.26764(10) 0.5494(3) 0.0371(6) Uani 1 1 d . . . H21A H 0.5047 0.2579 0.4888 0.045 Uiso 1 1 calc R . . H21B H 0.3871 0.2903 0.4910 0.045 Uiso 1 1 calc R . . C22 C 0.5492(2) 0.29765(9) 0.6847(3) 0.0317(5) Uani 1 1 d . . . C23 C 0.6689(2) 0.27744(11) 0.7687(3) 0.0444(6) Uani 1 1 d . . . H23 H 0.6964 0.2453 0.7398 0.053 Uiso 1 1 calc R . . C24 C 0.7485(3) 0.30414(11) 0.8947(3) 0.0489(7) Uani 1 1 d . . . H24 H 0.8301 0.2900 0.9518 0.059 Uiso 1 1 calc R . . C25 C 0.7102(3) 0.35093(11) 0.9378(3) 0.0433(6) Uani 1 1 d . . . H25 H 0.7648 0.3690 1.0244 0.052 Uiso 1 1 calc R . . C26 C 0.5914(3) 0.37132(11) 0.8538(3) 0.0404(6) Uani 1 1 d . . . H26 H 0.5642 0.4036 0.8827 0.048 Uiso 1 1 calc R . . C27 C 0.5118(2) 0.34488(10) 0.7277(3) 0.0337(5) Uani 1 1 d . . . H27 H 0.4306 0.3594 0.6702 0.040 Uiso 1 1 calc R . . C28 C 0.0209(2) 0.09989(9) 0.3771(2) 0.0277(4) Uani 1 1 d . . . O28 O -0.03818(17) 0.06818(7) 0.4025(2) 0.0398(4) Uani 1 1 d . . . C29 C -0.0319(2) 0.17842(9) 0.1947(2) 0.0296(5) Uani 1 1 d . . . O29 O -0.12644(16) 0.19573(8) 0.1121(2) 0.0418(4) Uani 1 1 d . . . C30 C 0.0956(2) 0.19858(9) 0.4635(2) 0.0272(4) Uani 1 1 d . . . O30 O 0.08362(18) 0.22832(7) 0.54214(19) 0.0386(4) Uani 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 Cr1 0.02527(18) 0.02071(17) 0.01967(17) 0.00117(12) 0.00622(14) 0.00105(12) C1 0.0237(10) 0.0214(10) 0.0219(10) 0.0008(8) 0.0062(8) 0.0008(8) C2 0.0226(10) 0.0223(10) 0.0190(9) 0.0022(7) 0.0050(8) 0.0005(8) C3 0.0241(10) 0.0247(10) 0.0208(10) 0.0009(8) 0.0068(8) -0.0006(8) C4 0.0274(10) 0.0240(10) 0.0234(10) 0.0032(8) 0.0090(9) 0.0006(8) C5 0.0270(10) 0.0284(11) 0.0197(10) 0.0048(8) 0.0073(8) 0.0036(8) C6 0.0256(10) 0.0274(11) 0.0196(10) -0.0001(8) 0.0058(8) 0.0019(8) S1 0.0320(3) 0.0203(2) 0.0223(3) 0.00108(19) 0.0016(2) 0.0011(2) C7 0.0336(12) 0.0260(11) 0.0215(10) -0.0006(8) 0.0030(9) -0.0014(9) C8 0.0259(10) 0.0258(10) 0.0191(10) -0.0022(8) 0.0022(8) -0.0002(8) C9 0.0279(11) 0.0332(12) 0.0258(11) -0.0049(9) 0.0089(9) -0.0002(9) C10 0.0346(12) 0.0285(11) 0.0255(11) -0.0061(9) 0.0079(9) 0.0027(9) C11 0.0396(13) 0.0264(11) 0.0258(11) -0.0001(9) 0.0091(10) -0.0040(9) C12 0.0385(13) 0.0365(13) 0.0350(13) -0.0002(10) 0.0194(11) -0.0008(10) C13 0.0373(13) 0.0273(11) 0.0330(12) -0.0019(9) 0.0145(10) 0.0057(9) S2 0.0239(2) 0.0263(3) 0.0176(2) 0.00394(18) 0.00430(19) 0.00122(19) C14 0.0260(11) 0.0422(13) 0.0220(11) 0.0057(9) 0.0059(9) 0.0083(9) C15 0.0223(10) 0.0335(11) 0.0216(10) 0.0058(8) 0.0062(8) 0.0049(8) C16 0.0309(12) 0.0316(12) 0.0287(11) 0.0005(9) 0.0050(9) 0.0018(9) C17 0.0366(13) 0.0342(13) 0.0355(13) 0.0119(10) 0.0070(11) 0.0039(10) C18 0.0280(11) 0.0491(15) 0.0225(11) 0.0093(10) 0.0034(9) 0.0022(10) C19 0.0265(11) 0.0425(13) 0.0252(11) -0.0031(9) 0.0069(9) -0.0017(10) C20 0.0264(11) 0.0302(11) 0.0293(11) 0.0034(9) 0.0091(9) 0.0016(9) S3 0.0318(3) 0.0259(3) 0.0225(3) -0.0013(2) 0.0053(2) -0.0071(2) C21 0.0407(13) 0.0294(12) 0.0314(12) 0.0017(10) 0.0063(10) -0.0111(10) C22 0.0314(11) 0.0262(11) 0.0305(12) 0.0031(9) 0.0068(10) -0.0071(9) C23 0.0346(13) 0.0291(12) 0.0552(17) -0.0041(11) 0.0061(12) 0.0003(10) C24 0.0326(13) 0.0386(14) 0.0503(17) 0.0058(12) -0.0056(12) 0.0005(11) C25 0.0482(15) 0.0395(14) 0.0279(12) 0.0007(10) 0.0030(11) -0.0105(12) C26 0.0508(15) 0.0351(13) 0.0365(13) -0.0015(10) 0.0202(12) 0.0006(11) C27 0.0285(11) 0.0354(12) 0.0331(12) 0.0054(10) 0.0097(10) 0.0011(9) C28 0.0303(11) 0.0251(11) 0.0234(10) -0.0019(8) 0.0077(9) 0.0004(9) O28 0.0414(10) 0.0367(9) 0.0409(10) -0.0011(8) 0.0173(8) -0.0094(8) C29 0.0340(12) 0.0292(11) 0.0238(10) 0.0032(9) 0.0108(9) 0.0027(9) O29 0.0313(9) 0.0444(10) 0.0408(10) 0.0110(8) 0.0073(8) 0.0094(8) C30 0.0343(12) 0.0214(10) 0.0218(10) 0.0017(8) 0.0082(9) -0.0048(8) O30 0.0520(11) 0.0281(9) 0.0399(10) -0.0030(7) 0.0237(9) -0.0006(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 C30 1.847(2) . ? Cr1 C29 1.854(2) . ? Cr1 C28 1.860(2) . ? Cr1 C5 2.185(2) . ? Cr1 C2 2.206(2) . ? Cr1 C6 2.227(2) . ? Cr1 C4 2.231(2) . ? Cr1 C1 2.231(2) . ? Cr1 C3 2.254(2) . ? C1 C6 1.408(3) . ? C1 C2 1.437(3) . ? C1 S1 1.767(2) . ? C2 C3 1.425(3) . ? C2 S2 1.769(2) . ? C3 C4 1.417(3) . ? C3 S3 1.769(2) . ? C4 C5 1.403(3) . ? C5 C6 1.407(3) . ? S1 C7 1.825(2) . ? C7 C8 1.510(3) . ? C8 C13 1.380(3) . ? C8 C9 1.396(3) . ? C9 C10 1.386(3) . ? C10 C11 1.374(3) . ? C11 C12 1.382(3) . ? C12 C13 1.390(3) . ? S2 C14 1.836(2) . ? C14 C15 1.505(3) . ? C15 C20 1.389(3) . ? C15 C16 1.398(3) . ? C16 C17 1.383(3) . ? C17 C18 1.382(4) . ? C18 C19 1.382(4) . ? C19 C20 1.389(3) . ? S3 C21 1.831(2) . ? C21 C22 1.514(3) . ? C22 C27 1.382(3) . ? C22 C23 1.389(3) . ? C23 C24 1.387(4) . ? C24 C25 1.379(4) . ? C25 C26 1.382(4) . ? C26 C27 1.385(4) . ? C28 O28 1.148(3) . ? C29 O29 1.150(3) . ? C30 O30 1.140(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Cr1 C29 86.85(10) . . ? C30 Cr1 C28 89.38(10) . . ? C29 Cr1 C28 87.52(10) . . ? C30 Cr1 C5 130.61(9) . . ? C29 Cr1 C5 89.65(9) . . ? C28 Cr1 C5 139.69(9) . . ? C30 Cr1 C2 103.96(9) . . ? C29 Cr1 C2 168.14(9) . . ? C28 Cr1 C2 97.32(9) . . ? C5 Cr1 C2 79.64(8) . . ? C30 Cr1 C6 164.31(9) . . ? C29 Cr1 C6 101.03(9) . . ? C28 Cr1 C6 104.38(9) . . ? C5 Cr1 C6 37.17(8) . . ? C2 Cr1 C6 67.31(8) . . ? C30 Cr1 C4 98.01(9) . . ? C29 Cr1 C4 106.83(9) . . ? C28 Cr1 C4 164.12(9) . . ? C5 Cr1 C4 37.03(8) . . ? C2 Cr1 C4 67.31(8) . . ? C6 Cr1 C4 66.81(8) . . ? C30 Cr1 C1 139.91(9) . . ? C29 Cr1 C1 132.57(9) . . ? C28 Cr1 C1 86.05(9) . . ? C5 Cr1 C1 66.91(8) . . ? C2 Cr1 C1 37.79(7) . . ? C6 Cr1 C1 36.83(7) . . ? C4 Cr1 C1 79.23(8) . . ? C30 Cr1 C3 86.81(9) . . ? C29 Cr1 C3 141.22(9) . . ? C28 Cr1 C3 130.60(9) . . ? C5 Cr1 C3 66.44(8) . . ? C2 Cr1 C3 37.24(8) . . ? C6 Cr1 C3 78.54(8) . . ? C4 Cr1 C3 36.82(7) . . ? C1 Cr1 C3 66.99(8) . . ? C6 C1 C2 119.40(19) . . ? C6 C1 S1 123.42(16) . . ? C2 C1 S1 117.17(15) . . ? C6 C1 Cr1 71.44(12) . . ? C2 C1 Cr1 70.15(11) . . ? S1 C1 Cr1 129.73(11) . . ? C3 C2 C1 119.74(18) . . ? C3 C2 S2 119.54(15) . . ? C1 C2 S2 120.73(15) . . ? C3 C2 Cr1 73.21(12) . . ? C1 C2 Cr1 72.06(11) . . ? S2 C2 Cr1 126.64(11) . . ? C4 C3 C2 119.85(19) . . ? C4 C3 S3 122.93(16) . . ? C2 C3 S3 117.21(15) . . ? C4 C3 Cr1 70.71(12) . . ? C2 C3 Cr1 69.55(11) . . ? S3 C3 Cr1 131.73(11) . . ? C5 C4 C3 119.26(19) . . ? C5 C4 Cr1 69.71(12) . . ? C3 C4 Cr1 72.46(12) . . ? C4 C5 C6 121.76(19) . . ? C4 C5 Cr1 73.26(13) . . ? C6 C5 Cr1 73.04(13) . . ? C5 C6 C1 119.74(19) . . ? C5 C6 Cr1 69.79(12) . . ? C1 C6 Cr1 71.73(12) . . ? C1 S1 C7 101.27(10) . . ? C8 C7 S1 107.84(15) . . ? C13 C8 C9 119.1(2) . . ? C13 C8 C7 120.3(2) . . ? C9 C8 C7 120.7(2) . . ? C10 C9 C8 120.1(2) . . ? C11 C10 C9 120.5(2) . . ? C10 C11 C12 119.8(2) . . ? C11 C12 C13 120.1(2) . . ? C8 C13 C12 120.5(2) . . ? C2 S2 C14 100.37(10) . . ? C15 C14 S2 107.13(16) . . ? C20 C15 C16 118.9(2) . . ? C20 C15 C14 120.3(2) . . ? C16 C15 C14 120.8(2) . . ? C17 C16 C15 120.2(2) . . ? C18 C17 C16 120.3(2) . . ? C19 C18 C17 120.1(2) . . ? C18 C19 C20 119.8(2) . . ? C19 C20 C15 120.7(2) . . ? C3 S3 C21 103.26(11) . . ? C22 C21 S3 105.65(16) . . ? C27 C22 C23 119.0(2) . . ? C27 C22 C21 121.0(2) . . ? C23 C22 C21 120.1(2) . . ? C24 C23 C22 120.1(3) . . ? C25 C24 C23 120.7(3) . . ? C24 C25 C26 119.3(2) . . ? C25 C26 C27 120.2(2) . . ? C22 C27 C26 120.7(2) . . ? O28 C28 Cr1 179.7(2) . . ? O29 C29 Cr1 176.6(2) . . ? O30 C30 Cr1 179.1(2) . . ? 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 C30 Cr1 C1 C6 -155.18(15) . . . . ? C29 Cr1 C1 C6 37.51(18) . . . . ? C28 Cr1 C1 C6 120.49(14) . . . . ? C5 Cr1 C1 C6 -28.87(12) . . . . ? C2 Cr1 C1 C6 -132.21(18) . . . . ? C4 Cr1 C1 C6 -65.51(13) . . . . ? C3 Cr1 C1 C6 -101.95(13) . . . . ? C30 Cr1 C1 C2 -22.97(19) . . . . ? C29 Cr1 C1 C2 169.72(14) . . . . ? C28 Cr1 C1 C2 -107.30(13) . . . . ? C5 Cr1 C1 C2 103.34(13) . . . . ? C6 Cr1 C1 C2 132.21(18) . . . . ? C4 Cr1 C1 C2 66.70(12) . . . . ? C3 Cr1 C1 C2 30.26(12) . . . . ? C30 Cr1 C1 S1 86.38(18) . . . . ? C29 Cr1 C1 S1 -80.93(18) . . . . ? C28 Cr1 C1 S1 2.05(14) . . . . ? C5 Cr1 C1 S1 -147.31(16) . . . . ? C2 Cr1 C1 S1 109.35(19) . . . . ? C6 Cr1 C1 S1 -118.4(2) . . . . ? C4 Cr1 C1 S1 176.05(15) . . . . ? C3 Cr1 C1 S1 139.61(16) . . . . ? C6 C1 C2 C3 -4.0(3) . . . . ? S1 C1 C2 C3 176.98(16) . . . . ? Cr1 C1 C2 C3 -57.68(18) . . . . ? C6 C1 C2 S2 176.20(16) . . . . ? S1 C1 C2 S2 -2.9(2) . . . . ? Cr1 C1 C2 S2 122.50(15) . . . . ? C6 C1 C2 Cr1 53.71(18) . . . . ? S1 C1 C2 Cr1 -125.35(14) . . . . ? C30 Cr1 C2 C3 -65.04(14) . . . . ? C29 Cr1 C2 C3 90.2(5) . . . . ? C28 Cr1 C2 C3 -156.23(13) . . . . ? C5 Cr1 C2 C3 64.48(13) . . . . ? C6 Cr1 C2 C3 101.20(13) . . . . ? C4 Cr1 C2 C3 27.92(12) . . . . ? C1 Cr1 C2 C3 129.96(18) . . . . ? C30 Cr1 C2 C1 164.99(13) . . . . ? C29 Cr1 C2 C1 -39.7(5) . . . . ? C28 Cr1 C2 C1 73.81(13) . . . . ? C5 Cr1 C2 C1 -65.49(12) . . . . ? C6 Cr1 C2 C1 -28.77(12) . . . . ? C4 Cr1 C2 C1 -102.05(13) . . . . ? C3 Cr1 C2 C1 -129.96(18) . . . . ? C30 Cr1 C2 S2 49.62(15) . . . . ? C29 Cr1 C2 S2 -155.1(4) . . . . ? C28 Cr1 C2 S2 -41.56(15) . . . . ? C5 Cr1 C2 S2 179.14(15) . . . . ? C6 Cr1 C2 S2 -144.14(15) . . . . ? C4 Cr1 C2 S2 142.58(15) . . . . ? C1 Cr1 C2 S2 -115.37(19) . . . . ? C3 Cr1 C2 S2 114.67(19) . . . . ? C1 C2 C3 C4 5.5(3) . . . . ? S2 C2 C3 C4 -174.71(16) . . . . ? Cr1 C2 C3 C4 -51.65(18) . . . . ? C1 C2 C3 S3 -175.51(16) . . . . ? S2 C2 C3 S3 4.3(2) . . . . ? Cr1 C2 C3 S3 127.38(14) . . . . ? C1 C2 C3 Cr1 57.11(17) . . . . ? S2 C2 C3 Cr1 -123.06(15) . . . . ? C30 Cr1 C3 C4 -107.90(14) . . . . ? C29 Cr1 C3 C4 -27.0(2) . . . . ? C28 Cr1 C3 C4 165.66(13) . . . . ? C5 Cr1 C3 C4 29.45(12) . . . . ? C2 Cr1 C3 C4 133.89(19) . . . . ? C6 Cr1 C3 C4 66.45(13) . . . . ? C1 Cr1 C3 C4 103.21(14) . . . . ? C30 Cr1 C3 C2 118.21(13) . . . . ? C29 Cr1 C3 C2 -160.84(15) . . . . ? C28 Cr1 C3 C2 31.77(17) . . . . ? C5 Cr1 C3 C2 -104.44(13) . . . . ? C6 Cr1 C3 C2 -67.44(12) . . . . ? C4 Cr1 C3 C2 -133.89(19) . . . . ? C1 Cr1 C3 C2 -30.68(12) . . . . ? C30 Cr1 C3 S3 9.47(15) . . . . ? C29 Cr1 C3 S3 90.42(19) . . . . ? C28 Cr1 C3 S3 -76.97(18) . . . . ? C5 Cr1 C3 S3 146.81(17) . . . . ? C2 Cr1 C3 S3 -108.75(19) . . . . ? C6 Cr1 C3 S3 -176.18(16) . . . . ? C4 Cr1 C3 S3 117.4(2) . . . . ? C1 Cr1 C3 S3 -139.43(17) . . . . ? C2 C3 C4 C5 -2.4(3) . . . . ? S3 C3 C4 C5 178.58(17) . . . . ? Cr1 C3 C4 C5 -53.57(18) . . . . ? C2 C3 C4 Cr1 51.13(18) . . . . ? S3 C3 C4 Cr1 -127.85(16) . . . . ? C30 Cr1 C4 C5 -154.82(13) . . . . ? C29 Cr1 C4 C5 -65.70(14) . . . . ? C28 Cr1 C4 C5 88.1(3) . . . . ? C2 Cr1 C4 C5 103.34(13) . . . . ? C6 Cr1 C4 C5 29.34(12) . . . . ? C1 Cr1 C4 C5 65.75(13) . . . . ? C3 Cr1 C4 C5 131.55(19) . . . . ? C30 Cr1 C4 C3 73.63(14) . . . . ? C29 Cr1 C4 C3 162.75(13) . . . . ? C28 Cr1 C4 C3 -43.4(4) . . . . ? C5 Cr1 C4 C3 -131.55(19) . . . . ? C2 Cr1 C4 C3 -28.21(12) . . . . ? C6 Cr1 C4 C3 -102.21(14) . . . . ? C1 Cr1 C4 C3 -65.80(13) . . . . ? C3 C4 C5 C6 -2.1(3) . . . . ? Cr1 C4 C5 C6 -57.01(19) . . . . ? C3 C4 C5 Cr1 54.88(18) . . . . ? C30 Cr1 C5 C4 33.71(17) . . . . ? C29 Cr1 C5 C4 119.26(14) . . . . ? C28 Cr1 C5 C4 -154.99(14) . . . . ? C2 Cr1 C5 C4 -65.87(13) . . . . ? C6 Cr1 C5 C4 -131.79(18) . . . . ? C1 Cr1 C5 C4 -103.17(13) . . . . ? C3 Cr1 C5 C4 -29.30(12) . . . . ? C30 Cr1 C5 C6 165.50(13) . . . . ? C29 Cr1 C5 C6 -108.95(13) . . . . ? C28 Cr1 C5 C6 -23.19(19) . . . . ? C2 Cr1 C5 C6 65.93(12) . . . . ? C4 Cr1 C5 C6 131.79(18) . . . . ? C1 Cr1 C5 C6 28.62(12) . . . . ? C3 Cr1 C5 C6 102.49(13) . . . . ? C4 C5 C6 C1 3.6(3) . . . . ? Cr1 C5 C6 C1 -53.49(19) . . . . ? C4 C5 C6 Cr1 57.11(19) . . . . ? C2 C1 C6 C5 -0.5(3) . . . . ? S1 C1 C6 C5 178.48(17) . . . . ? Cr1 C1 C6 C5 52.59(18) . . . . ? C2 C1 C6 Cr1 -53.10(18) . . . . ? S1 C1 C6 Cr1 125.88(17) . . . . ? C30 Cr1 C6 C5 -44.6(4) . . . . ? C29 Cr1 C6 C5 74.49(14) . . . . ? C28 Cr1 C6 C5 164.75(13) . . . . ? C2 Cr1 C6 C5 -103.23(13) . . . . ? C4 Cr1 C6 C5 -29.24(12) . . . . ? C1 Cr1 C6 C5 -132.69(18) . . . . ? C3 Cr1 C6 C5 -65.94(13) . . . . ? C30 Cr1 C6 C1 88.1(3) . . . . ? C29 Cr1 C6 C1 -152.81(13) . . . . ? C28 Cr1 C6 C1 -62.56(14) . . . . ? C5 Cr1 C6 C1 132.69(18) . . . . ? C2 Cr1 C6 C1 29.47(12) . . . . ? C4 Cr1 C6 C1 103.46(13) . . . . ? C3 Cr1 C6 C1 66.75(12) . . . . ? C6 C1 S1 C7 -12.1(2) . . . . ? C2 C1 S1 C7 166.90(17) . . . . ? Cr1 C1 S1 C7 80.89(15) . . . . ? C1 S1 C7 C8 -167.20(16) . . . . ? S1 C7 C8 C13 78.3(2) . . . . ? S1 C7 C8 C9 -101.8(2) . . . . ? C13 C8 C9 C10 0.0(3) . . . . ? C7 C8 C9 C10 -179.9(2) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C9 C10 C11 C12 0.2(3) . . . . ? C10 C11 C12 C13 -1.0(4) . . . . ? C9 C8 C13 C12 -0.8(3) . . . . ? C7 C8 C13 C12 179.1(2) . . . . ? C11 C12 C13 C8 1.3(4) . . . . ? C3 C2 S2 C14 -86.45(19) . . . . ? C1 C2 S2 C14 93.38(19) . . . . ? Cr1 C2 S2 C14 -176.88(13) . . . . ? C2 S2 C14 C15 169.28(16) . . . . ? S2 C14 C15 C20 -79.5(2) . . . . ? S2 C14 C15 C16 99.3(2) . . . . ? C20 C15 C16 C17 0.0(4) . . . . ? C14 C15 C16 C17 -178.8(2) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 0.5(4) . . . . ? C18 C19 C20 C15 -0.5(4) . . . . ? C16 C15 C20 C19 0.2(3) . . . . ? C14 C15 C20 C19 179.1(2) . . . . ? C4 C3 S3 C21 -18.4(2) . . . . ? C2 C3 S3 C21 162.60(18) . . . . ? Cr1 C3 S3 C21 -111.29(16) . . . . ? C3 S3 C21 C22 -174.15(17) . . . . ? S3 C21 C22 C27 -107.4(2) . . . . ? S3 C21 C22 C23 71.7(3) . . . . ? C27 C22 C23 C24 0.8(4) . . . . ? C21 C22 C23 C24 -178.3(3) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C23 C24 C25 C26 -0.2(5) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C23 C22 C27 C26 -1.0(4) . . . . ? C21 C22 C27 C26 178.1(2) . . . . ? C25 C26 C27 C22 0.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.798 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.072 #===END