# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Fontenot, Sean' 'Cangelosi, Virginia' 'Pitt, Melanie' 'Sather, Aaron' 'Zakharov, Lev' 'Berryman, Orion' 'Johnson, Darren' _publ_contact_author_name 'Dr Darren Johnson' _publ_contact_author_email dwj@uoregon.edu _publ_section_title ; Design, Synthesis and Characterization of Self-Assembled As2L3 and Sb2L3 Cryptands ; # Attachment '- AS263 - map22.cif' data_map22 _database_code_depnum_ccdc_archive 'CCDC 824398' #TrackingRef '- AS263 - map22.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 As2 S6' _chemical_formula_weight 967.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.468(3) _cell_length_b 13.6420(12) _cell_length_c 11.0855(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.3970(10) _cell_angle_gamma 90.00 _cell_volume 4420.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5192 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 24.79 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5509 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24133 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4837 _reflns_number_gt 3704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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^)+(0.0708P)^2^+9.6896P] 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 4837 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 As1 As 0.185561(12) 0.24551(3) 0.19518(4) 0.03529(14) Uani 1 1 d . . . S1 S 0.20822(3) 0.31945(8) 0.04293(9) 0.0397(2) Uani 1 1 d . . . S2 S 0.22969(3) 0.11219(8) 0.20797(10) 0.0454(3) Uani 1 1 d . . . S3 S 0.23256(3) 0.33435(8) 0.34884(9) 0.0432(3) Uani 1 1 d . . . C1 C 0.16963(14) 0.2591(3) -0.0942(4) 0.0443(10) Uani 1 1 d . . . H1A H 0.1729 0.2904 -0.1718 0.053 Uiso 1 1 calc R . . H1B H 0.1785 0.1894 -0.0954 0.053 Uiso 1 1 calc R . . C2 C 0.12043(13) 0.2649(3) -0.0929(4) 0.0378(9) Uani 1 1 d . . . C3 C 0.09855(15) 0.1840(3) -0.0615(4) 0.0486(10) Uani 1 1 d . . . H3A H 0.1140 0.1227 -0.0474 0.058 Uiso 1 1 calc R . . C4 C 0.05484(16) 0.1909(4) -0.0504(5) 0.0603(13) Uani 1 1 d . . . H4A H 0.0409 0.1346 -0.0266 0.072 Uiso 1 1 calc R . . C5 C 0.03111(16) 0.2761(4) -0.0725(5) 0.0627(13) Uani 1 1 d . . . C6 C 0.05237(16) 0.3576(4) -0.1042(5) 0.0628(13) Uani 1 1 d . . . H6A H 0.0363 0.4181 -0.1192 0.075 Uiso 1 1 calc R . . C7 C 0.09701(14) 0.3531(3) -0.1147(4) 0.0485(10) Uani 1 1 d . . . H7A H 0.1111 0.4099 -0.1364 0.058 Uiso 1 1 calc R . . C8 C -0.01760(19) 0.2785(4) -0.0553(7) 0.0770(16) Uani 1 1 d . . . H8A H -0.0404 0.2740 -0.1388 0.092 Uiso 1 1 calc R . . H8B H -0.0217 0.2207 -0.0056 0.092 Uiso 1 1 calc R . . C9 C -0.0258(3) 0.3619(9) 0.0040(10) 0.179(6) Uani 1 1 d . . . H9A H -0.0261 0.4181 -0.0526 0.215 Uiso 1 1 calc R . . H9B H 0.0002 0.3717 0.0800 0.215 Uiso 1 1 calc R . . C10 C -0.0707(2) 0.3654(6) 0.0447(7) 0.100(2) Uani 1 1 d . . . C11 C -0.1132(2) 0.3681(5) -0.0434(5) 0.088(2) Uani 1 1 d . . . H11A H -0.1153 0.3564 -0.1294 0.106 Uiso 1 1 calc R . . C12 C -0.15288(16) 0.3875(4) -0.0094(4) 0.0566(12) Uani 1 1 d . . . H12A H -0.1816 0.3901 -0.0717 0.068 Uiso 1 1 calc R . . C13 C -0.15044(12) 0.4030(3) 0.1152(4) 0.0387(8) Uani 1 1 d . . . C14 C -0.10848(14) 0.3940(4) 0.2042(4) 0.0512(11) Uani 1 1 d . . . H14A H -0.1064 0.4011 0.2909 0.061 Uiso 1 1 calc R . . C15 C -0.06990(16) 0.3750(5) 0.1676(6) 0.0838(19) Uani 1 1 d . . . H15A H -0.0415 0.3682 0.2305 0.101 Uiso 1 1 calc R . . C16 C -0.19188(13) 0.4337(3) 0.1533(4) 0.0425(9) Uani 1 1 d . . . H16A H -0.2078 0.4863 0.0960 0.051 Uiso 1 1 calc R . . H16B H -0.1818 0.4615 0.2392 0.051 Uiso 1 1 calc R . . C17 C 0.21020(14) 0.0403(4) 0.3235(4) 0.0509(11) Uani 1 1 d . . . H17A H 0.2216 -0.0276 0.3242 0.061 Uiso 1 1 calc R . . H17B H 0.2238 0.0685 0.4082 0.061 Uiso 1 1 calc R . . C18 C 0.15910(13) 0.0376(3) 0.2981(4) 0.0396(9) Uani 1 1 d . . . C19 C 0.13196(16) -0.0199(3) 0.2024(4) 0.0500(10) Uani 1 1 d . . . H19A H 0.1459 -0.0606 0.1542 0.060 Uiso 1 1 calc R . . C20 C 0.08508(17) -0.0187(4) 0.1767(4) 0.0623(13) Uani 1 1 d . . . H20A H 0.0673 -0.0593 0.1115 0.075 Uiso 1 1 calc R . . C21 C 0.06315(15) 0.0400(4) 0.2428(4) 0.0623(14) Uani 1 1 d . . . C22 C 0.09007(15) 0.0970(4) 0.3386(4) 0.0544(11) Uani 1 1 d . . . H22A H 0.0759 0.1374 0.3866 0.065 Uiso 1 1 calc R . . C23 C 0.13767(14) 0.0963(3) 0.3660(4) 0.0457(10) Uani 1 1 d . . . H23A H 0.1555 0.1364 0.4318 0.055 Uiso 1 1 calc R . . C24 C 0.01159(17) 0.0441(8) 0.2118(5) 0.142(4) Uani 1 1 d . . . H24A H 0.0024 0.1038 0.1601 0.170 Uiso 1 1 calc R . . H24B H 0.0003 -0.0120 0.1550 0.170 Uiso 1 1 calc R . . 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 As1 0.0247(2) 0.0468(3) 0.0370(2) -0.00220(16) 0.01298(15) 0.00511(15) S1 0.0291(4) 0.0533(6) 0.0393(5) -0.0032(4) 0.0139(4) -0.0028(4) S2 0.0368(5) 0.0494(6) 0.0550(6) 0.0012(5) 0.0213(5) 0.0116(4) S3 0.0290(5) 0.0615(7) 0.0376(5) -0.0048(4) 0.0071(4) 0.0059(4) C1 0.035(2) 0.064(3) 0.037(2) -0.0096(18) 0.0157(17) 0.0009(18) C2 0.0317(19) 0.052(2) 0.0307(18) -0.0093(16) 0.0107(15) -0.0014(16) C3 0.045(2) 0.053(3) 0.049(2) -0.005(2) 0.0159(19) -0.008(2) C4 0.048(3) 0.078(4) 0.058(3) 0.001(3) 0.021(2) -0.013(3) C5 0.042(2) 0.095(4) 0.056(3) 0.004(3) 0.022(2) -0.009(3) C6 0.048(3) 0.076(3) 0.064(3) 0.009(3) 0.015(2) 0.024(2) C7 0.040(2) 0.057(3) 0.052(2) 0.005(2) 0.0181(19) 0.0029(19) C8 0.056(3) 0.079(4) 0.103(5) 0.004(3) 0.034(3) 0.001(3) C9 0.090(5) 0.261(12) 0.218(11) -0.172(10) 0.093(7) -0.079(7) C10 0.052(3) 0.162(7) 0.101(5) -0.051(5) 0.046(3) -0.018(4) C11 0.082(4) 0.138(6) 0.061(3) -0.024(4) 0.049(3) -0.024(4) C12 0.049(3) 0.083(3) 0.042(2) 0.000(2) 0.020(2) -0.003(2) C13 0.0352(19) 0.042(2) 0.043(2) 0.0036(17) 0.0182(16) -0.0039(16) C14 0.039(2) 0.068(3) 0.050(2) -0.002(2) 0.0178(18) 0.000(2) C15 0.034(2) 0.137(6) 0.080(4) -0.026(4) 0.016(2) 0.006(3) C16 0.039(2) 0.043(2) 0.048(2) 0.0035(18) 0.0171(17) 0.0010(17) C17 0.042(2) 0.063(3) 0.046(2) 0.009(2) 0.0097(19) 0.009(2) C18 0.042(2) 0.039(2) 0.038(2) 0.0081(17) 0.0113(16) 0.0002(17) C19 0.064(3) 0.040(2) 0.045(2) 0.0000(18) 0.013(2) -0.003(2) C20 0.067(3) 0.074(3) 0.041(2) 0.001(2) 0.009(2) -0.033(3) C21 0.043(2) 0.105(4) 0.038(2) 0.024(3) 0.0108(19) -0.018(3) C22 0.049(2) 0.070(3) 0.053(3) 0.008(2) 0.028(2) -0.001(2) C23 0.046(2) 0.052(3) 0.043(2) -0.0046(19) 0.0183(18) -0.0112(19) C24 0.040(3) 0.336(13) 0.048(3) 0.039(5) 0.009(2) -0.032(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 As1 S1 2.2362(10) . ? As1 S2 2.2424(11) . ? As1 S3 2.2458(11) . ? S1 C1 1.834(4) . ? S2 C17 1.839(4) . ? S3 C16 1.833(4) 2 ? C1 C2 1.505(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.384(6) . ? C2 C7 1.385(6) . ? C3 C4 1.375(6) . ? C3 H3A 0.9500 . ? C4 C5 1.353(8) . ? C4 H4A 0.9500 . ? C5 C6 1.382(7) . ? C5 C8 1.549(7) . ? C6 C7 1.399(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.371(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.556(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.363(8) . ? C10 C11 1.385(9) . ? C11 C12 1.390(7) . ? C11 H11A 0.9500 . ? C12 C13 1.378(6) . ? C12 H12A 0.9500 . ? C13 C14 1.382(6) . ? C13 C16 1.500(5) . ? C14 C15 1.372(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 S3 1.833(4) 2 ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.502(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.382(6) . ? C18 C19 1.389(6) . ? C19 C20 1.376(7) . ? C19 H19A 0.9500 . ? C20 C21 1.379(7) . ? C20 H20A 0.9500 . ? C21 C22 1.383(7) . ? C21 C24 1.511(7) . ? C22 C23 1.396(6) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C24 1.247(10) 2 ? C24 H24A 0.9900 . ? C24 H24B 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 S1 As1 S2 96.10(4) . . ? S1 As1 S3 93.58(4) . . ? S2 As1 S3 98.46(4) . . ? C1 S1 As1 99.24(14) . . ? C17 S2 As1 99.82(14) . . ? C16 S3 As1 96.04(13) 2 . ? C2 C1 S1 112.1(3) . . ? C2 C1 H1A 109.2 . . ? S1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? S1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C7 118.4(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 120.7(4) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C8 118.5(5) . . ? C6 C5 C8 123.2(5) . . ? C5 C6 C7 121.5(5) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C2 C7 C6 119.3(4) . . ? C2 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C9 C8 C5 112.8(5) . . ? C9 C8 H8A 109.0 . . ? C5 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C5 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 117.3(7) . . ? C8 C9 H9A 108.0 . . ? C10 C9 H9A 108.0 . . ? C8 C9 H9B 108.0 . . ? C10 C9 H9B 108.0 . . ? H9A C9 H9B 107.2 . . ? C15 C10 C11 116.8(5) . . ? C15 C10 C9 121.6(6) . . ? C11 C10 C9 121.3(7) . . ? C10 C11 C12 121.7(5) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 118.6(4) . . ? C12 C13 C16 120.9(4) . . ? C14 C13 C16 120.4(4) . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C10 C15 C14 122.6(5) . . ? C10 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C13 C16 S3 114.2(3) . 2 ? C13 C16 H16A 108.7 . . ? S3 C16 H16A 108.7 2 . ? C13 C16 H16B 108.7 . . ? S3 C16 H16B 108.7 2 . ? H16A C16 H16B 107.6 . . ? C18 C17 S2 113.8(3) . . ? C18 C17 H17A 108.8 . . ? S2 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? S2 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C23 C18 C19 118.2(4) . . ? C23 C18 C17 120.5(4) . . ? C19 C18 C17 121.3(4) . . ? C20 C19 C18 120.7(4) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C19 C20 C21 121.9(4) . . ? C19 C20 H20A 119.1 . . ? C21 C20 H20A 119.1 . . ? C20 C21 C22 117.6(4) . . ? C20 C21 C24 121.9(5) . . ? C22 C21 C24 120.5(6) . . ? C21 C22 C23 121.2(4) . . ? C21 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C18 C23 C22 120.5(4) . . ? C18 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C24 C24 C21 126.7(7) 2 . ? C24 C24 H24A 105.6 2 . ? C21 C24 H24A 105.6 . . ? C24 C24 H24B 105.6 2 . ? C21 C24 H24B 105.6 . . ? H24A C24 H24B 106.1 . . ? 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 S2 As1 S1 C1 84.36(14) . . . . ? S3 As1 S1 C1 -176.72(14) . . . . ? S1 As1 S2 C17 -175.66(15) . . . . ? S3 As1 S2 C17 89.78(15) . . . . ? S1 As1 S3 C16 90.11(13) . . . 2 ? S2 As1 S3 C16 -173.18(13) . . . 2 ? As1 S1 C1 C2 51.9(3) . . . . ? S1 C1 C2 C3 -104.5(4) . . . . ? S1 C1 C2 C7 71.0(5) . . . . ? C7 C2 C3 C4 -0.8(6) . . . . ? C1 C2 C3 C4 174.8(4) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C3 C4 C5 C6 -1.4(8) . . . . ? C3 C4 C5 C8 -178.7(5) . . . . ? C4 C5 C6 C7 0.6(8) . . . . ? C8 C5 C6 C7 177.8(5) . . . . ? C3 C2 C7 C6 0.0(6) . . . . ? C1 C2 C7 C6 -175.6(4) . . . . ? C5 C6 C7 C2 0.1(7) . . . . ? C4 C5 C8 C9 137.8(8) . . . . ? C6 C5 C8 C9 -39.4(10) . . . . ? C5 C8 C9 C10 -170.9(7) . . . . ? C8 C9 C10 C15 118.8(10) . . . . ? C8 C9 C10 C11 -67.3(14) . . . . ? C15 C10 C11 C12 5.0(12) . . . . ? C9 C10 C11 C12 -169.1(7) . . . . ? C10 C11 C12 C13 -1.1(10) . . . . ? C11 C12 C13 C14 -3.1(7) . . . . ? C11 C12 C13 C16 174.0(5) . . . . ? C12 C13 C14 C15 3.2(7) . . . . ? C16 C13 C14 C15 -173.9(5) . . . . ? C11 C10 C15 C14 -4.9(12) . . . . ? C9 C10 C15 C14 169.2(8) . . . . ? C13 C14 C15 C10 0.9(10) . . . . ? C12 C13 C16 S3 76.6(5) . . . 2 ? C14 C13 C16 S3 -106.4(4) . . . 2 ? As1 S2 C17 C18 45.5(3) . . . . ? S2 C17 C18 C23 -101.8(4) . . . . ? S2 C17 C18 C19 75.1(5) . . . . ? C23 C18 C19 C20 -0.3(6) . . . . ? C17 C18 C19 C20 -177.3(4) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C19 C20 C21 C22 -1.1(7) . . . . ? C19 C20 C21 C24 177.9(5) . . . . ? C20 C21 C22 C23 1.0(7) . . . . ? C24 C21 C22 C23 -178.1(5) . . . . ? C19 C18 C23 C22 0.1(6) . . . . ? C17 C18 C23 C22 177.1(4) . . . . ? C21 C22 C23 C18 -0.5(7) . . . . ? C20 C21 C24 C24 137.0(4) . . . 2 ? C22 C21 C24 C24 -44.0(7) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.064 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.113 # Attachment '- As243 - gr29.cif' data_gr29 _database_code_depnum_ccdc_archive 'CCDC 824399' #TrackingRef '- As243 - gr29.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 As2 S6' _chemical_formula_weight 738.79 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' As As 0.0499 2.0058 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 14.4540(6) _cell_length_b 12.6952(5) _cell_length_c 17.6319(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.1500(10) _cell_angle_gamma 90.00 _cell_volume 3235.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4433 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.54 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 2.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5050 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30492 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5689 _reflns_number_gt 4371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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^)+(0.0547P)^2^+1.0730P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5689 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 As1 As 0.22508(3) 0.23682(4) -0.11187(2) 0.04352(16) Uani 1 1 d . . . As2 As 0.27378(3) 0.15233(4) 0.16739(2) 0.03669(14) Uani 1 1 d . . . S1 S 0.09391(9) 0.31833(14) -0.14734(8) 0.0689(5) Uani 1 1 d . . . S2 S 0.17101(9) 0.18646(11) 0.25992(7) 0.0507(3) Uani 1 1 d . . . S3 S 0.21535(10) 0.11479(12) -0.20445(7) 0.0589(4) Uani 1 1 d . . . S4 S 0.29101(8) -0.01629(10) 0.20375(6) 0.0441(3) Uani 1 1 d . . . S5 S 0.32101(9) 0.34044(10) -0.17817(7) 0.0491(3) Uani 1 1 d . . . S6 S 0.40033(9) 0.20000(11) 0.23165(7) 0.0502(3) Uani 1 1 d . . . C1 C 0.0112(4) 0.2266(6) -0.1028(3) 0.0746(19) Uani 1 1 d . . . H1A H -0.0521 0.2544 -0.1106 0.089 Uiso 1 1 calc R . . H1B H 0.0150 0.1581 -0.1295 0.089 Uiso 1 1 calc R . . C2 C 0.0253(3) 0.2073(5) -0.0190(3) 0.0526(13) Uani 1 1 d . . . C3 C -0.0022(4) 0.2791(4) 0.0356(3) 0.0585(14) Uani 1 1 d . . . C4 C 0.0120(4) 0.2559(4) 0.1134(3) 0.0544(13) Uani 1 1 d . . . C5 C 0.0516(3) 0.1619(4) 0.1333(3) 0.0458(12) Uani 1 1 d . . . C6 C 0.0783(3) 0.0904(4) 0.0790(3) 0.0495(12) Uani 1 1 d . . . H6A H 0.1048 0.0249 0.0935 0.059 Uiso 1 1 calc R . . C7 C 0.0663(3) 0.1149(5) 0.0021(3) 0.0548(14) Uani 1 1 d . . . H7A H 0.0868 0.0669 -0.0357 0.066 Uiso 1 1 calc R . . C8 C 0.0655(3) 0.1314(5) 0.2154(3) 0.0572(14) Uani 1 1 d . . . H8A H 0.0682 0.0536 0.2188 0.069 Uiso 1 1 calc R . . H8B H 0.0110 0.1550 0.2447 0.069 Uiso 1 1 calc R . . C9 C -0.0549(5) 0.3774(5) 0.0140(4) 0.095(2) Uani 1 1 d . . . H9A H -0.0586 0.3826 -0.0414 0.142 Uiso 1 1 calc R . . H9B H -0.0228 0.4393 0.0343 0.142 Uiso 1 1 calc R . . H9C H -0.1174 0.3740 0.0351 0.142 Uiso 1 1 calc R . . C10 C -0.0189(4) 0.3340(5) 0.1733(4) 0.0784(18) Uani 1 1 d . . . H10A H -0.0043 0.3061 0.2238 0.118 Uiso 1 1 calc R . . H10B H -0.0858 0.3453 0.1690 0.118 Uiso 1 1 calc R . . H10C H 0.0135 0.4010 0.1659 0.118 Uiso 1 1 calc R . . C11 C 0.3175(4) 0.0340(4) -0.1822(2) 0.0530(13) Uani 1 1 d . . . H11A H 0.3134 -0.0328 -0.2109 0.064 Uiso 1 1 calc R . . H11B H 0.3735 0.0717 -0.1994 0.064 Uiso 1 1 calc R . . C12 C 0.3277(3) 0.0091(4) -0.0995(2) 0.0403(11) Uani 1 1 d . . . C13 C 0.2784(3) -0.0732(4) -0.0647(2) 0.0400(11) Uani 1 1 d . . . C14 C 0.2932(3) -0.0951(3) 0.0125(2) 0.0369(10) Uani 1 1 d . . . C15 C 0.3566(3) -0.0350(3) 0.0540(2) 0.0343(10) Uani 1 1 d . . . C16 C 0.4010(3) 0.0486(3) 0.0198(2) 0.0385(11) Uani 1 1 d . . . H16A H 0.4417 0.0917 0.0486 0.046 Uiso 1 1 calc R . . C17 C 0.3867(3) 0.0699(4) -0.0559(2) 0.0402(11) Uani 1 1 d . . . H17A H 0.4180 0.1276 -0.0786 0.048 Uiso 1 1 calc R . . C18 C 0.3793(3) -0.0586(4) 0.1358(2) 0.0423(11) Uani 1 1 d . . . H18A H 0.4384 -0.0236 0.1489 0.051 Uiso 1 1 calc R . . H18B H 0.3886 -0.1354 0.1413 0.051 Uiso 1 1 calc R . . C19 C 0.2117(4) -0.1400(4) -0.1104(3) 0.0563(14) Uani 1 1 d . . . H19A H 0.2094 -0.1142 -0.1628 0.085 Uiso 1 1 calc R . . H19B H 0.1499 -0.1357 -0.0880 0.085 Uiso 1 1 calc R . . H19C H 0.2327 -0.2135 -0.1101 0.085 Uiso 1 1 calc R . . C20 C 0.2404(3) -0.1850(4) 0.0502(3) 0.0467(12) Uani 1 1 d . . . H20A H 0.2585 -0.1898 0.1036 0.070 Uiso 1 1 calc R . . H20B H 0.2550 -0.2514 0.0245 0.070 Uiso 1 1 calc R . . H20C H 0.1738 -0.1715 0.0466 0.070 Uiso 1 1 calc R . . C21 C 0.3457(4) 0.4462(4) -0.1106(3) 0.0539(13) Uani 1 1 d . . . H21A H 0.3995 0.4866 -0.1297 0.065 Uiso 1 1 calc R . . H21B H 0.2920 0.4946 -0.1100 0.065 Uiso 1 1 calc R . . C22 C 0.3661(3) 0.4134(4) -0.0300(3) 0.0437(11) Uani 1 1 d . . . C23 C 0.4507(3) 0.3677(4) -0.0090(3) 0.0419(11) Uani 1 1 d . . . C24 C 0.4670(3) 0.3411(3) 0.0675(3) 0.0403(11) Uani 1 1 d . . . C25 C 0.3995(3) 0.3620(3) 0.1220(2) 0.0390(11) Uani 1 1 d . . . C26 C 0.3157(3) 0.4055(4) 0.0997(3) 0.0460(12) Uani 1 1 d . . . H26A H 0.2691 0.4184 0.1365 0.055 Uiso 1 1 calc R . . C27 C 0.2992(3) 0.4303(4) 0.0249(3) 0.0446(11) Uani 1 1 d . . . H27A H 0.2412 0.4594 0.0107 0.054 Uiso 1 1 calc R . . C28 C 0.4137(3) 0.3389(4) 0.2050(2) 0.0444(12) Uani 1 1 d . . . H28A H 0.3689 0.3812 0.2345 0.053 Uiso 1 1 calc R . . H28B H 0.4766 0.3622 0.2196 0.053 Uiso 1 1 calc R . . C29 C 0.5246(3) 0.3483(4) -0.0670(3) 0.0510(13) Uani 1 1 d . . . H29A H 0.5025 0.3709 -0.1170 0.077 Uiso 1 1 calc R . . H29B H 0.5394 0.2729 -0.0685 0.077 Uiso 1 1 calc R . . H29C H 0.5802 0.3882 -0.0535 0.077 Uiso 1 1 calc R . . C30 C 0.5573(3) 0.2906(4) 0.0901(3) 0.0517(13) Uani 1 1 d . . . H30A H 0.5574 0.2773 0.1448 0.078 Uiso 1 1 calc R . . H30B H 0.6085 0.3379 0.0773 0.078 Uiso 1 1 calc R . . H30C H 0.5647 0.2239 0.0629 0.078 Uiso 1 1 calc R . . 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 As1 0.0423(3) 0.0601(3) 0.0282(3) 0.0109(2) -0.0051(2) -0.0095(2) As2 0.0368(3) 0.0499(3) 0.0234(2) -0.0029(2) 0.00124(18) -0.0031(2) S1 0.0447(8) 0.1080(13) 0.0541(9) 0.0353(8) -0.0047(6) -0.0017(8) S2 0.0484(7) 0.0732(9) 0.0305(6) -0.0156(6) 0.0068(5) 0.0013(6) S3 0.0715(9) 0.0737(9) 0.0315(7) 0.0029(6) -0.0137(6) -0.0219(7) S4 0.0478(7) 0.0533(8) 0.0312(6) 0.0055(5) 0.0103(5) -0.0013(6) S5 0.0543(8) 0.0621(9) 0.0309(6) 0.0070(6) 0.0034(5) -0.0153(6) S6 0.0464(7) 0.0695(9) 0.0347(6) -0.0010(6) -0.0089(5) -0.0084(6) C1 0.047(3) 0.127(6) 0.050(3) 0.021(3) -0.005(3) -0.025(3) C2 0.039(3) 0.076(4) 0.043(3) 0.009(3) -0.001(2) -0.014(3) C3 0.054(3) 0.059(4) 0.063(4) 0.007(3) -0.007(3) -0.007(3) C4 0.049(3) 0.063(4) 0.051(3) -0.003(3) 0.007(2) -0.007(3) C5 0.028(2) 0.063(3) 0.046(3) 0.005(2) 0.000(2) -0.003(2) C6 0.039(3) 0.070(4) 0.039(3) -0.004(3) -0.001(2) -0.007(2) C7 0.038(3) 0.083(4) 0.044(3) -0.005(3) 0.003(2) -0.014(3) C8 0.048(3) 0.086(4) 0.038(3) 0.001(3) 0.007(2) 0.001(3) C9 0.106(6) 0.074(5) 0.103(6) 0.026(4) -0.018(4) -0.014(4) C10 0.081(4) 0.078(4) 0.076(4) -0.019(3) 0.004(3) 0.010(3) C11 0.068(3) 0.062(3) 0.029(2) -0.003(2) 0.007(2) -0.017(3) C12 0.043(3) 0.050(3) 0.028(2) -0.001(2) 0.007(2) -0.004(2) C13 0.046(3) 0.043(3) 0.031(2) -0.003(2) 0.006(2) -0.007(2) C14 0.040(2) 0.037(3) 0.035(2) -0.003(2) 0.009(2) -0.003(2) C15 0.030(2) 0.043(3) 0.030(2) -0.0034(19) 0.0067(18) 0.0033(19) C16 0.033(2) 0.046(3) 0.037(3) -0.007(2) 0.0059(19) -0.005(2) C17 0.037(2) 0.044(3) 0.040(3) 0.002(2) 0.009(2) -0.006(2) C18 0.041(3) 0.054(3) 0.033(2) 0.000(2) 0.006(2) 0.002(2) C19 0.067(4) 0.063(3) 0.039(3) -0.003(2) -0.004(3) -0.019(3) C20 0.048(3) 0.047(3) 0.045(3) 0.007(2) 0.004(2) -0.004(2) C21 0.065(3) 0.049(3) 0.047(3) 0.005(2) 0.006(3) -0.009(3) C22 0.051(3) 0.043(3) 0.038(3) -0.001(2) 0.005(2) -0.014(2) C23 0.045(3) 0.041(3) 0.040(3) -0.012(2) 0.009(2) -0.017(2) C24 0.034(2) 0.042(3) 0.045(3) -0.013(2) 0.007(2) -0.013(2) C25 0.040(3) 0.042(3) 0.035(2) -0.009(2) 0.005(2) -0.008(2) C26 0.044(3) 0.053(3) 0.041(3) -0.011(2) 0.014(2) -0.003(2) C27 0.041(3) 0.043(3) 0.049(3) -0.005(2) 0.004(2) -0.003(2) C28 0.044(3) 0.056(3) 0.034(2) -0.016(2) 0.001(2) -0.008(2) C29 0.047(3) 0.061(3) 0.045(3) -0.014(2) 0.015(2) -0.014(2) C30 0.040(3) 0.061(3) 0.055(3) -0.014(3) 0.003(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 S5 2.2424(12) . ? As1 S1 2.2472(15) . ? As1 S3 2.2547(15) . ? As2 S6 2.2327(12) . ? As2 S4 2.2482(13) . ? As2 S2 2.2513(12) . ? S1 C1 1.845(5) . ? S2 C8 1.851(5) . ? S3 C11 1.839(6) . ? S4 C18 1.833(4) . ? S5 C21 1.829(5) . ? S6 C28 1.835(5) . ? C1 C2 1.511(7) . ? C2 C7 1.365(7) . ? C2 C3 1.384(7) . ? C3 C4 1.417(7) . ? C3 C9 1.510(8) . ? C4 C5 1.370(7) . ? C4 C10 1.517(7) . ? C5 C6 1.375(7) . ? C5 C8 1.511(6) . ? C6 C7 1.403(6) . ? C11 C12 1.499(6) . ? C12 C17 1.382(6) . ? C12 C13 1.405(6) . ? C13 C14 1.405(6) . ? C13 C19 1.515(6) . ? C14 C15 1.398(6) . ? C14 C20 1.526(6) . ? C15 C16 1.380(6) . ? C15 C18 1.508(6) . ? C16 C17 1.377(6) . ? C21 C22 1.509(6) . ? C22 C27 1.386(6) . ? C22 C23 1.402(6) . ? C23 C24 1.409(6) . ? C23 C29 1.502(6) . ? C24 C25 1.397(6) . ? C24 C30 1.507(6) . ? C25 C26 1.387(6) . ? C25 C28 1.506(6) . ? C26 C27 1.376(6) . ? 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 S5 As1 S1 96.15(5) . . ? S5 As1 S3 93.62(5) . . ? S1 As1 S3 93.66(6) . . ? S6 As2 S4 91.34(5) . . ? S6 As2 S2 96.97(5) . . ? S4 As2 S2 92.83(5) . . ? C1 S1 As1 97.9(2) . . ? C8 S2 As2 99.45(16) . . ? C11 S3 As1 100.36(16) . . ? C18 S4 As2 99.73(16) . . ? C21 S5 As1 102.19(16) . . ? C28 S6 As2 102.52(15) . . ? C2 C1 S1 115.7(4) . . ? C7 C2 C3 120.1(5) . . ? C7 C2 C1 117.5(5) . . ? C3 C2 C1 122.3(5) . . ? C2 C3 C4 119.7(5) . . ? C2 C3 C9 121.0(5) . . ? C4 C3 C9 119.1(5) . . ? C5 C4 C3 119.2(5) . . ? C5 C4 C10 120.9(5) . . ? C3 C4 C10 119.8(5) . . ? C4 C5 C6 121.0(5) . . ? C4 C5 C8 121.6(5) . . ? C6 C5 C8 117.4(5) . . ? C5 C6 C7 119.5(5) . . ? C2 C7 C6 120.4(5) . . ? C5 C8 S2 114.7(3) . . ? C12 C11 S3 113.8(3) . . ? C17 C12 C13 119.1(4) . . ? C17 C12 C11 118.8(4) . . ? C13 C12 C11 122.1(4) . . ? C14 C13 C12 119.5(4) . . ? C14 C13 C19 119.9(4) . . ? C12 C13 C19 120.5(4) . . ? C15 C14 C13 119.8(4) . . ? C15 C14 C20 120.5(4) . . ? C13 C14 C20 119.7(4) . . ? C16 C15 C14 119.7(4) . . ? C16 C15 C18 118.1(4) . . ? C14 C15 C18 122.2(4) . . ? C15 C16 C17 120.4(4) . . ? C12 C17 C16 121.3(4) . . ? C15 C18 S4 114.7(3) . . ? C22 C21 S5 116.6(3) . . ? C27 C22 C23 119.2(4) . . ? C27 C22 C21 118.8(4) . . ? C23 C22 C21 122.0(4) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 C29 119.7(4) . . ? C22 C23 C29 120.7(4) . . ? C25 C24 C23 119.8(4) . . ? C25 C24 C30 120.3(4) . . ? C23 C24 C30 119.9(4) . . ? C26 C25 C24 119.5(4) . . ? C26 C25 C28 117.9(4) . . ? C24 C25 C28 122.6(4) . . ? C27 C26 C25 120.7(4) . . ? C26 C27 C22 121.0(4) . . ? C25 C28 S6 115.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.571 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.082 # Attachment '- As253 - ob171.cif' data_ob171 _database_code_depnum_ccdc_archive 'CCDC 824400' #TrackingRef '- As253 - ob171.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H42 As2 S6' _chemical_formula_weight 1033.08 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.660(7) _cell_length_b 10.399(3) _cell_length_c 20.779(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.192(7) _cell_angle_gamma 90.00 _cell_volume 4708(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 490 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 17.70 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9188 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9193 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.1695 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4993 _reflns_number_gt 2550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4993 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 As1 As 0.70123(3) 0.91499(7) 0.80965(4) 0.0332(2) Uani 1 1 d . . . S1 S 0.69344(9) 0.87632(18) 0.69784(11) 0.0412(5) Uani 1 1 d . . . S2 S 0.76839(9) 1.0762(2) 0.84514(12) 0.0443(5) Uani 1 1 d . . . S3 S 0.77332(8) 0.76532(19) 0.88295(11) 0.0402(5) Uani 1 1 d . . . C1 C 0.6399(3) 1.0066(7) 0.6398(4) 0.040(2) Uani 1 1 d . . . H1A H 0.6587 1.0890 0.6671 0.048 Uiso 1 1 calc R . . H1B H 0.6341 1.0101 0.5882 0.048 Uiso 1 1 calc R . . C2 C 0.5776(3) 0.9948(7) 0.6254(4) 0.0353(18) Uani 1 1 d . . . C3 C 0.5395(3) 0.8894(7) 0.5805(4) 0.043(2) Uani 1 1 d . . . H3A H 0.5544 0.8242 0.5636 0.052 Uiso 1 1 calc R . . C4 C 0.4815(3) 0.8817(7) 0.5617(4) 0.0389(19) Uani 1 1 d . . . H4A H 0.4568 0.8096 0.5328 0.047 Uiso 1 1 calc R . . C5 C 0.4569(3) 0.9797(7) 0.5844(4) 0.0314(17) Uani 1 1 d . . . C6 C 0.4717(3) 1.1824(6) 0.6509(4) 0.0346(18) Uani 1 1 d . . . H6A H 0.4972 1.2530 0.6810 0.041 Uiso 1 1 calc R . . C7 C 0.4955(3) 1.0852(7) 0.6300(4) 0.0327(17) Uani 1 1 d . . . C8 C 0.5569(3) 1.0883(7) 0.6506(4) 0.0380(18) Uani 1 1 d . . . H8A H 0.5835 1.1565 0.6823 0.046 Uiso 1 1 calc R . . C9 C 0.7718(3) 1.1486(7) 0.9279(4) 0.043(2) Uani 1 1 d . . . H9A H 0.7978 1.0944 0.9753 0.052 Uiso 1 1 calc R . . H9B H 0.7913 1.2344 0.9392 0.052 Uiso 1 1 calc R . . C10 C 0.7095(3) 1.1629(7) 0.9118(4) 0.0367(19) Uani 1 1 d . . . C11 C 0.6711(3) 1.2670(7) 0.8674(4) 0.0360(18) Uani 1 1 d . . . H11A H 0.6861 1.3321 0.8504 0.043 Uiso 1 1 calc R . . C12 C 0.6135(3) 1.2762(7) 0.8485(4) 0.0383(19) Uani 1 1 d . . . H12A H 0.5894 1.3492 0.8197 0.046 Uiso 1 1 calc R . . C13 C 0.5876(3) 1.1797(7) 0.8703(4) 0.0322(17) Uani 1 1 d . . . C14 C 0.6258(3) 1.0722(7) 0.9148(4) 0.0306(17) Uani 1 1 d . . . C15 C 0.6870(3) 1.0695(7) 0.9352(4) 0.0348(18) Uani 1 1 d . . . H15A H 0.7130 1.0002 0.9662 0.042 Uiso 1 1 calc R . . C16 C 0.6023(3) 0.9768(6) 0.9361(4) 0.0330(18) Uani 1 1 d . . . H16A H 0.6278 0.9062 0.9661 0.040 Uiso 1 1 calc R . . C17 C 0.7273(3) 0.6200(6) 0.8449(4) 0.0381(19) Uani 1 1 d . . . H17A H 0.7184 0.6009 0.7926 0.046 Uiso 1 1 calc R . . H17B H 0.7518 0.5476 0.8804 0.046 Uiso 1 1 calc R . . C18 C 0.6677(3) 0.6265(6) 0.8369(4) 0.0326(18) Uani 1 1 d . . . C19 C 0.6671(3) 0.6342(6) 0.9051(4) 0.0324(18) Uani 1 1 d . . . H19A H 0.7050 0.6403 0.9555 0.039 Uiso 1 1 calc R . . C20 C 0.6141(3) 0.6330(6) 0.8998(4) 0.0355(18) Uani 1 1 d . . . H20A H 0.6156 0.6360 0.9465 0.043 Uiso 1 1 calc R . . C21 C 0.5565(3) 0.6273(6) 0.8257(4) 0.0274(16) Uani 1 1 d . . . C22 C 0.5551(3) 0.6249(6) 0.7555(4) 0.0277(16) Uani 1 1 d . . . C23 C 0.6128(3) 0.6230(6) 0.7645(4) 0.0313(17) Uani 1 1 d . . . H23A H 0.6128 0.6191 0.7187 0.038 Uiso 1 1 calc R . . C24 C 0.4988(3) 0.6242(6) 0.6820(4) 0.0339(18) Uani 1 1 d . . . H24A H 0.4982 0.6215 0.6359 0.041 Uiso 1 1 calc R . . C25 C 0.5587(5) 0.4622(11) 0.5502(6) 0.071(3) Uani 1 1 d . . . H25A H 0.6001 0.4354 0.5859 0.085 Uiso 1 1 calc R . . C26 C 0.5452(5) 0.5623(10) 0.5027(8) 0.073(3) Uani 1 1 d . . . H26A H 0.5770 0.6065 0.5041 0.088 Uiso 1 1 calc R . . C27 C 0.4867(7) 0.6005(9) 0.4528(6) 0.081(3) Uani 1 1 d . . . H27A H 0.4773 0.6724 0.4195 0.097 Uiso 1 1 calc R . . 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 As1 0.0325(4) 0.0339(4) 0.0344(4) -0.0004(4) 0.0199(4) 0.0000(4) S1 0.0448(12) 0.0417(13) 0.0399(12) 0.0003(10) 0.0261(11) 0.0053(10) S2 0.0487(13) 0.0423(12) 0.0511(13) -0.0086(11) 0.0340(12) -0.0122(11) S3 0.0291(11) 0.0423(13) 0.0383(12) 0.0035(10) 0.0131(10) 0.0020(9) C1 0.037(5) 0.047(5) 0.029(4) 0.009(4) 0.015(4) 0.001(4) C2 0.037(5) 0.040(5) 0.028(4) 0.010(4) 0.017(4) 0.002(4) C3 0.048(5) 0.037(5) 0.038(5) 0.004(4) 0.021(4) 0.007(4) C4 0.041(5) 0.033(5) 0.037(5) 0.007(4) 0.020(4) 0.002(4) C5 0.028(4) 0.035(4) 0.017(4) 0.004(3) 0.004(3) 0.000(4) C6 0.041(5) 0.024(4) 0.032(4) -0.004(3) 0.017(4) -0.011(4) C7 0.034(4) 0.035(4) 0.024(4) 0.009(4) 0.014(4) 0.003(4) C8 0.039(5) 0.035(4) 0.029(4) 0.007(4) 0.014(4) -0.004(4) C9 0.038(5) 0.042(5) 0.044(5) -0.011(4) 0.020(4) -0.007(4) C10 0.043(5) 0.035(5) 0.029(4) -0.013(4) 0.019(4) -0.006(4) C11 0.039(5) 0.025(4) 0.036(5) -0.006(3) 0.017(4) -0.016(4) C12 0.039(5) 0.023(4) 0.042(5) -0.007(4) 0.017(4) -0.003(4) C13 0.038(5) 0.034(4) 0.022(4) -0.005(3) 0.016(4) 0.000(4) C14 0.033(4) 0.033(4) 0.026(4) -0.011(3) 0.018(4) 0.004(4) C15 0.039(4) 0.033(4) 0.024(4) 0.000(3) 0.013(4) 0.010(4) C16 0.033(5) 0.028(4) 0.023(4) 0.002(3) 0.008(4) 0.006(4) C17 0.036(4) 0.037(5) 0.038(5) 0.009(4) 0.020(4) 0.003(4) C18 0.036(5) 0.019(4) 0.047(5) 0.002(3) 0.027(4) 0.000(3) C19 0.026(4) 0.034(4) 0.026(4) 0.001(3) 0.009(4) 0.004(3) C20 0.038(5) 0.038(5) 0.030(4) -0.001(3) 0.019(4) 0.004(4) C21 0.032(4) 0.025(4) 0.019(4) 0.006(3) 0.011(4) 0.003(3) C22 0.030(4) 0.018(4) 0.028(4) -0.001(3) 0.013(4) -0.002(3) C23 0.036(5) 0.023(4) 0.036(4) 0.000(3) 0.022(4) -0.001(3) C24 0.039(5) 0.026(4) 0.033(4) 0.002(3) 0.018(4) 0.001(4) C25 0.054(7) 0.080(8) 0.058(7) -0.003(6) 0.021(6) 0.022(6) C26 0.078(8) 0.059(8) 0.118(10) -0.028(7) 0.077(8) -0.024(6) C27 0.122(10) 0.058(7) 0.100(9) 0.044(6) 0.085(9) 0.034(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 As1 S2 2.244(2) . ? As1 S1 2.246(2) . ? As1 S3 2.250(2) . ? S1 C1 1.828(7) . ? S2 C9 1.831(7) . ? S3 C17 1.815(7) . ? C1 C2 1.513(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C8 1.364(9) . ? C2 C3 1.418(9) . ? C3 C4 1.361(8) . ? C3 H3A 0.9500 . ? C4 C5 1.431(9) . ? C4 H4A 0.9500 . ? C5 C16 1.377(9) 2_656 ? C5 C7 1.427(9) . ? C6 C13 1.373(8) 2_656 ? C6 C7 1.391(8) . ? C6 H6A 0.9500 . ? C7 C8 1.434(8) . ? C8 H8A 0.9500 . ? C9 C10 1.502(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.369(9) . ? C10 C11 1.407(9) . ? C11 C12 1.352(8) . ? C11 H11A 0.9500 . ? C12 C13 1.434(9) . ? C12 H12A 0.9500 . ? C13 C6 1.373(8) 2_656 ? C13 C14 1.434(9) . ? C14 C16 1.378(8) . ? C14 C15 1.428(8) . ? C15 H15A 0.9500 . ? C16 C5 1.377(9) 2_656 ? C16 H16A 0.9500 . ? C17 C18 1.500(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.368(9) . ? C18 C19 1.428(8) . ? C19 C20 1.353(8) . ? C19 H19A 0.9500 . ? C20 C21 1.417(8) . ? C20 H20A 0.9500 . ? C21 C24 1.387(8) 2_656 ? C21 C22 1.438(8) . ? C22 C24 1.394(8) . ? C22 C23 1.441(8) . ? C23 H23A 0.9500 . ? C24 C21 1.387(8) 2_656 ? C24 H24A 0.9500 . ? C25 C27 1.343(11) 5_666 ? C25 C26 1.333(12) . ? C25 H25A 0.9500 . ? C26 C27 1.342(12) . ? C26 H26A 0.9500 . ? C27 C25 1.343(11) 5_666 ? C27 H27A 0.9500 . ? 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 S2 As1 S1 93.11(7) . . ? S2 As1 S3 94.92(8) . . ? S1 As1 S3 96.32(8) . . ? C1 S1 As1 97.0(2) . . ? C9 S2 As1 102.4(2) . . ? C17 S3 As1 100.5(2) . . ? C2 C1 S1 114.9(5) . . ? C2 C1 H1A 108.5 . . ? S1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? S1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C8 C2 C3 120.5(7) . . ? C8 C2 C1 120.6(7) . . ? C3 C2 C1 118.8(7) . . ? C4 C3 C2 119.9(7) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 121.6(7) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C16 C5 C7 118.8(7) 2_656 . ? C16 C5 C4 122.9(7) 2_656 . ? C7 C5 C4 118.3(6) . . ? C13 C6 C7 122.2(7) 2_656 . ? C13 C6 H6A 118.9 2_656 . ? C7 C6 H6A 118.9 . . ? C6 C7 C5 118.8(6) . . ? C6 C7 C8 122.6(7) . . ? C5 C7 C8 118.5(7) . . ? C2 C8 C7 121.0(7) . . ? C2 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C10 C9 S2 112.5(5) . . ? C10 C9 H9A 109.1 . . ? S2 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? S2 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C15 C10 C11 118.5(7) . . ? C15 C10 C9 120.4(7) . . ? C11 C10 C9 121.0(7) . . ? C12 C11 C10 121.3(7) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C13 122.2(7) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C6 C13 C14 118.9(7) 2_656 . ? C6 C13 C12 124.0(7) 2_656 . ? C14 C13 C12 117.1(6) . . ? C16 C14 C15 123.0(7) . . ? C16 C14 C13 118.8(6) . . ? C15 C14 C13 118.2(7) . . ? C10 C15 C14 122.6(7) . . ? C10 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C5 C16 C14 122.6(7) 2_656 . ? C5 C16 H16A 118.7 2_656 . ? C14 C16 H16A 118.7 . . ? C18 C17 S3 114.7(5) . . ? C18 C17 H17A 108.6 . . ? S3 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? S3 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C23 C18 C19 118.4(6) . . ? C23 C18 C17 121.0(6) . . ? C19 C18 C17 120.6(7) . . ? C20 C19 C18 121.8(7) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C24 C21 C20 122.8(6) 2_656 . ? C24 C21 C22 118.6(6) 2_656 . ? C20 C21 C22 118.7(6) . . ? C24 C22 C21 119.6(6) . . ? C24 C22 C23 122.5(6) . . ? C21 C22 C23 117.9(6) . . ? C18 C23 C22 121.9(6) . . ? C18 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C21 C24 C22 121.8(6) 2_656 . ? C21 C24 H24A 119.1 2_656 . ? C22 C24 H24A 119.1 . . ? C27 C25 C26 119.5(9) 5_666 . ? C27 C25 H25A 120.2 5_666 . ? C26 C25 H25A 120.2 . . ? C27 C26 C25 120.0(9) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C25 120.5(9) . 5_666 ? C26 C27 H27A 119.8 . . ? C25 C27 H27A 119.8 5_666 . ? 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 S2 As1 S1 C1 -80.0(2) . . . . ? S3 As1 S1 C1 -175.3(2) . . . . ? S1 As1 S2 C9 169.3(3) . . . . ? S3 As1 S2 C9 -94.1(3) . . . . ? S2 As1 S3 C17 -168.5(2) . . . . ? S1 As1 S3 C17 -74.8(2) . . . . ? As1 S1 C1 C2 -63.9(5) . . . . ? S1 C1 C2 C8 120.4(6) . . . . ? S1 C1 C2 C3 -63.9(8) . . . . ? C8 C2 C3 C4 0.6(11) . . . . ? C1 C2 C3 C4 -175.1(6) . . . . ? C2 C3 C4 C5 1.6(11) . . . . ? C3 C4 C5 C16 177.7(7) . . . 2_656 ? C3 C4 C5 C7 -2.0(10) . . . . ? C13 C6 C7 C5 0.5(10) 2_656 . . . ? C13 C6 C7 C8 178.7(6) 2_656 . . . ? C16 C5 C7 C6 -1.1(10) 2_656 . . . ? C4 C5 C7 C6 178.6(6) . . . . ? C16 C5 C7 C8 -179.4(6) 2_656 . . . ? C4 C5 C7 C8 0.2(9) . . . . ? C3 C2 C8 C7 -2.4(10) . . . . ? C1 C2 C8 C7 173.2(6) . . . . ? C6 C7 C8 C2 -176.3(6) . . . . ? C5 C7 C8 C2 1.9(10) . . . . ? As1 S2 C9 C10 -43.8(6) . . . . ? S2 C9 C10 C15 93.8(7) . . . . ? S2 C9 C10 C11 -81.3(7) . . . . ? C15 C10 C11 C12 0.6(11) . . . . ? C9 C10 C11 C12 175.8(6) . . . . ? C10 C11 C12 C13 -1.8(11) . . . . ? C11 C12 C13 C6 -176.8(7) . . . 2_656 ? C11 C12 C13 C14 1.0(10) . . . . ? C6 C13 C14 C16 -1.4(10) 2_656 . . . ? C12 C13 C14 C16 -179.3(6) . . . . ? C6 C13 C14 C15 178.8(6) 2_656 . . . ? C12 C13 C14 C15 0.9(9) . . . . ? C11 C10 C15 C14 1.4(10) . . . . ? C9 C10 C15 C14 -173.8(6) . . . . ? C16 C14 C15 C10 178.1(6) . . . . ? C13 C14 C15 C10 -2.2(10) . . . . ? C15 C14 C16 C5 -179.4(6) . . . 2_656 ? C13 C14 C16 C5 0.8(10) . . . 2_656 ? As1 S3 C17 C18 -46.1(5) . . . . ? S3 C17 C18 C23 113.7(6) . . . . ? S3 C17 C18 C19 -67.5(7) . . . . ? C23 C18 C19 C20 2.6(10) . . . . ? C17 C18 C19 C20 -176.3(6) . . . . ? C18 C19 C20 C21 -1.6(10) . . . . ? C19 C20 C21 C24 179.1(6) . . . 2_656 ? C19 C20 C21 C22 -1.0(10) . . . . ? C24 C21 C22 C24 2.2(8) 2_656 . . . ? C20 C21 C22 C24 -177.6(6) . . . . ? C24 C21 C22 C23 -177.6(6) 2_656 . . . ? C20 C21 C22 C23 2.6(9) . . . . ? C19 C18 C23 C22 -0.9(10) . . . . ? C17 C18 C23 C22 178.0(6) . . . . ? C24 C22 C23 C18 178.6(6) . . . . ? C21 C22 C23 C18 -1.6(10) . . . . ? C21 C22 C24 C21 0.8(9) . . . 2_656 ? C23 C22 C24 C21 -179.4(6) . . . 2_656 ? C27 C25 C26 C27 0.7(17) 5_666 . . . ? C25 C26 C27 C25 -0.7(18) . . . 5_666 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.752 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.105 # Attachment '- As273 - sean6.cif' data_sean6 _database_code_depnum_ccdc_archive 'CCDC 824401' #TrackingRef '- As273 - sean6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 As2 S6' _chemical_formula_weight 954.97 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.093(2) _cell_length_b 13.5902(10) _cell_length_c 10.6951(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.0900(10) _cell_angle_gamma 90.00 _cell_volume 4319.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3553 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 23.37 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.8066 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19714 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4719 _reflns_number_gt 3603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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^)+(0.0406P)^2^+1.3454P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4719 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 As1 As 0.177688(10) 0.24366(2) 1.19440(3) 0.04030(12) Uani 1 1 d . . . S1 S 0.23162(3) 0.34075(7) 1.16229(9) 0.0513(2) Uani 1 1 d . . . S2 S -0.18364(3) 0.29015(7) 0.10063(8) 0.0522(2) Uani 1 1 d . . . S3 S 0.21799(3) 0.10547(6) 1.24650(8) 0.0474(2) Uani 1 1 d . . . C1 C 0.19469(13) 0.4437(3) 1.0864(4) 0.0517(9) Uani 1 1 d . . . C2 C 0.15784(10) 0.4169(2) 0.9651(3) 0.0417(7) Uani 1 1 d . . . C3 C 0.16674(12) 0.3986(3) 0.8484(3) 0.0514(9) Uani 1 1 d . . . C4 C 0.13269(12) 0.3764(3) 0.7370(4) 0.0513(9) Uani 1 1 d . . . C5 C 0.08837(10) 0.3698(2) 0.7392(3) 0.0399(7) Uani 1 1 d . . . C6 C 0.07936(11) 0.3854(3) 0.8562(3) 0.0481(8) Uani 1 1 d . . . C7 C 0.11379(11) 0.4098(3) 0.9676(3) 0.0472(8) Uani 1 1 d . . . C8 C 0.05264(10) 0.3462(2) 0.6220(3) 0.0444(8) Uani 1 1 d . . . C9 C 0.02231(10) 0.3269(3) 0.5272(3) 0.0453(8) Uani 1 1 d . . . C10 C -0.01538(10) 0.3036(2) 0.4155(3) 0.0409(7) Uani 1 1 d . . . C11 C -0.03022(12) 0.2081(3) 0.3914(3) 0.0480(8) Uani 1 1 d . . . C12 C -0.06704(12) 0.1860(3) 0.2878(3) 0.0482(8) Uani 1 1 d . . . C13 C -0.09006(11) 0.2587(2) 0.2042(3) 0.0417(8) Uani 1 1 d . . . C14 C -0.07526(11) 0.3541(3) 0.2277(3) 0.0470(8) Uani 1 1 d . . . C15 C -0.03829(11) 0.3771(3) 0.3311(3) 0.0470(8) Uani 1 1 d . . . C16 C -0.13101(12) 0.2326(3) 0.0921(4) 0.0528(9) Uani 1 1 d . . . C17 C 0.20589(12) 0.0522(3) 1.0820(4) 0.0494(9) Uani 1 1 d . . . C18 C 0.15666(10) 0.0552(2) 1.0050(3) 0.0406(7) Uani 1 1 d . . . C19 C 0.12510(11) 0.0039(3) 1.0456(3) 0.0505(9) Uani 1 1 d . . . C20 C 0.08014(12) 0.0060(3) 0.9746(4) 0.0517(9) Uani 1 1 d . . . C21 C 0.06577(10) 0.0613(2) 0.8600(3) 0.0419(7) Uani 1 1 d . . . C22 C 0.09728(11) 0.1140(2) 0.8213(3) 0.0443(8) Uani 1 1 d . . . C23 C 0.14215(11) 0.1114(3) 0.8930(3) 0.0450(8) Uani 1 1 d . . . C24 C 0.01904(10) 0.0616(2) 0.7832(3) 0.0473(8) Uani 1 1 d . . . H1A H 0.1798(11) 0.472(3) 1.149(3) 0.063(11) Uiso 1 1 d . . . H1B H 0.2130(13) 0.489(3) 1.070(4) 0.073(13) Uiso 1 1 d . . . H3 H 0.1967(12) 0.402(2) 0.847(3) 0.061(11) Uiso 1 1 d . . . H4 H 0.1386(11) 0.367(2) 0.663(3) 0.054(10) Uiso 1 1 d . . . H6 H 0.0493(12) 0.381(3) 0.860(3) 0.072(12) Uiso 1 1 d . . . H7 H 0.1072(10) 0.419(2) 1.041(3) 0.047(10) Uiso 1 1 d . . . H11 H -0.0163(11) 0.159(2) 0.444(3) 0.056(10) Uiso 1 1 d . . . H12 H -0.0762(11) 0.117(2) 0.277(3) 0.053(10) Uiso 1 1 d . . . H14 H -0.0892(10) 0.406(2) 0.169(3) 0.049(9) Uiso 1 1 d . . . H15 H -0.0304(10) 0.441(2) 0.353(3) 0.046(9) Uiso 1 1 d . . . H16A H -0.1350(12) 0.160(3) 0.086(4) 0.073(12) Uiso 1 1 d . . . H16B H -0.1274(11) 0.260(2) 0.013(3) 0.051(10) Uiso 1 1 d . . . H17A H 0.2223(12) 0.088(3) 1.035(3) 0.058(11) Uiso 1 1 d . . . H17B H 0.2158(11) -0.011(3) 1.100(3) 0.053(10) Uiso 1 1 d . . . H19 H 0.1335(10) -0.031(2) 1.118(3) 0.049(10) Uiso 1 1 d . . . H20 H 0.0608(10) -0.030(2) 1.003(3) 0.046(9) Uiso 1 1 d . . . H22 H 0.0871(9) 0.154(2) 0.746(3) 0.040(8) Uiso 1 1 d . . . H23 H 0.1622(10) 0.143(2) 0.866(3) 0.042(9) 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 As1 0.02696(18) 0.0473(2) 0.04120(19) 0.00217(14) 0.00162(13) 0.00171(14) S1 0.0303(4) 0.0629(6) 0.0564(5) 0.0053(4) 0.0060(4) -0.0041(4) S2 0.0395(5) 0.0636(6) 0.0466(5) 0.0114(4) 0.0018(4) -0.0008(4) S3 0.0363(4) 0.0524(5) 0.0455(5) 0.0040(4) -0.0006(3) 0.0086(4) C1 0.046(2) 0.049(2) 0.054(2) -0.0019(17) 0.0057(17) -0.0070(18) C2 0.0390(17) 0.0386(17) 0.0418(17) 0.0047(14) 0.0029(14) -0.0042(14) C3 0.0340(18) 0.069(2) 0.050(2) -0.0029(17) 0.0112(16) -0.0144(17) C4 0.0423(19) 0.065(2) 0.048(2) -0.0094(18) 0.0152(16) -0.0126(17) C5 0.0347(16) 0.0387(17) 0.0433(18) 0.0060(14) 0.0069(13) -0.0024(14) C6 0.0341(18) 0.057(2) 0.053(2) 0.0141(16) 0.0125(16) 0.0061(16) C7 0.044(2) 0.059(2) 0.0378(18) 0.0086(16) 0.0119(15) 0.0080(17) C8 0.0386(18) 0.0459(19) 0.0483(19) 0.0068(15) 0.0121(15) -0.0010(15) C9 0.0355(17) 0.054(2) 0.0469(19) 0.0032(15) 0.0128(15) -0.0014(16) C10 0.0330(16) 0.050(2) 0.0411(17) 0.0007(14) 0.0131(13) -0.0014(15) C11 0.045(2) 0.046(2) 0.050(2) 0.0047(17) 0.0087(16) 0.0062(17) C12 0.047(2) 0.042(2) 0.054(2) -0.0042(16) 0.0119(16) -0.0017(17) C13 0.0346(17) 0.054(2) 0.0378(17) -0.0030(14) 0.0130(13) -0.0026(15) C14 0.0416(19) 0.050(2) 0.047(2) 0.0063(16) 0.0098(15) -0.0022(17) C15 0.044(2) 0.043(2) 0.053(2) 0.0035(16) 0.0130(16) -0.0037(16) C16 0.045(2) 0.071(3) 0.040(2) -0.0025(18) 0.0082(16) -0.0044(19) C17 0.0345(19) 0.056(2) 0.055(2) -0.0026(18) 0.0082(16) 0.0060(17) C18 0.0311(16) 0.0457(18) 0.0432(18) -0.0065(14) 0.0080(13) 0.0019(14) C19 0.0409(19) 0.057(2) 0.047(2) 0.0073(17) 0.0040(16) -0.0006(17) C20 0.041(2) 0.057(2) 0.057(2) 0.0034(18) 0.0128(17) -0.0084(18) C21 0.0363(17) 0.0428(18) 0.0435(18) -0.0063(14) 0.0069(14) 0.0015(15) C22 0.0432(19) 0.0448(19) 0.0401(18) -0.0009(15) 0.0049(15) 0.0011(15) C23 0.0389(19) 0.050(2) 0.0460(19) -0.0021(15) 0.0125(15) -0.0081(16) C24 0.0386(17) 0.052(2) 0.0479(19) -0.0036(15) 0.0080(14) 0.0013(15) _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 As1 S3 2.2355(9) . ? As1 S2 2.2362(9) 2_556 ? As1 S1 2.2381(9) . ? S1 C1 1.840(4) . ? S2 C16 1.840(4) . ? S2 As1 2.2362(9) 2_556 ? S3 C17 1.836(4) . ? C1 C2 1.502(4) . ? C1 H1A 1.00(4) . ? C1 H1B 0.89(4) . ? C2 C3 1.378(5) . ? C2 C7 1.381(4) . ? C3 C4 1.374(5) . ? C3 H3 0.94(3) . ? C4 C5 1.388(4) . ? C4 H4 0.88(3) . ? C5 C6 1.377(5) . ? C5 C8 1.446(4) . ? C6 C7 1.388(5) . ? C6 H6 0.95(4) . ? C7 H7 0.87(3) . ? C8 C9 1.193(4) . ? C9 C10 1.442(4) . ? C10 C11 1.376(5) . ? C10 C15 1.394(4) . ? C11 C12 1.373(5) . ? C11 H11 0.90(3) . ? C12 C13 1.382(5) . ? C12 H12 0.97(3) . ? C13 C14 1.374(4) . ? C13 C16 1.513(5) . ? C14 C15 1.377(5) . ? C14 H14 0.95(3) . ? C15 H15 0.91(3) . ? C16 H16A 0.99(4) . ? C16 H16B 0.96(3) . ? C17 C18 1.510(4) . ? C17 H17A 0.95(3) . ? C17 H17B 0.91(3) . ? C18 C19 1.374(5) . ? C18 C23 1.379(4) . ? C19 C20 1.381(5) . ? C19 H19 0.89(3) . ? C20 C21 1.394(5) . ? C20 H20 0.90(3) . ? C21 C22 1.372(5) . ? C21 C24 1.444(4) . ? C22 C23 1.381(4) . ? C22 H22 0.95(3) . ? C23 H23 0.87(3) . ? C24 C24 1.188(6) 2_556 ? 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 S3 As1 S2 96.56(3) . 2_556 ? S3 As1 S1 98.23(3) . . ? S2 As1 S1 97.70(4) 2_556 . ? C1 S1 As1 96.74(14) . . ? C16 S2 As1 96.32(13) . 2_556 ? C17 S3 As1 98.64(13) . . ? C2 C1 S1 114.6(3) . . ? C2 C1 H1A 106.6(19) . . ? S1 C1 H1A 111(2) . . ? C2 C1 H1B 111(2) . . ? S1 C1 H1B 105(3) . . ? H1A C1 H1B 108(3) . . ? C3 C2 C7 118.0(3) . . ? C3 C2 C1 121.4(3) . . ? C7 C2 C1 120.6(3) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 121(2) . . ? C2 C3 H3 118(2) . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 120(2) . . ? C5 C4 H4 119(2) . . ? C6 C5 C4 118.3(3) . . ? C6 C5 C8 120.9(3) . . ? C4 C5 C8 120.9(3) . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6 120(2) . . ? C7 C6 H6 120(2) . . ? C2 C7 C6 121.3(3) . . ? C2 C7 H7 120(2) . . ? C6 C7 H7 119(2) . . ? C9 C8 C5 178.1(4) . . ? C8 C9 C10 178.0(4) . . ? C11 C10 C15 118.4(3) . . ? C11 C10 C9 120.6(3) . . ? C15 C10 C9 121.0(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119(2) . . ? C10 C11 H11 120(2) . . ? C11 C12 C13 121.1(3) . . ? C11 C12 H12 117.0(19) . . ? C13 C12 H12 121.9(19) . . ? C14 C13 C12 118.3(3) . . ? C14 C13 C16 121.7(3) . . ? C12 C13 C16 120.0(3) . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 120.8(19) . . ? C15 C14 H14 118.0(19) . . ? C14 C15 C10 120.3(3) . . ? C14 C15 H15 121(2) . . ? C10 C15 H15 118.0(19) . . ? C13 C16 S2 114.5(3) . . ? C13 C16 H16A 110(2) . . ? S2 C16 H16A 109(2) . . ? C13 C16 H16B 109(2) . . ? S2 C16 H16B 103(2) . . ? H16A C16 H16B 112(3) . . ? C18 C17 S3 113.7(2) . . ? C18 C17 H17A 108(2) . . ? S3 C17 H17A 108(2) . . ? C18 C17 H17B 111(2) . . ? S3 C17 H17B 102(2) . . ? H17A C17 H17B 114(3) . . ? C19 C18 C23 118.3(3) . . ? C19 C18 C17 121.1(3) . . ? C23 C18 C17 120.6(3) . . ? C18 C19 C20 121.1(3) . . ? C18 C19 H19 120(2) . . ? C20 C19 H19 119(2) . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 118(2) . . ? C21 C20 H20 121(2) . . ? C22 C21 C20 118.3(3) . . ? C22 C21 C24 121.0(3) . . ? C20 C21 C24 120.7(3) . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 117.9(18) . . ? C23 C22 H22 121.2(18) . . ? C18 C23 C22 121.0(3) . . ? C18 C23 H23 118(2) . . ? C22 C23 H23 120(2) . . ? C24 C24 C21 178.2(5) 2_556 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.609 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.067 # Attachment '- As283 - g36.cif' data_g36 _database_code_depnum_ccdc_archive 'CCDC 824402' #TrackingRef '- As283 - g36.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.33 H30.33 As2 Cl S6' _chemical_formula_weight 844.59 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 Hexagonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 21.3256(7) _cell_length_b 21.3256(7) _cell_length_c 41.358(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16288.8(13) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8087 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.61 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7692 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4924 _exptl_absorpt_correction_T_max 0.6830 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector Bruker Apex' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58788 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3969 _reflns_number_gt 3478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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. In the crystal structure solvent molecule, CHCl3, is disordered around a -3 axis. The solvate molecule were treated by SQUEEZE [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.]. Corrections of the X-ray data by SQUEEZE (343 electron/cell) was close to the required values (348 electron/cell) corresponding to six CHCl3 molecules in the full unit cell. ; _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^)+(0.0597P)^2^+29.1844P] 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 3969 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 As1 As 0.117472(15) 0.582828(14) 0.067699(8) 0.04870(12) Uani 1 1 d . . . S1 S 0.22052(4) 0.62369(4) 0.04013(3) 0.0741(3) Uani 1 1 d . . . S2 S -0.11091(4) 0.82647(5) 0.05467(2) 0.0714(3) Uani 1 1 d . . . S3 S 0.06335(4) 0.46834(4) 0.04920(2) 0.0553(2) Uani 1 1 d . . . C1 C 0.20710(18) 0.67141(18) 0.00634(10) 0.0679(9) Uani 1 1 d . . . H1A H 0.2547 0.7040 -0.0037 0.082 Uiso 1 1 calc R . . H1B H 0.1765 0.6354 -0.0102 0.082 Uiso 1 1 calc R . . C2 C 0.17273(15) 0.71486(15) 0.01555(7) 0.0506(6) Uani 1 1 d . . . C3 C 0.21265(14) 0.77976(15) 0.03330(7) 0.0485(6) Uani 1 1 d . . . H3A H 0.2611 0.7949 0.0394 0.058 Uiso 1 1 calc R . . C4 C 0.18295(14) 0.82075(14) 0.04171(6) 0.0444(6) Uani 1 1 d . . . H4A H 0.2109 0.8641 0.0537 0.053 Uiso 1 1 calc R . . C5 C 0.11078(13) 0.79986(14) 0.03291(6) 0.0425(5) Uani 1 1 d . . . C6 C 0.06993(14) 0.73424(14) 0.01551(7) 0.0474(6) Uani 1 1 d . . . C7 C 0.10260(16) 0.69330(15) 0.00734(7) 0.0532(7) Uani 1 1 d . . . H7A H 0.0752 0.6493 -0.0042 0.064 Uiso 1 1 calc R . . C8 C -0.00216(16) 0.71309(17) 0.00646(8) 0.0571(7) Uani 1 1 d . . . H8A H -0.0306 0.6687 -0.0047 0.069 Uiso 1 1 calc R . . C9 C -0.03080(16) 0.75565(18) 0.01356(8) 0.0613(8) Uani 1 1 d . . . H9A H -0.0791 0.7405 0.0073 0.074 Uiso 1 1 calc R . . C10 C 0.00951(16) 0.82175(17) 0.03005(7) 0.0540(7) Uani 1 1 d . . . C11 C 0.07881(15) 0.84253(15) 0.04021(7) 0.0474(6) Uani 1 1 d . . . H11A H 0.1054 0.8860 0.0522 0.057 Uiso 1 1 calc R . . C12 C -0.02137(18) 0.8706(2) 0.03562(9) 0.0684(9) Uani 1 1 d . . . H12A H -0.0247 0.8909 0.0146 0.082 Uiso 1 1 calc R . . H12B H 0.0126 0.9116 0.0494 0.082 Uiso 1 1 calc R . . C13 C -0.01952(17) 0.43085(15) 0.07329(8) 0.0560(7) Uani 1 1 d . . . H13A H -0.0532 0.3810 0.0657 0.067 Uiso 1 1 calc R . . H13B H -0.0074 0.4277 0.0961 0.067 Uiso 1 1 calc R . . C14 C -0.05777(15) 0.47429(14) 0.07180(7) 0.0519(6) Uani 1 1 d . . . C15 C -0.07518(16) 0.49303(16) 0.04121(7) 0.0550(7) Uani 1 1 d . . . H15A H -0.0610 0.4796 0.0218 0.066 Uiso 1 1 calc R . . C16 C -0.11198(16) 0.53007(16) 0.03971(7) 0.0542(7) Uani 1 1 d . . . H16A H -0.1235 0.5420 0.0193 0.065 Uiso 1 1 calc R . . C17 C -0.07711(15) 0.49475(15) 0.09943(7) 0.0527(7) Uani 1 1 d . . . H17A H -0.0647 0.4831 0.1197 0.063 Uiso 1 1 calc R . . C18 C -0.11594(15) 0.53373(14) 0.09854(6) 0.0491(6) 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 As1 0.04649(18) 0.03592(16) 0.0696(2) -0.00241(12) -0.00858(12) 0.02503(13) S1 0.0429(4) 0.0488(4) 0.1358(9) 0.0114(5) 0.0080(4) 0.0267(3) S2 0.0502(4) 0.0863(6) 0.0922(6) 0.0307(5) 0.0054(4) 0.0450(4) S3 0.0595(4) 0.0399(3) 0.0650(4) -0.0061(3) 0.0072(3) 0.0238(3) C1 0.0528(17) 0.0501(17) 0.094(3) -0.0018(16) 0.0100(16) 0.0202(14) C2 0.0449(14) 0.0390(13) 0.0611(16) 0.0081(12) 0.0032(12) 0.0157(11) C3 0.0343(13) 0.0396(13) 0.0617(16) 0.0092(12) -0.0048(11) 0.0110(10) C4 0.0357(12) 0.0351(12) 0.0515(14) 0.0055(10) -0.0053(10) 0.0095(10) C5 0.0389(12) 0.0405(12) 0.0415(12) 0.0116(10) -0.0029(10) 0.0148(10) C6 0.0385(13) 0.0418(13) 0.0494(14) 0.0100(11) -0.0079(11) 0.0106(11) C7 0.0482(15) 0.0389(13) 0.0584(16) -0.0004(12) -0.0060(12) 0.0111(12) C8 0.0423(14) 0.0548(17) 0.0609(18) 0.0034(13) -0.0159(13) 0.0142(13) C9 0.0393(14) 0.0652(19) 0.0681(19) 0.0145(15) -0.0131(13) 0.0176(14) C10 0.0468(15) 0.0597(17) 0.0565(16) 0.0246(13) 0.0061(12) 0.0274(13) C11 0.0439(14) 0.0411(13) 0.0521(15) 0.0118(11) 0.0002(11) 0.0173(11) C12 0.0575(18) 0.072(2) 0.084(2) 0.0327(18) 0.0128(16) 0.0389(17) C13 0.0617(18) 0.0377(13) 0.0601(17) 0.0044(12) 0.0099(14) 0.0185(13) C14 0.0452(14) 0.0352(13) 0.0607(16) -0.0022(12) 0.0076(12) 0.0090(11) C15 0.0544(16) 0.0477(15) 0.0514(15) -0.0059(12) 0.0029(13) 0.0168(13) C16 0.0552(16) 0.0526(16) 0.0432(14) -0.0054(12) -0.0028(12) 0.0184(13) C17 0.0503(15) 0.0422(14) 0.0517(15) 0.0037(12) 0.0047(12) 0.0127(12) C18 0.0443(14) 0.0410(13) 0.0426(13) -0.0014(10) 0.0038(11) 0.0067(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 S1 2.2302(9) . ? As1 S2 2.2417(9) 16_454 ? As1 S3 2.2496(8) . ? S1 C1 1.834(4) . ? S2 C12 1.832(3) . ? S2 As1 2.2417(9) 16_454 ? S3 C13 1.828(3) . ? C1 C2 1.490(4) . ? C2 C7 1.370(4) . ? C2 C3 1.414(4) . ? C3 C4 1.356(4) . ? C4 C5 1.419(3) . ? C5 C11 1.416(4) . ? C5 C6 1.420(4) . ? C6 C7 1.404(4) . ? C6 C8 1.419(4) . ? C8 C9 1.356(5) . ? C9 C10 1.407(5) . ? C10 C11 1.379(4) . ? C10 C12 1.503(5) . ? C13 C14 1.511(4) . ? C14 C17 1.359(4) . ? C14 C15 1.430(4) . ? C15 C16 1.365(4) . ? C16 C18 1.404(4) 16_454 ? C17 C18 1.438(4) . ? C18 C16 1.404(4) 16_454 ? C18 C18 1.405(6) 16_454 ? 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 S1 As1 S2 94.21(4) . 16_454 ? S1 As1 S3 96.93(3) . . ? S2 As1 S3 93.01(3) 16_454 . ? C1 S1 As1 102.11(11) . . ? C12 S2 As1 98.42(11) . 16_454 ? C13 S3 As1 98.53(10) . . ? C2 C1 S1 114.3(3) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 121.5(3) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 121.1(2) . . ? C3 C4 C5 121.0(2) . . ? C11 C5 C4 122.6(2) . . ? C11 C5 C6 119.1(2) . . ? C4 C5 C6 118.3(2) . . ? C7 C6 C8 122.3(3) . . ? C7 C6 C5 119.0(2) . . ? C8 C6 C5 118.7(3) . . ? C2 C7 C6 122.0(3) . . ? C9 C8 C6 120.6(3) . . ? C8 C9 C10 121.5(3) . . ? C11 C10 C9 119.3(3) . . ? C11 C10 C12 120.1(3) . . ? C9 C10 C12 120.6(3) . . ? C10 C11 C5 120.8(3) . . ? C10 C12 S2 114.5(2) . . ? C14 C13 S3 114.2(2) . . ? C17 C14 C15 119.4(3) . . ? C17 C14 C13 120.4(3) . . ? C15 C14 C13 120.2(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C16 C18 120.6(3) . 16_454 ? C14 C17 C18 121.3(3) . . ? C16 C18 C18 120.3(4) 16_454 16_454 ? C16 C18 C17 121.7(3) 16_454 . ? C18 C18 C17 118.0(3) 16_454 . ? 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 S2 As1 S1 C1 -165.75(12) 16_454 . . . ? S3 As1 S1 C1 100.69(12) . . . . ? S1 As1 S3 C13 176.46(11) . . . . ? S2 As1 S3 C13 81.84(11) 16_454 . . . ? As1 S1 C1 C2 41.3(2) . . . . ? S1 C1 C2 C7 -107.6(3) . . . . ? S1 C1 C2 C3 72.1(3) . . . . ? C7 C2 C3 C4 -1.0(4) . . . . ? C1 C2 C3 C4 179.3(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C11 -177.6(2) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C11 C5 C6 C7 177.8(2) . . . . ? C4 C5 C6 C7 -0.8(4) . . . . ? C11 C5 C6 C8 -1.0(4) . . . . ? C4 C5 C6 C8 -179.7(2) . . . . ? C3 C2 C7 C6 1.2(4) . . . . ? C1 C2 C7 C6 -179.1(3) . . . . ? C8 C6 C7 C2 178.6(3) . . . . ? C5 C6 C7 C2 -0.3(4) . . . . ? C7 C6 C8 C9 -177.1(3) . . . . ? C5 C6 C8 C9 1.7(4) . . . . ? C6 C8 C9 C10 -0.1(5) . . . . ? C8 C9 C10 C11 -2.3(4) . . . . ? C8 C9 C10 C12 175.7(3) . . . . ? C9 C10 C11 C5 3.0(4) . . . . ? C12 C10 C11 C5 -175.0(2) . . . . ? C4 C5 C11 C10 177.3(2) . . . . ? C6 C5 C11 C10 -1.3(4) . . . . ? C11 C10 C12 S2 -129.5(3) . . . . ? C9 C10 C12 S2 52.6(4) . . . . ? As1 S2 C12 C10 55.9(3) 16_454 . . . ? As1 S3 C13 C14 50.7(2) . . . . ? S3 C13 C14 C17 -128.8(2) . . . . ? S3 C13 C14 C15 52.4(3) . . . . ? C17 C14 C15 C16 -1.1(4) . . . . ? C13 C14 C15 C16 177.7(3) . . . . ? C14 C15 C16 C18 0.4(4) . . . 16_454 ? C15 C14 C17 C18 1.2(4) . . . . ? C13 C14 C17 C18 -177.6(2) . . . . ? C14 C17 C18 C16 179.6(3) . . . 16_454 ? C14 C17 C18 C18 -0.5(3) . . . 16_454 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.145 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.065 # Attachment '- Sb283 - g44p.cif' data_g44p _database_code_depnum_ccdc_archive 'CCDC 824403' #TrackingRef '- Sb283 - g44p.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.25 H31.38 Cl3 N0.13 S6 Sb2' _chemical_formula_weight 1022.96 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 21.0255(7) _cell_length_b 21.0255(7) _cell_length_c 21.0255(7) _cell_angle_alpha 69.14 _cell_angle_beta 69.14 _cell_angle_gamma 69.14 _cell_volume 7831.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6306 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.68 _exptl_crystal_description cut-block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4038 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7474 _exptl_absorpt_correction_T_max 0.8607 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector Bruker Apex' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88616 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.00 _reflns_number_total 11413 _reflns_number_gt 9195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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' _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. In the crystal structure solvent molecule, CH3CN, is disordered around a -3 axis. The solvate molecule were treated by SQUEEZE [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.]. Corrections of the X-ray data by SQUEEZE (23 electron/cell) was close to the required values (22 electron/cell) corresponding to one CH3CN molecule in the full unit cell. ; _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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11413 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_restrained_S_all 1.370 _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 Sb1 Sb 0.427849(18) 0.427849(18) 0.427849(18) 0.0686(3) Uani 1 3 d S . . Sb2 Sb 0.280830(16) 0.280830(16) 0.280830(16) 0.0455(2) Uani 1 3 d S . . Sb3 Sb 0.32671(2) 0.82570(2) 0.27071(2) 0.03546(13) Uani 1 1 d . . . Sb4 Sb 0.36810(3) 0.85719(2) -0.05678(2) 0.04521(15) Uani 1 1 d . . . S1 S 0.54199(13) 0.45268(15) 0.37401(14) 0.0819(7) Uani 1 1 d . . . S2 S 0.26978(10) 0.32427(10) 0.16081(10) 0.0541(5) Uani 1 1 d . . . S3 S 0.41555(10) 0.75601(10) 0.33423(10) 0.0527(5) Uani 1 1 d . . . S4 S 0.33471(13) 0.78162(10) -0.09725(12) 0.0638(6) Uani 1 1 d . . . S5 S 0.23354(9) 0.78329(10) 0.36936(9) 0.0501(4) Uani 1 1 d . . . S6 S 0.30796(14) 0.96084(10) -0.13315(10) 0.0678(6) Uani 1 1 d . . . S7 S 0.30710(9) 0.92683(9) 0.31341(8) 0.0449(4) Uani 1 1 d . . . S8 S 0.47861(12) 0.85191(11) -0.14930(10) 0.0608(5) Uani 1 1 d . . . C1 C 0.5480(6) 0.4820(5) 0.2814(5) 0.082(3) Uani 1 1 d . . . H1A H 0.5240 0.5330 0.2696 0.098 Uiso 1 1 calc R . . H1B H 0.5984 0.4764 0.2553 0.098 Uiso 1 1 calc R . . C2 C 0.5170(4) 0.4445(4) 0.2550(4) 0.0551(18) Uani 1 1 d . . . C3 C 0.5517(5) 0.3753(4) 0.2506(5) 0.066(2) Uani 1 1 d . . . H3A H 0.5933 0.3524 0.2664 0.079 Uiso 1 1 calc R . . C4 C 0.5289(4) 0.3397(4) 0.2253(4) 0.0585(19) Uani 1 1 d . . . H4A H 0.5546 0.2928 0.2229 0.070 Uiso 1 1 calc R . . C5 C 0.4674(3) 0.3715(3) 0.2024(3) 0.0433(15) Uani 1 1 d . . . C6 C 0.4411(4) 0.3381(4) 0.1716(4) 0.0479(16) Uani 1 1 d . . . H6A H 0.4650 0.2909 0.1690 0.057 Uiso 1 1 calc R . . C7 C 0.3841(4) 0.3712(4) 0.1464(4) 0.0459(15) Uani 1 1 d . . . C8 C 0.3483(4) 0.4404(4) 0.1522(5) 0.063(2) Uani 1 1 d . . . H8A H 0.3075 0.4642 0.1350 0.075 Uiso 1 1 calc R . . C9 C 0.3698(4) 0.4744(4) 0.1816(5) 0.062(2) Uani 1 1 d . . . H9A H 0.3436 0.5207 0.1854 0.074 Uiso 1 1 calc R . . C10 C 0.4293(4) 0.4421(3) 0.2057(4) 0.0472(16) Uani 1 1 d . . . C11 C 0.4567(4) 0.4776(4) 0.2338(4) 0.0545(18) Uani 1 1 d . . . H11A H 0.4322 0.5244 0.2375 0.065 Uiso 1 1 calc R . . C12 C 0.3586(4) 0.3366(5) 0.1131(4) 0.062(2) Uani 1 1 d . . . H12A H 0.3921 0.2900 0.1103 0.075 Uiso 1 1 calc R . . H12B H 0.3583 0.3656 0.0643 0.075 Uiso 1 1 calc R . . C13 C 0.4540(5) 0.6749(4) 0.3040(4) 0.066(2) Uani 1 1 d . . . H13A H 0.5057 0.6616 0.2970 0.079 Uiso 1 1 calc R . . H13B H 0.4357 0.6365 0.3420 0.079 Uiso 1 1 calc R . . C14 C 0.4402(4) 0.6787(3) 0.2386(4) 0.0467(16) Uani 1 1 d . . . C15 C 0.4904(5) 0.6902(4) 0.1775(5) 0.076(3) Uani 1 1 d . . . H15A H 0.5313 0.6951 0.1827 0.091 Uiso 1 1 calc R . . C16 C 0.4940(6) 0.6962(5) 0.1109(6) 0.088(3) Uani 1 1 d . . . H16A H 0.5332 0.7042 0.0718 0.105 Uiso 1 1 calc R . . C17 C 0.4358(4) 0.6894(3) 0.1067(4) 0.0522(18) Uani 1 1 d . . . C18 C 0.4343(6) 0.6925(4) 0.0310(6) 0.085(3) Uani 1 1 d . . . H18A H 0.4739 0.6972 -0.0086 0.101 Uiso 1 1 calc R . . C19 C 0.3739(4) 0.6881(3) 0.0254(4) 0.0550(19) Uani 1 1 d . . . C20 C 0.3148(6) 0.6812(4) 0.0877(5) 0.085(3) Uani 1 1 d . . . H20A H 0.2728 0.6794 0.0818 0.102 Uiso 1 1 calc R . . C21 C 0.3148(5) 0.6772(5) 0.1532(6) 0.086(3) Uani 1 1 d . . . H21A H 0.2752 0.6726 0.1928 0.103 Uiso 1 1 calc R . . C22 C 0.3756(4) 0.6805(3) 0.1573(5) 0.060(2) Uani 1 1 d . . . C23 C 0.3783(5) 0.6732(4) 0.2370(6) 0.073(3) Uani 1 1 d . . . H23A H 0.3404 0.6659 0.2778 0.088 Uiso 1 1 calc R . . C24 C 0.3638(5) 0.6924(4) -0.0417(4) 0.059(2) Uani 1 1 d . . . H24A H 0.3286 0.6664 -0.0313 0.071 Uiso 1 1 calc R . . H24B H 0.4089 0.6676 -0.0694 0.071 Uiso 1 1 calc R . . C25 C 0.1531(4) 0.8417(4) 0.3414(4) 0.0561(19) Uani 1 1 d . . . H25A H 0.1137 0.8193 0.3673 0.067 Uiso 1 1 calc R . . H25B H 0.1400 0.8869 0.3535 0.067 Uiso 1 1 calc R . . C26 C 0.1636(3) 0.8562(4) 0.2640(4) 0.0463(16) Uani 1 1 d . . . C27 C 0.1587(3) 0.8049(4) 0.2372(4) 0.0477(16) Uani 1 1 d . . . H27A H 0.1482 0.7625 0.2691 0.057 Uiso 1 1 calc R . . C28 C 0.1688(4) 0.8156(4) 0.1680(4) 0.0491(16) Uani 1 1 d . . . H28A H 0.1655 0.7805 0.1516 0.059 Uiso 1 1 calc R . . C29 C 0.1843(3) 0.8787(3) 0.1184(4) 0.0397(14) Uani 1 1 d . . . C30 C 0.1931(3) 0.8923(4) 0.0440(4) 0.0485(16) Uani 1 1 d . . . H30A H 0.1891 0.8585 0.0264 0.058 Uiso 1 1 calc R . . C31 C 0.2071(4) 0.9532(3) -0.0008(4) 0.0482(16) Uani 1 1 d . . . C32 C 0.2145(4) 1.0024(4) 0.0260(4) 0.0582(19) Uani 1 1 d . . . H32A H 0.2261 1.0442 -0.0061 0.070 Uiso 1 1 calc R . . C33 C 0.2058(4) 0.9924(4) 0.0951(4) 0.0568(19) Uani 1 1 d . . . H33A H 0.2102 1.0270 0.1113 0.068 Uiso 1 1 calc R . . C34 C 0.1902(3) 0.9307(3) 0.1424(4) 0.0430(15) Uani 1 1 d . . . C35 C 0.1799(3) 0.9174(4) 0.2170(4) 0.0482(16) Uani 1 1 d . . . H35A H 0.1843 0.9512 0.2343 0.058 Uiso 1 1 calc R . . C36 C 0.2154(5) 0.9692(5) -0.0771(4) 0.074(3) Uani 1 1 d . . . H36A H 0.1872 1.0179 -0.0930 0.089 Uiso 1 1 calc R . . H36B H 0.1957 0.9371 -0.0848 0.089 Uiso 1 1 calc R . . C37 C 0.3835(5) 0.9580(5) 0.2557(4) 0.072(3) Uani 1 1 d . . . H37A H 0.3746 1.0076 0.2557 0.087 Uiso 1 1 calc R . . H37B H 0.4243 0.9298 0.2756 0.087 Uiso 1 1 calc R . . C38 C 0.4029(3) 0.9549(3) 0.1818(3) 0.0389(14) Uani 1 1 d . . . C39 C 0.3636(4) 1.0049(4) 0.1364(4) 0.060(2) Uani 1 1 d . . . H39A H 0.3246 1.0391 0.1555 0.073 Uiso 1 1 calc R . . C40 C 0.3750(4) 1.0094(4) 0.0689(5) 0.060(2) Uani 1 1 d . . . H40A H 0.3465 1.0463 0.0410 0.072 Uiso 1 1 calc R . . C41 C 0.4282(4) 0.9603(3) 0.0413(4) 0.0446(15) Uani 1 1 d . . . C42 C 0.4438(4) 0.9627(4) -0.0345(4) 0.0553(18) Uani 1 1 d . . . H42A H 0.4163 0.9989 -0.0638 0.066 Uiso 1 1 calc R . . C43 C 0.4973(4) 0.9129(4) -0.0603(4) 0.0511(18) Uani 1 1 d . . . C44 C 0.5408(5) 0.8584(5) -0.0174(4) 0.063(2) Uani 1 1 d . . . H44A H 0.5789 0.8243 -0.0376 0.075 Uiso 1 1 calc R . . C45 C 0.5283(4) 0.8552(4) 0.0508(5) 0.066(2) Uani 1 1 d . . . H45A H 0.5570 0.8193 0.0792 0.079 Uiso 1 1 calc R . . C46 C 0.4724(3) 0.9059(3) 0.0785(4) 0.0436(15) Uani 1 1 d . . . C47 C 0.4580(4) 0.9044(4) 0.1558(4) 0.0554(19) Uani 1 1 d . . . H47A H 0.4867 0.8693 0.1846 0.067 Uiso 1 1 calc R . . C48 C 0.5149(5) 0.9114(5) -0.1368(4) 0.069(2) Uani 1 1 d . . . H48A H 0.5668 0.8976 -0.1553 0.083 Uiso 1 1 calc R . . H48B H 0.4971 0.9597 -0.1650 0.083 Uiso 1 1 calc R . . Cl1S Cl 0.23983(10) 0.18312(10) 0.10084(9) 0.0586(5) Uani 1 1 d . . . Cl2S Cl 0.4404(3) 0.5024(3) 0.9703(3) 0.195(3) Uani 1 1 d . . . Cl3S Cl 0.3999(3) 0.4514(2) 0.8974(3) 0.213(3) Uani 1 1 d . . . Cl4S Cl 0.29709(19) 0.5483(2) 0.9739(3) 0.167(2) Uani 1 1 d . . . C1S C 0.1862(2) 0.1862(2) 0.1862(2) 0.039(2) Uani 1 3 d S . . H1SA H 0.2072 0.2072 0.2072 0.047 Uiso 1 3 calc SR . . C2S C 0.3766(6) 0.5245(5) 0.9258(6) 0.087(3) Uani 1 1 d . . . H2SA H 0.3852 0.5649 0.8837 0.104 Uiso 1 1 calc R . . 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 Sb1 0.0786(4) 0.0786(4) 0.0786(4) -0.0320(2) -0.0320(2) -0.0320(2) Sb2 0.0489(2) 0.0489(2) 0.0489(2) -0.01662(15) -0.01662(15) -0.01662(15) Sb3 0.0315(2) 0.0432(2) 0.0308(2) -0.01059(17) -0.00746(16) -0.00867(17) Sb4 0.0686(3) 0.0366(2) 0.0378(2) -0.00900(18) -0.0202(2) -0.0168(2) S1 0.0781(15) 0.110(2) 0.0878(17) -0.0401(15) -0.0349(13) -0.0324(14) S2 0.0571(11) 0.0584(11) 0.0566(11) -0.0023(9) -0.0279(9) -0.0261(9) S3 0.0493(10) 0.0635(11) 0.0504(10) -0.0231(9) -0.0260(8) 0.0004(8) S4 0.0951(15) 0.0464(10) 0.0759(13) -0.0176(9) -0.0594(12) -0.0097(10) S5 0.0436(9) 0.0628(11) 0.0367(9) -0.0064(8) -0.0039(7) -0.0189(8) S6 0.1020(17) 0.0444(10) 0.0454(10) 0.0001(8) -0.0257(11) -0.0117(10) S7 0.0477(9) 0.0495(9) 0.0329(8) -0.0157(7) -0.0008(7) -0.0123(7) S8 0.0886(15) 0.0570(11) 0.0460(10) -0.0283(9) -0.0055(9) -0.0271(10) C1 0.092(7) 0.087(7) 0.094(7) -0.028(6) -0.036(6) -0.041(6) C2 0.072(5) 0.046(4) 0.058(4) -0.016(3) -0.023(4) -0.019(4) C3 0.068(5) 0.059(5) 0.078(6) -0.024(4) -0.031(4) -0.007(4) C4 0.060(5) 0.039(4) 0.075(5) -0.017(4) -0.024(4) -0.003(3) C5 0.045(4) 0.033(3) 0.046(4) -0.011(3) -0.007(3) -0.008(3) C6 0.050(4) 0.042(4) 0.052(4) -0.017(3) -0.006(3) -0.015(3) C7 0.044(4) 0.047(4) 0.044(4) -0.010(3) -0.006(3) -0.017(3) C8 0.059(5) 0.049(4) 0.076(6) -0.011(4) -0.018(4) -0.015(4) C9 0.042(4) 0.044(4) 0.090(6) -0.019(4) -0.012(4) -0.004(3) C10 0.045(4) 0.039(3) 0.050(4) -0.009(3) -0.003(3) -0.014(3) C11 0.066(5) 0.039(4) 0.060(5) -0.015(3) -0.013(4) -0.019(3) C12 0.058(5) 0.081(6) 0.060(5) -0.023(4) -0.012(4) -0.032(4) C13 0.095(6) 0.042(4) 0.056(5) -0.012(3) -0.041(4) 0.008(4) C14 0.056(4) 0.030(3) 0.054(4) -0.006(3) -0.028(3) -0.002(3) C15 0.093(7) 0.054(5) 0.061(5) -0.014(4) -0.030(5) 0.010(4) C16 0.077(7) 0.079(7) 0.103(8) -0.008(6) -0.036(6) -0.020(5) C17 0.041(4) 0.030(3) 0.070(5) -0.010(3) 0.000(3) -0.009(3) C18 0.100(7) 0.040(4) 0.131(9) -0.010(5) -0.081(7) -0.001(4) C19 0.074(5) 0.029(3) 0.072(5) -0.013(3) -0.036(4) -0.009(3) C20 0.143(10) 0.044(5) 0.057(5) -0.013(4) -0.040(6) 0.000(5) C21 0.064(6) 0.067(6) 0.122(9) -0.028(6) -0.013(6) -0.021(5) C22 0.047(4) 0.019(3) 0.110(7) -0.009(3) -0.029(4) -0.004(3) C23 0.076(6) 0.033(4) 0.121(8) -0.027(4) -0.045(6) -0.001(4) C24 0.085(6) 0.042(4) 0.069(5) -0.017(4) -0.032(4) -0.023(4) C25 0.038(4) 0.077(5) 0.052(4) -0.024(4) -0.004(3) -0.013(3) C26 0.017(3) 0.068(5) 0.051(4) -0.025(3) -0.004(3) -0.004(3) C27 0.039(3) 0.057(4) 0.048(4) -0.010(3) -0.010(3) -0.018(3) C28 0.050(4) 0.048(4) 0.055(4) -0.008(3) -0.014(3) -0.025(3) C29 0.029(3) 0.037(3) 0.057(4) -0.013(3) -0.017(3) -0.008(2) C30 0.044(4) 0.045(4) 0.061(4) -0.010(3) -0.020(3) -0.014(3) C31 0.055(4) 0.031(3) 0.056(4) 0.000(3) -0.024(3) -0.011(3) C32 0.064(5) 0.039(4) 0.071(5) -0.007(4) -0.025(4) -0.013(3) C33 0.061(5) 0.035(4) 0.081(6) -0.012(4) -0.030(4) -0.012(3) C34 0.025(3) 0.037(3) 0.068(4) -0.018(3) -0.016(3) -0.002(2) C35 0.030(3) 0.051(4) 0.070(5) -0.026(4) -0.018(3) -0.004(3) C36 0.102(7) 0.057(5) 0.073(6) 0.006(4) -0.056(5) -0.023(5) C37 0.086(6) 0.103(7) 0.052(5) -0.036(5) 0.006(4) -0.060(5) C38 0.041(3) 0.043(3) 0.038(3) -0.016(3) -0.001(3) -0.021(3) C39 0.060(5) 0.067(5) 0.057(5) -0.008(4) -0.012(4) -0.031(4) C40 0.056(5) 0.051(4) 0.073(5) -0.015(4) -0.015(4) -0.016(4) C41 0.047(4) 0.033(3) 0.064(4) -0.008(3) -0.022(3) -0.019(3) C42 0.057(4) 0.050(4) 0.063(5) -0.018(4) -0.001(4) -0.030(4) C43 0.073(5) 0.050(4) 0.040(4) -0.021(3) 0.004(3) -0.037(4) C44 0.078(6) 0.072(5) 0.052(5) -0.015(4) -0.009(4) -0.045(5) C45 0.049(4) 0.058(5) 0.092(6) -0.024(4) -0.012(4) -0.018(4) C46 0.032(3) 0.038(3) 0.061(4) -0.021(3) 0.005(3) -0.020(3) C47 0.037(4) 0.049(4) 0.076(5) -0.015(4) 0.000(3) -0.022(3) C48 0.092(6) 0.082(6) 0.048(4) -0.030(4) 0.004(4) -0.048(5) Cl1S 0.0599(11) 0.0596(11) 0.0408(9) -0.0134(8) -0.0042(8) -0.0069(9) Cl2S 0.140(4) 0.158(4) 0.189(5) 0.028(4) -0.028(3) -0.015(3) Cl3S 0.260(6) 0.144(4) 0.203(5) -0.104(4) 0.105(5) -0.123(4) Cl4S 0.089(2) 0.112(3) 0.300(6) -0.090(3) -0.009(3) -0.032(2) C1S 0.041(3) 0.041(3) 0.041(3) -0.013(2) -0.013(2) -0.013(2) C2S 0.113(8) 0.053(5) 0.095(7) -0.026(5) -0.034(6) -0.008(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 Sb1 S1 2.419(3) 3 ? Sb1 S1 2.419(3) 2 ? Sb1 S1 2.419(3) . ? Sb2 S2 2.4251(19) 2 ? Sb2 S2 2.4251(19) . ? Sb2 S2 2.4251(19) 3 ? Sb3 S3 2.4193(17) . ? Sb3 S7 2.4430(17) . ? Sb3 S5 2.4428(17) . ? Sb4 S6 2.433(2) . ? Sb4 S4 2.4339(18) . ? Sb4 S8 2.438(2) . ? S1 C1 1.793(10) . ? S2 C12 1.841(8) . ? S3 C13 1.842(8) . ? S4 C24 1.841(8) . ? S5 C25 1.853(7) . ? S6 C36 1.864(10) . ? S7 C37 1.810(8) . ? S8 C48 1.810(8) . ? C1 C2 1.513(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C11 1.358(10) . ? C2 C3 1.396(11) . ? C3 C4 1.340(11) . ? C3 H3A 0.9500 . ? C4 C5 1.396(10) . ? C4 H4A 0.9500 . ? C5 C10 1.427(9) . ? C5 C6 1.441(10) . ? C6 C7 1.341(10) . ? C6 H6A 0.9500 . ? C7 C8 1.407(10) . ? C7 C12 1.487(10) . ? C8 C9 1.357(11) . ? C8 H8A 0.9500 . ? C9 C10 1.373(10) . ? C9 H9A 0.9500 . ? C10 C11 1.450(10) . ? C11 H11A 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.472(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C23 1.361(11) . ? C14 C15 1.349(11) . ? C15 C16 1.337(13) . ? C15 H15A 0.9500 . ? C16 C17 1.317(12) . ? C16 H16A 0.9500 . ? C17 C22 1.354(10) . ? C17 C18 1.580(13) . ? C18 C19 1.355(11) . ? C18 H18A 0.9500 . ? C19 C20 1.453(13) . ? C19 C24 1.468(10) . ? C20 C21 1.348(14) . ? C20 H20A 0.9500 . ? C21 C22 1.339(12) . ? C21 H21A 0.9500 . ? C22 C23 1.648(13) . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.493(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C35 1.384(10) . ? C26 C27 1.428(10) . ? C27 C28 1.340(10) . ? C27 H27A 0.9500 . ? C28 C29 1.426(9) . ? C28 H28A 0.9500 . ? C29 C34 1.415(9) . ? C29 C30 1.441(10) . ? C30 C31 1.350(9) . ? C30 H30A 0.9500 . ? C31 C32 1.417(10) . ? C31 C36 1.474(11) . ? C32 C33 1.344(11) . ? C32 H32A 0.9500 . ? C33 C34 1.389(9) . ? C33 H33A 0.9500 . ? C34 C35 1.441(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.479(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C47 1.362(9) . ? C38 C39 1.389(10) . ? C39 C40 1.325(11) . ? C39 H39A 0.9500 . ? C40 C41 1.340(10) . ? C40 H40A 0.9500 . ? C41 C46 1.382(9) . ? C41 C42 1.494(10) . ? C42 C43 1.336(10) . ? C42 H42A 0.9500 . ? C43 C44 1.438(11) . ? C43 C48 1.525(10) . ? C44 C45 1.344(11) . ? C44 H44A 0.9500 . ? C45 C46 1.385(10) . ? C45 H45A 0.9500 . ? C46 C47 1.533(11) . ? C47 H47A 0.9500 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? Cl1S C1S 1.757(4) . ? Cl2S C2S 1.741(12) . ? Cl3S C2S 1.695(10) . ? Cl4S C2S 1.621(11) . ? C1S Cl1S 1.757(4) 3 ? C1S Cl1S 1.757(4) 2 ? C1S H1SA 1.0000 . ? C2S H2SA 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Sb1 S1 91.78(8) 3 2 ? S1 Sb1 S1 91.78(8) 3 . ? S1 Sb1 S1 91.78(8) 2 . ? S2 Sb2 S2 90.33(6) 2 . ? S2 Sb2 S2 90.33(6) 2 3 ? S2 Sb2 S2 90.33(6) . 3 ? S3 Sb3 S7 91.10(6) . . ? S3 Sb3 S5 92.05(7) . . ? S7 Sb3 S5 92.15(6) . . ? S6 Sb4 S4 90.05(7) . . ? S6 Sb4 S8 90.99(8) . . ? S4 Sb4 S8 91.64(8) . . ? C1 S1 Sb1 104.1(3) . . ? C12 S2 Sb2 99.9(3) . . ? C13 S3 Sb3 104.1(3) . . ? C24 S4 Sb4 104.4(2) . . ? C25 S5 Sb3 101.9(2) . . ? C36 S6 Sb4 99.6(2) . . ? C37 S7 Sb3 99.7(3) . . ? C48 S8 Sb4 102.3(3) . . ? C2 C1 S1 116.0(7) . . ? C2 C1 H1A 108.3 . . ? S1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? S1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C11 C2 C3 119.3(7) . . ? C11 C2 C1 121.1(7) . . ? C3 C2 C1 119.6(8) . . ? C4 C3 C2 123.1(8) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C10 119.7(6) . . ? C4 C5 C6 123.5(6) . . ? C10 C5 C6 116.7(6) . . ? C7 C6 C5 122.3(6) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C8 118.1(7) . . ? C6 C7 C12 121.7(7) . . ? C8 C7 C12 120.2(7) . . ? C9 C8 C7 122.3(8) . . ? C9 C8 H8A 118.8 . . ? C7 C8 H8A 118.8 . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C5 120.1(7) . . ? C9 C10 C11 122.4(7) . . ? C5 C10 C11 117.5(6) . . ? C2 C11 C10 120.4(7) . . ? C2 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C7 C12 S2 113.7(5) . . ? C7 C12 H12A 108.8 . . ? S2 C12 H12A 108.8 . . ? C7 C12 H12B 108.8 . . ? S2 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C14 C13 S3 116.0(5) . . ? C14 C13 H13A 108.3 . . ? S3 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? S3 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C23 C14 C15 118.6(8) . . ? C23 C14 C13 122.8(8) . . ? C15 C14 C13 118.5(8) . . ? C16 C15 C14 132.8(10) . . ? C16 C15 H15A 113.6 . . ? C14 C15 H15A 113.6 . . ? C17 C16 C15 110.9(10) . . ? C17 C16 H16A 124.5 . . ? C15 C16 H16A 124.5 . . ? C16 C17 C22 130.4(9) . . ? C16 C17 C18 116.0(8) . . ? C22 C17 C18 113.6(8) . . ? C19 C18 C17 116.7(10) . . ? C19 C18 H18A 121.6 . . ? C17 C18 H18A 121.6 . . ? C18 C19 C20 119.4(9) . . ? C18 C19 C24 123.0(9) . . ? C20 C19 C24 117.6(8) . . ? C21 C20 C19 125.3(11) . . ? C21 C20 H20A 117.3 . . ? C19 C20 H20A 117.3 . . ? C20 C21 C22 113.9(10) . . ? C20 C21 H21A 123.0 . . ? C22 C21 H21A 123.0 . . ? C21 C22 C17 131.0(10) . . ? C21 C22 C23 115.2(9) . . ? C17 C22 C23 113.8(7) . . ? C14 C23 C22 113.4(8) . . ? C14 C23 H23A 123.3 . . ? C22 C23 H23A 123.3 . . ? C19 C24 S4 116.4(5) . . ? C19 C24 H24A 108.2 . . ? S4 C24 H24A 108.2 . . ? C19 C24 H24B 108.2 . . ? S4 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? C26 C25 S5 111.8(5) . . ? C26 C25 H25A 109.3 . . ? S5 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? S5 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C35 C26 C27 119.0(6) . . ? C35 C26 C25 121.6(7) . . ? C27 C26 C25 119.4(7) . . ? C28 C27 C26 121.1(7) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C27 C28 C29 121.3(7) . . ? C27 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C34 C29 C28 119.5(6) . . ? C34 C29 C30 118.2(6) . . ? C28 C29 C30 122.3(6) . . ? C31 C30 C29 120.0(6) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 119.2(7) . . ? C30 C31 C36 121.4(7) . . ? C32 C31 C36 119.4(7) . . ? C33 C32 C31 122.8(7) . . ? C33 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? C32 C33 C34 119.1(7) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? C33 C34 C29 120.7(7) . . ? C33 C34 C35 121.5(7) . . ? C29 C34 C35 117.9(6) . . ? C26 C35 C34 121.2(6) . . ? C26 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C31 C36 S6 115.2(6) . . ? C31 C36 H36A 108.5 . . ? S6 C36 H36A 108.5 . . ? C31 C36 H36B 108.5 . . ? S6 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 S7 115.5(5) . . ? C38 C37 H37A 108.4 . . ? S7 C37 H37A 108.4 . . ? C38 C37 H37B 108.4 . . ? S7 C37 H37B 108.4 . . ? H37A C37 H37B 107.5 . . ? C47 C38 C39 117.7(7) . . ? C47 C38 C37 122.9(7) . . ? C39 C38 C37 119.5(7) . . ? C40 C39 C38 126.4(8) . . ? C40 C39 H39A 116.8 . . ? C38 C39 H39A 116.8 . . ? C39 C40 C41 117.9(8) . . ? C39 C40 H40A 121.0 . . ? C41 C40 H40A 121.0 . . ? C40 C41 C46 124.0(7) . . ? C40 C41 C42 120.4(7) . . ? C46 C41 C42 115.5(6) . . ? C43 C42 C41 118.8(7) . . ? C43 C42 H42A 120.6 . . ? C41 C42 H42A 120.6 . . ? C42 C43 C44 121.6(7) . . ? C42 C43 C48 121.4(8) . . ? C44 C43 C48 117.0(7) . . ? C45 C44 C43 120.9(8) . . ? C45 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? C44 C45 C46 118.1(9) . . ? C44 C45 H45A 120.9 . . ? C46 C45 H45A 120.9 . . ? C45 C46 C41 125.0(7) . . ? C45 C46 C47 119.2(7) . . ? C41 C46 C47 115.8(6) . . ? C38 C47 C46 118.2(7) . . ? C38 C47 H47A 120.9 . . ? C46 C47 H47A 120.9 . . ? C43 C48 S8 114.5(5) . . ? C43 C48 H48A 108.6 . . ? S8 C48 H48A 108.6 . . ? C43 C48 H48B 108.6 . . ? S8 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? Cl1S C1S Cl1S 110.6(3) 3 . ? Cl1S C1S Cl1S 110.6(3) 3 2 ? Cl1S C1S Cl1S 110.6(3) . 2 ? Cl1S C1S H1SA 108.3 3 . ? Cl1S C1S H1SA 108.3 . . ? Cl1S C1S H1SA 108.3 2 . ? Cl4S C2S Cl3S 118.6(7) . . ? Cl4S C2S Cl2S 112.7(7) . . ? Cl3S C2S Cl2S 100.6(6) . . ? Cl4S C2S H2SA 108.1 . . ? Cl3S C2S H2SA 108.1 . . ? Cl2S C2S H2SA 108.1 . . ? 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 S1 Sb1 S1 C1 170.9(4) 3 . . . ? S1 Sb1 S1 C1 -97.3(4) 2 . . . ? S2 Sb2 S2 C12 -179.1(3) 2 . . . ? S2 Sb2 S2 C12 -88.8(3) 3 . . . ? S7 Sb3 S3 C13 -172.2(3) . . . . ? S5 Sb3 S3 C13 95.6(3) . . . . ? S6 Sb4 S4 C24 -173.8(3) . . . . ? S8 Sb4 S4 C24 95.2(3) . . . . ? S3 Sb3 S5 C25 170.1(3) . . . . ? S7 Sb3 S5 C25 79.0(3) . . . . ? S4 Sb4 S6 C36 80.8(3) . . . . ? S8 Sb4 S6 C36 172.4(3) . . . . ? S3 Sb3 S7 C37 77.5(3) . . . . ? S5 Sb3 S7 C37 169.6(3) . . . . ? S6 Sb4 S8 C48 85.8(3) . . . . ? S4 Sb4 S8 C48 175.8(3) . . . . ? Sb1 S1 C1 C2 -37.6(8) . . . . ? S1 C1 C2 C11 109.2(9) . . . . ? S1 C1 C2 C3 -72.3(10) . . . . ? C11 C2 C3 C4 1.2(13) . . . . ? C1 C2 C3 C4 -177.4(9) . . . . ? C2 C3 C4 C5 -0.7(13) . . . . ? C3 C4 C5 C10 0.4(11) . . . . ? C3 C4 C5 C6 177.1(8) . . . . ? C4 C5 C6 C7 -176.2(7) . . . . ? C10 C5 C6 C7 0.6(10) . . . . ? C5 C6 C7 C8 -1.6(10) . . . . ? C5 C6 C7 C12 178.4(6) . . . . ? C6 C7 C8 C9 0.6(12) . . . . ? C12 C7 C8 C9 -179.4(7) . . . . ? C7 C8 C9 C10 1.4(13) . . . . ? C8 C9 C10 C5 -2.3(12) . . . . ? C8 C9 C10 C11 176.5(7) . . . . ? C4 C5 C10 C9 178.3(7) . . . . ? C6 C5 C10 C9 1.4(10) . . . . ? C4 C5 C10 C11 -0.6(10) . . . . ? C6 C5 C10 C11 -177.5(6) . . . . ? C3 C2 C11 C10 -1.3(12) . . . . ? C1 C2 C11 C10 177.2(7) . . . . ? C9 C10 C11 C2 -177.8(7) . . . . ? C5 C10 C11 C2 1.1(10) . . . . ? C6 C7 C12 S2 117.1(7) . . . . ? C8 C7 C12 S2 -62.9(9) . . . . ? Sb2 S2 C12 C7 -44.4(6) . . . . ? Sb3 S3 C13 C14 17.2(8) . . . . ? S3 C13 C14 C23 -79.7(9) . . . . ? S3 C13 C14 C15 98.3(8) . . . . ? C23 C14 C15 C16 -2.1(14) . . . . ? C13 C14 C15 C16 179.8(9) . . . . ? C14 C15 C16 C17 0.3(15) . . . . ? C15 C16 C17 C22 2.7(14) . . . . ? C15 C16 C17 C18 -177.8(7) . . . . ? C16 C17 C18 C19 -177.7(8) . . . . ? C22 C17 C18 C19 1.9(9) . . . . ? C17 C18 C19 C20 0.2(10) . . . . ? C17 C18 C19 C24 178.0(6) . . . . ? C18 C19 C20 C21 -1.4(12) . . . . ? C24 C19 C20 C21 -179.4(8) . . . . ? C19 C20 C21 C22 0.2(13) . . . . ? C20 C21 C22 C17 2.6(13) . . . . ? C20 C21 C22 C23 -178.1(7) . . . . ? C16 C17 C22 C21 176.0(9) . . . . ? C18 C17 C22 C21 -3.6(11) . . . . ? C16 C17 C22 C23 -3.4(11) . . . . ? C18 C17 C22 C23 177.1(5) . . . . ? C15 C14 C23 C22 1.0(9) . . . . ? C13 C14 C23 C22 179.1(6) . . . . ? C21 C22 C23 C14 -178.3(7) . . . . ? C17 C22 C23 C14 1.2(8) . . . . ? C18 C19 C24 S4 -84.5(9) . . . . ? C20 C19 C24 S4 93.3(7) . . . . ? Sb4 S4 C24 C19 21.4(7) . . . . ? Sb3 S5 C25 C26 38.2(6) . . . . ? S5 C25 C26 C35 -97.9(7) . . . . ? S5 C25 C26 C27 80.4(7) . . . . ? C35 C26 C27 C28 -0.8(10) . . . . ? C25 C26 C27 C28 -179.1(6) . . . . ? C26 C27 C28 C29 -0.4(10) . . . . ? C27 C28 C29 C34 0.9(10) . . . . ? C27 C28 C29 C30 -178.0(6) . . . . ? C34 C29 C30 C31 0.5(9) . . . . ? C28 C29 C30 C31 179.3(6) . . . . ? C29 C30 C31 C32 1.4(10) . . . . ? C29 C30 C31 C36 -179.2(7) . . . . ? C30 C31 C32 C33 -2.4(12) . . . . ? C36 C31 C32 C33 178.2(8) . . . . ? C31 C32 C33 C34 1.3(12) . . . . ? C32 C33 C34 C29 0.6(10) . . . . ? C32 C33 C34 C35 -179.6(7) . . . . ? C28 C29 C34 C33 179.6(6) . . . . ? C30 C29 C34 C33 -1.5(9) . . . . ? C28 C29 C34 C35 -0.2(8) . . . . ? C30 C29 C34 C35 178.7(5) . . . . ? C27 C26 C35 C34 1.5(9) . . . . ? C25 C26 C35 C34 179.8(6) . . . . ? C33 C34 C35 C26 179.3(6) . . . . ? C29 C34 C35 C26 -1.0(9) . . . . ? C30 C31 C36 S6 -105.4(8) . . . . ? C32 C31 C36 S6 74.1(8) . . . . ? Sb4 S6 C36 C31 38.4(6) . . . . ? Sb3 S7 C37 C38 39.3(7) . . . . ? S7 C37 C38 C47 -103.4(8) . . . . ? S7 C37 C38 C39 76.2(9) . . . . ? C47 C38 C39 C40 -1.4(11) . . . . ? C37 C38 C39 C40 179.0(7) . . . . ? C38 C39 C40 C41 2.2(12) . . . . ? C39 C40 C41 C46 -1.0(11) . . . . ? C39 C40 C41 C42 -179.9(7) . . . . ? C40 C41 C42 C43 179.9(7) . . . . ? C46 C41 C42 C43 1.0(9) . . . . ? C41 C42 C43 C44 -1.5(10) . . . . ? C41 C42 C43 C48 178.6(6) . . . . ? C42 C43 C44 C45 1.1(11) . . . . ? C48 C43 C44 C45 -179.0(7) . . . . ? C43 C44 C45 C46 0.0(11) . . . . ? C44 C45 C46 C41 -0.4(11) . . . . ? C44 C45 C46 C47 -178.7(6) . . . . ? C40 C41 C46 C45 -178.9(7) . . . . ? C42 C41 C46 C45 0.0(9) . . . . ? C40 C41 C46 C47 -0.6(9) . . . . ? C42 C41 C46 C47 178.2(5) . . . . ? C39 C38 C47 C46 -0.5(9) . . . . ? C37 C38 C47 C46 179.1(6) . . . . ? C45 C46 C47 C38 179.7(6) . . . . ? C41 C46 C47 C38 1.4(8) . . . . ? C42 C43 C48 S8 -97.3(8) . . . . ? C44 C43 C48 S8 82.8(8) . . . . ? Sb4 S8 C48 C43 32.9(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.900 _refine_diff_density_min -1.630 _refine_diff_density_rms 0.130