# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1675 data_s8macc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety C11H16S8.0.5CS2 _chemical_formula_sum 'C23 H32 S18' _chemical_formula_weight 885.58 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 35.970(3) _cell_length_b 9.9454(5) _cell_length_c 5.3287(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.660(8) _cell_angle_gamma 90.00 _cell_volume 1904.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 241 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.940 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11384 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.85 _reflns_number_total 3573 _reflns_number_gt 2926 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.3950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3573 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.686488(18) 0.09793(7) 0.49330(11) 0.04658(17) Uani 1 d . . . C2 C 0.66669(7) 0.2395(2) 0.6552(5) 0.0415(5) Uani 1 d . . . H2A H 0.6864 0.2868 0.7487 0.050 Uiso 1 calc R . . H2B H 0.6557 0.3013 0.5320 0.050 Uiso 1 calc R . . C3 C 0.63734(7) 0.1974(2) 0.8337(5) 0.0465(6) Uani 1 d . . . H3A H 0.6489 0.1489 0.9746 0.056 Uiso 1 calc R . . H3B H 0.6195 0.1382 0.7480 0.056 Uiso 1 calc R . . S4 S 0.61376(2) 0.34474(7) 0.94604(17) 0.0626(2) Uani 1 d . . . C5 C 0.5866(3) 0.2612(11) 1.197(2) 0.095(3) Uani 0.50 d P A 1 H5A H 0.6019 0.1936 1.2826 0.114 Uiso 0.50 calc PR A 1 H5B H 0.5797 0.3276 1.3201 0.114 Uiso 0.50 calc PR A 1 C6 C 0.5547(2) 0.2013(10) 1.0916(17) 0.087(2) Uani 0.50 d P A 1 H6A H 0.5610 0.1394 0.9594 0.104 Uiso 0.50 calc PR A 1 H6B H 0.5379 0.2690 1.0205 0.104 Uiso 0.50 calc PR A 1 C5A C 0.57034(15) 0.2728(6) 1.0318(12) 0.0467(12) Uani 0.50 d P A 2 H5AA H 0.5518 0.3433 1.0376 0.056 Uiso 0.50 calc PR A 2 H5AB H 0.5620 0.2086 0.9042 0.056 Uiso 0.50 calc PR A 2 C6A C 0.57365(15) 0.2003(6) 1.2927(11) 0.0450(13) Uani 0.50 d P A 2 H6AA H 0.5783 0.2668 1.4237 0.054 Uiso 0.50 calc PR A 2 H6AB H 0.5947 0.1393 1.2956 0.054 Uiso 0.50 calc PR A 2 S7 S 0.53206(2) 0.10751(10) 1.35588(18) 0.0723(2) Uani 1 d . . . C8 C 0.54284(19) -0.0449(6) 1.2075(14) 0.0466(14) Uani 0.50 d P A 1 H8A H 0.5199 -0.0935 1.1698 0.056 Uiso 0.50 calc PR A 1 H8B H 0.5538 -0.0245 1.0491 0.056 Uiso 0.50 calc PR A 1 C9 C 0.5709(2) -0.1418(6) 1.3689(14) 0.0463(14) Uani 0.50 d P A 1 H9A H 0.5585 -0.1730 1.5157 0.056 Uiso 0.50 calc PR A 1 H9B H 0.5924 -0.0895 1.4276 0.056 Uiso 0.50 calc PR A 1 C8A C 0.5622(3) -0.0610(14) 1.3765(18) 0.118(5) Uani 0.50 d P A 2 H8AA H 0.5882 -0.0430 1.3484 0.142 Uiso 0.50 calc PR A 2 H8AB H 0.5603 -0.1043 1.5385 0.142 Uiso 0.50 calc PR A 2 C9A C 0.5478(3) -0.1314(15) 1.204(2) 0.120(5) Uani 0.50 d P A 2 H9AA H 0.5460 -0.0837 1.0456 0.144 Uiso 0.50 calc PR A 2 H9AB H 0.5234 -0.1644 1.2452 0.144 Uiso 0.50 calc PR A 2 S10 S 0.58643(2) -0.28152(8) 1.20440(17) 0.0642(2) Uani 1 d . . . C11 C 0.61888(8) -0.1959(3) 1.0069(6) 0.0509(6) Uani 1 d . . . H11A H 0.6052 -0.1398 0.8854 0.061 Uiso 1 calc R . . H11B H 0.6352 -0.1385 1.1096 0.061 Uiso 1 calc R . . C12 C 0.64166(7) -0.2980(2) 0.8716(6) 0.0507(6) Uani 1 d . . . H12A H 0.6252 -0.3654 0.7962 0.061 Uiso 1 calc R . . H12B H 0.6584 -0.3429 0.9924 0.061 Uiso 1 calc R . . S13 S 0.668485(18) -0.22286(7) 0.63015(13) 0.05028(18) Uani 1 d . . . C14 C 0.69993(6) -0.1207(2) 0.8028(4) 0.0366(5) Uani 1 d . . . S15 S 0.727785(17) -0.19059(6) 1.04769(12) 0.04175(16) Uani 1 d . . . S16 S 0.788439(19) -0.04879(6) 1.33459(13) 0.04868(18) Uani 1 d . . . C16 C 0.75528(6) -0.0509(2) 1.1134(4) 0.0349(5) Uani 1 d . . . S17 S 0.744638(16) 0.08265(6) 0.91567(11) 0.03937(15) Uani 1 d . . . C18 C 0.70764(6) 0.0075(2) 0.7435(4) 0.0359(5) Uani 1 d . . . C20 C 0.5000 0.5000 0.5000 0.0885(17) Uani 1 d S . . S21 S 0.52769(5) 0.55857(18) 0.6959(4) 0.1371(6) Uani 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 S1 0.0485(4) 0.0608(4) 0.0300(3) 0.0028(2) -0.0028(2) 0.0087(3) C2 0.0370(12) 0.0443(12) 0.0428(14) 0.0068(10) -0.0009(10) -0.0008(9) C3 0.0489(14) 0.0436(12) 0.0476(15) 0.0078(10) 0.0094(12) 0.0034(10) S4 0.0564(4) 0.0486(4) 0.0846(6) -0.0005(3) 0.0217(4) 0.0033(3) C5 0.074(6) 0.120(8) 0.090(7) -0.040(6) 0.002(6) 0.012(5) C6 0.063(5) 0.118(7) 0.080(6) -0.002(5) 0.001(4) 0.021(5) C5A 0.027(2) 0.067(3) 0.047(4) 0.018(3) 0.006(2) 0.001(2) C6A 0.032(2) 0.065(3) 0.039(3) 0.008(2) 0.008(2) -0.011(2) S7 0.0537(4) 0.0915(6) 0.0739(6) 0.0008(4) 0.0279(4) 0.0009(4) C8 0.035(3) 0.056(3) 0.048(3) 0.002(3) 0.001(2) -0.001(2) C9 0.047(3) 0.050(3) 0.042(3) 0.003(2) 0.001(2) 0.001(2) C8A 0.067(6) 0.237(15) 0.050(5) 0.021(8) -0.004(4) -0.055(8) C9A 0.061(6) 0.236(15) 0.063(6) 0.028(9) -0.003(4) -0.045(8) S10 0.0575(4) 0.0670(4) 0.0688(5) 0.0082(4) 0.0118(4) -0.0144(3) C11 0.0495(14) 0.0516(14) 0.0518(16) 0.0074(11) 0.0040(12) -0.0051(11) C12 0.0439(14) 0.0418(13) 0.0658(18) 0.0053(11) -0.0038(12) -0.0070(10) S13 0.0402(3) 0.0621(4) 0.0481(4) -0.0105(3) -0.0023(3) -0.0100(3) C14 0.0299(10) 0.0447(12) 0.0351(12) -0.0039(9) 0.0020(9) 0.0007(8) S15 0.0420(3) 0.0363(3) 0.0463(4) 0.0016(2) -0.0056(3) -0.0020(2) S16 0.0526(4) 0.0433(3) 0.0482(4) -0.0037(2) -0.0184(3) 0.0038(2) C16 0.0340(11) 0.0368(11) 0.0339(12) -0.0029(8) 0.0023(9) 0.0051(8) S17 0.0423(3) 0.0399(3) 0.0353(3) 0.0039(2) -0.0039(2) -0.0045(2) C18 0.0330(11) 0.0476(12) 0.0271(11) 0.0008(9) 0.0004(8) 0.0022(9) C20 0.075(4) 0.091(4) 0.101(5) 0.030(3) 0.020(3) 0.009(3) S21 0.1232(12) 0.1447(13) 0.1414(14) 0.0301(10) -0.0149(11) -0.0171(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C18 1.752(2) . ? S1 C2 1.814(3) . ? C2 C3 1.512(3) . ? C3 S4 1.809(3) . ? S4 C5A 1.796(6) . ? S4 C5 1.886(12) . ? C5 C6 1.389(12) . ? C6 S7 1.903(10) . ? C5A C6A 1.565(7) . ? C6A S7 1.803(5) . ? S7 C8 1.761(6) . ? S7 C8A 1.997(15) . ? C8 C9 1.615(8) . ? C9 S10 1.748(6) . ? C8A C9A 1.247(16) . ? C9A S10 2.040(14) . ? S10 C11 1.819(3) . ? C11 C12 1.509(4) . ? C12 S13 1.806(3) . ? S13 C14 1.749(2) . ? C14 C18 1.346(3) . ? C14 S15 1.751(2) . ? S15 C16 1.731(2) . ? S16 C16 1.638(2) . ? C16 S17 1.727(2) . ? S17 C18 1.749(2) . ? C20 S21 1.5247(18) 3_666 ? C20 S21 1.5247(18) . ? 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 C18 S1 C2 101.69(11) . . ? C3 C2 S1 112.66(17) . . ? C2 C3 S4 109.62(17) . . ? C5A S4 C3 100.8(2) . . ? C5A S4 C5 32.7(3) . . ? C3 S4 C5 98.3(3) . . ? C6 C5 S4 110.3(8) . . ? C5 C6 S7 106.5(8) . . ? C6A C5A S4 112.2(4) . . ? C5A C6A S7 111.8(4) . . ? C8 S7 C6A 98.9(3) . . ? C8 S7 C6 88.8(4) . . ? C6A S7 C6 39.1(3) . . ? C8 S7 C8A 34.1(4) . . ? C6A S7 C8A 89.2(3) . . ? C6 S7 C8A 101.7(4) . . ? C9 C8 S7 114.8(5) . . ? C8 C9 S10 114.4(5) . . ? C9A C8A S7 102.9(10) . . ? C8A C9A S10 98.7(9) . . ? C9 S10 C11 98.4(3) . . ? C9 S10 C9A 35.4(4) . . ? C11 S10 C9A 96.5(3) . . ? C12 C11 S10 109.81(18) . . ? C11 C12 S13 112.47(18) . . ? C14 S13 C12 102.66(12) . . ? C18 C14 S13 124.19(18) . . ? C18 C14 S15 115.69(17) . . ? S13 C14 S15 119.68(13) . . ? C16 S15 C14 97.71(11) . . ? S16 C16 S17 124.22(13) . . ? S16 C16 S15 123.09(13) . . ? S17 C16 S15 112.67(13) . . ? C16 S17 C18 97.64(11) . . ? C14 C18 S17 116.23(17) . . ? C14 C18 S1 125.30(18) . . ? S17 C18 S1 118.22(13) . . ? S21 C20 S21 180.0 3_666 . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.357 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.052