data_r105m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 N O2 S2' _chemical_formula_weight 487.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6527(18) _cell_length_b 9.7093(15) _cell_length_c 12.4847(19) _cell_angle_alpha 90.00 _cell_angle_beta 110.860(3) _cell_angle_gamma 90.00 _cell_volume 1319.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.824244 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 8918 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.28 _reflns_number_total 3788 _reflns_number_gt 3554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0521P)^2^+0.2421P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(7) _refine_ls_number_reflns 3788 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 C1 C 0.7799(2) 0.4704(2) 0.40660(19) 0.0501(6) Uani 1 1 d . . . H1 H 0.8479 0.4073 0.4444 0.060 Uiso 1 1 calc R . . C2 C 0.6576(2) 0.3971(3) 0.3911(2) 0.0511(6) Uani 1 1 d . . . H2 H 0.5914 0.4642 0.3592 0.061 Uiso 1 1 calc R . . S2 S 0.77741(7) 0.50773(9) 0.26037(5) 0.0721(2) Uani 1 1 d . . . C3 C 0.8899(4) 0.6409(4) 0.2843(3) 0.0962(11) Uani 1 1 d . . . H3A H 0.8618 0.7224 0.3109 0.144 Uiso 1 1 calc R . . H3B H 0.9025 0.6607 0.2140 0.144 Uiso 1 1 calc R . . H3C H 0.9659 0.6111 0.3410 0.144 Uiso 1 1 calc R . . C11 C 1.0287(2) 0.4883(3) 0.7567(2) 0.0552(6) Uani 1 1 d . . . C12 C 0.9348(3) 0.4175(4) 0.7703(2) 0.0824(9) Uani 1 1 d . . . H12 H 0.8717 0.3837 0.7065 0.099 Uiso 1 1 calc R . . C13 C 0.9325(3) 0.3954(5) 0.8785(3) 0.0996(13) Uani 1 1 d . . . H13 H 0.8684 0.3446 0.8867 0.119 Uiso 1 1 calc R . . C14 C 1.0210(4) 0.4455(5) 0.9731(3) 0.0950(12) Uani 1 1 d . . . C15 C 1.1159(5) 0.5143(6) 0.9583(3) 0.1225(14) Uani 1 1 d . . . H15 H 1.1791 0.5471 1.0224 0.147 Uiso 1 1 calc R . . C16 C 1.1215(3) 0.5372(5) 0.8505(3) 0.0994(12) Uani 1 1 d . . . H16 H 1.1872 0.5848 0.8423 0.119 Uiso 1 1 calc R . . C17 C 1.0152(5) 0.4237(7) 1.0920(3) 0.151(2) Uani 1 1 d . . . H17A H 1.0463 0.3339 1.1196 0.226 Uiso 1 1 calc R . . H17B H 0.9316 0.4312 1.0879 0.226 Uiso 1 1 calc R . . H17C H 1.0641 0.4925 1.1434 0.226 Uiso 1 1 calc R . . S1 S 1.03322(5) 0.51279(7) 0.61582(5) 0.05275(18) Uani 1 1 d . . . O1 O 1.14695(16) 0.5927(2) 0.63029(18) 0.0754(6) Uani 1 1 d . . . C21 C 0.9073(2) 0.6327(2) 0.56569(19) 0.0487(5) Uani 1 1 d . . . C22 C 0.9259(2) 0.7616(3) 0.6182(2) 0.0586(6) Uani 1 1 d . . . H22 H 0.9994 0.7805 0.6777 0.070 Uiso 1 1 calc R . . C23 C 0.8370(3) 0.8603(3) 0.5828(2) 0.0666(7) Uani 1 1 d . . . H23 H 0.8495 0.9464 0.6177 0.080 Uiso 1 1 calc R . . C24 C 0.7287(3) 0.8311(3) 0.4950(3) 0.0684(7) Uani 1 1 d . . . H24 H 0.6674 0.8977 0.4710 0.082 Uiso 1 1 calc R . . C25 C 0.7102(2) 0.7048(3) 0.4426(2) 0.0609(7) Uani 1 1 d . . . H25 H 0.6361 0.6870 0.3835 0.073 Uiso 1 1 calc R . . C26 C 0.7994(2) 0.6024(2) 0.47538(19) 0.0493(6) Uani 1 1 d . . . C31 C 0.6514(2) 0.3463(3) 0.5038(2) 0.0513(6) Uani 1 1 d . . . C32 C 0.6850(3) 0.2119(3) 0.5399(3) 0.0669(7) Uani 1 1 d . . . H32 H 0.7150 0.1545 0.4963 0.080 Uiso 1 1 calc R . . C33 C 0.6745(3) 0.1628(3) 0.6394(3) 0.0813(9) Uani 1 1 d . . . H33 H 0.6963 0.0723 0.6616 0.098 Uiso 1 1 calc R . . C34 C 0.6321(3) 0.2464(4) 0.7063(3) 0.0765(8) Uani 1 1 d . . . C35 C 0.5991(3) 0.3805(3) 0.6735(2) 0.0685(7) Uani 1 1 d . . . H35 H 0.5713 0.4380 0.7187 0.082 Uiso 1 1 calc R . . C36 C 0.6080(2) 0.4284(3) 0.5721(2) 0.0587(6) Uani 1 1 d . . . H36 H 0.5842 0.5183 0.5491 0.070 Uiso 1 1 calc R . . O2 O 0.6245(3) 0.1844(3) 0.8024(3) 0.1196(10) Uani 1 1 d . . . C37 C 0.5740(5) 0.2542(7) 0.8706(4) 0.1410(18) Uani 1 1 d . . . H37A H 0.6284 0.3269 0.9103 0.212 Uiso 1 1 calc R . . H37B H 0.5620 0.1919 0.9253 0.212 Uiso 1 1 calc R . . H37C H 0.4965 0.2927 0.8238 0.212 Uiso 1 1 calc R . . N1 N 0.6410(2) 0.2895(3) 0.30704(19) 0.0609(6) Uani 1 1 d . . . C41 C 0.5274(2) 0.2429(3) 0.2367(2) 0.0637(7) Uani 1 1 d . . . C42 C 0.5185(4) 0.1614(4) 0.1440(3) 0.0965(12) Uani 1 1 d . . . H42 H 0.5896 0.1334 0.1327 0.116 Uiso 1 1 calc R . . C43 C 0.4046(5) 0.1202(6) 0.0669(3) 0.132(2) Uani 1 1 d . . . H43 H 0.3994 0.0701 0.0018 0.159 Uiso 1 1 calc R . . C44 C 0.2999(4) 0.1544(6) 0.0877(4) 0.1344(19) Uani 1 1 d . . . H44 H 0.2235 0.1278 0.0361 0.161 Uiso 1 1 calc R . . C45 C 0.3070(3) 0.2274(5) 0.1838(5) 0.1219(15) Uani 1 1 d . . . H45 H 0.2361 0.2459 0.1992 0.146 Uiso 1 1 calc R . . C46 C 0.4193(3) 0.2734(4) 0.2578(3) 0.0893(10) Uani 1 1 d . . . H46 H 0.4236 0.3249 0.3219 0.107 Uiso 1 1 calc R . . H3 H 0.697(2) 0.249(2) 0.3060(18) 0.028(6) 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 C1 0.0474(12) 0.0531(15) 0.0480(12) 0.0001(10) 0.0148(10) -0.0013(10) C2 0.0436(12) 0.0538(13) 0.0502(13) -0.0040(11) 0.0099(10) 0.0012(10) S2 0.0914(5) 0.0759(4) 0.0537(4) -0.0022(4) 0.0314(3) -0.0111(4) C3 0.123(3) 0.095(2) 0.091(2) -0.004(2) 0.063(2) -0.025(2) C11 0.0485(12) 0.0626(16) 0.0513(13) -0.0032(12) 0.0137(10) 0.0072(11) C12 0.0560(16) 0.129(3) 0.0595(17) 0.0150(18) 0.0175(13) -0.0018(17) C13 0.0703(19) 0.162(4) 0.075(2) 0.035(2) 0.0367(18) 0.021(2) C14 0.099(2) 0.127(3) 0.0610(19) 0.021(2) 0.0306(19) 0.050(2) C15 0.133(3) 0.157(4) 0.0513(18) -0.008(3) 0.0010(19) -0.008(4) C16 0.098(2) 0.127(3) 0.0607(18) -0.0075(19) 0.0122(16) -0.028(2) C17 0.169(4) 0.230(6) 0.063(2) 0.037(3) 0.054(2) 0.092(4) S1 0.0468(3) 0.0605(3) 0.0519(3) -0.0061(3) 0.0189(2) -0.0004(3) O1 0.0515(10) 0.0933(14) 0.0846(13) -0.0075(11) 0.0283(9) -0.0117(10) C21 0.0514(13) 0.0525(14) 0.0464(12) -0.0018(10) 0.0227(10) -0.0027(11) C22 0.0621(15) 0.0617(16) 0.0521(14) -0.0108(13) 0.0204(12) -0.0062(13) C23 0.0818(19) 0.0502(15) 0.0732(17) -0.0109(13) 0.0343(15) -0.0035(14) C24 0.0719(18) 0.0511(16) 0.086(2) 0.0014(14) 0.0330(16) 0.0091(13) C25 0.0541(15) 0.0566(16) 0.0672(17) 0.0046(13) 0.0156(13) 0.0032(12) C26 0.0503(13) 0.0483(13) 0.0524(14) 0.0007(11) 0.0223(11) -0.0041(11) C31 0.0431(12) 0.0516(14) 0.0589(14) -0.0030(11) 0.0179(11) -0.0049(10) C32 0.0801(19) 0.0554(16) 0.0737(18) 0.0009(14) 0.0379(15) 0.0016(14) C33 0.100(2) 0.0650(18) 0.092(2) 0.0131(16) 0.0498(19) 0.0065(17) C34 0.0733(19) 0.087(2) 0.0760(19) 0.0096(17) 0.0343(16) -0.0081(17) C35 0.0638(16) 0.082(2) 0.0694(17) -0.0109(15) 0.0362(14) -0.0058(15) C36 0.0540(14) 0.0572(15) 0.0672(16) -0.0050(12) 0.0243(12) -0.0009(12) O2 0.158(3) 0.129(2) 0.1009(19) 0.0303(17) 0.082(2) 0.0008(19) C37 0.162(4) 0.189(5) 0.103(3) 0.011(4) 0.084(3) -0.013(4) N1 0.0468(13) 0.0691(15) 0.0609(13) -0.0156(11) 0.0120(11) -0.0025(12) C41 0.0629(16) 0.0680(17) 0.0507(15) -0.0003(13) 0.0087(12) -0.0156(13) C42 0.102(3) 0.132(3) 0.0598(18) -0.0251(19) 0.0348(17) -0.057(2) C43 0.148(4) 0.178(5) 0.063(2) -0.029(3) 0.029(2) -0.091(4) C44 0.097(3) 0.168(5) 0.100(3) 0.002(3) -0.012(3) -0.049(3) C45 0.064(2) 0.134(4) 0.144(4) -0.011(3) 0.007(2) -0.009(2) C46 0.0533(18) 0.090(2) 0.108(3) -0.012(2) 0.0084(17) -0.0039(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C26 1.514(3) . ? C1 C2 1.542(3) . ? C1 S2 1.851(2) . ? C2 N1 1.444(3) . ? C2 C31 1.516(3) . ? S2 C3 1.789(4) . ? C11 C12 1.353(4) . ? C11 C16 1.365(4) . ? C11 S1 1.794(2) . ? C12 C13 1.378(4) . ? C13 C14 1.352(6) . ? C14 C15 1.360(6) . ? C14 C17 1.525(5) . ? C15 C16 1.388(5) . ? S1 O1 1.4903(19) . ? S1 C21 1.802(2) . ? C21 C26 1.389(3) . ? C21 C22 1.393(4) . ? C22 C23 1.365(4) . ? C23 C24 1.375(4) . ? C24 C25 1.371(4) . ? C25 C26 1.390(4) . ? C31 C36 1.388(4) . ? C31 C32 1.390(4) . ? C32 C33 1.375(4) . ? C33 C34 1.376(5) . ? C34 O2 1.374(4) . ? C34 C35 1.378(5) . ? C35 C36 1.387(4) . ? O2 C37 1.373(6) . ? N1 C41 1.379(3) . ? C41 C42 1.375(4) . ? C41 C46 1.407(4) . ? C42 C43 1.392(5) . ? C43 C44 1.377(7) . ? C44 C45 1.370(7) . ? C45 C46 1.380(5) . ? 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 C26 C1 C2 114.06(19) . . ? C26 C1 S2 109.89(16) . . ? C2 C1 S2 106.13(15) . . ? N1 C2 C31 113.6(2) . . ? N1 C2 C1 107.68(19) . . ? C31 C2 C1 112.44(18) . . ? C3 S2 C1 102.91(14) . . ? C12 C11 C16 119.9(3) . . ? C12 C11 S1 119.8(2) . . ? C16 C11 S1 120.3(2) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 121.7(4) . . ? C13 C14 C15 117.5(3) . . ? C13 C14 C17 121.1(4) . . ? C15 C14 C17 121.4(4) . . ? C14 C15 C16 122.1(4) . . ? C11 C16 C15 118.7(4) . . ? O1 S1 C11 106.58(11) . . ? O1 S1 C21 106.53(12) . . ? C11 S1 C21 96.98(11) . . ? C26 C21 C22 121.1(2) . . ? C26 C21 S1 122.32(18) . . ? C22 C21 S1 116.46(18) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C24 119.3(2) . . ? C25 C24 C23 120.6(3) . . ? C24 C25 C26 121.7(3) . . ? C21 C26 C25 117.0(2) . . ? C21 C26 C1 123.4(2) . . ? C25 C26 C1 119.5(2) . . ? C36 C31 C32 117.5(3) . . ? C36 C31 C2 122.1(2) . . ? C32 C31 C2 120.4(2) . . ? C33 C32 C31 120.8(3) . . ? C32 C33 C34 120.7(3) . . ? O2 C34 C33 114.9(3) . . ? O2 C34 C35 125.1(3) . . ? C33 C34 C35 120.0(3) . . ? C34 C35 C36 118.9(3) . . ? C35 C36 C31 122.0(3) . . ? C37 O2 C34 120.0(4) . . ? C41 N1 C2 123.4(2) . . ? C42 C41 N1 119.5(3) . . ? C42 C41 C46 118.3(3) . . ? N1 C41 C46 122.1(3) . . ? C41 C42 C43 121.0(4) . . ? C44 C43 C42 119.4(4) . . ? C45 C44 C43 120.6(4) . . ? C44 C45 C46 120.1(5) . . ? C45 C46 C41 120.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.320 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.029