# Supplementary Material (ESI) for Chemical Communications # This journal is The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Tanaka, Kazuhiko' 'Kitahara, Yoshinori' _publ_contact_author_name 'Prof Kazuhiko Tanaka' _publ_contact_author_address ; Materials Science and Chemistry Faculty of Systems Engineering Wakayama University 930@Sakaedani Wakayama 640-8510 JAPAN ; _publ_contact_author_email 'KTANAKA@SYS.WAKAYAMA-U.AC.JP' _publ_section_title ; Synthesis, crystal structure and properties of thiaheterohelicenes containing phenolic hydroxy functions ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; <<2MeO.CIF>> <> <> data_crystal (P)-4 or (M)-4; dimethoxyhelicene _database_code_CSD 175385 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 25 10:24:29 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 450.57 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H18 O2 S2 ' _chemical_formula_moiety 'C28 H18 O2 S2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.719(6) _cell_length_b 17.730(4) _cell_length_c 9.974(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2072(1) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.2 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pail' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 936.00 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.975 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 1.25 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -1 2 0 0 3 -1 1 _diffrn_reflns_number 2720 _reflns_number_total 2720 _reflns_number_observed 1759 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06044 _diffrn_orient_matrix_UB_12 0.03912 _diffrn_orient_matrix_UB_13 0.01315 _diffrn_orient_matrix_UB_21 0.05788 _diffrn_orient_matrix_UB_22 -0.04062 _diffrn_orient_matrix_UB_23 0.01461 _diffrn_orient_matrix_UB_31 0.01669 _diffrn_orient_matrix_UB_32 -0.00081 _diffrn_orient_matrix_UB_33 -0.09832 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 112 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S(9) 0.6821(1) 0.03775(9) 1.0833(2) 0.0591(5) Uani d . 1.00 . S(14) 0.7643(2) 0.3396(1) 1.3835(2) 0.0772(6) Uani d . 1.00 . O(29) 0.5092(4) 0.4204(2) 0.8484(5) 0.057(1) Uani d . 1.00 . O(31) 0.9248(5) 0.2594(3) 0.6731(5) 0.073(2) Uani d . 1.00 . C(1) 0.5843(4) 0.3002(3) 0.9171(5) 0.037(1) Uani d . 1.00 . C(2) 0.5397(4) 0.3472(3) 0.8251(6) 0.042(1) Uani d . 1.00 . C(3) 0.5206(5) 0.3228(4) 0.6900(6) 0.053(2) Uani d . 1.00 . C(4) 0.5397(5) 0.2509(4) 0.6567(6) 0.057(2) Uani d . 1.00 . C(5) 0.5835(5) 0.1979(3) 0.7515(6) 0.046(1) Uani d . 1.00 . C(6) 0.5933(6) 0.1201(4) 0.7216(7) 0.060(2) Uani d . 1.00 . C(7) 0.6216(6) 0.0688(3) 0.8160(8) 0.058(2) Uani d . 1.00 . C(8) 0.6531(5) 0.0937(3) 0.9450(6) 0.045(1) Uani d . 1.00 . C(10) 0.7043(5) 0.1170(4) 1.1843(6) 0.051(2) Uani d . 1.00 . C(11) 0.7157(6) 0.1164(4) 1.3240(7) 0.067(2) Uani d . 1.00 . C(12) 0.7287(6) 0.1834(5) 1.3892(6) 0.068(2) Uani d . 1.00 . C(13) 0.7395(6) 0.2492(4) 1.3152(6) 0.061(2) Uani d . 1.00 . C(15) 0.7883(6) 0.3774(4) 1.2241(7) 0.065(2) Uani d . 1.00 . C(16) 0.8175(7) 0.4524(4) 1.198(1) 0.079(3) Uani d . 1.00 . C(17) 0.8448(6) 0.4722(4) 1.070(1) 0.084(3) Uani d . 1.00 . C(18) 0.8555(5) 0.4179(4) 0.9661(8) 0.059(2) Uani d . 1.00 . C(19) 0.8938(7) 0.4368(5) 0.833(1) 0.083(3) Uani d . 1.00 . C(20) 0.9140(7) 0.3840(5) 0.7426(10) 0.079(3) Uani d . 1.00 . C(21) 0.8939(5) 0.3075(4) 0.7736(7) 0.063(2) Uani d . 1.00 . C(22) 0.8558(4) 0.2867(3) 0.8960(6) 0.044(1) Uani d . 1.00 . C(23) 0.8290(5) 0.3412(3) 0.9945(7) 0.048(2) Uani d . 1.00 . C(24) 0.7840(4) 0.3222(3) 1.1249(6) 0.045(1) Uani d . 1.00 . C(25) 0.7416(5) 0.2509(3) 1.1751(5) 0.044(1) Uani d . 1.00 . C(26) 0.7058(4) 0.1838(3) 1.1097(5) 0.041(1) Uani d . 1.00 . C(27) 0.6595(4) 0.1715(3) 0.9737(5) 0.037(1) Uani d . 1.00 . C(28) 0.6118(4) 0.2227(3) 0.8815(5) 0.037(1) Uani d . 1.00 . C(30) 0.5145(7) 0.4455(4) 0.9822(8) 0.068(2) Uani d . 1.00 . C(32) 0.9223(7) 0.1819(5) 0.7003(7) 0.074(2) Uani d . 1.00 . H(1) 0.5989 0.3174 1.0061 0.0424 Uiso calc . 1.00 . H(2) 0.4929 0.3566 0.6240 0.0618 Uiso calc . 1.00 . H(3) 0.5236 0.2341 0.5683 0.0643 Uiso calc . 1.00 . H(4) 0.5745 0.1029 0.6337 0.0694 Uiso calc . 1.00 . H(5) 0.6215 0.0160 0.7969 0.0674 Uiso calc . 1.00 . H(6) 0.7153 0.0711 1.3741 0.0762 Uiso calc . 1.00 . H(7) 0.7279 0.1846 1.4853 0.0771 Uiso calc . 1.00 . H(8) 0.8197 0.4909 1.2619 0.0949 Uiso calc . 1.00 . H(9) 0.8585 0.5234 1.0443 0.0955 Uiso calc . 1.00 . H(10) 0.9050 0.4880 0.8126 0.0947 Uiso calc . 1.00 . H(11) 0.9401 0.3976 0.6565 0.0890 Uiso calc . 1.00 . H(12) 0.8451 0.2345 0.9157 0.0490 Uiso calc . 1.00 . H(13) 0.4946 0.4976 0.9902 0.0779 Uiso calc . 1.00 . H(14) 0.5921 0.4402 1.0158 0.0779 Uiso calc . 1.00 . H(15) 0.4662 0.4168 1.0399 0.0779 Uiso calc . 1.00 . H(16) 0.8450 0.1673 0.7174 0.0858 Uiso calc . 1.00 . H(17) 0.9503 0.1550 0.6258 0.0858 Uiso calc . 1.00 . H(18) 0.9671 0.1724 0.7770 0.0858 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(9) 0.0614(9) 0.0416(7) 0.074(1) 0.0081(7) 0.0150(9) 0.0151(8) S(14) 0.076(1) 0.103(1) 0.0534(9) 0.028(1) -0.0197(9) -0.0362(10) O(29) 0.063(3) 0.043(2) 0.064(3) 0.005(2) -0.013(2) 0.014(2) O(31) 0.086(4) 0.087(4) 0.046(3) 0.008(3) 0.019(3) 0.018(3) C(1) 0.033(2) 0.046(3) 0.034(3) -0.005(2) -0.007(2) 0.004(2) C(2) 0.032(2) 0.052(3) 0.042(3) -0.004(2) 0.001(2) 0.009(3) C(3) 0.050(3) 0.070(4) 0.038(3) -0.001(3) -0.006(3) 0.015(3) C(4) 0.049(3) 0.095(5) 0.028(3) -0.011(4) -0.010(3) 0.002(3) C(5) 0.035(3) 0.054(3) 0.050(3) -0.007(2) -0.002(3) -0.001(3) C(6) 0.057(4) 0.071(4) 0.053(4) -0.006(3) -0.009(3) -0.024(3) C(7) 0.056(4) 0.040(3) 0.079(4) -0.003(3) 0.003(4) -0.024(3) C(8) 0.041(3) 0.040(3) 0.054(3) 0.004(2) 0.015(3) 0.003(3) C(10) 0.046(3) 0.056(3) 0.052(3) 0.020(3) 0.010(3) 0.009(3) C(11) 0.068(4) 0.080(5) 0.053(4) 0.032(4) 0.009(4) 0.038(4) C(12) 0.062(4) 0.106(6) 0.035(3) 0.029(4) -0.001(3) 0.011(4) C(13) 0.054(4) 0.093(5) 0.036(3) 0.024(4) 0.002(3) -0.004(3) C(15) 0.050(4) 0.074(4) 0.071(4) 0.015(3) -0.019(3) -0.022(4) C(16) 0.063(4) 0.063(4) 0.112(7) 0.012(4) -0.032(5) -0.048(5) C(17) 0.055(4) 0.045(4) 0.151(9) 0.000(3) -0.033(6) 0.001(5) C(18) 0.038(3) 0.049(3) 0.090(5) -0.002(3) -0.018(3) 0.005(4) C(19) 0.052(4) 0.072(5) 0.125(8) -0.015(4) -0.018(5) 0.043(6) C(20) 0.058(4) 0.077(5) 0.102(6) -0.012(4) 0.010(5) 0.038(5) C(21) 0.036(3) 0.080(5) 0.071(5) -0.002(3) -0.003(3) 0.035(4) C(22) 0.032(2) 0.053(3) 0.045(3) -0.005(2) -0.006(2) 0.010(3) C(23) 0.034(3) 0.044(3) 0.067(4) -0.007(2) -0.015(3) 0.006(3) C(24) 0.036(3) 0.049(3) 0.050(3) 0.008(2) -0.015(2) -0.006(3) C(25) 0.040(3) 0.063(4) 0.029(2) 0.015(3) -0.006(2) -0.003(2) C(26) 0.041(3) 0.046(3) 0.036(3) 0.013(2) 0.005(2) 0.005(2) C(27) 0.039(3) 0.034(2) 0.038(3) 0.001(2) 0.004(2) -0.002(2) C(28) 0.033(2) 0.041(3) 0.035(3) 0.000(2) 0.001(2) 0.002(2) C(30) 0.087(5) 0.043(3) 0.075(5) 0.015(3) -0.010(4) 0.006(3) C(32) 0.069(4) 0.109(6) 0.044(4) 0.017(4) 0.010(3) 0.014(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00265|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.004(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1759 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0528 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0770 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.229 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.24 _refine_diff_density_max 0.17 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(9) C(8) 1.732(6) 1_555 1_555 yes S(9) C(10) 1.748(7) 1_555 1_555 yes S(14) C(13) 1.766(7) 1_555 1_555 yes S(14) C(15) 1.748(8) 1_555 1_555 yes O(29) C(2) 1.367(7) 1_555 1_555 yes O(29) C(30) 1.407(9) 1_555 1_555 yes O(31) C(21) 1.365(10) 1_555 1_555 yes O(31) C(32) 1.40(1) 1_555 1_555 yes C(1) C(2) 1.345(7) 1_555 1_555 yes C(1) C(28) 1.455(7) 1_555 1_555 yes C(2) C(3) 1.432(9) 1_555 1_555 yes C(3) C(4) 1.337(10) 1_555 1_555 yes C(4) C(5) 1.428(9) 1_555 1_555 yes C(5) C(6) 1.415(9) 1_555 1_555 yes C(5) C(28) 1.409(8) 1_555 1_555 yes C(6) C(7) 1.35(1) 1_555 1_555 yes C(7) C(8) 1.410(9) 1_555 1_555 yes C(8) C(27) 1.412(7) 1_555 1_555 yes C(10) C(11) 1.399(9) 1_555 1_555 yes C(10) C(26) 1.400(8) 1_555 1_555 yes C(11) C(12) 1.36(1) 1_555 1_555 yes C(12) C(13) 1.386(10) 1_555 1_555 yes C(13) C(25) 1.398(8) 1_555 1_555 yes C(15) C(16) 1.40(1) 1_555 1_555 yes C(15) C(24) 1.393(9) 1_555 1_555 yes C(16) C(17) 1.36(1) 1_555 1_555 yes C(17) C(18) 1.42(1) 1_555 1_555 yes C(18) C(19) 1.44(1) 1_555 1_555 yes C(18) C(23) 1.424(8) 1_555 1_555 yes C(19) C(20) 1.32(1) 1_555 1_555 yes C(20) C(21) 1.41(1) 1_555 1_555 yes C(21) C(22) 1.352(9) 1_555 1_555 yes C(22) C(23) 1.413(9) 1_555 1_555 yes C(23) C(24) 1.442(9) 1_555 1_555 yes C(24) C(25) 1.447(8) 1_555 1_555 yes C(25) C(26) 1.421(8) 1_555 1_555 yes C(26) C(27) 1.477(7) 1_555 1_555 yes C(27) C(28) 1.408(7) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(8) S(9) C(10) 91.6(3) 1_555 1_555 1_555 yes C(13) S(14) C(15) 91.4(3) 1_555 1_555 1_555 yes C(2) O(29) C(30) 116.7(4) 1_555 1_555 1_555 yes C(21) O(31) C(32) 117.7(5) 1_555 1_555 1_555 yes C(2) C(1) C(28) 120.2(5) 1_555 1_555 1_555 yes C(2) C(1) H(1) 120.5(5) 1_555 1_555 1_555 no C(28) C(1) H(1) 119.3(5) 1_555 1_555 1_555 no O(29) C(2) C(1) 125.0(5) 1_555 1_555 1_555 yes O(29) C(2) C(3) 114.0(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 121.1(6) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.7(6) 1_555 1_555 1_555 yes C(2) C(3) H(2) 121.0(7) 1_555 1_555 1_555 no C(4) C(3) H(2) 119.2(7) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.6(5) 1_555 1_555 1_555 yes C(3) C(4) H(3) 119.7(7) 1_555 1_555 1_555 no C(5) C(4) H(3) 118.7(7) 1_555 1_555 1_555 no C(4) C(5) C(6) 122.0(6) 1_555 1_555 1_555 yes C(4) C(5) C(28) 119.2(5) 1_555 1_555 1_555 yes C(6) C(5) C(28) 118.7(6) 1_555 1_555 1_555 yes C(5) C(6) C(7) 121.9(6) 1_555 1_555 1_555 yes C(5) C(6) H(4) 119.2(7) 1_555 1_555 1_555 no C(7) C(6) H(4) 118.8(7) 1_555 1_555 1_555 no C(6) C(7) C(8) 119.4(5) 1_555 1_555 1_555 yes C(6) C(7) H(5) 121.4(7) 1_555 1_555 1_555 no C(8) C(7) H(5) 119.3(7) 1_555 1_555 1_555 no S(9) C(8) C(7) 126.8(4) 1_555 1_555 1_555 yes S(9) C(8) C(27) 112.8(5) 1_555 1_555 1_555 yes C(7) C(8) C(27) 120.3(5) 1_555 1_555 1_555 yes S(9) C(10) C(11) 125.6(6) 1_555 1_555 1_555 yes S(9) C(10) C(26) 112.1(5) 1_555 1_555 1_555 yes C(11) C(10) C(26) 122.3(7) 1_555 1_555 1_555 yes C(10) C(11) C(12) 118.6(6) 1_555 1_555 1_555 yes C(10) C(11) H(6) 122.2(9) 1_555 1_555 1_555 no C(12) C(11) H(6) 119.2(7) 1_555 1_555 1_555 no C(11) C(12) C(13) 119.3(6) 1_555 1_555 1_555 yes C(11) C(12) H(7) 119.7(8) 1_555 1_555 1_555 no C(13) C(12) H(7) 121.0(8) 1_555 1_555 1_555 no S(14) C(13) C(12) 125.0(5) 1_555 1_555 1_555 yes S(14) C(13) C(25) 111.2(5) 1_555 1_555 1_555 yes C(12) C(13) C(25) 123.6(6) 1_555 1_555 1_555 yes S(14) C(15) C(16) 125.1(6) 1_555 1_555 1_555 yes S(14) C(15) C(24) 111.7(6) 1_555 1_555 1_555 yes C(16) C(15) C(24) 122.9(7) 1_555 1_555 1_555 yes C(15) C(16) C(17) 118.7(7) 1_555 1_555 1_555 yes C(15) C(16) H(8) 124(1) 1_555 1_555 1_555 no C(17) C(16) H(8) 116.4(10) 1_555 1_555 1_555 no C(16) C(17) C(18) 122.0(7) 1_555 1_555 1_555 yes C(16) C(17) H(9) 122(1) 1_555 1_555 1_555 no C(18) C(17) H(9) 115(1) 1_555 1_555 1_555 no C(17) C(18) C(19) 122.9(7) 1_555 1_555 1_555 yes C(17) C(18) C(23) 118.8(8) 1_555 1_555 1_555 yes C(19) C(18) C(23) 118.3(7) 1_555 1_555 1_555 yes C(18) C(19) C(20) 121.3(7) 1_555 1_555 1_555 yes C(18) C(19) H(10) 117(1) 1_555 1_555 1_555 no C(20) C(19) H(10) 120(1) 1_555 1_555 1_555 no C(19) C(20) C(21) 120.1(8) 1_555 1_555 1_555 yes C(19) C(20) H(11) 119.8(8) 1_555 1_555 1_555 no C(21) C(20) H(11) 120.0(10) 1_555 1_555 1_555 no O(31) C(21) C(20) 113.3(7) 1_555 1_555 1_555 yes O(31) C(21) C(22) 125.5(6) 1_555 1_555 1_555 yes C(20) C(21) C(22) 121.0(8) 1_555 1_555 1_555 yes C(21) C(22) C(23) 121.0(6) 1_555 1_555 1_555 yes C(21) C(22) H(12) 119.5(7) 1_555 1_555 1_555 no C(23) C(22) H(12) 119.4(6) 1_555 1_555 1_555 no C(18) C(23) C(22) 117.7(6) 1_555 1_555 1_555 yes C(18) C(23) C(24) 118.8(6) 1_555 1_555 1_555 yes C(22) C(23) C(24) 123.3(5) 1_555 1_555 1_555 yes C(15) C(24) C(23) 117.6(6) 1_555 1_555 1_555 yes C(15) C(24) C(25) 112.3(6) 1_555 1_555 1_555 yes C(23) C(24) C(25) 129.9(5) 1_555 1_555 1_555 yes C(13) C(25) C(24) 111.8(6) 1_555 1_555 1_555 yes C(13) C(25) C(26) 115.8(6) 1_555 1_555 1_555 yes C(24) C(25) C(26) 132.4(5) 1_555 1_555 1_555 yes C(10) C(26) C(25) 118.0(5) 1_555 1_555 1_555 yes C(10) C(26) C(27) 111.0(5) 1_555 1_555 1_555 yes C(25) C(26) C(27) 130.8(5) 1_555 1_555 1_555 yes C(8) C(27) C(26) 110.5(5) 1_555 1_555 1_555 yes C(8) C(27) C(28) 118.5(5) 1_555 1_555 1_555 yes C(26) C(27) C(28) 130.6(5) 1_555 1_555 1_555 yes C(1) C(28) C(5) 117.9(5) 1_555 1_555 1_555 yes C(1) C(28) C(27) 122.5(5) 1_555 1_555 1_555 yes C(5) C(28) C(27) 119.5(5) 1_555 1_555 1_555 yes O(29) C(30) H(13) 111.9(6) 1_555 1_555 1_555 no O(29) C(30) H(14) 109.7(7) 1_555 1_555 1_555 no O(29) C(30) H(15) 112.2(7) 1_555 1_555 1_555 no H(13) C(30) H(14) 107.0(7) 1_555 1_555 1_555 no H(13) C(30) H(15) 108.6(8) 1_555 1_555 1_555 no H(14) C(30) H(15) 107.2(7) 1_555 1_555 1_555 no O(31) C(32) H(16) 108.6(7) 1_555 1_555 1_555 no O(31) C(32) H(17) 109.6(7) 1_555 1_555 1_555 no O(31) C(32) H(18) 108.6(8) 1_555 1_555 1_555 no H(16) C(32) H(17) 109.6(9) 1_555 1_555 1_555 no H(16) C(32) H(18) 109.5(7) 1_555 1_555 1_555 no H(17) C(32) H(18) 110.9(8) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(9) C(19) 3.510(8) 1_555 3_457 ? O(29) C(16) 3.386(8) 1_555 2_664 ? O(29) C(7) 3.458(7) 1_555 4_656 ? O(31) C(4) 3.559(7) 1_555 3_556 ? C(3) C(12) 3.512(10) 1_555 3_457 ? C(3) C(13) 3.533(9) 1_555 3_457 ? C(4) C(13) 3.530(9) 1_555 3_457 ? C(6) C(16) 3.57(1) 1_555 3_457 ? C(7) C(17) 3.513(10) 1_555 3_457 ? C(7) C(16) 3.59(1) 1_555 3_457 ? C(10) C(20) 3.48(1) 1_555 3_457 ? C(11) C(20) 3.60(1) 1_555 3_457 ? C(16) C(19) 3.44(1) 1_555 2_665 ? #------------------------------------------------------------------------------ data_(PM-5)(acetone) _database_code_CSD 175386 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Nov 8 16:06:11 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 480.60 _chemical_formula_analytical ? _chemical_formula_sum 'C29 H20 O3 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.612(3) _cell_length_b 10.361(1) _cell_length_c 19.180(2) _cell_angle_alpha 90.00(1) _cell_angle_beta 91.31(2) _cell_angle_gamma 90.00(2) _cell_volume 2306.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 90.0 _cell_measurement_theta_max -90.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.856 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0.15 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 1 -4 -2 0 -2 -1 1 -2 _diffrn_reflns_number 5758 _reflns_number_total 5612 _reflns_number_observed 3562 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.055 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05742 _diffrn_orient_matrix_UB_12 0.06554 _diffrn_orient_matrix_UB_13 -0.01681 _diffrn_orient_matrix_UB_21 0.06407 _diffrn_orient_matrix_UB_22 0.06115 _diffrn_orient_matrix_UB_23 -0.01024 _diffrn_orient_matrix_UB_31 0.00427 _diffrn_orient_matrix_UB_32 -0.03579 _diffrn_orient_matrix_UB_33 -0.04830 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 116 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 12 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S(9) 0.60926(5) -0.09898(7) 0.36724(4) 0.0584(2) Uani d . 1.00 . S(14) 0.39496(6) 0.37682(7) 0.50864(3) 0.0586(2) Uani d . 1.00 . O(29) 0.1135(1) 0.2726(2) 0.22664(9) 0.0607(5) Uani d . 1.00 . O(30) 0.0485(1) -0.1843(1) 0.37887(9) 0.0496(4) Uani d . 1.00 . O(31) 0.2426(2) -0.3184(2) 0.3780(1) 0.0694(6) Uani d . 1.00 . C(1) 0.2553(2) 0.1373(2) 0.27512(10) 0.0339(5) Uani d . 1.00 . C(2) 0.1723(2) 0.1589(2) 0.2243(1) 0.0426(6) Uani d . 1.00 . C(3) 0.1506(2) 0.0666(3) 0.1726(1) 0.0613(8) Uani d . 1.00 . C(4) 0.2145(3) -0.0427(3) 0.1711(1) 0.0661(8) Uani d . 1.00 . C(5) 0.3030(2) -0.0672(2) 0.2213(1) 0.0461(6) Uani d . 1.00 . C(6) 0.3782(2) -0.1761(2) 0.2155(1) 0.0586(8) Uani d . 1.00 . C(7) 0.4692(2) -0.1921(2) 0.2590(1) 0.0565(7) Uani d . 1.00 . C(8) 0.4861(2) -0.1037(2) 0.3142(1) 0.0453(6) Uani d . 1.00 . C(10) 0.5597(2) 0.0359(2) 0.4102(1) 0.0472(6) Uani d . 1.00 . C(11) 0.6258(2) 0.1080(3) 0.4588(1) 0.0585(8) Uani d . 1.00 . C(12) 0.5816(2) 0.2163(3) 0.4865(1) 0.0576(7) Uani d . 1.00 . C(13) 0.4652(2) 0.2466(2) 0.4721(1) 0.0475(6) Uani d . 1.00 . C(15) 0.2644(2) 0.3222(2) 0.4760(1) 0.0460(6) Uani d . 1.00 . C(16) 0.1592(2) 0.3867(2) 0.4860(1) 0.0591(8) Uani d . 1.00 . C(17) 0.0608(2) 0.3289(3) 0.4649(1) 0.0596(8) Uani d . 1.00 . C(18) 0.0602(2) 0.2016(2) 0.4374(1) 0.0454(6) Uani d . 1.00 . C(19) -0.0442(2) 0.1359(3) 0.4238(1) 0.0538(7) Uani d . 1.00 . C(20) -0.0469(2) 0.0106(3) 0.4039(1) 0.0504(7) Uani d . 1.00 . C(21) 0.0569(2) -0.0566(2) 0.3965(1) 0.0381(5) Uani d . 1.00 . C(22) 0.1613(2) 0.0038(2) 0.40700(9) 0.0324(5) Uani d . 1.00 . C(23) 0.1658(2) 0.1356(2) 0.42637(10) 0.0335(5) Uani d . 1.00 . C(24) 0.2719(2) 0.2048(2) 0.44001(10) 0.0355(5) Uani d . 1.00 . C(25) 0.3918(2) 0.1677(2) 0.4304(1) 0.0362(5) Uani d . 1.00 . C(26) 0.4457(2) 0.0707(2) 0.3897(1) 0.0363(5) Uani d . 1.00 . C(27) 0.4098(2) -0.0029(2) 0.3282(1) 0.0348(5) Uani d . 1.00 . C(28) 0.3200(2) 0.0229(2) 0.27637(10) 0.0338(5) Uani d . 1.00 . C(32) 0.2588(2) -0.3979(2) 0.3330(1) 0.0605(8) Uani d . 1.00 . C(33) 0.3640(3) -0.4778(3) 0.3328(2) 0.086(1) Uani d . 1.00 . C(34) 0.1742(3) -0.4162(4) 0.2740(2) 0.105(1) Uani d . 1.00 . H(1) 0.2694 0.2009 0.3100 0.0428 Uiso calc . 1.00 . H(2) 0.0907 0.0798 0.1388 0.0765 Uiso calc . 1.00 . H(3) 0.2007 -0.1037 0.1351 0.0800 Uiso calc . 1.00 . H(4) 0.3625 -0.2376 0.1796 0.0714 Uiso calc . 1.00 . H(5) 0.5207 -0.2621 0.2533 0.0705 Uiso calc . 1.00 . H(6) 0.7008 0.0802 0.4716 0.0722 Uiso calc . 1.00 . H(7) 0.6273 0.2722 0.5151 0.0715 Uiso calc . 1.00 . H(8) 0.1586 0.4694 0.5074 0.0739 Uiso calc . 1.00 . H(9) -0.0100 0.3738 0.4685 0.0743 Uiso calc . 1.00 . H(10) -0.1148 0.1807 0.4291 0.0666 Uiso calc . 1.00 . H(11) -0.1186 -0.0310 0.3951 0.0625 Uiso calc . 1.00 . H(12) 0.2306 -0.0427 0.4011 0.0411 Uiso calc . 1.00 . H(13) 0.0618 0.2776 0.1884 0.0807 Uiso calc . 1.00 . H(14) 0.1235 -0.2338 0.3821 0.0807 Uiso calc . 1.00 . H(15) 0.4211 -0.4433 0.3654 0.1035 Uiso calc . 1.00 . H(16) 0.3971 -0.4811 0.2881 0.1035 Uiso calc . 1.00 . H(17) 0.3478 -0.5647 0.3476 0.1035 Uiso calc . 1.00 . H(18) 0.2104 -0.4397 0.2320 0.1265 Uiso calc . 1.00 . H(19) 0.1309 -0.3377 0.2653 0.1265 Uiso calc . 1.00 . H(20) 0.1186 -0.4823 0.2848 0.1265 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(9) 0.0327(3) 0.0756(5) 0.0673(4) 0.0178(3) 0.0078(3) 0.0266(3) S(14) 0.0675(4) 0.0560(4) 0.0517(4) -0.0240(3) -0.0099(3) -0.0095(3) O(29) 0.063(1) 0.0555(10) 0.063(1) 0.0188(8) -0.0268(9) -0.0007(8) O(30) 0.0383(8) 0.0454(9) 0.065(1) -0.0095(7) -0.0097(7) -0.0090(8) O(31) 0.069(1) 0.066(1) 0.073(1) 0.0146(10) -0.0109(10) -0.026(1) C(1) 0.0334(10) 0.035(1) 0.0328(10) -0.0017(8) -0.0017(8) 0.0001(8) C(2) 0.042(1) 0.042(1) 0.044(1) 0.0018(9) -0.0083(9) 0.0041(9) C(3) 0.063(2) 0.070(2) 0.050(1) 0.007(1) -0.026(1) -0.010(1) C(4) 0.080(2) 0.067(2) 0.050(1) 0.005(1) -0.015(1) -0.022(1) C(5) 0.051(1) 0.043(1) 0.045(1) 0.0015(10) 0.0033(10) -0.0073(10) C(6) 0.069(2) 0.048(1) 0.060(2) 0.005(1) 0.015(1) -0.014(1) C(7) 0.054(1) 0.047(1) 0.070(2) 0.014(1) 0.023(1) 0.001(1) C(8) 0.035(1) 0.049(1) 0.052(1) 0.0089(9) 0.0139(9) 0.014(1) C(10) 0.0284(10) 0.066(1) 0.047(1) -0.003(1) 0.0002(9) 0.023(1) C(11) 0.027(1) 0.099(2) 0.048(1) -0.012(1) -0.0086(10) 0.028(1) C(12) 0.040(1) 0.088(2) 0.044(1) -0.028(1) -0.0135(10) 0.011(1) C(13) 0.044(1) 0.059(1) 0.039(1) -0.019(1) -0.0062(9) 0.005(1) C(15) 0.051(1) 0.045(1) 0.042(1) -0.009(1) -0.0021(10) -0.0041(10) C(16) 0.069(2) 0.042(1) 0.066(2) 0.003(1) 0.006(1) -0.017(1) C(17) 0.052(1) 0.052(1) 0.075(2) 0.016(1) 0.008(1) -0.011(1) C(18) 0.037(1) 0.049(1) 0.050(1) 0.0026(9) 0.0040(9) -0.003(1) C(19) 0.029(1) 0.064(2) 0.069(2) 0.009(1) 0.002(1) -0.003(1) C(20) 0.0249(10) 0.066(2) 0.060(1) -0.0057(10) -0.0036(9) -0.001(1) C(21) 0.0328(10) 0.045(1) 0.036(1) -0.0067(9) -0.0021(8) -0.0028(9) C(22) 0.0249(9) 0.041(1) 0.0314(9) -0.0006(8) -0.0007(7) -0.0007(8) C(23) 0.0297(9) 0.039(1) 0.0314(9) -0.0008(8) -0.0004(7) 0.0001(8) C(24) 0.037(1) 0.036(1) 0.0333(10) -0.0049(8) -0.0015(8) -0.0008(8) C(25) 0.0324(10) 0.042(1) 0.0338(10) -0.0097(8) -0.0038(8) 0.0083(8) C(26) 0.0247(9) 0.046(1) 0.038(1) -0.0050(8) -0.0016(7) 0.0140(9) C(27) 0.0263(9) 0.038(1) 0.040(1) 0.0030(8) 0.0072(8) 0.0103(9) C(28) 0.0299(9) 0.035(1) 0.0363(10) -0.0027(8) 0.0031(8) 0.0009(8) C(32) 0.075(2) 0.045(1) 0.062(2) -0.001(1) 0.008(1) -0.009(1) C(33) 0.119(3) 0.063(2) 0.078(2) 0.035(2) 0.020(2) 0.008(2) C(34) 0.093(3) 0.120(3) 0.102(3) -0.007(2) -0.013(2) -0.059(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00137|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3562 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0422 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0625 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.272 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.17 _refine_diff_density_max 0.31 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(9) C(8) 1.736(2) 1_555 1_555 yes S(9) C(10) 1.728(3) 1_555 1_555 yes S(14) C(13) 1.733(3) 1_555 1_555 yes S(14) C(15) 1.723(2) 1_555 1_555 yes O(29) C(2) 1.363(3) 1_555 1_555 yes O(30) C(21) 1.369(3) 1_555 1_555 yes O(31) C(32) 1.211(3) 1_555 1_555 yes C(1) C(2) 1.373(3) 1_555 1_555 yes C(1) C(28) 1.403(3) 1_555 1_555 yes C(2) C(3) 1.396(3) 1_555 1_555 yes C(3) C(4) 1.355(4) 1_555 1_555 yes C(4) C(5) 1.415(3) 1_555 1_555 yes C(5) C(6) 1.433(3) 1_555 1_555 yes C(5) C(28) 1.420(3) 1_555 1_555 yes C(6) C(7) 1.341(4) 1_555 1_555 yes C(7) C(8) 1.411(4) 1_555 1_555 yes C(8) C(27) 1.399(3) 1_555 1_555 yes C(10) C(11) 1.408(4) 1_555 1_555 yes C(10) C(26) 1.419(3) 1_555 1_555 yes C(11) C(12) 1.347(4) 1_555 1_555 yes C(12) C(13) 1.409(3) 1_555 1_555 yes C(13) C(25) 1.414(3) 1_555 1_555 yes C(15) C(16) 1.410(3) 1_555 1_555 yes C(15) C(24) 1.402(3) 1_555 1_555 yes C(16) C(17) 1.344(4) 1_555 1_555 yes C(17) C(18) 1.420(3) 1_555 1_555 yes C(18) C(19) 1.409(3) 1_555 1_555 yes C(18) C(23) 1.424(3) 1_555 1_555 yes C(19) C(20) 1.353(4) 1_555 1_555 yes C(20) C(21) 1.403(3) 1_555 1_555 yes C(21) C(22) 1.374(3) 1_555 1_555 yes C(22) C(23) 1.415(3) 1_555 1_555 yes C(23) C(24) 1.444(3) 1_555 1_555 yes C(24) C(25) 1.461(3) 1_555 1_555 yes C(25) C(26) 1.426(3) 1_555 1_555 yes C(26) C(27) 1.458(3) 1_555 1_555 yes C(27) C(28) 1.448(3) 1_555 1_555 yes C(32) C(33) 1.475(4) 1_555 1_555 yes C(32) C(34) 1.493(4) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(8) S(9) C(10) 91.3(1) 1_555 1_555 1_555 yes C(13) S(14) C(15) 90.9(1) 1_555 1_555 1_555 yes C(2) O(29) H(13) 109.5(2) 1_555 1_555 1_555 no C(21) O(30) H(14) 114.8(1) 1_555 1_555 1_555 no C(2) C(1) C(28) 121.1(2) 1_555 1_555 1_555 yes C(2) C(1) H(1) 119.5(2) 1_555 1_555 1_555 no C(28) C(1) H(1) 119.3(2) 1_555 1_555 1_555 no O(29) C(2) C(1) 117.5(2) 1_555 1_555 1_555 yes O(29) C(2) C(3) 122.2(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.3(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.8(2) 1_555 1_555 1_555 yes C(2) C(3) H(2) 120.2(3) 1_555 1_555 1_555 no C(4) C(3) H(2) 120.0(2) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.7(2) 1_555 1_555 1_555 yes C(3) C(4) H(3) 119.3(3) 1_555 1_555 1_555 no C(5) C(4) H(3) 118.9(3) 1_555 1_555 1_555 no C(4) C(5) C(6) 121.6(2) 1_555 1_555 1_555 yes C(4) C(5) C(28) 118.4(2) 1_555 1_555 1_555 yes C(6) C(5) C(28) 120.0(2) 1_555 1_555 1_555 yes C(5) C(6) C(7) 121.5(2) 1_555 1_555 1_555 yes C(5) C(6) H(4) 118.4(3) 1_555 1_555 1_555 no C(7) C(6) H(4) 120.1(3) 1_555 1_555 1_555 no C(6) C(7) C(8) 118.7(2) 1_555 1_555 1_555 yes C(6) C(7) H(5) 120.9(3) 1_555 1_555 1_555 no C(8) C(7) H(5) 120.3(3) 1_555 1_555 1_555 no S(9) C(8) C(7) 123.8(2) 1_555 1_555 1_555 yes S(9) C(8) C(27) 112.6(2) 1_555 1_555 1_555 yes C(7) C(8) C(27) 123.4(2) 1_555 1_555 1_555 yes S(9) C(10) C(11) 124.2(2) 1_555 1_555 1_555 yes S(9) C(10) C(26) 113.1(2) 1_555 1_555 1_555 yes C(11) C(10) C(26) 122.7(2) 1_555 1_555 1_555 yes C(10) C(11) C(12) 119.7(2) 1_555 1_555 1_555 yes C(10) C(11) H(6) 119.7(3) 1_555 1_555 1_555 no C(12) C(11) H(6) 120.6(3) 1_555 1_555 1_555 no C(11) C(12) C(13) 118.8(2) 1_555 1_555 1_555 yes C(11) C(12) H(7) 121.4(3) 1_555 1_555 1_555 no C(13) C(12) H(7) 119.9(3) 1_555 1_555 1_555 no S(14) C(13) C(12) 123.5(2) 1_555 1_555 1_555 yes S(14) C(13) C(25) 113.3(2) 1_555 1_555 1_555 yes C(12) C(13) C(25) 123.0(2) 1_555 1_555 1_555 yes S(14) C(15) C(16) 123.6(2) 1_555 1_555 1_555 yes S(14) C(15) C(24) 113.6(2) 1_555 1_555 1_555 yes C(16) C(15) C(24) 122.9(2) 1_555 1_555 1_555 yes C(15) C(16) C(17) 118.7(2) 1_555 1_555 1_555 yes C(15) C(16) H(8) 120.1(3) 1_555 1_555 1_555 no C(17) C(16) H(8) 121.2(3) 1_555 1_555 1_555 no C(16) C(17) C(18) 121.5(2) 1_555 1_555 1_555 yes C(16) C(17) H(9) 119.4(3) 1_555 1_555 1_555 no C(18) C(17) H(9) 119.0(3) 1_555 1_555 1_555 no C(17) C(18) C(19) 120.9(2) 1_555 1_555 1_555 yes C(17) C(18) C(23) 120.3(2) 1_555 1_555 1_555 yes C(19) C(18) C(23) 118.7(2) 1_555 1_555 1_555 yes C(18) C(19) C(20) 122.0(2) 1_555 1_555 1_555 yes C(18) C(19) H(10) 119.1(2) 1_555 1_555 1_555 no C(20) C(19) H(10) 119.0(2) 1_555 1_555 1_555 no C(19) C(20) C(21) 119.3(2) 1_555 1_555 1_555 yes C(19) C(20) H(11) 120.1(2) 1_555 1_555 1_555 no C(21) C(20) H(11) 120.6(2) 1_555 1_555 1_555 no O(30) C(21) C(20) 116.6(2) 1_555 1_555 1_555 yes O(30) C(21) C(22) 122.3(2) 1_555 1_555 1_555 yes C(20) C(21) C(22) 121.1(2) 1_555 1_555 1_555 yes C(21) C(22) C(23) 120.3(2) 1_555 1_555 1_555 yes C(21) C(22) H(12) 120.0(2) 1_555 1_555 1_555 no C(23) C(22) H(12) 119.7(2) 1_555 1_555 1_555 no C(18) C(23) C(22) 118.4(2) 1_555 1_555 1_555 yes C(18) C(23) C(24) 117.9(2) 1_555 1_555 1_555 yes C(22) C(23) C(24) 123.6(2) 1_555 1_555 1_555 yes C(15) C(24) C(23) 117.2(2) 1_555 1_555 1_555 yes C(15) C(24) C(25) 111.1(2) 1_555 1_555 1_555 yes C(23) C(24) C(25) 131.2(2) 1_555 1_555 1_555 yes C(13) C(25) C(24) 109.9(2) 1_555 1_555 1_555 yes C(13) C(25) C(26) 116.8(2) 1_555 1_555 1_555 yes C(24) C(25) C(26) 133.3(2) 1_555 1_555 1_555 yes C(10) C(26) C(25) 116.4(2) 1_555 1_555 1_555 yes C(10) C(26) C(27) 109.9(2) 1_555 1_555 1_555 yes C(25) C(26) C(27) 133.7(2) 1_555 1_555 1_555 yes C(8) C(27) C(26) 112.0(2) 1_555 1_555 1_555 yes C(8) C(27) C(28) 117.1(2) 1_555 1_555 1_555 yes C(26) C(27) C(28) 130.3(2) 1_555 1_555 1_555 yes C(1) C(28) C(5) 118.5(2) 1_555 1_555 1_555 yes C(1) C(28) C(27) 123.0(2) 1_555 1_555 1_555 yes C(5) C(28) C(27) 118.4(2) 1_555 1_555 1_555 yes O(31) C(32) C(33) 121.7(3) 1_555 1_555 1_555 yes O(31) C(32) C(34) 121.0(3) 1_555 1_555 1_555 yes C(33) C(32) C(34) 117.3(3) 1_555 1_555 1_555 yes C(32) C(33) H(15) 110.3(3) 1_555 1_555 1_555 no C(32) C(33) H(16) 112.0(3) 1_555 1_555 1_555 no C(32) C(33) H(17) 110.9(3) 1_555 1_555 1_555 no H(15) C(33) H(16) 108.1(4) 1_555 1_555 1_555 no H(15) C(33) H(17) 106.9(3) 1_555 1_555 1_555 no H(16) C(33) H(17) 108.5(3) 1_555 1_555 1_555 no C(32) C(34) H(18) 112.3(3) 1_555 1_555 1_555 no C(32) C(34) H(19) 110.7(3) 1_555 1_555 1_555 no C(32) C(34) H(20) 111.1(4) 1_555 1_555 1_555 no H(18) C(34) H(19) 107.9(4) 1_555 1_555 1_555 no H(18) C(34) H(20) 108.1(3) 1_555 1_555 1_555 no H(19) C(34) H(20) 106.6(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(9) C(13) 3.564(2) 1_555 3_656 ? S(14) S(14) 3.551(1) 1_555 3_666 ? O(29) O(30) 2.768(2) 1_555 2_555 ? O(29) C(34) 3.419(4) 1_555 1_565 ? O(29) C(21) 3.524(2) 1_555 2_555 ? O(29) C(20) 3.587(3) 1_555 2_555 ? O(30) O(31) 2.648(2) 1_555 1_555 ? O(30) C(32) 3.426(3) 1_555 1_555 ? O(30) C(34) 3.476(4) 1_555 1_555 ? O(30) C(3) 3.588(3) 1_555 2_545 ? O(30) C(2) 3.591(3) 1_555 2_545 ? O(31) C(12) 3.435(3) 1_555 3_656 ? O(31) C(21) 3.489(3) 1_555 1_555 ? O(31) C(22) 3.517(3) 1_555 1_555 ? C(6) C(32) 3.524(4) 1_555 1_555 ? C(7) C(33) 3.455(4) 1_555 2_655 ? C(7) C(33) 3.513(4) 1_555 1_555 ? C(7) C(32) 3.562(4) 1_555 1_555 ? C(8) C(33) 3.594(4) 1_555 2_655 ? C(11) C(26) 3.559(3) 1_555 3_656 ? C(11) C(25) 3.568(3) 1_555 3_656 ? C(19) C(21) 3.549(3) 1_555 3_556 ? #------------------------------------------------------------------------------