Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_general _database_code_CSD 116636 _journal_coden_Cambridge 188 loop_ _publ_author_name 'Inoue, Megumi' 'Moriguchi, Tetsuji' 'Sakata, Kazunori' 'Simmyozu, Teruo' 'Tsuge, Akihiko' 'Yasutake, Miko' _publ_contact_author_name ' Dr. Tetsuji Moriguchi' _publ_contact_author_address ; Department of Applied Chemistry, Faculty of Engeneering, Kyushu Institute of Technology, 1-1 Sensui-cho, Tobata-ku, Kitakyushu 804-8550, JAPAN ; _publ_contact_author_email ' moriguch@che.kyutech.ac.jp ' _publ_contact_author_fax ' +81-93-884-3300 ' _publ_contact_author_phone ' +81-93-884-3330 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Perkin Transactions 2 ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; Preparation and Structural Properties of Dithia[3.3.1]metacylophanes ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; data_Nitrodithia[1.3.3]MCPLowTemp #--------------------------------------------------------------------- _audit_creation_date 'Mon Mar 15 02:49:46 1999' _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 579.81 _chemical_formula_analytical 'C33 H41 N O4 S2 ' _chemical_formula_sum 'C33 H41 N O4 S2 ' _chemical_formula_moiety 'C33 H41 N O4 S2 ' _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------- _cell_length_a 15.169(4) _cell_length_b 12.719(7) _cell_length_c 17.684(3) _cell_angle_alpha 90 _cell_angle_beta 114.97(1) _cell_angle_gamma 90 _cell_volume 3092.6599 _cell_formula_units_Z 4 _cell_measurement_temperature 103.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #--------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 'yellow' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240.00 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #--------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 103.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_measurement_method 'Imaging Plate' _diffrn_detector_area_resol_mean 0.010000 _diffrn_reflns_number 6686 _reflns_number_total 6686 _reflns_number_gt 6076 _reflns_threshold_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.011 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 55.10 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 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_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 S(1) S 0.79820(5) 0.11914(6) -0.12469(4) 0.0184(2) Uani 1.00 d . . . S(2) S 0.71014(6) -0.23804(6) 0.22102(5) 0.0206(2) Uani 1.00 d . . . O(1) O 0.9332(1) 0.1039(2) 0.1167(1) 0.0186(5) Uani 1.00 d . . . O(2) O 0.9043(1) -0.0246(2) 0.3025(1) 0.0191(5) Uani 1.00 d . . . O(3) O 0.8626(2) -0.2172(2) -0.0085(2) 0.0279(6) Uani 1.00 d . . . O(4) O 0.9429(2) -0.1649(2) 0.1196(2) 0.0374(7) Uani 1.00 d . . . N(1) N 0.8708(2) -0.1646(2) 0.0530(2) 0.0210(6) Uani 1.00 d . . . C(1) C 0.8122(2) -0.0061(2) -0.0726(2) 0.0192(7) Uani 1.00 d . . . C(2) C 0.8846(2) 0.2017(2) -0.0422(2) 0.0199(7) Uani 1.00 d . . . C(3) C 0.8509(2) 0.2438(2) 0.0216(2) 0.0168(7) Uani 1.00 d . . . C(4) C 0.7923(2) 0.3338(2) 0.0032(2) 0.0179(7) Uani 1.00 d . . . C(5) C 0.7650(2) 0.3798(2) 0.0620(2) 0.0161(6) Uani 1.00 d . . . C(6) C 0.7977(2) 0.3331(2) 0.1408(2) 0.0166(7) Uani 1.00 d . . . C(7) C 0.8527(2) 0.2394(2) 0.1607(2) 0.0148(6) Uani 1.00 d . . . C(8) C 0.8797(2) 0.1972(2) 0.1005(2) 0.0159(6) Uani 1.00 d . . . C(9) C 0.7016(2) 0.4790(2) 0.0401(2) 0.0187(7) Uani 1.00 d . . . C(10) C 0.7546(3) 0.5685(2) 0.0167(2) 0.0252(8) Uani 1.00 d . . . C(11) C 0.6054(2) 0.4557(3) -0.0351(2) 0.0270(8) Uani 1.00 d . . . C(12) C 0.6793(2) 0.5173(3) 0.1129(2) 0.0242(8) Uani 1.00 d . . . C(13) C 1.0362(2) 0.1203(3) 0.1626(2) 0.0257(8) Uani 1.00 d . . . C(14) C 0.8800(2) 0.1890(2) 0.2451(2) 0.0163(6) Uani 1.00 d . . . C(15) C 0.7982(2) 0.1265(2) 0.2530(2) 0.0140(6) Uani 1.00 d . . . C(16) C 0.7063(2) 0.1695(2) 0.2324(2) 0.0156(6) Uani 1.00 d . . . C(17) C 0.6306(2) 0.1134(2) 0.2398(2) 0.0158(6) Uani 1.00 d . . . C(18) C 0.6497(2) 0.0104(2) 0.2692(2) 0.0165(6) Uani 1.00 d . . . C(19) C 0.7409(2) -0.0363(2) 0.2902(2) 0.0151(6) Uani 1.00 d . . . C(20) C 0.8148(2) 0.0231(2) 0.2836(2) 0.0149(6) Uani 1.00 d . . . C(21) C 0.5318(2) 0.1667(2) 0.2172(2) 0.0186(7) Uani 1.00 d . . . C(22) C 0.4910(2) 0.2074(3) 0.1264(2) 0.0254(8) Uani 1.00 d . . . C(23) C 0.5451(2) 0.2606(3) 0.2766(2) 0.0256(8) Uani 1.00 d . . . C(24) C 0.4564(2) 0.0909(2) 0.2240(2) 0.0219(7) Uani 1.00 d . . . C(25) C 0.9714(2) -0.0106(3) 0.3886(2) 0.0279(8) Uani 1.00 d . . . C(26) C 0.7557(2) -0.1518(2) 0.3126(2) 0.0187(7) Uani 1.00 d . . . C(27) C 0.7849(2) -0.1994(2) 0.1680(2) 0.0197(7) Uani 1.00 d . . . C(28) C 0.7436(2) -0.1173(2) 0.0993(2) 0.0163(6) Uani 1.00 d . . . C(29) C 0.6626(2) -0.0561(2) 0.0870(2) 0.0197(7) Uani 1.00 d . . . C(30) C 0.6331(2) 0.0246(2) 0.0277(2) 0.0202(7) Uani 1.00 d . . . C(31) C 0.6817(2) 0.0431(2) -0.0228(2) 0.0177(7) Uani 1.00 d . . . C(32) C 0.7595(2) -0.0195(2) -0.0163(2) 0.0167(6) Uani 1.00 d . . . C(33) C 0.7875(2) -0.0979(2) 0.0448(2) 0.0161(6) Uani 1.00 d . . . H(1) H 0.889(3) -0.027(3) -0.037(2) 0.028(10) Uiso 1.00 calc . . . H(2) H 0.786(2) -0.057(3) -0.118(2) 0.017(8) Uiso 1.00 calc . . . H(3) H 0.944(3) 0.151(3) -0.016(2) 0.025(9) Uiso 1.00 calc . . . H(4) H 0.895(3) 0.256(3) -0.080(2) 0.03(1) Uiso 1.00 calc . . . H(5) H 0.772(2) 0.361(3) -0.052(2) 0.015(8) Uiso 1.00 calc . . . H(6) H 0.786(3) 0.372(4) 0.192(3) 0.05(1) Uiso 1.00 calc . . . H(7) H 0.819(2) 0.584(3) 0.064(2) 0.014(8) Uiso 1.00 calc . . . H(8) H 0.767(3) 0.543(4) -0.035(3) 0.05(1) Uiso 1.00 calc . . . H(9) H 0.710(3) 0.636(4) 0.002(3) 0.05(1) Uiso 1.00 calc . . . H(10) H 0.566(3) 0.519(4) -0.051(3) 0.05(1) Uiso 1.00 calc . . . H(11) H 0.573(3) 0.406(3) -0.018(3) 0.04(1) Uiso 1.00 calc . . . H(12) H 0.619(3) 0.431(3) -0.094(3) 0.04(1) Uiso 1.00 calc . . . H(13) H 0.633(3) 0.585(3) 0.094(3) 0.04(1) Uiso 1.00 calc . . . H(14) H 0.744(2) 0.538(3) 0.174(2) 0.020(9) Uiso 1.00 calc . . . H(15) H 0.646(2) 0.461(3) 0.136(2) 0.019(9) Uiso 1.00 calc . . . H(16) H 1.050(3) 0.157(3) 0.217(3) 0.03(1) Uiso 1.00 calc . . . H(17) H 1.065(4) 0.050(5) 0.173(4) 0.08(2) Uiso 1.00 calc . . . H(18) H 1.064(3) 0.167(3) 0.122(3) 0.04(1) Uiso 1.00 calc . . . H(19) H 0.901(3) 0.249(3) 0.288(2) 0.028(10) Uiso 1.00 calc . . . H(20) H 0.931(2) 0.145(2) 0.258(2) 0.009(7) Uiso 1.00 calc . . . H(21) H 0.697(3) 0.244(3) 0.213(2) 0.03(1) Uiso 1.00 calc . . . H(22) H 0.598(3) -0.036(4) 0.283(3) 0.05(1) Uiso 1.00 calc . . . H(23) H 0.436(4) 0.247(4) 0.122(3) 0.06(1) Uiso 1.00 calc . . . H(24) H 0.482(3) 0.153(4) 0.090(3) 0.05(1) Uiso 1.00 calc . . . H(25) H 0.537(3) 0.251(3) 0.120(2) 0.018(8) Uiso 1.00 calc . . . H(26) H 0.587(3) 0.322(3) 0.272(3) 0.04(1) Uiso 1.00 calc . . . H(27) H 0.577(3) 0.235(3) 0.342(2) 0.020(9) Uiso 1.00 calc . . . H(28) H 0.485(3) 0.290(3) 0.270(3) 0.04(1) Uiso 1.00 calc . . . H(29) H 0.395(3) 0.127(3) 0.205(2) 0.025(9) Uiso 1.00 calc . . . H(30) H 0.446(3) 0.024(3) 0.185(2) 0.021(9) Uiso 1.00 calc . . . H(31) H 0.478(3) 0.064(3) 0.288(2) 0.025(9) Uiso 1.00 calc . . . H(32) H 0.988(3) 0.063(3) 0.407(2) 0.029(10) Uiso 1.00 calc . . . H(33) H 0.941(3) -0.037(3) 0.422(2) 0.027(10) Uiso 1.00 calc . . . H(34) H 1.030(4) -0.046(4) 0.401(3) 0.05(1) Uiso 1.00 calc . . . H(35) H 0.717(3) -0.170(3) 0.348(3) 0.03(1) Uiso 1.00 calc . . . H(36) H 0.828(2) -0.161(3) 0.353(2) 0.015(8) Uiso 1.00 calc . . . H(37) H 0.845(3) -0.173(3) 0.208(2) 0.027(10) Uiso 1.00 calc . . . H(38) H 0.792(3) -0.271(3) 0.141(3) 0.04(1) Uiso 1.00 calc . . . H(39) H 0.631(3) -0.065(3) 0.124(2) 0.022(9) Uiso 1.00 calc . . . H(40) H 0.578(3) 0.071(3) 0.016(2) 0.021(9) Uiso 1.00 calc . . . H(41) H 0.660(3) 0.100(3) -0.066(2) 0.025(9) Uiso 1.00 calc . . . 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(1) 0.0226(3) 0.0176(3) 0.0161(3) 0.0016(3) 0.0092(3) 0.0010(3) S(2) 0.0279(4) 0.0153(3) 0.0252(4) -0.0033(3) 0.0175(3) -0.0025(3) O(1) 0.0154(9) 0.0158(10) 0.024(1) 0.0027(8) 0.0081(8) -0.0019(8) O(2) 0.0140(9) 0.021(1) 0.021(1) 0.0036(8) 0.0061(8) 0.0018(8) O(3) 0.034(1) 0.021(1) 0.038(1) 0.0011(10) 0.023(1) -0.0055(10) O(4) 0.025(1) 0.058(2) 0.029(1) 0.018(1) 0.011(1) 0.011(1) N(1) 0.022(1) 0.020(1) 0.026(1) 0.004(1) 0.014(1) 0.005(1) C(1) 0.022(1) 0.017(1) 0.023(1) 0.002(1) 0.014(1) 0.000(1) C(2) 0.023(1) 0.019(1) 0.023(1) -0.003(1) 0.015(1) -0.004(1) C(3) 0.017(1) 0.018(1) 0.018(1) -0.004(1) 0.010(1) -0.005(1) C(4) 0.020(1) 0.017(1) 0.019(1) -0.002(1) 0.010(1) 0.000(1) C(5) 0.015(1) 0.016(1) 0.018(1) -0.002(1) 0.008(1) -0.002(1) C(6) 0.017(1) 0.016(1) 0.019(1) -0.002(1) 0.009(1) -0.003(1) C(7) 0.012(1) 0.015(1) 0.017(1) -0.0026(10) 0.006(1) -0.002(1) C(8) 0.015(1) 0.013(1) 0.021(1) 0.000(1) 0.008(1) -0.001(1) C(9) 0.020(1) 0.016(1) 0.020(1) 0.001(1) 0.009(1) 0.000(1) C(10) 0.030(2) 0.017(1) 0.033(2) 0.003(1) 0.018(1) 0.005(1) C(11) 0.022(2) 0.026(2) 0.029(2) 0.005(1) 0.007(1) 0.000(1) C(12) 0.029(2) 0.021(1) 0.027(2) 0.005(1) 0.016(1) 0.000(1) C(13) 0.017(1) 0.030(2) 0.030(2) 0.004(1) 0.010(1) 0.000(1) C(14) 0.013(1) 0.018(1) 0.017(1) -0.001(1) 0.006(1) 0.000(1) C(15) 0.014(1) 0.015(1) 0.012(1) -0.002(1) 0.0052(10) -0.002(1) C(16) 0.015(1) 0.013(1) 0.019(1) 0.000(1) 0.007(1) -0.002(1) C(17) 0.016(1) 0.015(1) 0.016(1) 0.000(1) 0.007(1) -0.002(1) C(18) 0.018(1) 0.016(1) 0.016(1) -0.003(1) 0.009(1) -0.002(1) C(19) 0.018(1) 0.013(1) 0.015(1) -0.002(1) 0.009(1) -0.002(1) C(20) 0.013(1) 0.016(1) 0.015(1) 0.002(1) 0.006(1) 0.000(1) C(21) 0.014(1) 0.019(1) 0.023(1) 0.000(1) 0.008(1) -0.003(1) C(22) 0.018(1) 0.027(2) 0.029(2) 0.006(1) 0.007(1) 0.006(1) C(23) 0.018(1) 0.018(1) 0.042(2) 0.001(1) 0.014(1) -0.009(1) C(24) 0.015(1) 0.022(1) 0.028(2) -0.002(1) 0.009(1) -0.004(1) C(25) 0.016(1) 0.033(2) 0.024(2) 0.001(1) -0.001(1) 0.003(1) C(26) 0.026(1) 0.015(1) 0.020(1) 0.002(1) 0.013(1) 0.001(1) C(27) 0.023(1) 0.019(1) 0.021(1) 0.001(1) 0.014(1) 0.000(1) C(28) 0.017(1) 0.016(1) 0.015(1) -0.004(1) 0.006(1) -0.003(1) C(29) 0.019(1) 0.024(1) 0.018(1) -0.001(1) 0.010(1) -0.003(1) C(30) 0.017(1) 0.024(1) 0.018(1) 0.004(1) 0.006(1) -0.003(1) C(31) 0.016(1) 0.020(1) 0.016(1) 0.002(1) 0.005(1) 0.000(1) C(32) 0.017(1) 0.017(1) 0.018(1) -0.004(1) 0.008(1) -0.003(1) C(33) 0.015(1) 0.016(1) 0.018(1) -0.002(1) 0.009(1) -0.003(1) #--------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6076 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.674 _refine_ls_shift/su_max 0.1270 _refine_ls_shift/su_mean 0.0070 _refine_diff_density_min -0.46 _refine_diff_density_max 0.43 #--------------------------------------------------------------------- _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(1) C(1) 1.808(3) 1_555 1_555 yes S(1) C(2) 1.826(3) 1_555 1_555 yes S(2) C(26) 1.833(3) 1_555 1_555 yes S(2) C(27) 1.818(3) 1_555 1_555 yes O(1) C(8) 1.397(3) 1_555 1_555 yes O(1) C(13) 1.441(4) 1_555 1_555 yes O(2) C(20) 1.393(3) 1_555 1_555 yes O(2) C(25) 1.440(4) 1_555 1_555 yes O(3) N(1) 1.238(3) 1_555 1_555 yes O(4) N(1) 1.223(4) 1_555 1_555 yes N(1) C(33) 1.478(4) 1_555 1_555 yes C(1) C(32) 1.527(4) 1_555 1_555 yes C(2) C(3) 1.520(4) 1_555 1_555 yes C(3) C(4) 1.401(4) 1_555 1_555 yes C(3) C(8) 1.405(4) 1_555 1_555 yes C(4) C(5) 1.399(4) 1_555 1_555 yes C(5) C(6) 1.398(4) 1_555 1_555 yes C(5) C(9) 1.534(4) 1_555 1_555 yes C(6) C(7) 1.412(4) 1_555 1_555 yes C(7) C(8) 1.399(4) 1_555 1_555 yes C(7) C(14) 1.513(4) 1_555 1_555 yes C(9) C(10) 1.546(4) 1_555 1_555 yes C(9) C(11) 1.533(4) 1_555 1_555 yes C(9) C(12) 1.542(4) 1_555 1_555 yes C(14) C(15) 1.529(4) 1_555 1_555 yes C(15) C(16) 1.395(4) 1_555 1_555 yes C(15) C(20) 1.405(4) 1_555 1_555 yes C(16) C(17) 1.404(4) 1_555 1_555 yes C(17) C(18) 1.394(4) 1_555 1_555 yes C(17) C(21) 1.536(4) 1_555 1_555 yes C(18) C(19) 1.404(4) 1_555 1_555 yes C(19) C(20) 1.397(4) 1_555 1_555 yes C(19) C(26) 1.513(4) 1_555 1_555 yes C(21) C(22) 1.545(4) 1_555 1_555 yes C(21) C(23) 1.547(4) 1_555 1_555 yes C(21) C(24) 1.538(4) 1_555 1_555 yes C(27) C(28) 1.522(4) 1_555 1_555 yes C(28) C(29) 1.391(4) 1_555 1_555 yes C(28) C(33) 1.405(4) 1_555 1_555 yes C(29) C(30) 1.400(4) 1_555 1_555 yes C(30) C(31) 1.397(4) 1_555 1_555 yes C(31) C(32) 1.388(4) 1_555 1_555 yes C(32) C(33) 1.397(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(1) S(1) C(2) 102.1(1) 1_555 1_555 1_555 yes C(26) S(2) C(27) 102.1(1) 1_555 1_555 1_555 yes C(8) O(1) C(13) 112.9(2) 1_555 1_555 1_555 yes C(20) O(2) C(25) 112.5(2) 1_555 1_555 1_555 yes O(3) N(1) O(4) 124.2(3) 1_555 1_555 1_555 yes O(3) N(1) C(33) 117.4(3) 1_555 1_555 1_555 yes O(4) N(1) C(33) 118.4(3) 1_555 1_555 1_555 yes S(1) C(1) C(32) 116.7(2) 1_555 1_555 1_555 yes S(1) C(1) H(1) 111(1) 1_555 1_555 1_555 no S(1) C(1) H(2) 103(2) 1_555 1_555 1_555 no C(32) C(1) H(1) 108(1) 1_555 1_555 1_555 no C(32) C(1) H(2) 109(1) 1_555 1_555 1_555 no H(1) C(1) H(2) 105(2) 1_555 1_555 1_555 no S(1) C(2) C(3) 116.2(2) 1_555 1_555 1_555 yes S(1) C(2) H(3) 101(2) 1_555 1_555 1_555 no S(1) C(2) H(4) 97(2) 1_555 1_555 1_555 no C(3) C(2) H(3) 112(2) 1_555 1_555 1_555 no C(3) C(2) H(4) 116(2) 1_555 1_555 1_555 no H(3) C(2) H(4) 111(2) 1_555 1_555 1_555 no C(2) C(3) C(4) 119.6(3) 1_555 1_555 1_555 yes C(2) C(3) C(8) 121.9(3) 1_555 1_555 1_555 yes C(4) C(3) C(8) 118.5(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 121.8(3) 1_555 1_555 1_555 yes C(3) C(4) H(5) 115(1) 1_555 1_555 1_555 no C(5) C(4) H(5) 122(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 118.1(3) 1_555 1_555 1_555 yes C(4) C(5) C(9) 120.5(3) 1_555 1_555 1_555 yes C(6) C(5) C(9) 121.5(2) 1_555 1_555 1_555 yes C(5) C(6) C(7) 122.1(3) 1_555 1_555 1_555 yes C(5) C(6) H(6) 120(2) 1_555 1_555 1_555 no C(7) C(6) H(6) 116(2) 1_555 1_555 1_555 no C(6) C(7) C(8) 117.8(3) 1_555 1_555 1_555 yes C(6) C(7) C(14) 119.4(2) 1_555 1_555 1_555 yes C(8) C(7) C(14) 122.9(2) 1_555 1_555 1_555 yes O(1) C(8) C(3) 118.2(2) 1_555 1_555 1_555 yes O(1) C(8) C(7) 120.1(2) 1_555 1_555 1_555 yes C(3) C(8) C(7) 121.7(3) 1_555 1_555 1_555 yes C(5) C(9) C(10) 109.4(2) 1_555 1_555 1_555 yes C(5) C(9) C(11) 109.0(2) 1_555 1_555 1_555 yes C(5) C(9) C(12) 112.6(2) 1_555 1_555 1_555 yes C(10) C(9) C(11) 108.8(3) 1_555 1_555 1_555 yes C(10) C(9) C(12) 108.2(2) 1_555 1_555 1_555 yes C(11) C(9) C(12) 108.8(3) 1_555 1_555 1_555 yes C(9) C(10) H(7) 110(1) 1_555 1_555 1_555 no C(9) C(10) H(8) 108(2) 1_555 1_555 1_555 no C(9) C(10) H(9) 107(2) 1_555 1_555 1_555 no H(7) C(10) H(8) 107(3) 1_555 1_555 1_555 no H(7) C(10) H(9) 110(3) 1_555 1_555 1_555 no H(8) C(10) H(9) 111(3) 1_555 1_555 1_555 no C(9) C(11) H(10) 109(2) 1_555 1_555 1_555 no C(9) C(11) H(11) 106(2) 1_555 1_555 1_555 no C(9) C(11) H(12) 110(2) 1_555 1_555 1_555 no H(10) C(11) H(11) 108(3) 1_555 1_555 1_555 no H(10) C(11) H(12) 106(3) 1_555 1_555 1_555 no H(11) C(11) H(12) 115(3) 1_555 1_555 1_555 no C(9) C(12) H(13) 110(2) 1_555 1_555 1_555 no C(9) C(12) H(14) 117(1) 1_555 1_555 1_555 no C(9) C(12) H(15) 114(1) 1_555 1_555 1_555 no H(13) C(12) H(14) 107(2) 1_555 1_555 1_555 no H(13) C(12) H(15) 107(2) 1_555 1_555 1_555 no H(14) C(12) H(15) 98(2) 1_555 1_555 1_555 no O(1) C(13) H(16) 110(2) 1_555 1_555 1_555 no O(1) C(13) H(17) 104(3) 1_555 1_555 1_555 no O(1) C(13) H(18) 109(2) 1_555 1_555 1_555 no H(16) C(13) H(17) 110(3) 1_555 1_555 1_555 no H(16) C(13) H(18) 112(3) 1_555 1_555 1_555 no H(17) C(13) H(18) 109(3) 1_555 1_555 1_555 no C(7) C(14) C(15) 114.6(2) 1_555 1_555 1_555 yes C(7) C(14) H(19) 106(2) 1_555 1_555 1_555 no C(7) C(14) H(20) 110(1) 1_555 1_555 1_555 no C(15) C(14) H(19) 109(2) 1_555 1_555 1_555 no C(15) C(14) H(20) 107(1) 1_555 1_555 1_555 no H(19) C(14) H(20) 108(2) 1_555 1_555 1_555 no C(14) C(15) C(16) 122.2(2) 1_555 1_555 1_555 yes C(14) C(15) C(20) 120.1(2) 1_555 1_555 1_555 yes C(16) C(15) C(20) 117.7(2) 1_555 1_555 1_555 yes C(15) C(16) C(17) 122.9(3) 1_555 1_555 1_555 yes C(15) C(16) H(21) 116(2) 1_555 1_555 1_555 no C(17) C(16) H(21) 120(2) 1_555 1_555 1_555 no C(16) C(17) C(18) 117.6(3) 1_555 1_555 1_555 yes C(16) C(17) C(21) 119.9(2) 1_555 1_555 1_555 yes C(18) C(17) C(21) 122.5(3) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.5(3) 1_555 1_555 1_555 yes C(17) C(18) H(22) 122(2) 1_555 1_555 1_555 no C(19) C(18) H(22) 115(2) 1_555 1_555 1_555 no C(18) C(19) C(20) 119.0(3) 1_555 1_555 1_555 yes C(18) C(19) C(26) 120.1(3) 1_555 1_555 1_555 yes C(20) C(19) C(26) 120.7(2) 1_555 1_555 1_555 yes O(2) C(20) C(15) 119.9(2) 1_555 1_555 1_555 yes O(2) C(20) C(19) 118.7(2) 1_555 1_555 1_555 yes C(15) C(20) C(19) 121.2(2) 1_555 1_555 1_555 yes C(17) C(21) C(22) 109.7(2) 1_555 1_555 1_555 yes C(17) C(21) C(23) 109.3(2) 1_555 1_555 1_555 yes C(17) C(21) C(24) 112.3(2) 1_555 1_555 1_555 yes C(22) C(21) C(23) 109.1(3) 1_555 1_555 1_555 yes C(22) C(21) C(24) 107.8(2) 1_555 1_555 1_555 yes C(23) C(21) C(24) 108.6(2) 1_555 1_555 1_555 yes C(21) C(22) H(23) 102(2) 1_555 1_555 1_555 no C(21) C(22) H(24) 110(2) 1_555 1_555 1_555 no C(21) C(22) H(25) 109(2) 1_555 1_555 1_555 no H(23) C(22) H(24) 118(4) 1_555 1_555 1_555 no H(23) C(22) H(25) 111(3) 1_555 1_555 1_555 no H(24) C(22) H(25) 104(3) 1_555 1_555 1_555 no C(21) C(23) H(26) 116(2) 1_555 1_555 1_555 no C(21) C(23) H(27) 111(1) 1_555 1_555 1_555 no C(21) C(23) H(28) 112(2) 1_555 1_555 1_555 no H(26) C(23) H(27) 107(2) 1_555 1_555 1_555 no H(26) C(23) H(28) 106(3) 1_555 1_555 1_555 no H(27) C(23) H(28) 102(3) 1_555 1_555 1_555 no C(21) C(24) H(29) 108(2) 1_555 1_555 1_555 no C(21) C(24) H(30) 110(1) 1_555 1_555 1_555 no C(21) C(24) H(31) 111(1) 1_555 1_555 1_555 no H(29) C(24) H(30) 107(2) 1_555 1_555 1_555 no H(29) C(24) H(31) 108(2) 1_555 1_555 1_555 no H(30) C(24) H(31) 108(2) 1_555 1_555 1_555 no O(2) C(25) H(32) 115(2) 1_555 1_555 1_555 no O(2) C(25) H(33) 107(2) 1_555 1_555 1_555 no O(2) C(25) H(34) 111(2) 1_555 1_555 1_555 no H(32) C(25) H(33) 103(3) 1_555 1_555 1_555 no H(32) C(25) H(34) 107(3) 1_555 1_555 1_555 no H(33) C(25) H(34) 109(3) 1_555 1_555 1_555 no S(2) C(26) C(19) 113.0(2) 1_555 1_555 1_555 yes S(2) C(26) H(35) 107(2) 1_555 1_555 1_555 no S(2) C(26) H(36) 115(1) 1_555 1_555 1_555 no C(19) C(26) H(35) 108(2) 1_555 1_555 1_555 no C(19) C(26) H(36) 106(1) 1_555 1_555 1_555 no H(35) C(26) H(36) 105(2) 1_555 1_555 1_555 no S(2) C(27) C(28) 117.5(2) 1_555 1_555 1_555 yes S(2) C(27) H(37) 108(2) 1_555 1_555 1_555 no S(2) C(27) H(38) 101(2) 1_555 1_555 1_555 no C(28) C(27) H(37) 107(2) 1_555 1_555 1_555 no C(28) C(27) H(38) 108(2) 1_555 1_555 1_555 no H(37) C(27) H(38) 113(3) 1_555 1_555 1_555 no C(27) C(28) C(29) 123.1(3) 1_555 1_555 1_555 yes C(27) C(28) C(33) 120.9(2) 1_555 1_555 1_555 yes C(29) C(28) C(33) 116.0(3) 1_555 1_555 1_555 yes C(28) C(29) C(30) 120.6(3) 1_555 1_555 1_555 yes C(28) C(29) H(39) 119(2) 1_555 1_555 1_555 no C(30) C(29) H(39) 119(2) 1_555 1_555 1_555 no C(29) C(30) C(31) 121.0(3) 1_555 1_555 1_555 yes C(29) C(30) H(40) 125(2) 1_555 1_555 1_555 no C(31) C(30) H(40) 113(2) 1_555 1_555 1_555 no C(30) C(31) C(32) 120.7(3) 1_555 1_555 1_555 yes C(30) C(31) H(41) 121(2) 1_555 1_555 1_555 no C(32) C(31) H(41) 117(2) 1_555 1_555 1_555 no C(1) C(32) C(31) 122.9(3) 1_555 1_555 1_555 yes C(1) C(32) C(33) 120.8(2) 1_555 1_555 1_555 yes C(31) C(32) C(33) 116.3(3) 1_555 1_555 1_555 yes N(1) C(33) C(28) 117.7(2) 1_555 1_555 1_555 yes N(1) C(33) C(32) 117.0(2) 1_555 1_555 1_555 yes C(28) C(33) C(32) 125.3(3) 1_555 1_555 1_555 yes #--------------------------------------------------------------------- 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 S(1) C(1) C(32) C(31) 20.1(4) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(32) C(33) -160.8(2) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) C(4) -82.3(3) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) C(8) 100.2(3) 1_555 1_555 1_555 1_555 yes S(2) C(26) C(19) C(18) 80.0(3) 1_555 1_555 1_555 1_555 yes S(2) C(26) C(19) C(20) -94.8(3) 1_555 1_555 1_555 1_555 yes S(2) C(27) C(28) C(29) 13.5(4) 1_555 1_555 1_555 1_555 yes S(2) C(27) C(28) C(33) -167.7(2) 1_555 1_555 1_555 1_555 yes O(1) C(8) C(3) C(2) -6.2(4) 1_555 1_555 1_555 1_555 yes O(1) C(8) C(3) C(4) 176.2(2) 1_555 1_555 1_555 1_555 yes O(1) C(8) C(7) C(6) -179.2(2) 1_555 1_555 1_555 1_555 yes O(1) C(8) C(7) C(14) 0.8(4) 1_555 1_555 1_555 1_555 yes O(2) C(20) C(15) C(14) -3.5(4) 1_555 1_555 1_555 1_555 yes O(2) C(20) C(15) C(16) 177.9(2) 1_555 1_555 1_555 1_555 yes O(2) C(20) C(19) C(18) -178.3(2) 1_555 1_555 1_555 1_555 yes O(2) C(20) C(19) C(26) -3.4(4) 1_555 1_555 1_555 1_555 yes O(3) N(1) C(33) C(28) 120.0(3) 1_555 1_555 1_555 1_555 yes O(3) N(1) C(33) C(32) -60.6(3) 1_555 1_555 1_555 1_555 yes O(4) N(1) C(33) C(28) -59.8(4) 1_555 1_555 1_555 1_555 yes O(4) N(1) C(33) C(32) 119.5(3) 1_555 1_555 1_555 1_555 yes N(1) C(33) C(28) C(27) 4.0(4) 1_555 1_555 1_555 1_555 yes N(1) C(33) C(28) C(29) -177.1(3) 1_555 1_555 1_555 1_555 yes N(1) C(33) C(32) C(1) 1.2(4) 1_555 1_555 1_555 1_555 yes N(1) C(33) C(32) C(31) -179.6(2) 1_555 1_555 1_555 1_555 yes C(1) S(1) C(2) C(3) -79.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(32) C(31) C(30) 177.1(3) 1_555 1_555 1_555 1_555 yes C(1) C(32) C(33) C(28) -179.5(3) 1_555 1_555 1_555 1_555 yes C(2) S(1) C(1) C(32) 79.8(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -175.4(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(7) 176.5(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -0.2(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(9) 179.4(3) 1_555 1_555 1_555 1_555 yes C(3) C(8) O(1) C(13) 98.7(3) 1_555 1_555 1_555 1_555 yes C(3) C(8) C(7) C(6) -2.1(4) 1_555 1_555 1_555 1_555 yes C(3) C(8) C(7) C(14) 178.0(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(7) -1.0(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -3.1(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(9) C(10) -59.7(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(9) C(11) 59.1(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(9) C(12) 179.9(3) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(8) 2.2(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 4.2(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(14) -175.9(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(9) C(10) 119.8(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(9) C(11) -121.4(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(9) C(12) -0.6(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(14) C(15) 78.5(3) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(9) 177.3(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) O(1) C(13) -84.0(3) 1_555 1_555 1_555 1_555 yes C(7) C(14) C(15) C(16) -52.2(4) 1_555 1_555 1_555 1_555 yes C(7) C(14) C(15) C(20) 129.3(3) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(14) C(15) -101.6(3) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) -179.5(3) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(20) C(19) -179.0(2) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -0.1(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(21) 179.0(3) 1_555 1_555 1_555 1_555 yes C(15) C(20) O(2) C(25) 92.4(3) 1_555 1_555 1_555 1_555 yes C(15) C(20) C(19) C(18) -2.8(4) 1_555 1_555 1_555 1_555 yes C(15) C(20) C(19) C(26) 172.1(3) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(20) C(19) 2.4(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) -0.3(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(21) C(22) 56.5(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(21) C(23) -63.1(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(21) C(24) 176.3(3) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(20) -1.0(4) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 1.7(4) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(26) -173.2(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(21) C(22) -124.5(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(21) C(23) 115.9(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(21) C(24) -4.6(4) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(17) C(21) -179.4(3) 1_555 1_555 1_555 1_555 yes C(19) C(20) O(2) C(25) -92.1(3) 1_555 1_555 1_555 1_555 yes C(19) C(26) S(2) C(27) 61.9(2) 1_555 1_555 1_555 1_555 yes C(26) S(2) C(27) C(28) -94.8(2) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 174.2(3) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(32) -175.3(3) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 2.5(5) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(31) -0.3(4) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(32) 3.6(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 1.1(4) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) -4.6(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -2.1(4) 1_555 1_555 1_555 1_555 yes #-------------------------------------------------------------------- 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(1) C(16) 3.547(3) 1_555 4_554 ? S(2) C(12) 3.577(3) 1_555 1_545 ? O(3) C(10) 3.306(4) 1_555 1_545 ? O(3) C(26) 3.328(4) 1_555 4_544 ? O(3) C(2) 3.556(4) 1_555 3_755 ? O(4) C(14) 3.312(4) 1_555 2_745 ? O(4) C(2) 3.459(4) 1_555 3_755 ? #--------------------------------------------------------------------- data_outerNO2[3.3.1]MCP _database_code_CSD 165145 #----------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C33 H41 N O4 S2 ' _chemical_formula_moiety 'C33 H41 N O4 S2 ' _chemical_formula_weight 579.81 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 _cell_length_a 12.9636(5) _cell_length_b 12.7351(4) _cell_length_c 19.3901(7) _cell_angle_alpha 90 _cell_angle_beta 104.0528(8) _cell_angle_gamma 90 _cell_volume 3105.4(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 32666 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #----------------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27065 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9968 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7112 _reflns_number_gt 4629 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0401 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4629 _refine_ls_number_parameters 361 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.30 _refine_diff_density_min -0.24 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 S(1) S 1.03148(4) -0.06909(4) 0.31903(2) 0.0202(1) Uani 1.00 d . . . S(2) S 0.48956(4) 0.05365(3) 0.09893(2) 0.0203(1) Uani 1.00 d . . . O(1) O 0.61148(9) -0.16158(9) 0.24741(6) 0.0180(3) Uani 1.00 d . . . O(2) O 0.84759(9) -0.32293(9) 0.31893(6) 0.0164(3) Uani 1.00 d . . . O(3) O 0.80497(10) 0.33161(10) 0.35193(7) 0.0215(3) Uani 1.00 d . . . O(4) O 0.7018(1) 0.36723(9) 0.24868(7) 0.0243(3) Uani 1.00 d . . . N(1) N 0.7536(1) 0.3051(1) 0.29236(8) 0.0177(4) Uani 1.00 d . . . C(1) C 0.4601(1) -0.1457(1) 0.14735(9) 0.0151(4) Uani 1.00 d . . . C(2) C 0.3928(1) -0.1927(1) 0.08777(9) 0.0158(4) Uani 1.00 d . . . C(3) C 0.4056(1) -0.2960(1) 0.06869(9) 0.0150(4) Uani 1.00 d . . . C(4) C 0.4915(1) -0.3519(1) 0.11027(9) 0.0154(4) Uani 1.00 d . . . C(5) C 0.5607(1) -0.3090(1) 0.16942(9) 0.0141(4) Uani 1.00 d . . . C(6) C 0.5415(1) -0.2061(1) 0.18863(9) 0.0147(4) Uani 1.00 d . . . C(7) C 0.6606(1) -0.3651(1) 0.20841(9) 0.0168(4) Uani 1.00 d . . . C(8) C 0.7593(1) -0.3138(1) 0.19445(9) 0.0150(4) Uani 1.00 d . . . C(9) C 0.7624(1) -0.2824(1) 0.12599(9) 0.0155(4) Uani 1.00 d . . . C(10) C 0.8501(1) -0.2312(1) 0.11167(9) 0.0162(4) Uani 1.00 d . . . C(11) C 0.9359(1) -0.2100(1) 0.16929(9) 0.0170(4) Uani 1.00 d . . . C(12) C 0.9363(1) -0.2396(1) 0.23845(9) 0.0158(4) Uani 1.00 d . . . C(13) C 0.8480(1) -0.2928(1) 0.24995(9) 0.0148(4) Uani 1.00 d . . . C(14) C 1.0271(1) -0.2095(1) 0.29973(9) 0.0175(4) Uani 1.00 d . . . C(15) C 0.9050(1) -0.0521(1) 0.34397(9) 0.0199(5) Uani 1.00 d . . . C(16) C 0.8317(1) 0.0239(1) 0.29585(9) 0.0174(4) Uani 1.00 d . . . C(17) C 0.8247(1) 0.1271(1) 0.31689(9) 0.0172(4) Uani 1.00 d . . . C(18) C 0.7558(1) 0.1943(1) 0.27165(9) 0.0157(4) Uani 1.00 d . . . C(19) C 0.6917(1) 0.1628(1) 0.20733(9) 0.0165(4) Uani 1.00 d . . . C(20) C 0.6979(1) 0.0590(1) 0.18598(9) 0.0166(4) Uani 1.00 d . . . C(21) C 0.7693(1) -0.0085(1) 0.22969(9) 0.0173(4) Uani 1.00 d . . . C(22) C 0.6291(1) 0.0203(1) 0.11563(9) 0.0191(4) Uani 1.00 d . . . C(23) C 0.4480(1) -0.0311(1) 0.16274(9) 0.0189(4) Uani 1.00 d . . . C(24) C 0.5768(2) -0.1706(2) 0.31197(9) 0.0251(5) Uani 1.00 d . . . C(25) C 0.8829(2) -0.4297(1) 0.33219(10) 0.0259(5) Uani 1.00 d . . . C(26) C 0.3340(1) -0.3470(1) 0.00240(9) 0.0187(4) Uani 1.00 d . . . C(27) C 0.2945(2) -0.4547(2) 0.0210(1) 0.0259(5) Uani 1.00 d . . . C(28) C 0.3997(2) -0.3617(2) -0.05281(10) 0.0260(5) Uani 1.00 d . . . C(29) C 0.2368(2) -0.2794(2) -0.0302(1) 0.0267(5) Uani 1.00 d . . . C(30) C 0.8538(1) -0.1946(1) 0.03696(9) 0.0189(4) Uani 1.00 d . . . C(31) C 0.8662(2) -0.0752(2) 0.0376(1) 0.0330(6) Uani 1.00 d . . . C(32) C 0.7533(2) -0.2243(2) -0.01906(10) 0.0279(5) Uani 1.00 d . . . C(33) C 0.9489(2) -0.2456(2) 0.0160(1) 0.0353(6) Uani 1.00 d . . . H(1) H 0.3351 -0.1524 0.0599 0.0196 Uiso 1.00 calc . . . H(2) H 0.5023 -0.4234 0.0971 0.0189 Uiso 1.00 calc . . . H(3) H 0.6651 -0.3632 0.2588 0.0210 Uiso 1.00 calc . . . H(4) H 0.6578 -0.4366 0.1939 0.0210 Uiso 1.00 calc . . . H(5) H 0.7017 -0.2961 0.0874 0.0180 Uiso 1.00 calc . . . H(6) H 0.9961 -0.1732 0.1609 0.0214 Uiso 1.00 calc . . . H(7) H 1.0928 -0.2299 0.2893 0.0213 Uiso 1.00 calc . . . H(8) H 1.0207 -0.2471 0.3416 0.0213 Uiso 1.00 calc . . . H(9) H 0.8699 -0.1189 0.3423 0.0243 Uiso 1.00 calc . . . H(10) H 0.9183 -0.0266 0.3919 0.0243 Uiso 1.00 calc . . . H(11) H 0.8662 0.1515 0.3615 0.0220 Uiso 1.00 calc . . . H(12) H 0.6446 0.2114 0.1780 0.0198 Uiso 1.00 calc . . . H(13) H 0.7754 -0.0798 0.2146 0.0202 Uiso 1.00 calc . . . H(14) H 0.6358 -0.0545 0.1141 0.0227 Uiso 1.00 calc . .. . H(15) H 0.6570 0.0494 0.0781 0.0227 Uiso 1.00 calc . . . H(16) H 0.4892 -0.0148 0.2096 0.0227 Uiso 1.00 calc . . . H(17) H 0.3745 -0.0165 0.1615 0.0227 Uiso 1.00 calc . . . H(18) H 0.6266 -0.1388 0.3503 0.0312 Uiso 1.00 calc . . . H(19) H 0.5093 -0.1369 0.3065 0.0312 Uiso 1.00 calc . . . H(20) H 0.5691 -0.2430 0.3228 0.0312 Uiso 1.00 calc . . . H(21) H 0.8827 -0.4486 0.3800 0.0320 Uiso 1.00 calc . . . H(22) H 0.8369 -0.4757 0.3004 0.0320 Uiso 1.00 calc . . . H(23) H 0.9533 -0.4369 0.3263 0.0320 Uiso 1.00 calc . . . H(24) H 0.2510 -0.4459 0.0536 0.0337 Uiso 1.00 calc . . . H(25) H 0.2538 -0.4873 -0.0212 0.0337 Uiso 1.00 calc . . . H(26) H 0.3533 -0.4985 0.0417 0.0337 Uiso 1.00 calc . . . H(27) H 0.4607 -0.4039 -0.0339 0.0313 Uiso 1.00 calc . . . H(28) H 0.3580 -0.3935 -0.0944 0.0313 Uiso 1.00 calc . . . H(29) H 0.4236 -0.2943 -0.0652 0.0313 Uiso 1.00 calc . . . H(30) H 0.2584 -0.2120 -0.0424 0.0325 Uiso 1.00 calc . . . H(31) H 0.1959 -0.3124 -0.0728 0.0325 Uiso 1.00 calc . . . H(32) H 0.1929 -0.2718 0.0022 0.0325 Uiso 1.00 calc . . . H(33) H 0.9305 -0.0562 0.0708 0.0395 Uiso 1.00 calc . . . H(34) H 0.8690 -0.0519 -0.0084 0.0395 Uiso 1.00 calc . . . H(35) H 0.8079 -0.0432 0.0509 0.0395 Uiso 1.00 calc . . . H(36) H 0.6913 -0.1929 -0.0083 0.0358 Uiso 1.00 calc . . . H(37) H 0.7570 -0.2017 -0.0651 0.0358 Uiso 1.00 calc . . . H(38) H 0.7429 -0.2991 -0.0202 0.0358 Uiso 1.00 calc . . . H(39) H 0.9406 -0.3220 0.0148 0.0436 Uiso 1.00 calc . . . H(40) H 0.9542 -0.2240 -0.0297 0.0436 Uiso 1.00 calc . . . H(41) H 1.0139 -0.2306 0.0499 0.0436 Uiso 1.00 calc . . . 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(1) 0.0160(2) 0.0222(2) 0.0202(2) -0.0019(2) -0.0002(2) 0.0020(2) S(2) 0.0199(2) 0.0157(2) 0.0209(2) 0.0018(2) -0.0034(2) 0.0017(2) O(1) 0.0156(6) 0.0227(7) 0.0149(6) -0.0044(5) 0.0022(5) -0.0046(5) O(2) 0.0223(7) 0.0163(6) 0.0109(6) 0.0035(5) 0.0044(5) 0.0013(5) O(3) 0.0189(6) 0.0204(7) 0.0241(7) -0.0017(5) 0.0029(5) -0.0052(5) O(4) 0.0254(7) 0.0167(6) 0.0289(7) 0.0035(5) 0.0027(6) 0.0024(6) N(1) 0.0136(7) 0.0168(7) 0.0236(8) -0.0004(6) 0.0062(6) 0.0002(6) C(1) 0.0138(8) 0.0164(8) 0.0166(9) -0.0012(7) 0.0066(7) -0.0026(7) C(2) 0.0125(8) 0.0189(9) 0.0164(8) 0.0015(7) 0.0042(7) 0.0002(7) C(3) 0.0149(8) 0.0158(8) 0.0153(8) -0.0023(7) 0.0055(7) -0.0006(7) C(4) 0.0163(8) 0.0130(8) 0.0181(9) -0.0008(7) 0.0062(7) -0.0002(7) C(5) 0.0138(8) 0.0161(8) 0.0136(8) -0.0011(7) 0.0056(6) 0.0026(7) C(6) 0.0126(8) 0.0189(9) 0.0132(8) -0.0025(7) 0.0045(6) -0.0010(7) C(7) 0.0177(9) 0.0154(8) 0.0171(9) 0.0007(7) 0.0035(7) 0.0022(7) C(8) 0.0153(8) 0.0132(8) 0.0165(8) 0.0032(7) 0.0039(7) 0.0001(7) C(9) 0.0136(8) 0.0178(9) 0.0135(8) 0.0012(7) -0.0001(6) -0.0014(7) C(10) 0.0152(8) 0.0205(9) 0.0125(8) 0.0027(7) 0.0029(7) -0.0006(7) C(11) 0.0125(8) 0.0231(9) 0.0162(9) -0.0002(7) 0.0050(7) -0.0006(7) C(12) 0.0131(8) 0.0196(9) 0.0143(8) 0.0039(7) 0.0023(6) -0.0025(7) C(13) 0.0161(8) 0.0166(8) 0.0118(8) 0.0050(7) 0.0038(6) 0.0002(7) C(14) 0.0130(8) 0.0237(9) 0.0150(8) 0.0034(7) 0.0020(7) -0.0007(7) C(15) 0.0237(9) 0.0194(9) 0.0168(9) 0.0022(8) 0.0055(7) 0.0012(7) C(16) 0.0167(9) 0.0176(9) 0.0191(9) 0.0006(7) 0.0069(7) 0.0032(7) C(17) 0.0155(9) 0.0190(9) 0.0175(9) -0.0027(7) 0.0048(7) 0.0003(7) C(18) 0.0152(8) 0.0115(8) 0.0223(9) -0.0018(7) 0.0081(7) 0.0000(7) C(19) 0.0139(8) 0.0165(9) 0.0195(9) -0.0007(7) 0.0049(7) 0.0045(7) C(20) 0.0143(8) 0.0178(9) 0.0186(9) -0.0027(7) 0.0057(7) 0.0008(7) C(21) 0.0181(9) 0.0147(8) 0.0205(9) -0.0014(7) 0.0072(7) 0.0006(7) C(22) 0.0192(9) 0.0182(9) 0.0196(9) -0.0023(7) 0.0044(7) 0.0010(7) C(23) 0.0156(9) 0.0186(9) 0.0219(9) 0.0014(7) 0.0037(7) -0.0041(7) C(24) 0.025(1) 0.034(1) 0.0139(9) -0.0025(9) 0.0021(7) -0.0031(8) C(25) 0.040(1) 0.0193(9) 0.0174(9) 0.0071(9) 0.0059(8) 0.0035(8) C(26) 0.0209(9) 0.0176(9) 0.0156(9) -0.0010(7) 0.0007(7) -0.0017(7) C(27) 0.028(1) 0.0225(10) 0.0238(10) -0.0079(8) -0.0002(8) -0.0020(8) C(28) 0.034(1) 0.028(1) 0.0154(9) 0.0016(9) 0.0048(8) -0.0022(8) C(29) 0.0229(10) 0.027(1) 0.024(1) 0.0007(8) -0.0056(8) -0.0042(8) C(30) 0.0160(9) 0.0279(10) 0.0124(8) -0.0011(8) 0.0027(7) 0.0004(7) C(31) 0.050(1) 0.034(1) 0.0183(10) -0.010(1) 0.0128(9) 0.0014(9) C(32) 0.025(1) 0.042(1) 0.0133(9) -0.0089(9) -0.0018(8) 0.0064(8) C(33) 0.028(1) 0.064(2) 0.0163(10) 0.013(1) 0.0090(8) 0.0040(10) #----------------------------------------------------------------------- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #----------------------------------------------------------------------- _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(1) C(14) 1.825(2) . . yes S(1) C(15) 1.832(2) . . yes S(2) C(22) 1.809(2) . . yes S(2) C(23) 1.820(2) . . yes O(1) C(6) 1.393(2) . . yes O(1) C(24) 1.434(2) . . yes O(2) C(13) 1.393(2) . . yes O(2) C(25) 1.437(2) . . yes O(3) N(1) 1.232(2) . . yes O(4) N(1) 1.232(2) . . yes N(1) C(18) 1.470(2) . . yes C(1) C(2) 1.402(2) . . yes C(1) C(6) 1.392(2) . . yes C(1) C(23) 1.505(2) . . yes C(2) C(3) 1.388(3) . . yes C(3) C(4) 1.400(2) . . yes C(3) C(26) 1.534(2) . . yes C(4) C(5) 1.385(2) . . yes C(5) C(6) 1.400(2) . . yes C(5) C(7) 1.511(2) . . yes C(7) C(8) 1.519(3) . . yes C(8) C(9) 1.396(3) . . yes C(8) C(13) 1.396(2) . . yes C(9) C(10) 1.396(3) . . yes C(10) C(11) 1.398(2) . . yes C(10) C(30) 1.534(3) . . yes C(11) C(12) 1.392(3) . . yes C(12) C(13) 1.395(3) . . yes C(12) C(14) 1.505(2) . . yes C(15) C(16) 1.510(2) . . yes C(16) C(17) 1.386(2) . . yes C(16) C(21) 1.403(2) . . yes C(17) C(18) 1.385(2) . . yes C(18) C(19) 1.380(2) . . yes C(19) C(20) 1.394(2) . . yes C(20) C(21) 1.390(2) . . yes C(20) C(22) 1.519(2) . . yes C(26) C(27) 1.538(3) . . yes C(26) C(28) 1.533(3) . . yes C(26) C(29) 1.529(3) . . yes C(30) C(31) 1.529(3) . . yes C(30) C(32) 1.527(2) . . yes C(30) C(33) 1.533(3) . . 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(14) S(1) C(15) 100.63(8) . . . yes C(22) S(2) C(23) 100.79(8) . . . yes C(6) O(1) C(24) 113.7(1) . . . yes C(13) O(2) C(25) 110.9(1) . . . yes O(3) N(1) O(4) 123.3(1) . . . yes O(3) N(1) C(18) 118.5(1) . . . yes O(4) N(1) C(18) 118.2(1) . . . yes C(2) C(1) C(6) 118.1(2) . . . yes C(2) C(1) C(23) 120.2(1) . . . yes C(6) C(1) C(23) 121.5(1) . . . yes C(1) C(2) C(3) 122.3(1) . . . yes C(2) C(3) C(4) 117.3(1) . . . yes C(2) C(3) C(26) 122.5(1) . . . yes C(4) C(3) C(26) 120.1(1) . . . yes C(3) C(4) C(5) 122.7(2) . . . yes C(4) C(5) C(6) 117.9(1) . . . yes C(4) C(5) C(7) 122.1(2) . . . yes C(6) C(5) C(7) 119.7(1) . . . yes O(1) C(6) C(1) 119.8(1) . . . yes O(1) C(6) C(5) 118.4(1) . . . yes C(1) C(6) C(5) 121.5(1) . . . yes C(5) C(7) C(8) 111.4(1) . . . yes C(7) C(8) C(9) 120.8(1) . . . yes C(7) C(8) C(13) 121.1(2) . . . yes C(9) C(8) C(13) 118.1(2) . . . yes C(8) C(9) C(10) 122.4(1) . . . yes C(9) C(10) C(11) 117.4(2) . . . yes C(9) C(10) C(30) 122.9(1) . . . yes C(11) C(10) C(30) 119.7(2) . . . yes C(10) C(11) C(12) 122.3(2) . . . yes C(11) C(12) C(13) 118.3(1) . . . yes C(11) C(12) C(14) 120.8(2) . . . yes C(13) C(12) C(14) 120.8(2) . . . yes O(2) C(13) C(8) 119.6(2) . . . yes O(2) C(13) C(12) 118.8(1) . . . yes C(8) C(13) C(12) 121.6(2) . . . yes S(1) C(14) C(12) 113.0(1) . . . yes S(1) C(15) C(16) 112.5(1) . . . yes C(15) C(16) C(17) 120.2(1) . . . yes C(15) C(16) C(21) 120.9(2) . . . yes C(17) C(16) C(21) 118.9(1) . . . yes C(16) C(17) C(18) 118.5(1) . . . yes N(1) C(18) C(17) 118.2(1) . . . yes N(1) C(18) C(19) 118.6(1) . . . yes C(17) C(18) C(19) 123.2(2) . . . yes C(18) C(19) C(20) 118.6(1) . . . yes C(19) C(20) C(21) 118.9(1) . . . yes C(19) C(20) C(22) 120.7(1) . . . yes C(21) C(20) C(22) 120.4(2) . . . yes C(16) C(21) C(20) 121.8(2) . . . yes S(2) C(22) C(20) 115.4(1) . . . yes S(2) C(23) C(1) 112.2(1) . . . yes C(3) C(26) C(27) 110.4(1) . . . yes C(3) C(26) C(28) 108.1(1) . . . yes C(3) C(26) C(29) 112.2(1) . . . yes C(27) C(26) C(28) 109.1(2) . . . yes C(27) C(26) C(29) 108.1(2) . . . yes C(28) C(26) C(29) 108.8(1) . . . yes C(10) C(30) C(31) 108.8(1) . . . yes C(10) C(30) C(32) 112.3(2) . . . yes C(10) C(30) C(33) 109.4(1) . . . yes C(31) C(30) C(32) 108.7(1) . . . yes C(31) C(30) C(33) 109.5(2) . . . yes C(32) C(30) C(33) 108.0(2) . . . yes #----------------------------------------------------------------------- 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 S(1) C(14) C(12) C(11) 69.7(2) . . . . yes S(1) C(14) C(12) C(13) -106.9(2) . . . . yes S(1) C(15) C(16) C(17) -99.0(2) . . . . yes S(1) C(15) C(16) C(21) 81.5(2) . . . . yes S(2) C(22) C(20) C(19) -48.5(2) . . . . yes S(2) C(22) C(20) C(21) 132.5(2) . . . . yes S(2) C(23) C(1) C(2) -70.3(2) . . . . yes S(2) C(23) C(1) C(6) 105.7(2) . . . . yes O(1) C(6) C(1) C(2) 178.7(2) . . . . yes O(1) C(6) C(1) C(23) 2.6(3) . . . . yes O(1) C(6) C(5) C(4) -179.1(2) . . . . yes O(1) C(6) C(5) C(7) -5.2(3) . . . . yes O(2) C(13) C(8) C(7) 2.5(2) . . . . yes O(2) C(13) C(8) C(9) 179.9(2) . . . . yes O(2) C(13) C(12) C(11) 179.9(2) . . . . yes O(2) C(13) C(12) C(14) -3.5(2) . . . . yes O(3) N(1) C(18) C(17) -7.1(3) . . . . yes O(3) N(1) C(18) C(19) 174.9(2) . . . . yes O(4) N(1) C(18) C(17) 171.7(2) . . . . yes O(4) N(1) C(18) C(19) -6.3(3) . . . . yes N(1) C(18) C(17) C(16) -176.3(2) . . . . yes N(1) C(18) C(19) C(20) 176.7(2) . . . . yes C(1) C(2) C(3) C(4) -2.0(3) . . . . yes C(1) C(2) C(3) C(26) -178.3(2) . . . . yes C(1) C(6) O(1) C(24) 89.4(2) . . . . yes C(1) C(6) C(5) C(4) -4.3(3) . . . . yes C(1) C(6) C(5) C(7) 169.6(2) . . . . yes C(1) C(23) S(2) C(22) -63.2(1) . . . . yes C(2) C(1) C(6) C(5) 3.9(3) . . . . yes C(2) C(3) C(4) C(5) 1.6(3) . . . . yes C(2) C(3) C(26) C(27) -131.9(2) . . . . yes C(2) C(3) C(26) C(28) 108.8(2) . . . . yes C(2) C(3) C(26) C(29) -11.2(3) . . . . yes C(3) C(2) C(1) C(6) -0.7(3) . . . . yes C(3) C(2) C(1) C(23) 175.4(2) . . . . yes C(3) C(4) C(5) C(6) 1.4(3) . . . . yes C(3) C(4) C(5) C(7) -172.3(2) . . . . yes C(4) C(3) C(26) C(27) 51.9(2) . . . . yes C(4) C(3) C(26) C(28) -67.4(2) . . . . yes C(4) C(3) C(26) C(29) 172.6(2) . . . . yes C(4) C(5) C(7) C(8) 107.2(2) . . . . yes C(5) C(4) C(3) C(26) 178.0(2) . . . . yes C(5) C(6) O(1) C(24) -95.6(2) . . . . yes C(5) C(6) C(1) C(23) -172.2(2) . . . . yes C(5) C(7) C(8) C(9) -43.6(2) . . . . yes C(5) C(7) C(8) C(13) 133.8(2) . . . . yes C(6) C(5) C(7) C(8) -66.4(2) . . . . yes C(7) C(8) C(9) C(10) 177.3(2) . . . . yes C(7) C(8) C(13) C(12) -175.7(2) . . . . yes C(8) C(9) C(10) C(11) -1.3(3) . . . . yes C(8) C(9) C(10) C(30) -178.9(2) . . . . yes C(8) C(13) O(2) C(25) 86.3(2) . . . . yes C(8) C(13) C(12) C(11) -1.9(3) . . . . yes C(8) C(13) C(12) C(14) 174.7(2) . . . . yes C(9) C(8) C(13) C(12) 1.8(3) . . . . yes C(9) C(10) C(11) C(12) 1.1(3) . . . . yes C(9) C(10) C(30) C(31) 118.3(2) . . . . yes C(9) C(10) C(30) C(32) -2.2(2) . . . . yes C(9) C(10) C(30) C(33) -122.1(2) . . . . yes C(10) C(9) C(8) C(13) -0.1(3) . . . . yes C(10) C(11) C(12) C(13) 0.4(3) . . . . yes C(10) C(11) C(12) C(14) -176.2(2) . . . . yes C(11) C(10) C(30) C(31) -59.3(2) . . . . yes C(11) C(10) C(30) C(32) -179.7(2) . . . . yes C(11) C(10) C(30) C(33) 60.3(2) . . . . yes C(12) C(11) C(10) C(30) 178.8(2) . . . . yes C(12) C(13) O(2) C(25) -95.5(2) . . . . yes C(12) C(14) S(1) C(15) 62.9(1) . . . . yes C(14) S(1) C(15) C(16) -119.5(1) . . . . yes C(15) C(16) C(17) C(18) -179.3(2) . . . . yes C(15) C(16) C(21) C(20) 177.1(2) . . . . yes C(16) C(17) C(18) C(19) 1.6(3) . . . . yes C(16) C(21) C(20) C(19) 2.8(3) . . . . yes C(16) C(21) C(20) C(22) -178.2(2) . . . . yes C(17) C(16) C(21) C(20) -2.4(3) . . . . yes C(17) C(18) C(19) C(20) -1.3(3) . . . . yes C(18) C(17) C(16) C(21) 0.2(3) . . . . yes C(18) C(19) C(20) C(21) -0.9(3) . . . . yes C(18) C(19) C(20) C(22) -180.0(2) . . . . yes C(20) C(22) S(2) C(23) -70.8(1) . . . . yes C(20) C(22) S(2) C(23) -70.8(1) . . . . yes #----------------------------------------------------------------------- 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 O(3) C(2) 3.080(2) . 2_655 ? O(3) C(25) 3.255(2) . 1_565 ? O(3) C(1) 3.452(2) . 2_655 ? O(3) C(11) 3.522(2) . 2_755 ? O(4) C(23) 3.165(2) . 2_655 ? O(4) C(1) 3.248(2) . 2_655 ? O(4) C(7) 3.509(2) . 1_565 ? O(4) C(24) 3.549(2) . 2_655 ? N(1) C(1) 3.318(2) . 2_655 ? N(1) C(2) 3.338(3) . 2_655 ? #----------------------------------------------------------------------- #----------------------------------------------------------------------- data_dithia[3.3.1]MCP _database_code_CSD 165153 _audit_creation_date 'Mon Jun 11 15:26:42 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #----------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C33 H42 O2 S2 ' _chemical_formula_moiety 'C33 H42 O2 S2 ' _chemical_formula_weight 534.81 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.7609(6) _cell_length_b 18.671(2) _cell_length_c 9.1231(5) _cell_angle_alpha 90.878(4) _cell_angle_beta 116.678(2) _cell_angle_gamma 83.190(3) _cell_volume 1473.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7088 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #----------------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 0.959 #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12179 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9276 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9276 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6256 _reflns_number_gt 3397 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0491 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3397 _refine_ls_number_parameters 335 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]' _refine_ls_shift/su_max 0.0092 _refine_diff_density_max 0.26 _refine_diff_density_min -0.30 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 S(1) S -0.08712(8) 0.42666(4) 0.54779(9) 0.0228(2) Uani 1.00 d . . . S(2) S 0.41335(9) 0.09312(4) 0.49704(9) 0.0215(2) Uani 1.00 d . . . O(1) O 0.1202(2) 0.33269(10) 0.9924(2) 0.0170(5) Uani 1.00 d . . . O(2) O 0.5720(2) 0.14560(9) 0.9536(2) 0.0182(5) Uani 1.00 d . . . C(1) C 0.1905(3) 0.4072(1) 0.8295(3) 0.0154(7) Uani 1.00 d . . . C(2) C 0.2996(3) 0.4223(1) 0.7790(3) 0.0170(7) Uani 1.00 d . . . C(3) C 0.4422(3) 0.3807(1) 0.8309(3) 0.0154(7) Uani 1.00 d . . . C(4) C 0.4721(3) 0.3204(1) 0.9349(3) 0.0146(7) Uani 1.00 d . . . C(5) C 0.3661(3) 0.3032(1) 0.9892(3) 0.0138(7) Uani 1.00 d . . . C(6) C 0.2279(3) 0.3489(1) 0.9395(3) 0.0149(7) Uani 1.00 d . . . C(7) C 0.3932(3) 0.2323(1) 1.0835(3) 0.0156(7) Uani 1.00 d . . . C(8) C 0.3277(3) 0.1742(1) 0.9619(3) 0.0136(7) Uani 1.00 d . . . C(9) C 0.1737(3) 0.1622(1) 0.9030(3) 0.0137(7) Uani 1.00 d . . . C(10) C 0.1058(3) 0.1139(1) 0.7814(3) 0.0134(7) Uani 1.00 d . . . C(11) C 0.1980(3) 0.0788(1) 0.7140(3) 0.0164(7) Uani 1.00 d . . . C(12) C 0.3526(3) 0.0886(1) 0.7693(3) 0.0158(7) Uani 1.00 d . . . C(13) C 0.4173(3) 0.1353(1) 0.8960(3) 0.0147(7) Uani 1.00 d . . . C(14) C 0.4479(3) 0.0510(1) 0.6921(4) 0.0206(8) Uani 1.00 d . . . C(15) C 0.3704(3) 0.1891(1) 0.5199(3) 0.0176(7) Uani 1.00 d . . . C(16) C 0.2000(3) 0.2166(1) 0.4481(3) 0.0163(7) Uani 1.00 d . . . C(17) C 0.0994(4) 0.2008(2) 0.2881(3) 0.0221(8) Uani 1.00 d . . . C(18) C -0.0554(3) 0.2286(2) 0.2194(3) 0.0230(8) Uani 1.00 d . . . C(19) C -0.1134(3) 0.2714(1) 0.3101(3) 0.0208(8) Uani 1.00 d . . . C(20) C -0.0168(3) 0.2865(1) 0.4705(3) 0.0164(7) Uani 1.00 d . . . C(21) C 0.1398(3) 0.2597(1) 0.5372(3) 0.0164(7) Uani 1.00 d . . . C(22) C -0.0831(3) 0.3287(1) 0.5702(3) 0.0197(8) Uani 1.00 d . . . C(23) C 0.0326(3) 0.4505(1) 0.7574(3) 0.0201(8) Uani 1.00 d . . . C(24) C 0.1399(4) 0.3693(2) 1.1387(4) 0.0247(8) Uani 1.00 d . . . C(25) C 0.6713(3) 0.0935(2) 1.0838(4) 0.0261(8) Uani 1.00 d . . . C(26) C 0.5559(3) 0.4007(1) 0.7691(3) 0.0181(7) Uani 1.00 d . . . C(27) C 0.5908(4) 0.4779(2) 0.8123(4) 0.0330(10) Uani 1.00 d . . . C(28) C 0.7074(3) 0.3502(2) 0.8421(4) 0.0330(10) Uani 1.00 d . . . C(29) C 0.4837(3) 0.3958(2) 0.5821(4) 0.0265(9) Uani 1.00 d . . . C(30) C -0.0625(3) 0.0983(1) 0.7189(3) 0.0155(7) Uani 1.00 d . . . C(31) C -0.1436(3) 0.1418(2) 0.8072(4) 0.0265(9) Uani 1.00 d . . . C(32) C -0.1527(3) 0.1172(2) 0.5357(3) 0.0227(8) Uani 1.00 d . . . C(33) C -0.0638(3) 0.0179(1) 0.7496(3) 0.0212(8) Uani 1.00 d . . . H(1) H 0.2745 0.4634 0.7028 0.0216 Uiso 1.00 calc . . . H(2) H 0.5694 0.2896 0.9704 0.0165 Uiso 1.00 calc . . . H(3) H 0.5008 0.2184 1.1509 0.0193 Uiso 1.00 calc . . . H(4) H 0.3423 0.2370 1.1525 0.0193 Uiso 1.00 calc . . . H(5) H 0.1122 0.1883 0.9485 0.0162 Uiso 1.00 calc . . . H(6) H 0.1515 0.0458 0.6259 0.0198 Uiso 1.00 calc . . . H(7) H 0.4258 0.0024 0.6758 0.0249 Uiso 1.00 calc . . . H(8) H 0.5549 0.0507 0.7687 0.0249 Uiso 1.00 calc . . . H(9) H 0.4151 0.1985 0.6344 0.0241 Uiso 1.00 calc . . . H(10) H 0.4141 0.2159 0.4682 0.0241 Uiso 1.00 calc . . . H(11) H 0.1379 0.1707 0.2268 0.0277 Uiso 1.00 calc . . . H(12) H -0.1232 0.2177 0.1073 0.0281 Uiso 1.00 calc . . . H(13) H -0.2219 0.2910 0.2587 0.0253 Uiso 1.00 calc . . . H(14) H 0.2096 0.2703 0.6496 0.0188 Uiso 1.00 calc . . . H(15) H -0.0260 0.3135 0.6833 0.0244 Uiso 1.00 calc . . . H(16) H -0.1883 0.3181 0.5340 0.0244 Uiso 1.00 calc . . . H(17) H 0.0434 0.5010 0.7584 0.0250 Uiso 1.00 calc . . . H(18) H -0.0179 0.4424 0.8238 0.0250 Uiso 1.00 calc . . . H(19) H 0.2412 0.3551 1.2254 0.0319 Uiso 1.00 calc . . . H(20) H 0.1272 0.4204 1.1199 0.0319 Uiso 1.00 calc . . . H(21) H 0.0658 0.3579 1.1734 0.0319 Uiso 1.00 calc . . . H(22) H 0.6461 0.0986 1.1741 0.0323 Uiso 1.00 calc . . . H(23) H 0.6589 0.0458 1.0467 0.0323 Uiso 1.00 calc . . . H(24) H 0.7769 0.1009 1.1226 0.0323 Uiso 1.00 calc . . . H(25) H 0.6365 0.4822 0.9272 0.0403 Uiso 1.00 calc . . . H(26) H 0.6598 0.4906 0.7713 0.0403 Uiso 1.00 calc . . . H(27) H 0.4971 0.5101 0.7622 0.0403 Uiso 1.00 calc . . . H(28) H 0.6883 0.3010 0.8177 0.0380 Uiso 1.00 calc . . . H(29) H 0.7760 0.3619 0.8009 0.0380 Uiso 1.00 calc . . . H(30) H 0.7585 0.3527 0.9601 0.0380 Uiso 1.00 calc . . . H(31) H 0.3887 0.4281 0.5322 0.0340 Uiso 1.00 calc . . . H(32) H 0.5513 0.4092 0.5407 0.0340 Uiso 1.00 calc . . . H(33) H 0.4611 0.3481 0.5517 0.0340 Uiso 1.00 calc . . . H(34) H -0.0946 0.1291 0.9210 0.0345 Uiso 1.00 calc . . . H(35) H -0.1465 0.1921 0.7909 0.0345 Uiso 1.00 calc . . . H(36) H -0.2499 0.1312 0.7628 0.0345 Uiso 1.00 calc . . . H(37) H -0.1583 0.1671 0.5124 0.0298 Uiso 1.00 calc . . . H(38) H -0.1033 0.0904 0.4768 0.0298 Uiso 1.00 calc . . . H(39) H -0.2555 0.1044 0.4934 0.0298 Uiso 1.00 calc . . . H(40) H -0.1688 0.0070 0.7051 0.0269 Uiso 1.00 calc . . . H(41) H -0.0139 -0.0112 0.6956 0.0269 Uiso 1.00 calc . . . H(42) H -0.0133 0.0050 0.8631 0.0269 Uiso 1.00 calc . . . 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(1) 0.0200(4) 0.0166(4) 0.0261(4) 0.0029(3) 0.0060(4) 0.0030(3) S(2) 0.0248(4) 0.0210(4) 0.0234(4) -0.0013(3) 0.0151(4) -0.0069(3) O(1) 0.018(1) 0.019(1) 0.0210(10) -0.0076(8) 0.0139(9) -0.0067(8) O(2) 0.0106(10) 0.017(1) 0.024(1) 0.0016(8) 0.0057(9) 0.0060(8) C(1) 0.016(1) 0.014(1) 0.016(1) -0.001(1) 0.007(1) -0.004(1) C(2) 0.020(2) 0.013(1) 0.018(1) -0.001(1) 0.009(1) -0.001(1) C(3) 0.017(1) 0.016(1) 0.014(1) -0.004(1) 0.007(1) -0.004(1) C(4) 0.010(1) 0.017(1) 0.012(1) -0.002(1) 0.001(1) -0.003(1) C(5) 0.016(1) 0.016(1) 0.009(1) -0.005(1) 0.005(1) -0.004(1) C(6) 0.015(1) 0.016(1) 0.016(1) -0.006(1) 0.008(1) -0.007(1) C(7) 0.015(1) 0.019(1) 0.011(1) -0.003(1) 0.004(1) -0.001(1) C(8) 0.016(1) 0.014(1) 0.011(1) -0.002(1) 0.006(1) 0.004(1) C(9) 0.017(1) 0.013(1) 0.013(1) 0.000(1) 0.008(1) 0.001(1) C(10) 0.015(1) 0.014(1) 0.013(1) -0.002(1) 0.008(1) 0.001(1) C(11) 0.024(2) 0.011(1) 0.018(1) -0.004(1) 0.012(1) -0.002(1) C(12) 0.020(1) 0.010(1) 0.021(1) 0.000(1) 0.013(1) 0.002(1) C(13) 0.013(1) 0.014(1) 0.016(1) 0.000(1) 0.005(1) 0.006(1) C(14) 0.022(2) 0.014(1) 0.032(2) -0.001(1) 0.018(1) -0.002(1) C(15) 0.022(2) 0.017(1) 0.016(1) -0.007(1) 0.010(1) -0.002(1) C(16) 0.023(2) 0.013(1) 0.015(1) -0.006(1) 0.010(1) 0.001(1) C(17) 0.032(2) 0.019(2) 0.015(1) -0.005(1) 0.010(1) -0.002(1) C(18) 0.027(2) 0.024(2) 0.014(1) -0.006(1) 0.005(1) -0.001(1) C(19) 0.020(2) 0.020(2) 0.019(1) -0.003(1) 0.004(1) 0.003(1) C(20) 0.020(2) 0.012(1) 0.017(1) -0.003(1) 0.009(1) 0.002(1) C(21) 0.021(2) 0.016(1) 0.012(1) -0.005(1) 0.006(1) 0.000(1) C(22) 0.020(2) 0.018(1) 0.021(1) -0.003(1) 0.009(1) 0.001(1) C(23) 0.021(2) 0.014(1) 0.026(2) -0.001(1) 0.010(1) -0.004(1) C(24) 0.034(2) 0.024(2) 0.027(2) -0.009(1) 0.021(2) -0.009(1) C(25) 0.015(2) 0.029(2) 0.027(2) 0.001(1) 0.003(1) 0.009(1) C(26) 0.019(2) 0.018(1) 0.020(1) -0.004(1) 0.011(1) -0.001(1) C(27) 0.039(2) 0.031(2) 0.043(2) -0.019(2) 0.027(2) -0.013(2) C(28) 0.021(2) 0.042(2) 0.040(2) 0.004(1) 0.019(2) 0.015(2) C(29) 0.029(2) 0.032(2) 0.026(2) -0.007(1) 0.017(2) -0.002(1) C(30) 0.015(1) 0.015(1) 0.018(1) -0.006(1) 0.007(1) -0.004(1) C(31) 0.020(2) 0.030(2) 0.036(2) -0.008(1) 0.017(2) -0.014(1) C(32) 0.016(2) 0.028(2) 0.022(2) -0.006(1) 0.005(1) 0.002(1) C(33) 0.020(2) 0.021(2) 0.024(2) -0.008(1) 0.010(1) 0.000(1) #----------------------------------------------------------------------- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #----------------------------------------------------------------------- _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(1) C(22) 1.838(3) . . yes S(1) C(23) 1.819(3) . . yes S(2) C(14) 1.828(3) . . yes S(2) C(15) 1.822(3) . . yes O(1) C(6) 1.402(4) . . yes O(1) C(24) 1.436(4) . . yes O(2) C(13) 1.396(3) . . yes O(2) C(25) 1.440(3) . . yes C(1) C(2) 1.393(5) . . yes C(1) C(6) 1.391(4) . . yes C(1) C(23) 1.507(4) . . yes C(2) C(3) 1.389(4) . . yes C(3) C(4) 1.400(4) . . yes C(3) C(26) 1.535(5) . . yes C(4) C(5) 1.401(5) . . yes C(5) C(6) 1.395(4) . . yes C(5) C(7) 1.520(4) . . yes C(7) C(8) 1.519(4) . . yes C(8) C(9) 1.395(4) . . yes C(8) C(13) 1.400(4) . . yes C(9) C(10) 1.392(4) . . yes C(10) C(11) 1.401(5) . . yes C(10) C(30) 1.541(4) . . yes C(11) C(12) 1.394(4) . . yes C(12) C(13) 1.392(4) . . yes C(12) C(14) 1.508(5) . . yes C(15) C(16) 1.512(4) . . yes C(16) C(17) 1.396(4) . . yes C(16) C(21) 1.397(4) . . yes C(17) C(18) 1.385(4) . . yes C(18) C(19) 1.392(5) . . yes C(19) C(20) 1.386(4) . . yes C(20) C(21) 1.396(4) . . yes C(20) C(22) 1.501(5) . . yes C(26) C(27) 1.525(4) . . yes C(26) C(28) 1.525(4) . . yes C(26) C(29) 1.532(4) . . yes C(30) C(31) 1.528(5) . . yes C(30) C(32) 1.523(4) . . yes C(30) C(33) 1.533(4) . . 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(22) S(1) C(23) 102.4(1) . . . yes C(14) S(2) C(15) 104.1(1) . . . yes C(6) O(1) C(24) 111.3(2) . . . yes C(13) O(2) C(25) 111.0(2) . . . yes C(2) C(1) C(6) 118.4(2) . . . yes C(2) C(1) C(23) 120.2(2) . . . yes C(6) C(1) C(23) 121.2(3) . . . yes C(1) C(2) C(3) 122.7(3) . . . yes C(2) C(3) C(4) 117.0(3) . . . yes C(2) C(3) C(26) 119.6(2) . . . yes C(4) C(3) C(26) 123.4(2) . . . yes C(3) C(4) C(5) 122.2(2) . . . yes C(4) C(5) C(6) 118.2(2) . . . yes C(4) C(5) C(7) 120.7(2) . . . yes C(6) C(5) C(7) 120.8(3) . . . yes O(1) C(6) C(1) 119.5(2) . . . yes O(1) C(6) C(5) 119.1(2) . . . yes C(1) C(6) C(5) 121.2(3) . . . yes C(5) C(7) C(8) 109.0(2) . . . yes C(7) C(8) C(9) 121.0(3) . . . yes C(7) C(8) C(13) 120.5(3) . . . yes C(9) C(8) C(13) 118.3(2) . . . yes C(8) C(9) C(10) 122.8(3) . . . yes C(9) C(10) C(11) 116.8(3) . . . yes C(9) C(10) C(30) 123.5(3) . . . yes C(11) C(10) C(30) 119.8(2) . . . yes C(10) C(11) C(12) 122.5(2) . . . yes C(11) C(12) C(13) 118.6(3) . . . yes C(11) C(12) C(14) 121.1(2) . . . yes C(13) C(12) C(14) 120.2(3) . . . yes O(2) C(13) C(8) 119.6(2) . . . yes O(2) C(13) C(12) 119.5(3) . . . yes C(8) C(13) C(12) 120.9(3) . . . yes S(2) C(14) C(12) 114.2(2) . . . yes S(2) C(15) C(16) 114.7(2) . . . yes C(15) C(16) C(17) 120.3(3) . . . yes C(15) C(16) C(21) 121.3(2) . . . yes C(17) C(16) C(21) 118.3(3) . . . yes C(16) C(17) C(18) 120.5(3) . . . yes C(17) C(18) C(19) 120.5(2) . . . yes C(18) C(19) C(20) 120.2(3) . . . yes C(19) C(20) C(21) 118.9(3) . . . yes C(19) C(20) C(22) 119.6(2) . . . yes C(21) C(20) C(22) 121.5(2) . . . yes C(16) C(21) C(20) 121.7(2) . . . yes S(1) C(22) C(20) 112.9(2) . . . yes S(1) C(23) C(1) 111.9(2) . . . yes C(3) C(26) C(27) 110.0(3) . . . yes C(3) C(26) C(28) 112.2(3) . . . yes C(3) C(26) C(29) 109.4(2) . . . yes C(27) C(26) C(28) 108.9(2) . . . yes C(27) C(26) C(29) 108.6(2) . . . yes C(28) C(26) C(29) 107.7(3) . . . yes C(10) C(30) C(31) 111.8(2) . . . yes C(10) C(30) C(32) 109.8(3) . . . yes C(10) C(30) C(33) 109.3(2) . . . yes C(31) C(30) C(32) 108.5(2) . . . yes C(31) C(30) C(33) 108.0(3) . . . yes C(32) C(30) C(33) 109.3(2) . . . yes #----------------------------------------------------------------------- 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 S(1) C(22) C(20) C(19) -89.0(3) . . . . yes S(1) C(22) C(20) C(21) 93.1(3) . . . . yes S(1) C(23) C(1) C(2) 73.8(3) . . . . yes S(1) C(23) C(1) C(6) -102.3(3) . . . . yes S(2) C(14) C(12) C(11) 78.8(3) . . . . yes S(2) C(14) C(12) C(13) -100.0(2) . . . . yes S(2) C(15) C(16) C(17) -49.7(4) . . . . yes S(2) C(15) C(16) C(21) 132.1(3) . . . . yes O(1) C(6) C(1) C(2) 179.9(2) . . . . yes O(1) C(6) C(1) C(23) -4.0(4) . . . . yes O(1) C(6) C(5) C(4) 180.0(2) . . . . yes O(1) C(6) C(5) C(7) 6.7(4) . . . . yes O(2) C(13) C(8) C(7) 5.7(4) . . . . yes O(2) C(13) C(8) C(9) -179.4(2) . . .. . yes O(2) C(13) C(12) C(11) 179.7(2) . . . . yes O(2) C(13) C(12) C(14) -1.5(4) . . . . yes C(1) C(2) C(3) C(4) 1.7(4) . . . . yes C(1) C(2) C(3) C(26) 179.8(2) . . . . yes C(1) C(6) O(1) C(24) -90.7(3) . . . . yes C(1) C(6) C(5) C(4) 4.6(4) . . . . yes C(1) C(6) C(5) C(7) -168.6(2) . . . . yes C(1) C(23) S(1) C(22) 55.5(3) . . . . yes C(2) C(1) C(6) C(5) -4.8(4) . . . . yes C(2) C(3) C(4) C(5) -1.8(4) . . . . yes C(2) C(3) C(26) C(27) 57.3(3) . . . . yes C(2) C(3) C(26) C(28) 178.6(2) . . . . yes C(2) C(3) C(26) C(29) -61.9(3) . . . . yes C(3) C(2) C(1) C(6) 1.5(4) . . . . yes C(3) C(2) C(1) C(23) -174.6(2) . . . . yes C(3) C(4) C(5) C(6) -1.3(4) . . . . yes C(3) C(4) C(5) C(7) 172.0(2) . . . . yes C(4) C(3) C(26) C(27) -124.7(3) . . . . yes C(4) C(3) C(26) C(28) -3.4(4) . . . . yes C(4) C(3) C(26) C(29) 116.0(3) . . . . yes C(4) C(5) C(7) C(8) -86.5(3) . . . . yes C(5) C(4) C(3) C(26) -179.8(2) . . . . yes C(5) C(6) O(1) C(24) 93.9(3) . . . . yes C(5) C(6) C(1) C(23) 171.3(2) . . . . yes C(5) C(7) C(8) C(9) -88.2(3) . . . . yes C(5) C(7) C(8) C(13) 86.5(3) . . . . yes C(6) C(5) C(7) C(8) 86.5(3) . . . . yes C(7) C(8) C(9) C(10) 174.4(2) . . . . yes C(7) C(8) C(13) C(12) -171.7(2) . . . . yes C(8) C(9) C(10) C(11) -2.4(4) . . . . yes C(8) C(9) C(10) C(30) 178.0(2) . . . . yes C(8) C(13) O(2) C(25) 93.4(3) . . . . yes C(8) C(13) C(12) C(11) -2.9(4) . . . . yes C(8) C(13) C(12) C(14) 175.9(2) . . . . yes C(9) C(8) C(13) C(12) 3.1(4) . . . . yes C(9) C(10) C(11) C(12) 2.7(4) . . . . yes C(9) C(10) C(30) C(31) -0.3(4) . . . . yes C(9) C(10) C(30) C(32) 120.2(3) . . . . yes C(9) C(10) C(30) C(33) -119.9(3) . . . . yes C(10) C(9) C(8) C(13) -0.4(4) . . . . yes C(10) C(11) C(12) C(13) -0.2(4) . . . . yes C(10) C(11) C(12) C(14) -178.9(2) . . . . yes C(11) C(10) C(30) C(31) -179.9(2) . . . . yes C(11) C(10) C(30) C(32) -59.4(3) . . . . yes C(11) C(10) C(30) C(33) 60.5(3) . . . . yes C(12) C(11) C(10) C(30) -177.6(2) . . . . yes C(12) C(13) O(2) C(25) -89.1(3) . . . . yes C(12) C(14) S(2) C(15) 33.1(2) . . . . yes C(14) S(2) C(15) C(16) -96.3(2) . . . . yes C(15) C(16) C(17) C(18) -177.1(3) . . . . yes C(15) C(16) C(21) C(20) 178.7(3) . . . . yes C(16) C(17) C(18) C(19) -1.3(5) . . . . yes C(16) C(21) C(20) C(19) -1.9(5) . . . . yes C(16) C(21) C(20) C(22) 175.9(3) . . . . yes C(17) C(16) C(21) C(20) 0.4(5) . . . . yes C(17) C(18) C(19) C(20) -0.2(5) . . . . yes C(18) C(17) C(16) C(21) 1.2(5) . . . . yes C(18) C(19) C(20) C(21) 1.8(5) . . . . yes C(18) C(19) C(20) C(22) -176.1(3) . . . . yes C(20) C(22) S(1) C(23) -120.0(2) . . . . yes C(20) C(22) S(1) C(23) -120.0(2) . . . . yes #----------------------------------------------------------------------- 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 O(2) C(31) 3.573(5) . 1_655 ? C(11) C(25) 3.532(4) . 2_657 ? C(17) C(24) 3.580(4) . 1_554 ? #----------------------------------------------------------------------- data_Fluoro[3.3.1]MCP _database_code_CSD 163830 _audit_creation_date 'Sat Feb 10 15:27:29 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #----------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C33 H41 F O2 S2 ' _chemical_formula_moiety 'C33 H41 F O2 S2 ' _chemical_formula_weight 552.80 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 18.3159(6) _cell_length_b 8.4338(2) _cell_length_c 20.4494(5) _cell_angle_alpha 90 _cell_angle_beta 104.829(1) _cell_angle_gamma 90 _cell_volume 3053.7(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 29703 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #----------------------------------------------------------------------- _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0.010000 _diffrn_reflns_number 28279 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9986 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.00 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6994 _reflns_number_gt 5320 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0417 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5320 _refine_ls_number_parameters 508 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00084|Fo|^2^]' _refine_ls_shift/su_max 0.0012 _refine_diff_density_max 0.31 _refine_diff_density_min -0.24 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0017(10) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 S(1) S 0.09467(2) 0.62335(4) 0.93490(2) 0.02031(9) Uani 1.00 d . . . S(2) S 0.34494(2) 0.49424(4) 0.71555(2) 0.02057(9) Uani 1.00 d . . . F(1) F 0.16186(4) 0.51801(10) 0.79967(4) 0.0203(2) Uani 1.00 d . . . O(1) O 0.06836(5) 0.1680(1) 0.90103(4) 0.0178(2) Uani 1.00 d . . . O(2) O 0.22967(5) 0.2056(1) 0.83393(4) 0.0187(2) Uani 1.00 d . . . C(1) C 0.28127(8) 0.6332(2) 0.81101(7) 0.0184(3) Uani 1.00 d . . . C(2) C 0.34686(8) 0.6943(2) 0.85428(7) 0.0210(3) Uani 1.00 d . . . C(3) C 0.35659(8) 0.6944(2) 0.92386(7) 0.0222(3) Uani 1.00 d . . . C(4) C 0.30106(8) 0.6314(2) 0.95169(7) 0.0199(3) Uani 1.00 d . . . C(5) C 0.23443(7) 0.5704(2) 0.91019(7) 0.0175(3) Uani 1.00 d . . . C(6) C 0.22666(7) 0.5764(2) 0.84052(7) 0.0170(3) Uani 1.00 d . . . C(7) C 0.17511(8) 0.4920(2) 0.93786(7) 0.0182(3) Uani 1.00 d . . . C(8) C 0.01610(8) 0.4826(2) 0.91143(7) 0.0187(3) Uani 1.00 d . . . C(9) C 0.01289(7) 0.4053(2) 0.84430(6) 0.0159(3) Uani 1.00 d . . . C(10) C -0.01311(7) 0.4906(2) 0.78426(7) 0.0166(3) Uani 1.00 d . . . C(11) C -0.01080(7) 0.4280(2) 0.72161(6) 0.0155(3) Uani 1.00 d . . . C(12) C 0.02133(7) 0.2786(2) 0.72150(6) 0.0156(3) Uani 1.00 d . . . C(13) C 0.04952(7) 0.1904(2) 0.78027(6) 0.0155(3) Uani 1.00 d . . . C(14) C 0.04184(7) 0.2536(2) 0.84127(6) 0.0154(3) Uani 1.00 d . . . C(15) C 0.09327(8) 0.0392(2) 0.77698(7) 0.0173(3) Uani 1.00 d . . . C(16) C 0.15123(7) 0.0730(2) 0.73738(6) 0.0162(3) Uani 1.00 d . . . C(17) C 0.13710(7) 0.0338(2) 0.66923(7) 0.0167(3) Uani 1.00 d . . . C(18) C 0.18341(7) 0.0855(2) 0.62846(7) 0.0167(3) Uani 1.00 d . . . C(19) C 0.24549(8) 0.1778(2) 0.65866(7) 0.0171(3) Uani 1.00 d . . . C(20) C 0.26324(7) 0.2169(2) 0.72746(7) 0.0162(3) Uani 1.00 d . . . C(21) C 0.21565(7) 0.1629(2) 0.76619(6) 0.0157(3) Uani 1.00 d . . . C(22) C 0.33298(8) 0.3125(2) 0.75938(7) 0.0188(3) Uani 1.00 d . . . C(23) C 0.27217(8) 0.6186(2) 0.73549(7) 0.0207(3) Uani 1.00 d . . . C(24) C 0.01486(9) 0.0524(2) 0.91067(8) 0.0246(4) Uani 1.00 d . . . C(25) C 0.28025(9) 0.0992(2) 0.87790(8) 0.0292(4) Uani 1.00 d . . . C(26) C -0.03519(8) 0.5251(2) 0.65625(7) 0.0179(3) Uani 1.00 d . . . C(27) C -0.05977(9) 0.4181(2) 0.59415(7) 0.0243(4) Uani 1.00 d . . . C(28) C 0.03283(10) 0.6239(2) 0.64965(9) 0.0353(5) Uani 1.00 d . . . C(29) C -0.10121(10) 0.6347(2) 0.65806(8) 0.0275(4) Uani 1.00 d . . . C(30) C 0.16148(8) 0.0445(2) 0.55285(7) 0.0205(3) Uani 1.00 d . . . C(31) C 0.1502(1) -0.1337(2) 0.54345(9) 0.0305(4) Uani 1.00 d . . . C(32) C 0.08748(9) 0.1307(2) 0.51895(8) 0.0314(4) Uani 1.00 d . . . C(33) C 0.22153(9) 0.0963(2) 0.51709(8) 0.0286(4) Uani 1.00 d . . . H(1) H 0.3859(9) 0.737(2) 0.8338(8) 0.026(4) Uiso 1.00 calc . . . H(2) H 0.4030(10) 0.737(2) 0.9528(8) 0.026(4) Uiso 1.00 calc . . . H(3) H 0.3094(9) 0.626(2) 1.0019(8) 0.018(4) Uiso 1.00 calc . . . H(4) H 0.1554(8) 0.397(2) 0.9118(7) 0.015(4) Uiso 1.00 calc . . . H(5) H 0.1973(8) 0.457(2) 0.9860(8) 0.019(4) Uiso 1.00 calc . . . H(6) H 0.0209(8) 0.398(2) 0.9481(8) 0.017(4) Uiso 1.00 calc . . . H(7) H -0.0280(9) 0.549(2) 0.9092(8) 0.021(4) Uiso 1.00 calc . . . H(8) H -0.0298(9) 0.598(2) 0.7879(8) 0.024(4) Uiso 1.00 calc . . . H(9) H 0.0286(9) 0.236(2) 0.6816(8) 0.019(4) Uiso 1.00 calc . . . H(10) H 0.0598(9) -0.046(2) 0.7556(8) 0.022(4) Uiso 1.00 calc . . . H(11) H 0.1152(9) 0.001(2) 0.8231(8) 0.020(4) Uiso 1.00 calc . . . H(12) H 0.0912(9) -0.029(2) 0.6494(7) 0.018(4) Uiso 1.00 calc . . . H(13) H 0.2769(9) 0.217(2) 0.6332(8) 0.021(4) Uiso 1.00 calc . . . H(14) H 0.3354(9) 0.338(2) 0.8063(8) 0.020(4) Uiso 1.00 calc . . . H(15) H 0.3790(10) 0.249(2) 0.7603(8) 0.028(4) Uiso 1.00 calc . . . H(16) H 0.2223(9) 0.576(2) 0.7137(8) 0.018(4) Uiso 1.00 calc . . . H(17) H 0.2818(9) 0.725(2) 0.7178(8) 0.025(4) Uiso 1.00 calc . . . H(18) H -0.002(1) -0.016(2) 0.8719(10) 0.038(5) Uiso 1.00 calc . . . H(19) H 0.040(1) -0.012(2) 0.9499(9) 0.036(5) Uiso 1.00 calc . . . H(20) H -0.031(1) 0.106(2) 0.9184(9) 0.037(5) Uiso 1.00 calc . . . H(21) H 0.256(1) -0.006(2) 0.8781(9) 0.038(5) Uiso 1.00 calc . . . H(22) H 0.2924(10) 0.149(2) 0.9234(9) 0.033(5) Uiso 1.00 calc . . . H(23) H 0.327(1) 0.087(2) 0.8634(9) 0.035(5) Uiso 1.00 calc . . . H(24) H -0.018(1) 0.354(2) 0.5872(9) 0.035(5) Uiso 1.00 calc . . . H(25) H -0.099(1) 0.339(2) 0.6020(10) 0.042(5) Uiso 1.00 calc . . . H(26) H -0.080(1) 0.486(2) 0.5534(9) 0.032(5) Uiso 1.00 calc . . . H(27) H 0.021(1) 0.691(2) 0.609(1) 0.048(6) Uiso 1.00 calc . . . H(28) H 0.077(1) 0.554(2) 0.6482(9) 0.034(5) Uiso 1.00 calc . . . H(29) H 0.052(1) 0.696(2) 0.689(1) 0.049(6) Uiso 1.00 calc . . . H(30) H -0.086(1) 0.716(2) 0.6928(9) 0.037(5) Uiso 1.00 calc . . . H(31) H -0.144(1) 0.570(2) 0.6664(9) 0.037(5) Uiso 1.00 calc . . . H(32) H -0.119(1) 0.687(2) 0.6138(9) 0.036(5) Uiso 1.00 calc . . . H(33) H 0.194(1) -0.190(2) 0.5654(9) 0.035(5) Uiso 1.00 calc . . . H(34) H 0.110(1) -0.177(2) 0.5616(9) 0.036(5) Uiso 1.00 calc . . . H(35) H 0.138(1) -0.163(2) 0.495(1) 0.041(5) Uiso 1.00 calc . . . H(36) H 0.074(1) 0.106(2) 0.4714(10) 0.039(5) Uiso 1.00 calc . . . H(37) H 0.095(1) 0.251(3) 0.526(1) 0.054(6) Uiso 1.00 calc . . . H(38) H 0.046(1) 0.097(2) 0.5386(9) 0.041(5) Uiso 1.00 calc . . . H(39) H 0.2292(10) 0.214(2) 0.5193(9) 0.034(5) Uiso 1.00 calc . . . H(40) H 0.271(1) 0.044(2) 0.5368(9) 0.032(5) Uiso 1.00 calc . . . H(41) H 0.2060(10) 0.062(2) 0.4701(9) 0.033(5) Uiso 1.00 calc . . . 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(1) 0.0207(2) 0.0213(2) 0.0185(2) 0.0010(1) 0.0044(1) -0.0058(1) S(2) 0.0200(2) 0.0238(2) 0.0198(2) -0.0058(1) 0.0087(1) -0.0025(1) F(1) 0.0149(4) 0.0279(4) 0.0164(4) -0.0041(3) 0.0007(3) -0.0021(3) O(1) 0.0179(4) 0.0228(5) 0.0126(4) -0.0003(4) 0.0036(3) 0.0034(4) O(2) 0.0215(5) 0.0229(5) 0.0110(4) 0.0034(4) 0.0030(4) 0.0005(4) C(1) 0.0185(6) 0.0172(6) 0.0185(6) 0.0016(5) 0.0030(5) -0.0003(5) C(2) 0.0199(7) 0.0193(7) 0.0238(7) -0.0033(6) 0.0055(6) -0.0014(6) C(3) 0.0195(7) 0.0223(7) 0.0221(7) -0.0038(6) 0.0005(5) -0.0041(6) C(4) 0.0217(7) 0.0201(7) 0.0163(6) -0.0004(6) 0.0020(5) -0.0035(6) C(5) 0.0179(6) 0.0158(6) 0.0186(6) 0.0013(5) 0.0043(5) -0.0009(5) C(6) 0.0147(6) 0.0170(6) 0.0169(6) 0.0001(5) 0.0000(5) -0.0035(5) C(7) 0.0179(6) 0.0201(7) 0.0154(6) 0.0000(5) 0.0024(5) -0.0016(5) C(8) 0.0171(6) 0.0240(7) 0.0152(6) 0.0021(6) 0.0044(5) -0.0033(6) C(9) 0.0123(6) 0.0222(7) 0.0136(6) -0.0013(5) 0.0039(5) -0.0024(5) C(10) 0.0142(6) 0.0184(7) 0.0170(6) 0.0010(5) 0.0037(5) -0.0013(5) C(11) 0.0121(6) 0.0192(6) 0.0147(6) -0.0021(5) 0.0025(5) 0.0002(5) C(12) 0.0159(6) 0.0187(6) 0.0128(6) -0.0020(5) 0.0049(5) -0.0021(5) C(13) 0.0131(6) 0.0178(6) 0.0160(6) -0.0028(5) 0.0046(5) -0.0007(5) C(14) 0.0123(6) 0.0210(7) 0.0125(6) -0.0018(5) 0.0024(5) 0.0016(5) C(15) 0.0202(6) 0.0161(7) 0.0176(6) -0.0004(5) 0.0082(5) 0.0010(5) C(16) 0.0185(6) 0.0133(6) 0.0186(6) 0.0028(5) 0.0079(5) 0.0022(5) C(17) 0.0162(6) 0.0162(6) 0.0183(6) -0.0012(5) 0.0055(5) -0.0018(5) C(18) 0.0177(6) 0.0169(6) 0.0166(6) 0.0009(5) 0.0062(5) -0.0002(5) C(19) 0.0167(6) 0.0202(7) 0.0160(6) 0.0001(5) 0.0071(5) 0.0000(5) C(20) 0.0154(6) 0.0158(6) 0.0169(6) 0.0020(5) 0.0033(5) -0.0002(5) C(21) 0.0177(6) 0.0162(6) 0.0132(6) 0.0044(5) 0.0039(5) 0.0005(5) C(22) 0.0174(6) 0.0213(7) 0.0172(7) -0.0008(5) 0.0038(5) -0.0016(5) C(23) 0.0197(7) 0.0244(7) 0.0181(6) -0.0013(6) 0.0050(5) 0.0010(6) C(24) 0.0268(7) 0.0265(8) 0.0222(7) -0.0031(7) 0.0092(6) 0.0050(7) C(25) 0.0294(8) 0.0377(10) 0.0187(7) 0.0079(7) 0.0027(6) 0.0082(7) C(26) 0.0192(6) 0.0202(7) 0.0133(6) -0.0010(5) 0.0021(5) 0.0011(5) C(27) 0.0275(7) 0.0290(8) 0.0139(6) 0.0084(7) 0.0006(5) -0.0010(6) C(28) 0.0307(9) 0.041(1) 0.0293(9) -0.0137(8) -0.0004(7) 0.0153(8) C(29) 0.0362(9) 0.0241(8) 0.0199(7) 0.0110(7) 0.0030(6) 0.0016(7) C(30) 0.0193(6) 0.0279(8) 0.0152(6) -0.0035(6) 0.0056(5) -0.0036(6) C(31) 0.0391(9) 0.0314(9) 0.0254(8) -0.0087(8) 0.0162(7) -0.0125(7) C(32) 0.0244(8) 0.050(1) 0.0179(7) 0.0032(8) 0.0018(6) -0.0008(7) C(33) 0.0251(8) 0.047(1) 0.0156(7) -0.0105(7) 0.0085(6) -0.0056(7) #----------------------------------------------------------------------- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #----------------------------------------------------------------------- _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(1) C(7) 1.832(1) . . yes S(1) C(8) 1.832(1) . . yes S(2) C(22) 1.817(2) . . yes S(2) C(23) 1.823(2) . . yes F(1) C(6) 1.357(1) . . yes O(1) C(14) 1.395(2) . . yes O(1) C(24) 1.431(2) . . yes O(2) C(21) 1.390(2) . . yes O(2) C(25) 1.430(2) . . yes C(1) C(2) 1.395(2) . . yes C(1) C(6) 1.380(2) . . yes C(1) C(23) 1.515(2) . . yes C(2) C(3) 1.388(2) . . yes C(3) C(4) 1.392(2) . . yes C(4) C(5) 1.394(2) . . yes C(5) C(6) 1.396(2) . . yes C(5) C(7) 1.501(2) . . yes C(8) C(9) 1.507(2) . . yes C(9) C(10) 1.397(2) . . yes C(9) C(14) 1.392(2) . . yes C(10) C(11) 1.396(2) . . yes C(11) C(12) 1.391(2) . . yes C(11) C(26) 1.533(2) . . yes C(12) C(13) 1.395(2) . . yes C(13) C(14) 1.396(2) . . yes C(13) C(15) 1.516(2) . . yes C(15) C(16) 1.518(2) . . yes C(16) C(17) 1.390(2) . . yes C(16) C(21) 1.400(2) . . yes C(17) C(18) 1.402(2) . . yes C(18) C(19) 1.386(2) . . yes C(18) C(30) 1.534(2) . . yes C(19) C(20) 1.400(2) . . yes C(20) C(21) 1.395(2) . . yes C(20) C(22) 1.510(2) . . yes C(26) C(27) 1.529(2) . . yes C(26) C(28) 1.533(2) . . yes C(26) C(29) 1.530(2) . . yes C(30) C(31) 1.523(2) . . yes C(30) C(32) 1.538(2) . . yes C(30) C(33) 1.532(2) . . 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(7) S(1) C(8) 100.84(7) . 1_555 1_555 yes C(22) S(2) C(23) 100.83(7) . 1_555 1_555 yes C(14) O(1) C(24) 112.1(1) . 1_555 1_555 yes C(21) O(2) C(25) 112.9(1) . 1_555 1_555 yes C(2) C(1) C(6) 117.0(1) . 1_555 1_555 yes C(2) C(1) C(23) 121.9(1) . 1_555 1_555 yes C(6) C(1) C(23) 121.0(1) . 1_555 1_555 yes C(1) C(2) C(3) 120.9(1) . 1_555 1_555 yes C(2) C(3) C(4) 120.2(1) . 1_555 1_555 yes C(3) C(4) C(5) 120.6(1) . 1_555 1_555 yes C(4) C(5) C(6) 116.9(1) . 1_555 1_555 yes C(4) C(5) C(7) 122.6(1) . 1_555 1_555 yes C(6) C(5) C(7) 120.4(1) . 1_555 1_555 yes F(1) C(6) C(1) 118.3(1) . 1_555 1_555 yes F(1) C(6) C(5) 117.4(1) . 1_555 1_555 yes C(1) C(6) C(5) 124.3(1) . 1_555 1_555 yes S(1) C(7) C(5) 112.04(10) . 1_555 1_555 yes S(1) C(8) C(9) 111.33(9) . 1_555 1_555 yes C(8) C(9) C(10) 120.2(1) . 1_555 1_555 yes C(8) C(9) C(14) 120.8(1) . 1_555 1_555 yes C(10) C(9) C(14) 118.8(1) . 1_555 1_555 yes C(9) C(10) C(11) 121.9(1) . 1_555 1_555 yes C(10) C(11) C(12) 117.1(1) . 1_555 1_555 yes C(10) C(11) C(26) 121.8(1) . 1_555 1_555 yes C(12) C(11) C(26) 120.8(1) . 1_555 1_555 yes C(11) C(12) C(13) 123.0(1) . 1_555 1_555 yes C(12) C(13) C(14) 117.8(1) . 1_555 1_555 yes C(12) C(13) C(15) 119.6(1) . 1_555 1_555 yes C(14) C(13) C(15) 122.4(1) . 1_555 1_555 yes O(1) C(14) C(9) 119.2(1) . 1_555 1_555 yes O(1) C(14) C(13) 119.5(1) . 1_555 1_555 yes C(9) C(14) C(13) 121.2(1) . 1_555 1_555 yes C(13) C(15) C(16) 108.4(1) . 1_555 1_555 yes C(15) C(16) C(17) 120.9(1) . 1_555 1_555 yes C(15) C(16) C(21) 120.4(1) . 1_555 1_555 yes C(17) C(16) C(21) 118.1(1) . 1_555 1_555 yes C(16) C(17) C(18) 122.4(1) . 1_555 1_555 yes C(17) C(18) C(19) 117.5(1) . 1_555 1_555 yes C(17) C(18) C(30) 119.1(1) . 1_555 1_555 yes C(19) C(18) C(30) 123.3(1) . 1_555 1_555 yes C(18) C(19) C(20) 122.2(1) . 1_555 1_555 yes C(19) C(20) C(21) 118.4(1) . 1_555 1_555 yes C(19) C(20) C(22) 120.9(1) . 1_555 1_555 yes C(21) C(20) C(22) 120.7(1) . 1_555 1_555 yes O(2) C(21) C(16) 118.7(1) . 1_555 1_555 yes O(2) C(21) C(20) 119.9(1) . 1_555 1_555 yes C(16) C(21) C(20) 121.3(1) . 1_555 1_555 yes S(2) C(22) C(20) 115.62(9) . 1_555 1_555 yes S(2) C(23) C(1) 112.25(10) . 1_555 1_555 yes C(11) C(26) C(27) 111.5(1) . 1_555 1_555 yes C(11) C(26) C(28) 107.8(1) . 1_555 1_555 yes C(11) C(26) C(29) 110.9(1) . 1_555 1_555 yes C(27) C(26) C(28) 108.7(1) . 1_555 1_555 yes C(27) C(26) C(29) 108.1(1) . 1_555 1_555 yes C(28) C(26) C(29) 109.8(1) . 1_555 1_555 yes C(18) C(30) C(31) 110.0(1) . 1_555 1_555 yes C(18) C(30) C(32) 108.7(1) . 1_555 1_555 yes C(18) C(30) C(33) 112.5(1) . 1_555 1_555 yes C(31) C(30) C(32) 109.5(1) . 1_555 1_555 yes C(31) C(30) C(33) 108.1(1) . 1_555 1_555 yes C(32) C(30) C(33) 107.9(1) . 1_555 1_555 yes #----------------------------------------------------------------------- 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 S(1) C(7) C(5) C(4) 102.3(1) 1_555 1_555 1_555 1_555 yes S(1) C(7) C(5) C(6) -81.6(1) 1_555 1_555 1_555 1_555 yes S(1) C(8) C(9) C(10) -74.3(1) 1_555 1_555 1_555 1_555 yes S(1) C(8) C(9) C(14) 100.0(1) 1_555 1_555 1_555 1_555 yes S(2) C(22) C(20) C(19) 50.5(2) 1_555 1_555 1_555 1_555 yes S(2) C(22) C(20) C(21) -130.7(1) 1_555 1_555 1_555 1_555 yes S(2) C(23) C(1) C(2) 58.9(2) 1_555 1_555 1_555 1_555 yes S(2) C(23) C(1) C(6) -116.7(1) 1_555 1_555 1_555 1_555 yes F(1) C(6) C(1) C(2) 179.2(1) 1_555 1_555 1_555 1_555 yes F(1) C(6) C(1) C(23) -5.0(2) 1_555 1_555 1_555 1_555 yes F(1) C(6) C(5) C(4) -179.7(1) 1_555 1_555 1_555 1_555 yes F(1) C(6) C(5) C(7) 4.0(2) 1_555 1_555 1_555 1_555 yes O(1) C(14) C(9) C(8) 5.3(2) 1_555 1_555 1_555 1_555 yes O(1) C(14) C(9) C(10) 179.6(1) 1_555 1_555 1_555 1_555 yes O(1) C(14) C(13) C(12) 179.1(1) 1_555 1_555 1_555 1_555 yes O(1) C(14) C(13) C(15) -6.7(2) 1_555 1_555 1_555 1_555 yes O(2) C(21) C(16) C(15) 7.0(2) 1_555 1_555 1_555 1_555 yes O(2) C(21) C(16) C(17) 178.7(1) 1_555 1_555 1_555 1_555 yes O(2) C(21) C(20) C(19) -177.1(1) 1_555 1_555 1_555 1_555 yes O(2) C(21) C(20) C(22) 4.1(2) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 0.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 2.3(2) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(7) -174.0(1) 1_555 1_555 1_555 1_555 yes C(1) C(23) S(2) C(22) 55.9(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) -2.8(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -1.3(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 1.2(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(23) -174.6(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -0.2(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(7) 176.1(1) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(1) C(23) 173.0(1) 1_555 1_555 1_555 1_555 yes C(5) C(7) S(1) C(8) 141.44(10) 1_555 1_555 1_555 1_555 yes C(7) S(1) C(8) C(9) -60.1(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 174.3(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(14) C(13) -170.3(1) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) -2.4(2) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(26) -176.5(1) 1_555 1_555 1_555 1_555 yes C(9) C(14) O(1) C(24) 101.0(1) 1_555 1_555 1_555 1_555 yes C(9) C(14) C(13) C(12) -5.3(2) 1_555 1_555 1_555 1_555 yes C(9) C(14) C(13) C(15) 168.8(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(14) C(13) 4.0(2) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) 1.0(2) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(27) -155.7(1) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(28) 85.1(2) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(29) -35.1(2) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(14) 0.0(2) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 2.8(2) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(15) -171.6(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(27) 30.5(2) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(28) -88.8(2) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(29) 151.0(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(15) C(16) 47.3(2) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(11) C(26) 175.2(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) O(1) C(24) -83.4(1) 1_555 1_555 1_555 1_555 yes C(13) C(15) C(16) C(17) -98.2(1) 1_555 1_555 1_555 1_555 yes C(13) C(15) C(16) C(21) 73.2(2) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(15) C(16) -126.8(1) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) 169.5(1) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(21) C(20) -169.5(1) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) 0.5(2) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(30) -176.7(1) 1_555 1_555 1_555 1_555 yes C(16) C(21) O(2) C(25) 95.6(1) 1_555 1_555 1_555 1_555 yes C(16) C(21) C(20) C(19) -0.5(2) 1_555 1_555 1_555 1_555 yes C(16) C(21) C(20) C(22) -179.4(1) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(21) C(20) 2.2(2) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 1.2(2) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(31) -54.1(2) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(32) 65.8(2) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(33) -174.7(1) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(16) C(21) -2.2(2) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) -1.2(2) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(22) 177.6(1) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(31) 128.8(1) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(32) -111.3(2) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(33) 8.2(2) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(18) C(30) 178.3(1) 1_555 1_555 1_555 1_555 yes C(20) C(21) O(2) C(25) -87.8(2) 1_555 1_555 1_555 1_555 yes C(20) C(22) S(2) C(23) 72.7(1) 1_555 1_555 1_555 1_555 yes #----------------------------------------------------------------------- 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(2) C(29) 3.569(2) . 4_565 ? O(1) C(4) 3.346(2) . 2_547 ? O(1) C(3) 3.499(2) . 2_547 ? #----------------------------------------------------------------------- data_Amino[1.3.3]MCP _database_code_CSD 119382 #---------------------------------------------------------------------- _audit_creation_date 'Tue Apr 27 12:34:30 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #---------------------------------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #---------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 549.83 _chemical_formula_analytical 'C33 H43 N O2 S2 ' _chemical_formula_sum 'C33 H43 N O2 S2 ' _chemical_formula_moiety 'C33 H43 N O2 S2 ' _chemical_formula_structural ? _chemical_melting_point ? #---------------------------------------------------------------------- _cell_length_a 13.415(2) _cell_length_b 14.115(4) _cell_length_c 16.489(6) _cell_angle_alpha 90 _cell_angle_beta 95.63(2) _cell_angle_gamma 90 _cell_volume 3107(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 28.3 _cell_measurement_theta_max 28.5 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1184.00 _exptl_absorpt_coefficient_mu 1.765 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #---------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.40 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -2 3 0 -3 2 0 -3 1 _diffrn_reflns_number 5029 _reflns_number_total 4845 _reflns_number_gt 3433 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 60.09 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05550 _diffrn_orient_matrix_UB_12 -0.04744 _diffrn_orient_matrix_UB_13 0.00755 _diffrn_orient_matrix_UB_21 0.04848 _diffrn_orient_matrix_UB_22 0.05189 _diffrn_orient_matrix_UB_23 0.01671 _diffrn_orient_matrix_UB_31 -0.01344 _diffrn_orient_matrix_UB_32 -0.00876 _diffrn_orient_matrix_UB_33 0.05812 #---------------------------------------------------------------------- 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 S 0 8 0.333 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 132 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 172 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #---------------------------------------------------------------------- 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 S(1) S 0.22549(9) 0.20983(10) 0.46110(7) 0.0834(4) Uani 1.00 d . . . S(2) S 0.66900(9) 0.1286(1) 0.69013(8) 0.0892(4) Uani 1.00 d . . . O(1) O 0.4055(2) -0.0274(2) 0.5820(2) 0.0711(9) Uani 1.00 d . . . O(2) O 0.5711(2) -0.0854(2) 0.7113(2) 0.0746(9) Uani 1.00 d . . . N(1) N 0.4002(3) 0.1902(3) 0.6834(2) 0.082(1) Uani 1.00 d . . . C(1) C 0.2694(3) 0.2771(3) 0.5510(3) 0.081(2) Uani 1.00 d . . . C(2) C 0.2794(3) 0.0948(3) 0.4842(3) 0.075(1) Uani 1.00 d . . . C(3) C 0.2439(3) 0.0439(3) 0.5583(2) 0.063(1) Uani 1.00 d . . . C(4) C 0.1488(3) 0.0592(3) 0.5826(3) 0.066(1) Uani 1.00 d . . . C(5) C 0.1179(3) 0.0133(3) 0.6511(2) 0.063(1) Uani 1.00 d . . . C(6) C 0.1859(3) -0.0462(3) 0.6943(2) 0.064(1) Uani 1.00 d . . . C(7) C 0.2810(3) -0.0621(3) 0.6726(2) 0.059(1) Uani 1.00 d . . . C(8) C 0.3088(3) -0.0159(3) 0.6025(2) 0.062(1) Uani 1.00 d . . . C(9) C 0.4192(4) -0.1049(4) 0.5281(3) 0.103(2) Uani 1.00 d . . . C(10) C 0.0146(3) 0.0313(3) 0.6801(3) 0.075(1) Uani 1.00 d . . . C(11) C -0.0478(4) 0.0985(5) 0.6271(4) 0.124(2) Uani 1.00 d . . . C(12) C -0.0428(4) -0.0623(4) 0.6778(4) 0.121(2) Uani 1.00 d . . . C(13) C 0.0247(4) 0.0668(5) 0.7669(4) 0.134(3) Uani 1.00 d . . . C(14) C 0.3585(3) -0.1178(3) 0.7258(3) 0.068(1) Uani 1.00 d . . . C(15) C 0.4242(3) -0.0505(3) 0.7785(2) 0.062(1) Uani 1.00 d . . . C(16) C 0.3791(3) 0.0053(3) 0.8359(2) 0.064(1) Uani 1.00 d . . . C(17) C 0.4306(3) 0.0751(3) 0.8811(2) 0.064(1) Uani 1.00 d . . . C(18) C 0.5288(3) 0.0924(3) 0.8661(2) 0.069(1) Uani 1.00 d . . . C(19) C 0.5767(3) 0.0389(3) 0.8097(2) 0.068(1) Uani 1.00 d . . . C(20) C 0.5229(3) -0.0330(3) 0.7683(2) 0.065(1) Uani 1.00 d . . . C(21) C 0.6124(4) -0.1716(4) 0.7420(4) 0.113(2) Uani 1.00 d . . . C(22) C 0.3782(3) 0.1373(4) 0.9405(3) 0.079(1) Uani 1.00 d . . . C(23) C 0.3352(9) 0.2166(6) 0.9016(4) 0.362(4) Uani 1.00 d . . . C(24) C 0.3027(6) 0.0782(7) 0.9800(5) 0.226(3) Uani 1.00 d . . . C(25) C 0.4481(5) 0.1624(6) 1.0130(4) 0.163(3) Uani 1.00 d . . . C(26) C 0.6789(3) 0.0669(4) 0.7886(3) 0.079(1) Uani 1.00 d . . . C(27) C 0.6079(3) 0.2385(3) 0.7144(3) 0.079(1) Uani 1.00 d . . . C(28) C 0.5425(3) 0.2753(3) 0.6424(3) 0.073(1) Uani 1.00 d . . . C(29) C 0.5833(4) 0.3372(4) 0.5889(3) 0.092(2) Uani 1.00 d . . . C(30) C 0.5256(4) 0.3746(4) 0.5233(3) 0.103(2) Uani 1.00 d . . . C(31) C 0.4255(4) 0.3544(4) 0.5117(3) 0.093(2) Uani 1.00 d . . . C(32) C 0.3805(3) 0.2921(3) 0.5643(3) 0.072(1) Uani 1.00 d . . . C(33) C 0.4409(3) 0.2523(3) 0.6288(3) 0.068(1) Uani 1.00 d . . . H(1) H 0.2351 0.3381 0.5492 0.0959 Uiso 1.00 calc . . . H(2) H 0.2475 0.2448 0.5989 0.0959 Uiso 1.00 calc . . . H(3) H 0.3515 0.1004 0.4918 0.0905 Uiso 1.00 calc . . . H(4) H 0.2650 0.0541 0.4362 0.0905 Uiso 1.00 calc . . . H(5) H 0.1034 0.1041 0.5520 0.0797 Uiso 1.00 calc . . . H(6) H 0.1655 -0.0772 0.7428 0.0772 Uiso 1.00 calc . . . H(7) H 0.3996 -0.1648 0.5502 0.1207 Uiso 1.00 calc . . . H(8) H 0.3767 -0.0978 0.4761 0.1207 Uiso 1.00 calc . . . H(9) H 0.4862 -0.1111 0.5144 0.1207 Uiso 1.00 calc . . . H(10) H -0.0169 0.1602 0.6248 0.1410 Uiso 1.00 calc . . . H(11) H -0.0563 0.0760 0.5701 0.1410 Uiso 1.00 calc . . . H(12) H -0.1140 0.1076 0.6426 0.1410 Uiso 1.00 calc . . . H(13) H -0.0502 -0.0889 0.6228 0.1419 Uiso 1.00 calc . . . H(14) H -0.1080 -0.0575 0.6953 0.1419 Uiso 1.00 calc . . . H(15) H -0.0065 -0.1102 0.7116 0.1419 Uiso 1.00 calc . . . H(16) H -0.0372 0.0800 0.7880 0.1519 Uiso 1.00 calc . . . H(17) H 0.0621 0.0236 0.8036 0.1519 Uiso 1.00 calc . . . H(18) H 0.0634 0.1267 0.7711 0.1519 Uiso 1.00 calc . . . H(19) H 0.3985 -0.1554 0.6923 0.0821 Uiso 1.00 calc . . . H(20) H 0.3258 -0.1620 0.7596 0.0821 Uiso 1.00 calc . . . H(21) H 0.3086 -0.0050 0.8442 0.0762 Uiso 1.00 calc . . . H(22) H 0.5656 0.1440 0.8962 0.0826 Uiso 1.00 calc . . . H(23) H 0.6459 -0.2059 0.7031 0.1306 Uiso 1.00 calc . . . H(24) H 0.5621 -0.2128 0.7613 0.1306 Uiso 1.00 calc . . . H(25) H 0.6616 -0.1610 0.7893 0.1306 Uiso 1.00 calc . . . H(26) H 0.2792 0.1892 0.8595 0.3579 Uiso 1.00 calc . . . H(27) H 0.2938 0.2502 0.9380 0.3579 Uiso 1.00 calc . . . H(28) H 0.3734 0.2527 0.8759 0.3579 Uiso 1.00 calc . . . H(29) H 0.2510 0.0558 0.9404 0.2444 Uiso 1.00 calc . . . H(30) H 0.2725 0.1109 1.0216 0.2444 Uiso 1.00 calc . . . H(31) H 0.3349 0.0216 1.0053 0.2444 Uiso 1.00 calc . . . H(32) H 0.4178 0.1952 1.0559 0.1750 Uiso 1.00 calc . . . H(33) H 0.4800 0.1056 1.0402 0.1750 Uiso 1.00 calc . . . H(34) H 0.5046 0.2013 1.0005 0.1750 Uiso 1.00 calc . . . H(35) H 0.7207 0.0110 0.7869 0.0966 Uiso 1.00 calc . . . H(36) H 0.7112 0.1071 0.8312 0.0966 Uiso 1.00 calc . . . H(37) H 0.6576 0.2863 0.7336 0.0925 Uiso 1.00 calc . . . H(38) H 0.5679 0.2290 0.7608 0.0925 Uiso 1.00 calc . . . H(39) H 0.6541 0.3552 0.5973 0.1108 Uiso 1.00 calc . . . H(40) H 0.5560 0.4151 0.4839 0.1201 Uiso 1.00 calc . . . H(41) H 0.3832 0.3838 0.4648 0.1123 Uiso 1.00 calc . . . H(42) H 0.4406 0.1636 0.7298 0.0945 Uiso 1.00 calc . . . H(43) H 0.3306 0.1725 0.6767 0.0945 Uiso 1.00 calc . . . 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(1) 0.0717(7) 0.0983(9) 0.0781(7) 0.0024(7) -0.0026(6) 0.0216(7) S(2) 0.0697(7) 0.1106(10) 0.0895(8) 0.0074(7) 0.0199(6) -0.0061(8) O(1) 0.053(2) 0.082(2) 0.078(2) 0.001(1) 0.005(1) -0.003(2) O(2) 0.070(2) 0.081(2) 0.073(2) 0.021(2) 0.009(1) -0.002(2) N(1) 0.073(2) 0.097(3) 0.075(2) -0.023(2) 0.004(2) 0.014(2) C(1) 0.072(3) 0.082(3) 0.088(3) 0.007(3) 0.011(2) 0.004(3) C(2) 0.065(3) 0.087(3) 0.074(3) 0.004(2) 0.009(2) 0.010(3) C(3) 0.053(2) 0.072(3) 0.062(2) -0.006(2) -0.001(2) 0.005(2) C(4) 0.054(2) 0.073(3) 0.068(3) 0.001(2) -0.001(2) 0.004(2) C(5) 0.048(2) 0.068(3) 0.071(3) -0.005(2) 0.004(2) -0.001(2) C(6) 0.059(2) 0.065(3) 0.067(3) -0.008(2) 0.003(2) 0.004(2) C(7) 0.055(2) 0.056(2) 0.065(2) -0.003(2) -0.004(2) -0.005(2) C(8) 0.048(2) 0.068(3) 0.067(2) -0.005(2) -0.001(2) -0.009(2) C(9) 0.096(4) 0.107(4) 0.109(4) 0.005(3) 0.034(3) -0.030(3) C(10) 0.055(2) 0.085(3) 0.087(3) -0.003(2) 0.011(2) 0.008(3) C(11) 0.071(3) 0.160(6) 0.148(5) 0.035(3) 0.040(3) 0.051(4) C(12) 0.070(3) 0.116(5) 0.182(6) -0.017(3) 0.029(4) 0.019(4) C(13) 0.096(4) 0.200(7) 0.110(4) 0.018(4) 0.029(3) -0.038(5) C(14) 0.067(3) 0.064(3) 0.073(3) 0.000(2) 0.001(2) 0.001(2) C(15) 0.059(2) 0.066(3) 0.058(2) 0.011(2) -0.002(2) 0.002(2) C(16) 0.055(2) 0.076(3) 0.062(2) 0.006(2) 0.005(2) 0.004(2) C(17) 0.058(2) 0.075(3) 0.057(2) 0.008(2) -0.001(2) -0.002(2) C(18) 0.060(2) 0.081(3) 0.063(2) 0.004(2) -0.008(2) -0.006(2) C(19) 0.050(2) 0.087(3) 0.065(3) 0.007(2) -0.002(2) 0.000(2) C(20) 0.055(2) 0.077(3) 0.061(2) 0.015(2) 0.001(2) -0.002(2) C(21) 0.110(4) 0.114(4) 0.118(4) 0.053(3) 0.022(3) 0.005(4) C(22) 0.075(3) 0.095(3) 0.067(3) 0.012(3) 0.013(2) -0.016(3) C(23) 0.68(1) 0.309(6) 0.120(5) 0.414(6) 0.143(6) 0.081(5) C(24) 0.194(6) 0.257(9) 0.253(7) -0.075(6) 0.164(4) -0.147(6) C(25) 0.153(6) 0.208(7) 0.131(5) 0.010(6) 0.028(4) -0.087(5) C(26) 0.057(2) 0.103(4) 0.076(3) 0.009(3) -0.002(2) -0.005(3) C(27) 0.062(3) 0.083(3) 0.094(3) -0.006(2) 0.011(2) -0.020(3) C(28) 0.064(3) 0.069(3) 0.087(3) -0.005(2) 0.013(2) -0.008(3) C(29) 0.074(3) 0.089(4) 0.117(4) -0.016(3) 0.024(3) 0.007(3) C(30) 0.090(3) 0.103(4) 0.121(4) -0.016(3) 0.030(3) 0.026(3) C(31) 0.091(3) 0.083(3) 0.106(4) -0.001(3) 0.018(3) 0.019(3) C(32) 0.067(3) 0.068(3) 0.083(3) -0.002(2) 0.013(2) 0.000(3) C(33) 0.066(3) 0.062(3) 0.078(3) -0.006(2) 0.015(2) -0.007(2) #---------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0165(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3433 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0664 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.644 _refine_ls_shift/su_max 0.2400 _refine_ls_shift/su_mean 0.0080 _refine_diff_density_min -0.39 _refine_diff_density_max 0.53 #---------------------------------------------------------------------- _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(1) C(1) 1.810(5) 1_555 1_555 yes S(1) C(2) 1.803(5) 1_555 1_555 yes S(2) C(26) 1.837(5) 1_555 1_555 yes S(2) C(27) 1.817(5) 1_555 1_555 yes O(1) C(8) 1.383(4) 1_555 1_555 yes O(1) C(9) 1.433(6) 1_555 1_555 yes O(2) C(20) 1.402(5) 1_555 1_555 yes O(2) C(21) 1.410(6) 1_555 1_555 yes N(1) C(33) 1.405(5) 1_555 1_555 yes N(1) H(42) 0.970 1_555 1_555 no N(1) H(43) 0.962 1_555 1_555 no C(1) C(32) 1.501(6) 1_555 1_555 yes C(1) H(1) 0.975 1_555 1_555 no C(1) H(2) 0.981 1_555 1_555 no C(2) C(3) 1.534(6) 1_555 1_555 yes C(2) H(3) 0.966 1_555 1_555 no C(2) H(4) 0.981 1_555 1_555 no C(3) C(4) 1.390(5) 1_555 1_555 yes C(3) C(8) 1.370(5) 1_555 1_555 yes C(4) C(5) 1.400(6) 1_555 1_555 yes C(4) H(5) 0.983 1_555 1_555 no C(5) C(6) 1.385(5) 1_555 1_555 yes C(5) C(10) 1.531(6) 1_555 1_555 yes C(6) C(7) 1.376(5) 1_555 1_555 yes C(6) H(6) 0.975 1_555 1_555 no C(7) C(8) 1.408(5) 1_555 1_555 yes C(7) C(14) 1.513(5) 1_555 1_555 yes C(9) H(7) 0.968 1_555 1_555 no C(9) H(8) 0.986 1_555 1_555 no C(9) H(9) 0.952 1_555 1_555 no C(10) C(11) 1.490(7) 1_555 1_555 yes C(10) C(12) 1.527(7) 1_555 1_555 yes C(10) C(13) 1.509(7) 1_555 1_555 yes C(11) H(10) 0.967 1_555 1_555 no C(11) H(11) 0.987 1_555 1_555 no C(11) H(12) 0.956 1_555 1_555 no C(12) H(13) 0.977 1_555 1_555 no C(12) H(14) 0.950 1_555 1_555 no C(12) H(15) 0.976 1_555 1_555 no C(13) H(16) 0.950 1_555 1_555 no C(13) H(17) 0.965 1_555 1_555 no C(13) H(18) 0.990 1_555 1_555 no C(14) C(15) 1.512(6) 1_555 1_555 yes C(14) H(19) 0.967 1_555 1_555 no C(14) H(20) 0.969 1_555 1_555 no C(15) C(16) 1.411(6) 1_555 1_555 yes C(15) C(20) 1.374(5) 1_555 1_555 yes C(16) C(17) 1.380(6) 1_555 1_555 yes C(16) H(21) 0.980 1_555 1_555 no C(17) C(18) 1.385(6) 1_555 1_555 yes C(17) C(22) 1.537(6) 1_555 1_555 yes C(18) C(19) 1.402(6) 1_555 1_555 yes C(18) H(22) 0.986 1_555 1_555 no C(19) C(20) 1.385(6) 1_555 1_555 yes C(19) C(26) 1.499(6) 1_555 1_555 yes C(21) H(23) 0.951 1_555 1_555 no C(21) H(24) 0.968 1_555 1_555 no C(21) H(25) 0.981 1_555 1_555 no C(22) C(23) 1.387(8) 1_555 1_555 yes C(22) C(24) 1.509(9) 1_555 1_555 yes C(22) C(25) 1.488(8) 1_555 1_555 yes C(23) H(26) 1.046 1_555 1_555 no C(23) H(27) 0.980 1_555 1_555 no C(23) H(28) 0.863 1_555 1_555 no C(24) H(29) 0.958 1_555 1_555 no C(24) H(30) 0.950 1_555 1_555 no C(24) H(31) 0.981 1_555 1_555 no C(25) H(32) 0.968 1_555 1_555 no C(25) H(33) 0.995 1_555 1_555 no C(25) H(34) 0.975 1_555 1_555 no C(26) H(35) 0.970 1_555 1_555 no C(26) H(36) 0.970 1_555 1_555 no C(27) C(28) 1.498(6) 1_555 1_555 yes C(27) H(37) 0.978 1_555 1_555 no C(27) H(38) 0.985 1_555 1_555 no C(28) C(29) 1.392(6) 1_555 1_555 yes C(28) C(33) 1.398(6) 1_555 1_555 yes C(29) C(30) 1.372(7) 1_555 1_555 yes C(29) H(39) 0.980 1_555 1_555 no C(30) C(31) 1.368(7) 1_555 1_555 yes C(30) H(40) 0.983 1_555 1_555 no C(31) C(32) 1.411(6) 1_555 1_555 yes C(31) H(41) 1.003 1_555 1_555 no C(32) C(33) 1.391(6) 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(1) S(1) C(2) 102.0(2) 1_555 1_555 1_555 yes C(26) S(2) C(27) 101.8(2) 1_555 1_555 1_555 yes C(8) O(1) C(9) 114.9(3) 1_555 1_555 1_555 yes C(20) O(2) C(21) 114.0(4) 1_555 1_555 1_555 yes C(33) N(1) H(42) 121.7(4) 1_555 1_555 1_555 no C(33) N(1) H(43) 121.5(4) 1_555 1_555 1_555 no H(42) N(1) H(43) 116.8(4) 1_555 1_555 1_555 no S(1) C(1) C(32) 115.6(3) 1_555 1_555 1_555 yes S(1) C(1) H(1) 108.8(3) 1_555 1_555 1_555 no S(1) C(1) H(2) 108.5(4) 1_555 1_555 1_555 no C(32) C(1) H(1) 109.7(4) 1_555 1_555 1_555 no C(32) C(1) H(2) 108.7(4) 1_555 1_555 1_555 no H(1) C(1) H(2) 104.9(4) 1_555 1_555 1_555 no S(1) C(2) C(3) 116.1(3) 1_555 1_555 1_555 yes S(1) C(2) H(3) 109.2(4) 1_555 1_555 1_555 no S(1) C(2) H(4) 108.3(3) 1_555 1_555 1_555 no C(3) C(2) H(3) 108.7(4) 1_555 1_555 1_555 no C(3) C(2) H(4) 108.4(4) 1_555 1_555 1_555 no H(3) C(2) H(4) 105.6(4) 1_555 1_555 1_555 no C(2) C(3) C(4) 121.5(4) 1_555 1_555 1_555 yes C(2) C(3) C(8) 118.8(4) 1_555 1_555 1_555 yes C(4) C(3) C(8) 119.7(4) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.9(4) 1_555 1_555 1_555 yes C(3) C(4) H(5) 119.5(4) 1_555 1_555 1_555 no C(5) C(4) H(5) 119.6(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 117.5(4) 1_555 1_555 1_555 yes C(4) C(5) C(10) 121.6(4) 1_555 1_555 1_555 yes C(6) C(5) C(10) 120.8(4) 1_555 1_555 1_555 yes C(5) C(6) C(7) 123.1(4) 1_555 1_555 1_555 yes C(5) C(6) H(6) 118.0(4) 1_555 1_555 1_555 no C(7) C(6) H(6) 118.9(4) 1_555 1_555 1_555 no C(6) C(7) C(8) 117.7(4) 1_555 1_555 1_555 yes C(6) C(7) C(14) 122.3(4) 1_555 1_555 1_555 yes C(8) C(7) C(14) 119.7(3) 1_555 1_555 1_555 yes O(1) C(8) C(3) 120.3(4) 1_555 1_555 1_555 yes O(1) C(8) C(7) 118.5(3) 1_555 1_555 1_555 yes C(3) C(8) C(7) 121.1(4) 1_555 1_555 1_555 yes O(1) C(9) H(7) 112.2(4) 1_555 1_555 1_555 no O(1) C(9) H(8) 111.3(5) 1_555 1_555 1_555 no O(1) C(9) H(9) 113.5(5) 1_555 1_555 1_555 no H(7) C(9) H(8) 105.1(5) 1_555 1_555 1_555 no H(7) C(9) H(9) 107.8(5) 1_555 1_555 1_555 no H(8) C(9) H(9) 106.4(5) 1_555 1_555 1_555 no C(5) C(10) C(11) 113.3(4) 1_555 1_555 1_555 yes C(5) C(10) C(12) 108.5(4) 1_555 1_555 1_555 yes C(5) C(10) C(13) 110.6(4) 1_555 1_555 1_555 yes C(11) C(10) C(12) 106.4(4) 1_555 1_555 1_555 yes C(11) C(10) C(13) 109.8(5) 1_555 1_555 1_555 yes C(12) C(10) C(13) 108.0(5) 1_555 1_555 1_555 yes C(10) C(11) H(10) 112.2(5) 1_555 1_555 1_555 no C(10) C(11) H(11) 111.1(5) 1_555 1_555 1_555 no C(10) C(11) H(12) 114.3(5) 1_555 1_555 1_555 no H(10) C(11) H(11) 105.1(5) 1_555 1_555 1_555 no H(10) C(11) H(12) 107.6(6) 1_555 1_555 1_555 no H(11) C(11) H(12) 106.0(5) 1_555 1_555 1_555 no C(10) C(12) H(13) 111.2(5) 1_555 1_555 1_555 no C(10) C(12) H(14) 114.1(6) 1_555 1_555 1_555 no C(10) C(12) H(15) 111.3(5) 1_555 1_555 1_555 no H(13) C(12) H(14) 107.2(5) 1_555 1_555 1_555 no H(13) C(12) H(15) 105.2(6) 1_555 1_555 1_555 no H(14) C(12) H(15) 107.3(6) 1_555 1_555 1_555 no C(10) C(13) H(16) 114.4(5) 1_555 1_555 1_555 no C(10) C(13) H(17) 112.2(6) 1_555 1_555 1_555 no C(10) C(13) H(18) 110.4(5) 1_555 1_555 1_555 no H(16) C(13) H(17) 108.2(6) 1_555 1_555 1_555 no H(16) C(13) H(18) 106.1(7) 1_555 1_555 1_555 no H(17) C(13) H(18) 105.0(6) 1_555 1_555 1_555 no C(7) C(14) C(15) 109.6(3) 1_555 1_555 1_555 yes C(7) C(14) H(19) 110.0(4) 1_555 1_555 1_555 no C(7) C(14) H(20) 110.1(4) 1_555 1_555 1_555 no C(15) C(14) H(19) 110.4(4) 1_555 1_555 1_555 no C(15) C(14) H(20) 110.2(4) 1_555 1_555 1_555 no H(19) C(14) H(20) 106.5(4) 1_555 1_555 1_555 no C(14) C(15) C(16) 118.1(4) 1_555 1_555 1_555 yes C(14) C(15) C(20) 123.9(4) 1_555 1_555 1_555 yes C(16) C(15) C(20) 117.6(4) 1_555 1_555 1_555 yes C(15) C(16) C(17) 122.4(4) 1_555 1_555 1_555 yes C(15) C(16) H(21) 119.6(4) 1_555 1_555 1_555 no C(17) C(16) H(21) 118.0(4) 1_555 1_555 1_555 no C(16) C(17) C(18) 117.6(4) 1_555 1_555 1_555 yes C(16) C(17) C(22) 121.1(4) 1_555 1_555 1_555 yes C(18) C(17) C(22) 121.1(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 122.0(4) 1_555 1_555 1_555 yes C(17) C(18) H(22) 118.5(4) 1_555 1_555 1_555 no C(19) C(18) H(22) 119.5(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 118.0(4) 1_555 1_555 1_555 yes C(18) C(19) C(26) 120.1(4) 1_555 1_555 1_555 yes C(20) C(19) C(26) 121.5(4) 1_555 1_555 1_555 yes O(2) C(20) C(15) 120.0(4) 1_555 1_555 1_555 yes O(2) C(20) C(19) 117.7(4) 1_555 1_555 1_555 yes C(15) C(20) C(19) 122.2(4) 1_555 1_555 1_555 yes O(2) C(21) H(23) 113.1(5) 1_555 1_555 1_555 no O(2) C(21) H(24) 111.9(5) 1_555 1_555 1_555 no O(2) C(21) H(25) 111.3(5) 1_555 1_555 1_555 no H(23) C(21) H(24) 107.8(6) 1_555 1_555 1_555 no H(23) C(21) H(25) 106.7(5) 1_555 1_555 1_555 no H(24) C(21) H(25) 105.5(5) 1_555 1_555 1_555 no C(17) C(22) C(23) 111.2(4) 1_555 1_555 1_555 yes C(17) C(22) C(24) 109.1(5) 1_555 1_555 1_555 yes C(17) C(22) C(25) 110.9(4) 1_555 1_555 1_555 yes C(23) C(22) C(24) 112.3(7) 1_555 1_555 1_555 yes C(23) C(22) C(25) 112.4(6) 1_555 1_555 1_555 yes C(24) C(22) C(25) 100.5(5) 1_555 1_555 1_555 yes C(22) C(23) H(26) 104.4(8) 1_555 1_555 1_555 no C(22) C(23) H(27) 110.0(6) 1_555 1_555 1_555 no C(22) C(23) H(28) 117.7(9) 1_555 1_555 1_555 no H(26) C(23) H(27) 99.9(10) 1_555 1_555 1_555 no H(26) C(23) H(28) 108.4(7) 1_555 1_555 1_555 no H(27) C(23) H(28) 114.5(9) 1_555 1_555 1_555 no C(22) C(24) H(29) 111.1(7) 1_555 1_555 1_555 no C(22) C(24) H(30) 113.2(8) 1_555 1_555 1_555 no C(22) C(24) H(31) 110.3(6) 1_555 1_555 1_555 no H(29) C(24) H(30) 108.8(7) 1_555 1_555 1_555 no H(29) C(24) H(31) 106.3(8) 1_555 1_555 1_555 no H(30) C(24) H(31) 106.9(8) 1_555 1_555 1_555 no C(22) C(25) H(32) 115.1(6) 1_555 1_555 1_555 no C(22) C(25) H(33) 112.3(6) 1_555 1_555 1_555 no C(22) C(25) H(34) 114.0(6) 1_555 1_555 1_555 no H(32) C(25) H(33) 104.5(7) 1_555 1_555 1_555 no H(32) C(25) H(34) 106.0(7) 1_555 1_555 1_555 no H(33) C(25) H(34) 103.9(7) 1_555 1_555 1_555 no S(2) C(26) C(19) 110.0(3) 1_555 1_555 1_555 yes S(2) C(26) H(35) 110.5(3) 1_555 1_555 1_555 no S(2) C(26) H(36) 110.5(4) 1_555 1_555 1_555 no C(19) C(26) H(35) 109.7(4) 1_555 1_555 1_555 no C(19) C(26) H(36) 109.9(4) 1_555 1_555 1_555 no H(35) C(26) H(36) 106.2(4) 1_555 1_555 1_555 no S(2) C(27) C(28) 111.3(3) 1_555 1_555 1_555 yes S(2) C(27) H(37) 110.6(3) 1_555 1_555 1_555 no S(2) C(27) H(38) 110.3(4) 1_555 1_555 1_555 no C(28) C(27) H(37) 110.2(4) 1_555 1_555 1_555 no C(28) C(27) H(38) 109.9(4) 1_555 1_555 1_555 no H(37) C(27) H(38) 104.4(4) 1_555 1_555 1_555 no C(27) C(28) C(29) 119.0(4) 1_555 1_555 1_555 yes C(27) C(28) C(33) 122.2(4) 1_555 1_555 1_555 yes C(29) C(28) C(33) 118.8(4) 1_555 1_555 1_555 yes C(28) C(29) C(30) 121.0(5) 1_555 1_555 1_555 yes C(28) C(29) H(39) 120.5(5) 1_555 1_555 1_555 no C(30) C(29) H(39) 118.5(5) 1_555 1_555 1_555 no C(29) C(30) C(31) 120.0(5) 1_555 1_555 1_555 yes C(29) C(30) H(40) 120.4(5) 1_555 1_555 1_555 no C(31) C(30) H(40) 119.6(5) 1_555 1_555 1_555 no C(30) C(31) C(32) 121.1(5) 1_555 1_555 1_555 yes C(30) C(31) H(41) 119.7(5) 1_555 1_555 1_555 no C(32) C(31) H(41) 119.2(5) 1_555 1_555 1_555 no C(1) C(32) C(31) 118.5(4) 1_555 1_555 1_555 yes C(1) C(32) C(33) 123.3(4) 1_555 1_555 1_555 yes C(31) C(32) C(33) 118.1(4) 1_555 1_555 1_555 yes N(1) C(33) C(28) 118.4(4) 1_555 1_555 1_555 yes N(1) C(33) C(32) 120.6(4) 1_555 1_555 1_555 yes C(28) C(33) C(32) 121.0(4) 1_555 1_555 1_555 yes #---------------------------------------------------------------------- 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 C(12) C(27) 3.484(8) 1_555 2_546 ? #---------------------------------------------------------------------- data_[1.3.3]OH _database_code_CSD 163959 #----------------------------------------------------------------------- _audit_creation_date 'Fri Feb 23 17:05:15 2001' _audit_creation_method 'by teXsan' _audit_update_record ? # CHEMICAL DATA _chemical_formula_sum 'C33 H42 O3 S2 ' _chemical_formula_moiety 'C33 H42 O3 S2 ' _chemical_formula_weight 550.81 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.497(2) _cell_length_b 16.640(3) _cell_length_c 15.500(2) _cell_angle_alpha 90 _cell_angle_beta 94.727(4) _cell_angle_gamma 90 _cell_volume 2955.2(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12684 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 93.2 #----------------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13622 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.00 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6093 _reflns_number_gt 1914 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2359 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1914 _refine_ls_number_parameters 343 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 0.35 _refine_diff_density_min -0.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 S(1) S 1.0933(1) 0.2472(1) 1.1192(1) 0.0369(5) Uani 1.00 d . . . S(2) S 0.6853(2) 0.5046(1) 1.2801(1) 0.0374(5) Uani 1.00 d . . . O(1) O 0.9103(4) 0.3970(3) 1.1531(3) 0.034(1) Uani 1.00 d . . . O(2) O 0.9471(3) 0.3525(3) 0.9794(3) 0.033(1) Uani 1.00 d . . . O(3) O 0.7422(4) 0.4937(3) 0.9965(3) 0.035(1) Uani 1.00 d . . . C(1) C 0.8613(5) 0.3861(4) 1.2973(4) 0.032(2) Uani 1.00 d . . . C(2) C 0.8476(6) 0.3415(5) 1.3709(4) 0.035(2) Uani 1.00 d . . . C(3) C 0.8719(5) 0.2597(5) 1.3710(4) 0.039(2) Uani 1.00 d . . . C(4) C 0.9056(6) 0.2233(4) 1.2973(5) 0.037(2) Uani 1.00 d . . . C(5) C 0.9169(5) 0.2656(4) 1.2219(4) 0.027(1) Uani 1.00 d . . . C(6) C 0.8978(5) 0.3485(4) 1.2222(4) 0.030(2) Uani 1.00 d . . . C(7) C 0.9447(5) 0.2218(4) 1.1408(4) 0.034(2) Uani 1.00 d . . . C(8) C 1.0994(6) 0.2164(4) 1.0062(4) 0.038(2) Uani 1.00 d . . . C(9) C 0.9847(5) 0.2139(4) 0.9527(4) 0.032(2) Uani 1.00 d . . . C(10) C 0.9409(5) 0.1396(4) 0.9194(4) 0.031(2) Uani 1.00 d . . . C(11) C 0.8307(5) 0.1322(4) 0.8750(4) 0.031(2) Uani 1.00 d . . . C(12) C 0.7638(5) 0.2012(4) 0.8633(4) 0.028(1) Uani 1.00 d . . . C(13) C 0.8039(5) 0.2761(4) 0.8955(4) 0.030(2) Uani 1.00 d . . . C(14) C 0.9132(6) 0.2802(4) 0.9381(4) 0.030(2) Uani 1.00 d . . . C(15) C 0.7222(5) 0.3470(4) 0.8932(4) 0.030(2) Uani 1.00 d . . . C(16) C 0.6741(5) 0.3568(4) 0.9804(4) 0.029(1) Uani 1.00 d . . . C(17) C 0.6225(5) 0.2904(4) 1.0178(4) 0.028(1) Uani 1.00 d . . . C(18) C 0.5817(5) 0.2932(4) 1.1015(4) 0.029(2) Uani 1.00 d . . . C(19) C 0.5963(5) 0.3654(4) 1.1476(4) 0.030(2) Uani 1.00 d . . . C(20) C 0.6476(5) 0.4322(4) 1.1119(5) 0.035(2) Uani 1.00 d . . . C(21) C 0.6858(5) 0.4273(4) 1.0286(4) 0.032(2) Uani 1.00 d . . . C(22) C 0.6638(6) 0.5108(4) 1.1639(4) 0.038(2) Uani 1.00 d . . . C(23) C 0.8379(6) 0.4763(4) 1.2984(4) 0.039(2) Uani 1.00 d . . . C(24) C 1.0204(6) 0.4036(4) 0.9328(5) 0.047(2) Uani 1.00 d . . . C(25) C 0.6655(6) 0.5494(4) 0.9507(5) 0.043(2) Uani 1.00 d . . . C(26) C 0.7837(5) 0.0494(4) 0.8494(4) 0.033(2) Uani 1.00 d . . . C(27) C 0.8755(6) -0.0025(5) 0.8104(5) 0.051(2) Uani 1.00 d . . . C(28) C 0.6781(6) 0.0516(4) 0.7848(5) 0.045(2) Uani 1.00 d . . . C(29) C 0.7497(6) 0.0068(5) 0.9312(5) 0.049(2) Uani 1.00 d . . . C(30) C 0.5241(5) 0.2213(4) 1.1429(4) 0.031(2) Uani 1.00 d . . . C(31) C 0.5308(5) 0.1459(4) 1.0873(4) 0.033(2) Uani 1.00 d . . . C(32) C 0.5856(6) 0.2037(4) 1.2317(4) 0.039(2) Uani 1.00 d . . . C(33) C 0.3952(6) 0.2401(4) 1.1528(5) 0.044(2) Uani 1.00 d . . . H(1) H 0.9357 0.3650 1.1064 0.0404 Uiso 1.00 calc . . . H(2) H 0.8227 0.3671 1.4225 0.0455 Uiso 1.00 calc . . . H(3) H 0.8645 0.2283 1.4220 0.0473 Uiso 1.00 calc . . . H(4) H 0.9211 0.1663 1.2981 0.0424 Uiso 1.00 calc . . . H(5) H 0.9372 0.1649 1.1490 0.0419 Uiso 1.00 calc . . . H(6) H 0.8909 0.2373 1.0933 0.0419 Uiso 1.00 calc . . . H(7) H 1.1346 0.1638 1.0049 0.0502 Uiso 1.00 calc . . . H(8) H 1.1506 0.2528 0.9786 0.0502 Uiso 1.00 calc . . . H(9) H 0.9900 0.0926 0.9290 0.0405 Uiso 1.00 calc . . . H(10) H 0.6882 0.1988 0.8316 0.0368 Uiso 1.00 calc . . . H(11) H 0.7612 0.3953 0.8786 0.0381 Uiso 1.00 calc . . . H(12) H 0.6588 0.3382 0.8495 0.0381 Uiso 1.00 calc . . . H(13) H 0.6135 0.2408 0.9848 0.0354 Uiso 1.00 calc . . . H(14) H 0.5717 0.3689 1.2059 0.0384 Uiso 1.00 calc . . . H(15) H 0.7315 0.5378 1.1430 0.0460 Uiso 1.00 calc . . . H(16) H 0.5978 0.5446 1.1485 0.0460 Uiso 1.00 calc . . . H(17) H 0.8802 0.5009 1.2543 0.0487 Uiso 1.00 calc . . . H(18) H 0.8681 0.4966 1.3531 0.0487 Uiso 1.00 calc . . . H(19) H 1.0894 0.3771 0.9204 0.0547 Uiso 1.00 calc . . . H(20) H 0.9783 0.4193 0.8786 0.0547 Uiso 1.00 calc . . . H(21) H 1.0389 0.4514 0.9649 0.0547 Uiso 1.00 calc . . . H(22) H 0.6214 0.5238 0.9021 0.0533 Uiso 1.00 calc . . . H(23) H 0.7058 0.5938 0.9289 0.0533 Uiso 1.00 calc . . . H(24) H 0.6082 0.5701 0.9875 0.0533 Uiso 1.00 calc . . . H(25) H 0.9434 -0.0079 0.8516 0.0614 Uiso 1.00 calc . . . H(26) H 0.9005 0.0205 0.7591 0.0614 Uiso 1.00 calc . . . H(27) H 0.8463 -0.0553 0.7980 0.0614 Uiso 1.00 calc . . . H(28) H 0.6506 -0.0022 0.7725 0.0548 Uiso 1.00 calc . . . H(29) H 0.6936 0.0771 0.7332 0.0548 Uiso 1.00 calc . . . H(30) H 0.6150 0.0799 0.8098 0.0548 Uiso 1.00 calc . . . H(31) H 0.7200 -0.0451 0.9188 0.0604 Uiso 1.00 calc . . . H(32) H 0.6923 0.0376 0.9585 0.0604 Uiso 1.00 calc . . . H(33) H 0.8172 0.0021 0.9725 0.0604 Uiso 1.00 calc . . . H(34) H 0.4929 0.1553 1.0309 0.0397 Uiso 1.00 calc . . . H(35) H 0.4922 0.1024 1.1133 0.0397 Uiso 1.00 calc . . . H(36) H 0.6097 0.1315 1.0817 0.0397 Uiso 1.00 calc . . . H(37) H 0.6664 0.1897 1.2275 0.0521 Uiso 1.00 calc . . . H(38) H 0.5494 0.1597 1.2593 0.0521 Uiso 1.00 calc . . . H(39) H 0.5841 0.2495 1.2692 0.0521 Uiso 1.00 calc . . . H(40) H 0.3883 0.2876 1.1887 0.0565 Uiso 1.00 calc . . . H(41) H 0.3567 0.1973 1.1782 0.0565 Uiso 1.00 calc . . . H(42) H 0.3544 0.2524 1.0973 0.0565 Uiso 1.00 calc . . . 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(1) 0.0287(9) 0.037(1) 0.045(1) -0.0002(8) 0.0024(7) -0.0074(9) S(2) 0.0374(10) 0.030(1) 0.045(1) 0.0007(8) 0.0059(8) -0.0100(9) O(1) 0.042(3) 0.028(3) 0.032(3) 0.003(2) 0.010(2) 0.002(2) O(2) 0.033(3) 0.029(3) 0.037(3) -0.004(2) 0.007(2) -0.004(2) O(3) 0.038(3) 0.019(3) 0.049(3) -0.001(2) 0.001(2) 0.011(2) C(1) 0.023(3) 0.024(4) 0.049(5) -0.003(3) 0.000(3) -0.013(3) C(2) 0.035(4) 0.042(5) 0.028(4) -0.001(3) -0.002(3) -0.004(4) C(3) 0.036(4) 0.052(5) 0.031(4) 0.001(4) 0.003(3) 0.011(4) C(4) 0.034(4) 0.029(4) 0.046(4) 0.000(3) -0.002(3) 0.002(3) C(5) 0.027(3) 0.023(4) 0.032(4) 0.000(3) 0.002(3) 0.002(3) C(6) 0.026(3) 0.030(4) 0.034(4) -0.005(3) -0.002(3) -0.001(3) C(7) 0.035(4) 0.030(4) 0.038(4) 0.002(3) 0.003(3) -0.001(3) C(8) 0.030(4) 0.037(5) 0.049(5) 0.006(3) 0.008(3) -0.009(4) C(9) 0.023(3) 0.034(4) 0.039(4) 0.000(3) 0.005(3) -0.005(3) C(10) 0.029(4) 0.031(4) 0.035(4) 0.001(3) 0.010(3) -0.003(3) C(11) 0.030(4) 0.029(4) 0.036(4) -0.003(3) 0.011(3) -0.007(3) C(12) 0.025(3) 0.030(4) 0.027(4) -0.001(3) 0.000(3) -0.004(3) C(13) 0.030(3) 0.030(4) 0.031(4) 0.006(3) 0.011(3) 0.005(3) C(14) 0.034(4) 0.027(4) 0.031(4) -0.009(3) 0.008(3) -0.003(3) C(15) 0.032(4) 0.031(4) 0.026(4) -0.004(3) -0.001(3) 0.008(3) C(16) 0.025(3) 0.022(4) 0.039(4) -0.002(3) -0.003(3) -0.002(3) C(17) 0.031(4) 0.024(4) 0.027(4) -0.004(3) 0.002(3) -0.004(3) C(18) 0.023(3) 0.028(4) 0.035(4) -0.002(3) 0.000(3) 0.000(3) C(19) 0.033(4) 0.027(4) 0.031(4) 0.006(3) 0.006(3) 0.001(3) C(20) 0.028(4) 0.026(4) 0.051(5) 0.005(3) 0.000(3) -0.003(3) C(21) 0.023(3) 0.032(4) 0.042(4) 0.004(3) 0.006(3) 0.006(3) C(22) 0.044(4) 0.022(4) 0.047(4) 0.002(3) 0.002(3) -0.004(3) C(23) 0.037(4) 0.028(4) 0.051(5) -0.005(3) 0.005(3) -0.008(3) C(24) 0.058(5) 0.026(4) 0.060(5) -0.015(4) 0.023(4) -0.014(4) C(25) 0.048(4) 0.037(5) 0.042(4) 0.001(4) -0.005(4) 0.003(4) C(26) 0.027(3) 0.037(4) 0.035(4) -0.003(3) 0.008(3) -0.002(3) C(27) 0.035(4) 0.039(5) 0.079(6) -0.004(4) 0.008(4) -0.014(4) C(28) 0.043(4) 0.036(4) 0.055(5) 0.001(4) -0.003(4) 0.002(4) C(29) 0.053(5) 0.035(5) 0.058(5) -0.015(4) 0.005(4) -0.005(4) C(30) 0.031(4) 0.024(4) 0.037(4) 0.000(3) 0.006(3) 0.009(3) C(31) 0.032(4) 0.031(4) 0.035(4) -0.003(3) -0.004(3) 0.007(3) C(32) 0.050(4) 0.029(4) 0.037(4) -0.002(3) 0.000(3) 0.008(3) C(33) 0.033(4) 0.035(5) 0.066(5) -0.004(3) 0.009(3) 0.013(4) #----------------------------------------------------------------------- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #----------------------------------------------------------------------- _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(1) C(7) 1.817(7) . . yes S(1) C(8) 1.832(7) . . yes S(2) C(22) 1.801(7) . . yes S(2) C(23) 1.816(7) . . yes O(1) C(6) 1.357(8) . . yes O(2) C(14) 1.403(8) . . yes O(2) C(24) 1.433(9) . . yes O(3) C(21) 1.394(8) . . yes O(3) C(25) 1.426(8) . . yes C(1) C(2) 1.380(10) . . yes C(1) C(6) 1.414(9) . . yes C(1) C(23) 1.525(10) . . yes C(2) C(3) 1.39(1) . . yes C(3) C(4) 1.38(1) . . yes C(4) C(5) 1.380(9) . . yes C(5) C(6) 1.398(9) . . yes C(5) C(7) 1.509(9) . . yes C(8) C(9) 1.500(9) . . yes C(9) C(10) 1.416(9) . . yes C(9) C(14) 1.384(9) . . yes C(10) C(11) 1.396(9) . . yes C(11) C(12) 1.385(9) . . yes C(11) C(26) 1.521(9) . . yes C(12) C(13) 1.406(9) . . yes C(13) C(14) 1.373(9) . . yes C(13) C(15) 1.506(9) . . yes C(15) C(16) 1.510(9) . . yes C(16) C(17) 1.403(9) . . yes C(16) C(21) 1.391(9) . . yes C(17) C(18) 1.415(9) . . yes C(18) C(19) 1.401(9) . . yes C(18) C(30) 1.534(9) . . yes C(19) C(20) 1.394(9) . . yes C(20) C(21) 1.399(10) . . yes C(20) C(22) 1.538(10) . . yes C(26) C(27) 1.526(10) . . yes C(26) C(28) 1.508(9) . . yes C(26) C(29) 1.53(1) . . yes C(30) C(31) 1.528(9) . . yes C(30) C(32) 1.523(9) . . yes C(30) C(33) 1.535(9) . . 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(7) S(1) C(8) 102.8(3) . 1_555 1_555 yes C(22) S(2) C(23) 102.8(3) . 1_555 1_555 yes C(14) O(2) C(24) 115.6(5) . 1_555 1_555 yes C(21) O(3) C(25) 114.0(5) . 1_555 1_555 yes C(2) C(1) C(6) 120.2(6) . 1_555 1_555 yes C(2) C(1) C(23) 119.2(6) . 1_555 1_555 yes C(6) C(1) C(23) 120.6(6) . 1_555 1_555 yes C(1) C(2) C(3) 119.4(6) . 1_555 1_555 yes C(2) C(3) C(4) 120.0(6) . 1_555 1_555 yes C(3) C(4) C(5) 122.1(6) . 1_555 1_555 yes C(4) C(5) C(6) 118.3(6) . 1_555 1_555 yes C(4) C(5) C(7) 120.1(6) . 1_555 1_555 yes C(6) C(5) C(7) 121.6(6) . 1_555 1_555 yes O(1) C(6) C(1) 116.3(6) . 1_555 1_555 yes O(1) C(6) C(5) 123.8(6) . 1_555 1_555 yes C(1) C(6) C(5) 119.8(6) . 1_555 1_555 yes S(1) C(7) C(5) 107.9(4) . 1_555 1_555 yes S(1) C(8) C(9) 115.8(5) . 1_555 1_555 yes C(8) C(9) C(10) 119.7(6) . 1_555 1_555 yes C(8) C(9) C(14) 123.5(6) . 1_555 1_555 yes C(10) C(9) C(14) 116.7(5) . 1_555 1_555 yes C(9) C(10) C(11) 122.4(6) . 1_555 1_555 yes C(10) C(11) C(12) 117.6(6) . 1_555 1_555 yes C(10) C(11) C(26) 119.8(6) . 1_555 1_555 yes C(12) C(11) C(26) 122.3(5) . 1_555 1_555 yes C(11) C(12) C(13) 121.8(5) . 1_555 1_555 yes C(12) C(13) C(14) 118.4(6) . 1_555 1_555 yes C(12) C(13) C(15) 120.1(5) . 1_555 1_555 yes C(14) C(13) C(15) 121.1(6) . 1_555 1_555 yes O(2) C(14) C(9) 118.1(5) . 1_555 1_555 yes O(2) C(14) C(13) 118.1(6) . 1_555 1_555 yes C(9) C(14) C(13) 123.1(6) . 1_555 1_555 yes C(13) C(15) C(16) 109.8(5) . 1_555 1_555 yes C(15) C(16) C(17) 118.9(6) . 1_555 1_555 yes C(15) C(16) C(21) 123.1(6) . 1_555 1_555 yes C(17) C(16) C(21) 117.8(6) . 1_555 1_555 yes C(16) C(17) C(18) 122.4(6) . 1_555 1_555 yes C(17) C(18) C(19) 117.5(6) . 1_555 1_555 yes C(17) C(18) C(30) 123.0(6) . 1_555 1_555 yes C(19) C(18) C(30) 119.5(6) . 1_555 1_555 yes C(18) C(19) C(20) 121.2(6) . 1_555 1_555 yes C(19) C(20) C(21) 119.6(6) . 1_555 1_555 yes C(19) C(20) C(22) 120.4(6) . 1_555 1_555 yes C(21) C(20) C(22) 120.0(6) . 1_555 1_555 yes O(3) C(21) C(16) 120.2(6) . 1_555 1_555 yes O(3) C(21) C(20) 118.3(6) . 1_555 1_555 yes C(16) C(21) C(20) 121.5(6) . 1_555 1_555 yes S(2) C(22) C(20) 118.4(5) . 1_555 1_555 yes S(2) C(23) C(1) 115.0(4) . 1_555 1_555 yes C(11) C(26) C(27) 111.9(5) . 1_555 1_555 yes C(11) C(26) C(28) 113.6(6) . 1_555 1_555 yes C(11) C(26) C(29) 108.2(5) . 1_555 1_555 yes C(27) C(26) C(28) 107.2(5) . 1_555 1_555 yes C(27) C(26) C(29) 107.4(6) . 1_555 1_555 yes C(28) C(26) C(29) 108.3(5) . 1_555 1_555 yes C(18) C(30) C(31) 111.2(5) . 1_555 1_555 yes C(18) C(30) C(32) 110.1(5) . 1_555 1_555 yes C(18) C(30) C(33) 109.7(5) . 1_555 1_555 yes C(31) C(30) C(32) 108.1(5) . 1_555 1_555 yes C(31) C(30) C(33) 108.5(5) . 1_555 1_555 yes C(32) C(30) C(33) 109.2(5) . 1_555 1_555 yes #----------------------------------------------------------------------- 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 S(1) C(7) C(5) C(4) -109.6(6) 1_555 1_555 1_555 1_555 yes S(1) C(7) C(5) C(6) 72.8(6) 1_555 1_555 1_555 1_555 yes S(1) C(8) C(9) C(10) -115.4(6) 1_555 1_555 1_555 1_555 yes S(1) C(8) C(9) C(14) 59.9(8) 1_555 1_555 1_555 1_555 yes S(2) C(22) C(20) C(19) 30.1(8) 1_555 1_555 1_555 1_555 yes S(2) C(22) C(20) C(21) -149.1(5) 1_555 1_555 1_555 1_555 yes S(2) C(23) C(1) C(2) -81.9(7) 1_555 1_555 1_555 1_555 yes S(2) C(23) C(1) C(6) 98.8(6) 1_555 1_555 1_555 1_555 yes O(1) C(6) C(1) C(2) -179.3(5) 1_555 1_555 1_555 1_555 yes O(1) C(6) C(1) C(23) 0.0(8) 1_555 1_555 1_555 1_555 yes O(1) C(6) C(5) C(4) 177.6(5) 1_555 1_555 1_555 1_555 yes O(1) C(6) C(5) C(7) -4.7(9) 1_555 1_555 1_555 1_555 yes O(2) C(14) C(9) C(8) -3.5(10) 1_555 1_555 1_555 1_555 yes O(2) C(14) C(9) C(10) 172.0(6) 1_555 1_555 1_555 1_555 yes O(2) C(14) C(13) C(12) -172.2(6) 1_555 1_555 1_555 1_555 yes O(2) C(14) C(13) C(15) -0.2(9) 1_555 1_555 1_555 1_555 yes O(3) C(21) C(16) C(15) 1.3(9) 1_555 1_555 1_555 1_555 yes O(3) C(21) C(16) C(17) 176.5(5) 1_555 1_555 1_555 1_555 yes O(3) C(21) C(20) C(19) -176.7(5) 1_555 1_555 1_555 1_555 yes O(3) C(21) C(20) C(22) 2.4(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -2.0(9) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) -3.5(8) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(7) 174.1(5) 1_555 1_555 1_555 1_555 yes C(1) C(23) S(2) C(22) -87.5(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) 1.8(9) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 0.2(10) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 1.0(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(23) -178.3(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 2.6(9) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(7) -175.1(6) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(1) C(23) -178.9(5) 1_555 1_555 1_555 1_555 yes C(5) C(7) S(1) C(8) -163.7(4) 1_555 1_555 1_555 1_555 yes C(7) S(1) C(8) C(9) 24.6(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 174.8(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(14) C(13) -174.1(6) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 0.6(10) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(26) -173.5(6) 1_555 1_555 1_555 1_555 yes C(9) C(14) O(2) C(24) 89.0(7) 1_555 1_555 1_555 1_555 yes C(9) C(14) C(13) C(12) -1.6(10) 1_555 1_555 1_555 1_555 yes C(9) C(14) C(13) C(15) 170.4(6) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(14) C(13) 1.4(10) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) -0.8(10) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(27) -44.9(8) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(28) -166.5(6) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(26) C(29) 73.2(7) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(14) -0.9(10) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 1.2(10) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(15) -170.9(6) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(27) 141.3(6) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(28) 19.7(9) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(26) C(29) -100.6(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(15) C(16) 97.8(7) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(11) C(26) 173.2(6) 1_555 1_555 1_555 1_555 yes C(13) C(14) O(2) C(24) -99.9(7) 1_555 1_555 1_555 1_555 yes C(13) C(15) C(16) C(17) -52.1(7) 1_555 1_555 1_555 1_555 yes C(13) C(15) C(16) C(21) 123.1(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(15) C(16) -74.0(8) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) 176.1(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(21) C(20) -175.3(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) -1.1(9) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(30) 179.4(5) 1_555 1_555 1_555 1_555 yes C(16) C(21) O(3) C(25) 93.4(7) 1_555 1_555 1_555 1_555 yes C(16) C(21) C(20) C(19) -0.1(9) 1_555 1_555 1_555 1_555 yes C(16) C(21) C(20) C(22) 179.0(5) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(21) C(20) -0.1(9) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 0.9(9) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(31) 6.9(8) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(32) 126.7(6) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(30) C(33) -113.1(6) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(16) C(21) 0.7(9) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) -0.3(9) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(22) -179.4(5) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(31) -172.7(5) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(32) -52.9(7) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(30) C(33) 67.3(7) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(18) C(30) -179.6(5) 1_555 1_555 1_555 1_555 yes C(20) C(21) O(3) C(25) -89.9(7) 1_555 1_555 1_555 1_555 yes C(20) C(22) S(2) C(23) 78.6(5) 1_555 1_555 1_555 1_555 yes #----------------------------------------------------------------------- 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(1) C(33) 3.470(7) . 1_655 ? O(3) C(24) 3.329(8) . 3_767 ? C(19) C(25) 3.555(9) . 3_667 ? C(23) C(31) 3.597(9) . 2_657 ? #-----------------------------------------------------------------------