# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data____l-TTP _database_code_depnum_ccdc_archive 'CCDC 924738' #TrackingRef '17828_web_deposit_cif_file_0_YongfaXie_1361090605.l-TTP.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H8 N2 S4 ' _chemical_formula_moiety 'C20 H8 N2 S4 ' _chemical_formula_weight 404.54 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 17.064(19) _cell_length_b 3.894(4) _cell_length_c 25.72(3) _cell_angle_alpha 90.0000 _cell_angle_beta 108.820(15) _cell_angle_gamma 90.0000 _cell_volume 1618(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3959 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824.00 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.888 _diffrn_ambient_temperature 173.1 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.26 _diffrn_reflns_number 8676 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_max 27.88 _diffrn_measured_fraction_theta_max 0.785 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.950 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3021 _reflns_number_gt 2510 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.2638 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3021 _refine_ls_number_parameters 236 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0116P)^2^+34.2210P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.82 _refine_diff_density_min -0.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; N N 0.006 0.003 ; 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 THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.65346(15) 0.2078(8) 0.71068(9) 0.0328(6) Uani 1.00 1 d . . . S(2) S 0.21057(14) 0.2043(6) 0.34970(9) 0.0242(5) Uani 1.00 1 d . . . S(3) S 0.05697(15) 0.3591(7) 0.21204(9) 0.0286(6) Uani 1.00 1 d . . . S(4) S -0.13967(15) 0.7506(6) 0.15038(9) 0.0248(5) Uani 1.00 1 d . . . N(1) N -0.0779(4) 0.667(2) -0.0242(2) 0.0202(15) Uani 1.00 1 d . . . N(2) N 0.4456(4) 0.166(2) 0.5236(2) 0.0215(16) Uani 1.00 1 d . . . C(1) C 0.1417(5) 0.185(3) 0.1984(3) 0.032(2) Uani 1.00 1 d . . . C(2) C 0.1329(5) 0.203(2) 0.1447(3) 0.025(2) Uani 1.00 1 d . . . C(3) C 0.0580(5) 0.357(2) 0.1117(3) 0.0188(18) Uani 1.00 1 d . . . C(4) C 0.0098(5) 0.465(2) 0.1441(3) 0.0224(19) Uani 1.00 1 d . . . C(5) C -0.0680(5) 0.623(2) 0.1195(3) 0.0214(19) Uani 1.00 1 d . . . C(6) C -0.0970(5) 0.696(2) 0.0636(3) 0.0192(18) Uani 1.00 1 d . . . C(7) C -0.1758(5) 0.852(2) 0.0464(3) 0.0207(18) Uani 1.00 1 d . . . C(8) C -0.2060(5) 0.888(2) 0.0893(3) 0.028(2) Uani 1.00 1 d . . . C(9) C -0.0473(5) 0.598(2) 0.0294(3) 0.0173(17) Uani 1.00 1 d . . . C(10) C -0.0291(5) 0.572(2) -0.0539(3) 0.0186(18) Uani 1.00 1 d . . . C(11) C 0.2042(6) 0.369(2) 0.4108(3) 0.029(2) Uani 1.00 1 d . . . C(12) C 0.2769(5) 0.338(2) 0.4528(3) 0.025(2) Uani 1.00 1 d . . . C(13) C 0.3397(5) 0.174(2) 0.4359(3) 0.0194(18) Uani 1.00 1 d . . . C(14) C 0.3118(5) 0.086(2) 0.3807(3) 0.024(2) Uani 1.00 1 d . . . C(15) C 0.4221(5) 0.089(2) 0.4706(3) 0.0214(19) Uani 1.00 1 d . . . C(16) C 0.5241(5) 0.086(2) 0.5541(3) 0.0198(18) Uani 1.00 1 d . . . C(17) C 0.5526(5) 0.162(2) 0.6113(3) 0.0201(18) Uani 1.00 1 d . . . C(18) C 0.5086(5) 0.330(2) 0.6434(3) 0.024(2) Uani 1.00 1 d . . . C(19) C 0.5541(6) 0.360(2) 0.6966(3) 0.029(2) Uani 1.00 1 d . . . C(20) C 0.6334(5) 0.084(2) 0.6432(3) 0.027(2) Uani 1.00 1 d . . . H(1) H 0.1885 0.0888 0.2255 0.038 Uiso 1.00 1 c R . . H(2) H 0.1737 0.1198 0.1300 0.030 Uiso 1.00 1 c R . . H(3) H -0.2041 0.9220 0.0098 0.025 Uiso 1.00 1 c R . . H(4) H -0.2591 0.9805 0.0853 0.033 Uiso 1.00 1 c R . . H(5) H 0.1556 0.4701 0.4146 0.034 Uiso 1.00 1 c R . . H(6) H 0.2849 0.4155 0.4892 0.029 Uiso 1.00 1 c R . . H(7) H 0.4534 0.4114 0.6285 0.029 Uiso 1.00 1 c R . . H(8) H 0.5335 0.4544 0.7237 0.035 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0272(13) 0.0519(18) 0.0189(11) 0.0037(12) 0.0067(9) -0.0025(11) S(2) 0.0195(11) 0.0280(13) 0.0233(11) 0.0002(10) 0.0043(8) 0.0013(10) S(3) 0.0272(12) 0.0396(15) 0.0193(10) 0.0044(11) 0.0080(9) 0.0068(10) S(4) 0.0262(12) 0.0279(13) 0.0231(10) 0.0005(10) 0.0117(8) -0.0019(9) N(1) 0.020(3) 0.018(4) 0.022(3) -0.004(3) 0.007(2) 0.001(3) N(2) 0.019(3) 0.027(4) 0.019(3) 0.000(3) 0.007(2) 0.002(3) C(1) 0.022(4) 0.049(7) 0.024(4) 0.003(4) 0.008(3) 0.013(4) C(2) 0.022(4) 0.028(5) 0.024(4) -0.003(4) 0.007(3) -0.001(4) C(3) 0.021(4) 0.010(4) 0.026(4) -0.005(3) 0.009(3) 0.003(3) C(4) 0.023(4) 0.026(5) 0.016(4) 0.006(4) 0.004(3) 0.007(3) C(5) 0.020(4) 0.018(4) 0.027(4) 0.003(3) 0.009(3) 0.003(3) C(6) 0.016(4) 0.021(4) 0.021(4) -0.002(3) 0.007(3) -0.001(3) C(7) 0.018(4) 0.019(4) 0.023(4) 0.000(3) 0.004(3) -0.001(3) C(8) 0.021(4) 0.032(5) 0.032(5) -0.001(4) 0.011(3) -0.005(4) C(9) 0.017(4) 0.016(4) 0.020(4) -0.000(3) 0.009(3) 0.000(3) C(10) 0.017(4) 0.016(4) 0.022(4) -0.002(3) 0.005(3) 0.001(3) C(11) 0.027(5) 0.032(5) 0.031(5) 0.001(4) 0.014(3) -0.001(4) C(12) 0.024(4) 0.029(5) 0.024(4) 0.002(4) 0.014(3) 0.006(4) C(13) 0.017(4) 0.020(4) 0.024(4) -0.002(3) 0.011(3) 0.002(3) C(14) 0.021(4) 0.028(5) 0.025(4) -0.003(4) 0.008(3) 0.003(4) C(15) 0.024(4) 0.017(4) 0.026(4) -0.005(3) 0.012(3) -0.002(3) C(16) 0.015(4) 0.021(4) 0.025(4) -0.003(3) 0.009(3) 0.004(3) C(17) 0.017(4) 0.018(4) 0.028(4) 0.003(3) 0.012(3) 0.001(3) C(18) 0.019(4) 0.034(5) 0.023(4) -0.001(4) 0.010(3) -0.006(4) C(19) 0.028(5) 0.042(6) 0.021(4) 0.000(4) 0.013(3) -0.001(4) C(20) 0.024(4) 0.028(5) 0.030(4) -0.010(4) 0.012(3) -0.004(4) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S(1) C(19) 1.720(10) yes . . S(1) C(20) 1.725(10) yes . . S(2) C(11) 1.734(10) yes . . S(2) C(14) 1.717(9) yes . . S(3) C(1) 1.733(11) yes . . S(3) C(4) 1.722(8) yes . . S(4) C(5) 1.732(10) yes . . S(4) C(8) 1.700(8) yes . . N(1) C(9) 1.335(10) yes . . N(1) C(10) 1.351(13) yes . . N(2) C(15) 1.324(11) yes . . N(2) C(16) 1.353(10) yes . . C(1) C(2) 1.341(13) yes . . C(2) C(3) 1.421(11) yes . . C(3) C(4) 1.409(14) yes . . C(3) C(10) 1.433(12) yes . 3_565 C(4) C(5) 1.414(12) yes . . C(5) C(6) 1.389(11) yes . . C(6) C(7) 1.409(12) yes . . C(6) C(9) 1.456(13) yes . . C(7) C(8) 1.368(15) yes . . C(9) C(10) 1.415(11) yes . 3_565 C(11) C(12) 1.363(11) yes . . C(12) C(13) 1.430(14) yes . . C(13) C(14) 1.389(12) yes . . C(13) C(15) 1.440(11) yes . . C(14) C(20) 1.435(15) yes . 3_656 C(15) C(16) 1.447(14) yes . 3_656 C(16) C(17) 1.422(12) yes . . C(17) C(18) 1.439(14) yes . . C(17) C(20) 1.393(11) yes . . C(18) C(19) 1.344(11) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.950 no . . C(11) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(18) H(7) 0.950 no . . C(19) H(8) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(19) S(1) C(20) 91.3(4) yes . . . C(11) S(2) C(14) 91.6(4) yes . . . C(1) S(3) C(4) 92.0(4) yes . . . C(5) S(4) C(8) 91.4(4) yes . . . C(9) N(1) C(10) 115.0(7) yes . . . C(15) N(2) C(16) 117.3(8) yes . . . S(3) C(1) C(2) 111.3(7) yes . . . C(1) C(2) C(3) 114.8(9) yes . . . C(2) C(3) C(4) 110.8(7) yes . . . C(2) C(3) C(10) 130.1(9) yes . . 3_565 C(4) C(3) C(10) 119.0(7) yes . . 3_565 S(3) C(4) C(3) 111.0(6) yes . . . S(3) C(4) C(5) 128.5(8) yes . . . C(3) C(4) C(5) 120.5(7) yes . . . S(4) C(5) C(4) 128.3(7) yes . . . S(4) C(5) C(6) 110.3(6) yes . . . C(4) C(5) C(6) 121.4(9) yes . . . C(5) C(6) C(7) 113.5(8) yes . . . C(5) C(6) C(9) 119.2(7) yes . . . C(7) C(6) C(9) 127.2(7) yes . . . C(6) C(7) C(8) 111.1(7) yes . . . S(4) C(8) C(7) 113.7(7) yes . . . N(1) C(9) C(6) 117.4(7) yes . . . N(1) C(9) C(10) 123.4(9) yes . . 3_565 C(6) C(9) C(10) 119.1(7) yes . . 3_565 N(1) C(10) C(3) 117.8(7) yes . . 3_565 N(1) C(10) C(9) 121.5(7) yes . . 3_565 C(3) C(10) C(9) 120.7(8) yes 3_565 . 3_565 S(2) C(11) C(12) 112.2(8) yes . . . C(11) C(12) C(13) 112.3(8) yes . . . C(12) C(13) C(14) 112.2(7) yes . . . C(12) C(13) C(15) 126.3(8) yes . . . C(14) C(13) C(15) 121.4(9) yes . . . S(2) C(14) C(13) 111.7(7) yes . . . S(2) C(14) C(20) 128.5(6) yes . . 3_656 C(13) C(14) C(20) 119.8(7) yes . . 3_656 N(2) C(15) C(13) 119.7(9) yes . . . N(2) C(15) C(16) 122.4(7) yes . . 3_656 C(13) C(15) C(16) 117.9(7) yes . . 3_656 N(2) C(16) C(15) 120.2(7) yes . . 3_656 N(2) C(16) C(17) 119.8(8) yes . . . C(15) C(16) C(17) 119.9(7) yes 3_656 . . C(16) C(17) C(18) 128.2(7) yes . . . C(16) C(17) C(20) 120.5(9) yes . . . C(18) C(17) C(20) 111.2(7) yes . . . C(17) C(18) C(19) 112.7(8) yes . . . S(1) C(19) C(18) 113.0(8) yes . . . S(1) C(20) C(14) 127.9(6) yes . . 3_656 S(1) C(20) C(17) 111.7(8) yes . . . C(14) C(20) C(17) 120.4(8) yes 3_656 . . S(3) C(1) H(1) 124.3 no . . . C(2) C(1) H(1) 124.4 no . . . C(1) C(2) H(2) 122.6 no . . . C(3) C(2) H(2) 122.6 no . . . C(6) C(7) H(3) 124.5 no . . . C(8) C(7) H(3) 124.4 no . . . S(4) C(8) H(4) 123.2 no . . . C(7) C(8) H(4) 123.2 no . . . S(2) C(11) H(5) 123.9 no . . . C(12) C(11) H(5) 123.9 no . . . C(11) C(12) H(6) 123.8 no . . . C(13) C(12) H(6) 123.8 no . . . C(17) C(18) H(7) 123.6 no . . . C(19) C(18) H(7) 123.6 no . . . S(1) C(19) H(8) 123.5 no . . . C(18) C(19) H(8) 123.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(19) S(1) C(20) C(17) 0.5(8) ? . . . . C(19) S(1) C(20) C(14) -178.1(10) ? . . . 3_656 C(20) S(1) C(19) C(18) -2.1(9) ? . . . . C(11) S(2) C(14) C(13) -0.7(8) ? . . . . C(11) S(2) C(14) C(20) 179.3(10) ? . . . 3_656 C(14) S(2) C(11) C(12) 0.7(8) ? . . . . C(1) S(3) C(4) C(3) 1.8(7) ? . . . . C(1) S(3) C(4) C(5) 178.8(9) ? . . . . C(4) S(3) C(1) C(2) -1.0(9) ? . . . . C(5) S(4) C(8) C(7) -1.9(8) ? . . . . C(8) S(4) C(5) C(4) -178.8(9) ? . . . . C(8) S(4) C(5) C(6) 1.2(7) ? . . . . C(9) N(1) C(10) C(3) -179.3(8) ? . . . 3_565 C(9) N(1) C(10) C(9) 1.9(12) ? . . . 3_565 C(10) N(1) C(9) C(6) 179.6(7) ? . . . . C(10) N(1) C(9) C(10) -1.9(12) ? . . . 3_565 C(15) N(2) C(16) C(17) -179.8(6) ? . . . . C(15) N(2) C(16) C(15) -2.4(13) ? . . . 3_656 C(16) N(2) C(15) C(13) -178.8(8) ? . . . . C(16) N(2) C(15) C(16) 2.4(14) ? . . . 3_656 S(3) C(1) C(2) C(3) -0.0(11) ? . . . . C(1) C(2) C(3) C(4) 1.4(12) ? . . . . C(1) C(2) C(3) C(10) 178.0(9) ? . . . 3_565 C(2) C(3) C(4) S(3) -2.1(10) ? . . . . C(2) C(3) C(4) C(5) -179.4(8) ? . . . . C(2) C(3) C(10) N(1) 1.3(14) ? . . 3_565 3_565 C(2) C(3) C(10) C(9) -177.5(9) ? . . 3_565 . C(4) C(3) C(10) N(1) 177.7(8) ? . . 3_565 3_565 C(4) C(3) C(10) C(9) -1.2(13) ? . . 3_565 . C(10) C(3) C(4) S(3) -179.1(6) ? 3_565 . . . C(10) C(3) C(4) C(5) 3.6(13) ? 3_565 . . . S(3) C(4) C(5) S(4) -1.0(14) ? . . . . S(3) C(4) C(5) C(6) 179.1(7) ? . . . . C(3) C(4) C(5) S(4) 175.8(7) ? . . . . C(3) C(4) C(5) C(6) -4.1(14) ? . . . . S(4) C(5) C(6) C(7) -0.2(7) ? . . . . S(4) C(5) C(6) C(9) -177.8(6) ? . . . . C(4) C(5) C(6) C(7) 179.7(6) ? . . . . C(4) C(5) C(6) C(9) 2.1(13) ? . . . . C(5) C(6) C(7) C(8) -1.2(11) ? . . . . C(5) C(6) C(9) N(1) 178.9(8) ? . . . . C(5) C(6) C(9) C(10) 0.3(10) ? . . . 3_565 C(7) C(6) C(9) N(1) 1.6(14) ? . . . . C(7) C(6) C(9) C(10) -176.9(9) ? . . . 3_565 C(9) C(6) C(7) C(8) 176.2(9) ? . . . . C(6) C(7) C(8) S(4) 2.1(11) ? . . . . N(1) C(9) C(10) N(1) 2.0(14) ? . . 3_565 3_565 N(1) C(9) C(10) C(3) -179.2(8) ? . . 3_565 . C(6) C(9) C(10) N(1) -179.5(8) ? . . 3_565 3_565 C(6) C(9) C(10) C(3) -0.8(13) ? . . 3_565 . S(2) C(11) C(12) C(13) -0.5(10) ? . . . . C(11) C(12) C(13) C(14) -0.1(10) ? . . . . C(11) C(12) C(13) C(15) -177.1(9) ? . . . . C(12) C(13) C(14) S(2) 0.6(10) ? . . . . C(12) C(13) C(14) C(20) -179.4(9) ? . . . 3_656 C(12) C(13) C(15) N(2) -0.7(13) ? . . . . C(12) C(13) C(15) C(16) 178.1(9) ? . . . 3_656 C(14) C(13) C(15) N(2) -177.5(9) ? . . . . C(14) C(13) C(15) C(16) 1.3(14) ? . . . 3_656 C(15) C(13) C(14) S(2) 177.8(7) ? . . . . C(15) C(13) C(14) C(20) -2.2(15) ? . . . 3_656 S(2) C(14) C(20) S(1) 1.8(15) ? . . 3_656 3_656 S(2) C(14) C(20) C(17) -179.7(7) ? . . 3_656 3_656 C(13) C(14) C(20) S(1) -178.2(8) ? . . 3_656 3_656 C(13) C(14) C(20) C(17) 0.3(12) ? . . 3_656 3_656 N(2) C(15) C(16) N(2) -2.5(14) ? . . 3_656 3_656 N(2) C(15) C(16) C(17) -179.9(6) ? . . 3_656 3_656 C(13) C(15) C(16) N(2) 178.7(8) ? . . 3_656 3_656 C(13) C(15) C(16) C(17) 1.3(13) ? . . 3_656 3_656 N(2) C(16) C(17) C(18) -1.9(15) ? . . . . N(2) C(16) C(17) C(20) -179.4(9) ? . . . . C(15) C(16) C(17) C(18) -179.4(9) ? 3_656 . . . C(15) C(16) C(17) C(20) 3.1(14) ? 3_656 . . . C(16) C(17) C(18) C(19) 179.7(8) ? . . . . C(16) C(17) C(20) S(1) 178.9(7) ? . . . . C(16) C(17) C(20) C(14) -2.3(15) ? . . . 3_656 C(18) C(17) C(20) S(1) 1.0(11) ? . . . . C(18) C(17) C(20) C(14) 179.8(7) ? . . . 3_656 C(20) C(17) C(18) C(19) -2.6(13) ? . . . . C(17) C(18) C(19) S(1) 3.0(12) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(3) C(1) 3.590(12) ? . 1_565 C(1) S(3) 3.590(12) ? . 1_545 C(1) C(4) 3.585(14) ? . 1_545 C(2) C(3) 3.537(13) ? . 1_545 C(2) C(4) 3.558(14) ? . 1_545 C(3) C(2) 3.537(13) ? . 1_565 C(4) C(1) 3.585(14) ? . 1_565 C(4) C(2) 3.558(14) ? . 1_565 C(4) C(5) 3.518(13) ? . 1_545 C(5) C(4) 3.518(13) ? . 1_565 C(6) C(7) 3.526(13) ? . 1_545 C(7) C(6) 3.526(13) ? . 1_565 C(7) C(7) 3.464(11) ? . 2_445 C(7) C(7) 3.464(11) ? . 2_455 C(9) C(10) 3.467(12) ? . 3_575 C(10) C(9) 3.467(12) ? . 3_575 C(11) C(14) 3.560(15) ? . 1_565 C(12) C(12) 3.458(14) ? . 2_546 C(12) C(12) 3.458(14) ? . 2_556 C(12) C(13) 3.500(13) ? . 1_565 C(13) C(12) 3.500(13) ? . 1_545 C(14) C(11) 3.560(15) ? . 1_545 C(14) C(20) 3.474(14) ? . 3_666 C(15) C(16) 3.456(13) ? . 3_666 C(16) C(15) 3.456(13) ? . 3_666 C(17) C(18) 3.485(14) ? . 1_545 C(18) C(17) 3.485(14) ? . 1_565 C(19) C(20) 3.589(15) ? . 1_565 C(20) C(14) 3.474(14) ? . 3_666 C(20) C(19) 3.589(15) ? . 1_545 S(1) H(1) 2.907 ? . 3_656 S(2) H(1) 3.126 ? . . S(2) H(5) 3.585 ? . 1_545 S(2) H(7) 3.233 ? . 2_546 S(3) H(1) 3.568 ? . 1_565 S(3) H(8) 3.041 ? . 2_546 S(3) H(8) 3.484 ? . 2_556 S(4) H(2) 3.380 ? . 4_455 S(4) H(8) 3.258 ? . 2_556 N(1) H(4) 2.813 ? . 2_445 N(2) H(5) 2.804 ? . 2_546 C(2) H(4) 3.011 ? . 4_565 C(3) H(2) 3.512 ? . 1_565 C(3) H(4) 3.460 ? . 4_565 C(6) H(3) 3.565 ? . 1_545 C(6) H(3) 3.476 ? . 2_445 C(7) H(3) 2.678 ? . 2_445 C(7) H(3) 3.052 ? . 2_455 C(7) H(4) 3.516 ? . 2_445 C(8) H(2) 3.256 ? . 4_455 C(8) H(2) 3.222 ? . 4_465 C(8) H(3) 3.099 ? . 2_445 C(8) H(3) 3.263 ? . 2_455 C(10) H(4) 3.457 ? . 2_445 C(11) H(6) 3.076 ? . 2_546 C(11) H(6) 3.296 ? . 2_556 C(11) H(7) 3.110 ? . 2_546 C(11) H(7) 3.309 ? . 2_556 C(12) H(5) 3.532 ? . 2_546 C(12) H(6) 2.656 ? . 2_546 C(12) H(6) 3.068 ? . 2_556 C(13) H(6) 3.508 ? . 1_545 C(13) H(6) 3.448 ? . 2_546 C(16) H(5) 3.441 ? . 2_546 C(17) H(5) 3.478 ? . 2_546 C(17) H(7) 3.478 ? . 1_545 C(18) H(5) 3.056 ? . 2_546 H(1) S(1) 2.907 ? . 3_656 H(1) S(2) 3.126 ? . . H(1) S(3) 3.568 ? . 1_545 H(2) S(4) 3.380 ? . 4_555 H(2) C(3) 3.512 ? . 1_545 H(2) C(8) 3.256 ? . 4_555 H(2) C(8) 3.222 ? . 4_565 H(2) H(4) 2.992 ? . 4_555 H(2) H(4) 2.431 ? . 4_565 H(3) C(6) 3.565 ? . 1_565 H(3) C(6) 3.476 ? . 2_455 H(3) C(7) 3.052 ? . 2_445 H(3) C(7) 2.678 ? . 2_455 H(3) C(8) 3.263 ? . 2_445 H(3) C(8) 3.099 ? . 2_455 H(3) H(3) 2.447 ? . 2_445 H(3) H(3) 2.447 ? . 2_455 H(3) H(4) 2.887 ? . 2_445 H(3) H(4) 3.179 ? . 2_455 H(4) N(1) 2.813 ? . 2_455 H(4) C(2) 3.011 ? . 4_465 H(4) C(3) 3.460 ? . 4_465 H(4) C(7) 3.516 ? . 2_455 H(4) C(10) 3.457 ? . 2_455 H(4) H(2) 2.992 ? . 4_455 H(4) H(2) 2.431 ? . 4_465 H(4) H(3) 3.179 ? . 2_445 H(4) H(3) 2.887 ? . 2_455 H(5) S(2) 3.585 ? . 1_565 H(5) N(2) 2.804 ? . 2_556 H(5) C(12) 3.532 ? . 2_556 H(5) C(16) 3.441 ? . 2_556 H(5) C(17) 3.478 ? . 2_556 H(5) C(18) 3.056 ? . 2_556 H(5) H(6) 3.194 ? . 2_546 H(5) H(6) 2.923 ? . 2_556 H(5) H(7) 2.844 ? . 2_546 H(5) H(7) 2.511 ? . 2_556 H(6) C(11) 3.296 ? . 2_546 H(6) C(11) 3.076 ? . 2_556 H(6) C(12) 3.068 ? . 2_546 H(6) C(12) 2.656 ? . 2_556 H(6) C(13) 3.508 ? . 1_565 H(6) C(13) 3.448 ? . 2_556 H(6) H(5) 2.923 ? . 2_546 H(6) H(5) 3.194 ? . 2_556 H(6) H(6) 2.438 ? . 2_546 H(6) H(6) 2.438 ? . 2_556 H(7) S(2) 3.233 ? . 2_556 H(7) C(11) 3.309 ? . 2_546 H(7) C(11) 3.110 ? . 2_556 H(7) C(17) 3.478 ? . 1_565 H(7) H(5) 2.511 ? . 2_546 H(7) H(5) 2.844 ? . 2_556 H(8) S(3) 3.484 ? . 2_546 H(8) S(3) 3.041 ? . 2_556 H(8) S(4) 3.258 ? . 2_546 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_m-TTP _database_code_depnum_ccdc_archive 'CCDC 924748' #TrackingRef '17829_web_deposit_cif_file_0_YongfaXie_1361091424.m-TTP.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H8 N2 S4 ' _chemical_formula_sum 'C20 H8 N2 S4' _chemical_formula_weight 404.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.5806(12) _cell_length_b 4.8247(5) _cell_length_c 13.7178(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.563(2) _cell_angle_gamma 90.00 _cell_volume 827.18(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5672 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.25 _reflns_number_total 3654 _reflns_number_gt 3379 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.2011P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(10) _refine_ls_number_reflns 3654 _refine_ls_number_parameters 236 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.11817(6) 0.01158(18) 0.42182(6) 0.0402(2) Uani 1 1 d . . . S2 S 0.14158(7) 0.87587(18) 0.09091(6) 0.0417(2) Uani 1 1 d . . . S3 S 0.70820(7) -0.1418(2) 0.34033(7) 0.0504(2) Uani 1 1 d . . . S4 S 0.71721(7) 0.3132(2) 0.13883(7) 0.0496(3) Uani 1 1 d . . . N1 N 0.3266(2) 0.1323(6) 0.32915(19) 0.0356(6) Uani 1 1 d . . . N2 N 0.3374(2) 0.5217(6) 0.17601(19) 0.0366(6) Uani 1 1 d . . . C1 C -0.0155(3) 0.0980(8) 0.4096(2) 0.0421(8) Uani 1 1 d . . . H1 H -0.0660 0.0110 0.4480 0.055 Uiso 1 1 d . . . C2 C 0.0074(3) 0.9179(8) 0.1004(3) 0.0477(8) Uani 1 1 d . . . H2 H -0.0310 1.0650 0.0650 0.074 Uiso 1 1 d . . . C3 C 0.1406(2) 0.2408(7) 0.3302(2) 0.0338(6) Uani 1 1 d . . . C4 C 0.1516(3) 0.6262(7) 0.1810(2) 0.0359(6) Uani 1 1 d . . . C5 C -0.0421(3) 0.2954(8) 0.3412(2) 0.0411(7) Uani 1 1 d . . . H3 H -0.1070 0.3650 0.3310 0.041 Uiso 1 1 d . . . C6 C -0.0300(3) 0.7516(8) 0.1682(3) 0.0434(8) Uani 1 1 d . . . H4 H -0.0990 0.7720 0.1870 0.052 Uiso 1 1 d . . . C7 C 0.0487(2) 0.3798(7) 0.2934(2) 0.0349(6) Uani 1 1 d . . . C8 C 0.0539(2) 0.5801(7) 0.2162(2) 0.0352(6) Uani 1 1 d . . . C9 C 0.2420(2) 0.2820(7) 0.2935(2) 0.0336(6) Uani 1 1 d . . . C10 C 0.2466(2) 0.4787(7) 0.2162(2) 0.0344(6) Uani 1 1 d . . . C11 C 0.4179(3) 0.1743(7) 0.2887(2) 0.0344(6) Uani 1 1 d . . . C12 C 0.4223(2) 0.3707(8) 0.2111(2) 0.0345(6) Uani 1 1 d . . . C13 C 0.5115(2) 0.0181(7) 0.3250(2) 0.0362(6) Uani 1 1 d . . . C14 C 0.5225(2) 0.4054(7) 0.1696(2) 0.0371(7) Uani 1 1 d . . . C15 C 0.5239(3) -0.1846(8) 0.4033(2) 0.0380(7) Uani 1 1 d . . . H5 H 0.4760 -0.2300 0.4320 0.036 Uiso 1 1 d . . . C16 C 0.5432(3) 0.5925(7) 0.0916(2) 0.0395(7) Uani 1 1 d . . . H6 H 0.5020 0.7080 0.0680 0.033 Uiso 1 1 d . . . C17 C 0.6061(3) 0.0580(7) 0.2827(2) 0.0386(7) Uani 1 1 d . . . C18 C 0.6107(3) 0.2469(7) 0.2038(3) 0.0399(7) Uani 1 1 d . . . C19 C 0.6250(3) -0.2808(9) 0.4184(3) 0.0497(9) Uani 1 1 d . . . H7 H 0.6660 -0.3980 0.4730 0.076 Uiso 1 1 d . . . C20 C 0.6450(3) 0.5612(9) 0.0689(3) 0.0491(9) Uani 1 1 d . . . H8 H 0.6890 0.6740 0.0170 0.044 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0376(4) 0.0424(4) 0.0417(4) 0.0040(3) 0.0096(3) -0.0031(4) S2 0.0450(4) 0.0403(4) 0.0398(4) 0.0033(4) 0.0051(3) -0.0017(4) S3 0.0351(4) 0.0573(5) 0.0588(5) 0.0046(5) 0.0064(4) 0.0047(4) S4 0.0373(4) 0.0587(6) 0.0553(5) 0.0003(4) 0.0164(4) -0.0032(4) N1 0.0376(13) 0.0365(14) 0.0336(13) -0.0005(11) 0.0074(11) -0.0023(11) N2 0.0353(12) 0.0402(15) 0.0351(13) 0.0009(12) 0.0075(10) -0.0050(12) C1 0.0360(15) 0.050(2) 0.0417(18) -0.0005(15) 0.0109(13) -0.0077(15) C2 0.0481(18) 0.047(2) 0.0473(19) 0.0059(16) 0.0006(14) 0.0092(16) C3 0.0320(14) 0.0326(15) 0.0376(16) -0.0011(13) 0.0072(12) -0.0020(12) C4 0.0403(16) 0.0333(15) 0.0340(15) -0.0021(12) 0.0040(13) -0.0022(13) C5 0.0351(15) 0.048(2) 0.0410(17) -0.0027(15) 0.0063(13) -0.0003(14) C6 0.0414(17) 0.0429(19) 0.0459(19) -0.0046(16) 0.0054(14) -0.0020(15) C7 0.0356(14) 0.0338(14) 0.0356(15) -0.0034(13) 0.0050(11) -0.0025(13) C8 0.0345(15) 0.0345(15) 0.0361(15) -0.0038(12) 0.0027(12) -0.0031(12) C9 0.0336(14) 0.0339(15) 0.0333(15) -0.0034(12) 0.0038(11) -0.0023(12) C10 0.0370(15) 0.0312(15) 0.0350(15) -0.0029(12) 0.0049(12) -0.0032(12) C11 0.0370(15) 0.0333(15) 0.0334(15) -0.0017(11) 0.0056(12) -0.0036(12) C12 0.0341(14) 0.0370(15) 0.0336(14) -0.0037(12) 0.0081(11) -0.0031(13) C13 0.0364(15) 0.0366(16) 0.0353(15) -0.0021(13) 0.0024(12) 0.0001(14) C14 0.0372(15) 0.0414(18) 0.0341(15) -0.0057(13) 0.0099(12) -0.0053(13) C15 0.0352(14) 0.0441(18) 0.0352(16) 0.0021(13) 0.0059(12) 0.0061(14) C16 0.0427(17) 0.0425(18) 0.0347(16) -0.0039(14) 0.0101(13) -0.0024(14) C17 0.0351(14) 0.0402(18) 0.0404(17) -0.0020(14) 0.0039(12) -0.0021(13) C18 0.0354(15) 0.0394(17) 0.0466(18) -0.0058(14) 0.0118(13) -0.0042(14) C19 0.0428(18) 0.057(2) 0.049(2) 0.0031(17) 0.0032(15) 0.0049(17) C20 0.0499(19) 0.056(2) 0.0436(18) -0.0006(16) 0.0154(15) -0.0088(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.721(3) . ? S1 C1 1.722(3) . ? S2 C4 1.720(3) . ? S2 C2 1.720(4) . ? S3 C19 1.717(4) . ? S3 C17 1.724(3) . ? S4 C18 1.723(3) . ? S4 C20 1.726(4) . ? N1 C9 1.332(4) . ? N1 C11 1.347(4) . ? N2 C12 1.336(4) . ? N2 C10 1.340(4) . ? C1 C5 1.352(5) . ? C1 H1 0.9663 . ? C2 C6 1.352(5) . ? C2 H2 0.9591 . ? C3 C7 1.382(4) . ? C3 C9 1.437(4) . ? C4 C8 1.389(4) . ? C4 C10 1.427(5) . ? C5 C7 1.439(4) . ? C5 H3 0.8796 . ? C6 C8 1.440(5) . ? C6 H4 0.9386 . ? C7 C8 1.441(4) . ? C9 C10 1.429(4) . ? C11 C12 1.432(5) . ? C11 C13 1.438(5) . ? C12 C14 1.450(4) . ? C13 C17 1.395(4) . ? C13 C15 1.448(4) . ? C14 C18 1.385(5) . ? C14 C16 1.446(4) . ? C15 C19 1.347(5) . ? C15 H5 0.7877 . ? C16 C20 1.360(5) . ? C16 H6 0.8035 . ? C17 C18 1.421(5) . ? C19 H7 1.0291 . ? C20 H8 1.0954 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 S1 C1 90.78(16) . . ? C4 S2 C2 91.15(17) . . ? C19 S3 C17 91.66(18) . . ? C18 S4 C20 91.44(17) . . ? C9 N1 C11 116.8(3) . . ? C12 N2 C10 116.9(3) . . ? C5 C1 S1 113.5(2) . . ? C5 C1 H1 123.9 . . ? S1 C1 H1 122.5 . . ? C6 C2 S2 113.8(3) . . ? C6 C2 H2 126.3 . . ? S2 C2 H2 119.4 . . ? C7 C3 C9 122.9(3) . . ? C7 C3 S1 112.2(2) . . ? C9 C3 S1 124.8(2) . . ? C8 C4 C10 122.9(3) . . ? C8 C4 S2 111.5(3) . . ? C10 C4 S2 125.6(3) . . ? C1 C5 C7 111.7(3) . . ? C1 C5 H3 122.1 . . ? C7 C5 H3 126.2 . . ? C2 C6 C8 111.1(3) . . ? C2 C6 H4 122.2 . . ? C8 C6 H4 125.9 . . ? C3 C7 C5 111.8(3) . . ? C3 C7 C8 119.2(3) . . ? C5 C7 C8 129.0(3) . . ? C4 C8 C6 112.4(3) . . ? C4 C8 C7 118.6(3) . . ? C6 C8 C7 129.0(3) . . ? N1 C9 C10 122.3(3) . . ? N1 C9 C3 120.0(3) . . ? C10 C9 C3 117.7(3) . . ? N2 C10 C4 120.3(3) . . ? N2 C10 C9 121.1(3) . . ? C4 C10 C9 118.6(3) . . ? N1 C11 C12 120.9(3) . . ? N1 C11 C13 118.8(3) . . ? C12 C11 C13 120.3(3) . . ? N2 C12 C11 122.1(3) . . ? N2 C12 C14 119.4(3) . . ? C11 C12 C14 118.5(3) . . ? C17 C13 C11 119.2(3) . . ? C17 C13 C15 112.1(3) . . ? C11 C13 C15 128.7(3) . . ? C18 C14 C16 113.0(3) . . ? C18 C14 C12 120.1(3) . . ? C16 C14 C12 126.9(3) . . ? C19 C15 C13 111.5(3) . . ? C19 C15 H5 126.2 . . ? C13 C15 H5 122.3 . . ? C20 C16 C14 110.7(3) . . ? C20 C16 H6 124.4 . . ? C14 C16 H6 124.6 . . ? C13 C17 C18 121.0(3) . . ? C13 C17 S3 111.0(2) . . ? C18 C17 S3 128.0(3) . . ? C14 C18 C17 120.8(3) . . ? C14 C18 S4 111.3(3) . . ? C17 C18 S4 127.9(3) . . ? C15 C19 S3 113.7(3) . . ? C15 C19 H7 133.4 . . ? S3 C19 H7 112.2 . . ? C16 C20 S4 113.5(3) . . ? C16 C20 H8 130.7 . . ? S4 C20 H8 115.6 . . ? 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 C3 S1 C1 C5 -1.3(3) . . . . ? C4 S2 C2 C6 -0.2(3) . . . . ? C1 S1 C3 C7 0.8(3) . . . . ? C1 S1 C3 C9 -177.8(3) . . . . ? C2 S2 C4 C8 0.0(3) . . . . ? C2 S2 C4 C10 179.3(3) . . . . ? S1 C1 C5 C7 1.4(4) . . . . ? S2 C2 C6 C8 0.3(4) . . . . ? C9 C3 C7 C5 178.4(3) . . . . ? S1 C3 C7 C5 -0.2(4) . . . . ? C9 C3 C7 C8 -1.4(5) . . . . ? S1 C3 C7 C8 179.9(2) . . . . ? C1 C5 C7 C3 -0.8(4) . . . . ? C1 C5 C7 C8 179.1(3) . . . . ? C10 C4 C8 C6 -179.2(3) . . . . ? S2 C4 C8 C6 0.2(4) . . . . ? C10 C4 C8 C7 1.7(5) . . . . ? S2 C4 C8 C7 -179.0(2) . . . . ? C2 C6 C8 C4 -0.4(4) . . . . ? C2 C6 C8 C7 178.7(3) . . . . ? C3 C7 C8 C4 0.2(4) . . . . ? C5 C7 C8 C4 -179.6(3) . . . . ? C3 C7 C8 C6 -178.8(3) . . . . ? C5 C7 C8 C6 1.3(6) . . . . ? C11 N1 C9 C10 -0.1(4) . . . . ? C11 N1 C9 C3 177.5(3) . . . . ? C7 C3 C9 N1 -177.0(3) . . . . ? S1 C3 C9 N1 1.5(4) . . . . ? C7 C3 C9 C10 0.8(5) . . . . ? S1 C3 C9 C10 179.3(2) . . . . ? C12 N2 C10 C4 -178.3(3) . . . . ? C12 N2 C10 C9 0.6(4) . . . . ? C8 C4 C10 N2 176.6(3) . . . . ? S2 C4 C10 N2 -2.7(5) . . . . ? C8 C4 C10 C9 -2.3(5) . . . . ? S2 C4 C10 C9 178.4(2) . . . . ? N1 C9 C10 N2 -0.2(5) . . . . ? C3 C9 C10 N2 -177.8(3) . . . . ? N1 C9 C10 C4 178.8(3) . . . . ? C3 C9 C10 C4 1.1(4) . . . . ? C9 N1 C11 C12 -0.1(4) . . . . ? C9 N1 C11 C13 179.8(3) . . . . ? C10 N2 C12 C11 -0.8(5) . . . . ? C10 N2 C12 C14 179.2(3) . . . . ? N1 C11 C12 N2 0.6(5) . . . . ? C13 C11 C12 N2 -179.3(3) . . . . ? N1 C11 C12 C14 -179.4(3) . . . . ? C13 C11 C12 C14 0.6(5) . . . . ? N1 C11 C13 C17 179.3(3) . . . . ? C12 C11 C13 C17 -0.7(5) . . . . ? N1 C11 C13 C15 -1.2(5) . . . . ? C12 C11 C13 C15 178.8(3) . . . . ? N2 C12 C14 C18 -178.8(3) . . . . ? C11 C12 C14 C18 1.2(5) . . . . ? N2 C12 C14 C16 0.2(5) . . . . ? C11 C12 C14 C16 -179.7(3) . . . . ? C17 C13 C15 C19 1.6(4) . . . . ? C11 C13 C15 C19 -177.9(3) . . . . ? C18 C14 C16 C20 1.6(4) . . . . ? C12 C14 C16 C20 -177.5(3) . . . . ? C11 C13 C17 C18 -1.0(5) . . . . ? C15 C13 C17 C18 179.4(3) . . . . ? C11 C13 C17 S3 178.0(2) . . . . ? C15 C13 C17 S3 -1.6(4) . . . . ? C19 S3 C17 C13 0.9(3) . . . . ? C19 S3 C17 C18 179.8(3) . . . . ? C16 C14 C18 C17 177.9(3) . . . . ? C12 C14 C18 C17 -3.0(5) . . . . ? C16 C14 C18 S4 -2.4(4) . . . . ? C12 C14 C18 S4 176.8(2) . . . . ? C13 C17 C18 C14 2.9(5) . . . . ? S3 C17 C18 C14 -175.9(3) . . . . ? C13 C17 C18 S4 -176.9(3) . . . . ? S3 C17 C18 S4 4.3(5) . . . . ? C20 S4 C18 C14 1.9(3) . . . . ? C20 S4 C18 C17 -178.3(3) . . . . ? C13 C15 C19 S3 -0.9(4) . . . . ? C17 S3 C19 C15 0.0(3) . . . . ? C14 C16 C20 S4 -0.1(4) . . . . ? C18 S4 C20 C16 -1.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.403 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.080 data___t-TTP _database_code_depnum_ccdc_archive 'CCDC 924749' #TrackingRef 'web_deposit_cif_file_1_YongfaXie_1361091424.t-TTP.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H8 N2 S4 ' _chemical_formula_moiety 'C20 H8 N2 S4 ' _chemical_formula_weight 404.54 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.247(5) _cell_length_b 5.014(2) _cell_length_c 14.169(6) _cell_angle_alpha 90.0000 _cell_angle_beta 91.668(7) _cell_angle_gamma 90.0000 _cell_volume 798.6(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1844 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412.00 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 0.984 _diffrn_ambient_temperature 173 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 5983 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1829 _reflns_number_gt 1506 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1027 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1829 _refine_ls_number_parameters 135 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.5374P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.40 _refine_diff_density_min -0.33 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; N N 0.006 0.003 ; 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 THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.80819(6) 0.91773(14) 0.48475(5) 0.02609(18) Uani 1.00 1 d . . . S(2) S 0.36651(6) 0.83526(14) 0.73419(5) 0.0271(2) Uani 1.00 1 d . . . N(2) N 0.39831(18) 0.4817(3) 0.55756(14) 0.0185(4) Uani 1.00 1 d . . . C(1) C 0.4332(2) 1.0932(5) 0.7957(2) 0.0293(6) Uani 1.00 1 d . . . C(2) C 0.5367(2) 1.1734(5) 0.75889(19) 0.0256(5) Uani 1.00 1 d . . . C(3) C 0.5666(2) 1.0214(4) 0.67743(17) 0.0204(5) Uani 1.00 1 d . . . C(4) C 0.4115(2) 0.3259(4) 0.48155(16) 0.0177(4) Uani 1.00 1 d . . . C(5) C 0.4806(2) 0.8305(4) 0.65597(17) 0.0194(5) Uani 1.00 1 d . . . C(6) C 0.7686(2) 1.2150(5) 0.62845(19) 0.0259(5) Uani 1.00 1 d . . . C(8) C 0.6684(2) 1.0401(4) 0.61980(17) 0.0199(5) Uani 1.00 1 d . . . C(9) C 0.6780(2) 0.8675(4) 0.54385(17) 0.0189(5) Uani 1.00 1 d . . . C(10) C 0.8492(2) 1.1713(5) 0.56183(19) 0.0271(5) Uani 1.00 1 d . . . C(11) C 0.4867(2) 0.6562(4) 0.57652(16) 0.0173(4) Uani 1.00 1 d . . . H(1) H 0.395(2) 1.163(6) 0.851(2) 0.046(9) Uiso 1.00 1 c . . . H(2) H 0.580(2) 1.308(5) 0.7843(19) 0.027(7) Uiso 1.00 1 c . . . H(3) H 0.779(2) 1.356(5) 0.6747(19) 0.025(7) Uiso 1.00 1 c . . . H(4) H 0.917(2) 1.250(5) 0.5549(19) 0.029(7) Uiso 1.00 1 c . . . 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) 0.0250(3) 0.0291(3) 0.0242(3) -0.0073(2) 0.0021(2) 0.0011(2) S(2) 0.0250(3) 0.0320(3) 0.0245(3) 0.0015(2) 0.0039(2) -0.0086(2) N(2) 0.0226(10) 0.0170(9) 0.0157(9) -0.0003(8) -0.0015(8) -0.0001(7) C(1) 0.0320(15) 0.0308(14) 0.0249(13) 0.0067(12) -0.0023(11) -0.0122(11) C(2) 0.0305(14) 0.0206(12) 0.0251(13) 0.0057(11) -0.0097(11) -0.0069(10) C(3) 0.0255(12) 0.0167(11) 0.0187(12) 0.0046(10) -0.0075(9) -0.0004(9) C(4) 0.0204(11) 0.0156(10) 0.0170(11) 0.0000(9) -0.0036(9) 0.0004(9) C(5) 0.0219(11) 0.0198(11) 0.0162(11) 0.0042(10) -0.0015(9) -0.0016(9) C(6) 0.0319(14) 0.0185(12) 0.0266(13) -0.0036(11) -0.0103(11) 0.0019(11) C(8) 0.0237(12) 0.0156(11) 0.0200(11) -0.0002(9) -0.0072(9) 0.0038(9) C(9) 0.0206(11) 0.0172(11) 0.0189(11) -0.0017(9) -0.0025(9) 0.0012(9) C(10) 0.0248(13) 0.0273(13) 0.0289(14) -0.0081(11) -0.0063(11) 0.0048(11) C(11) 0.0195(11) 0.0148(10) 0.0174(11) 0.0010(9) -0.0023(9) 0.0008(9) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S(1) C(9) 1.727(2) yes . . S(1) C(10) 1.730(2) yes . . S(2) C(1) 1.720(2) yes . . S(2) C(5) 1.720(2) yes . . N(2) C(4) 1.342(3) yes . . N(2) C(11) 1.346(3) yes . . C(1) C(2) 1.351(3) yes . . C(2) C(3) 1.431(3) yes . . C(3) C(5) 1.388(3) yes . . C(3) C(8) 1.428(3) yes . . C(4) C(9) 1.436(3) yes . 3_666 C(4) C(11) 1.432(3) yes . 3_666 C(5) C(11) 1.428(3) yes . . C(6) C(8) 1.431(3) yes . . C(6) C(10) 1.346(3) yes . . C(8) C(9) 1.388(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_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(9) S(1) C(10) 90.88(12) yes . . . C(1) S(2) C(5) 90.84(12) yes . . . C(4) N(2) C(11) 116.1(2) yes . . . S(2) C(1) C(2) 113.3(2) yes . . . C(1) C(2) C(3) 112.3(2) yes . . . C(2) C(3) C(5) 111.4(2) yes . . . C(2) C(3) C(8) 129.6(2) yes . . . C(5) C(3) C(8) 119.0(2) yes . . . N(2) C(4) C(9) 120.1(2) yes . . 3_666 N(2) C(4) C(11) 122.2(2) yes . . 3_666 C(9) C(4) C(11) 117.7(2) yes 3_666 . 3_666 S(2) C(5) C(3) 112.18(18) yes . . . S(2) C(5) C(11) 124.75(18) yes . . . C(3) C(5) C(11) 123.1(2) yes . . . C(8) C(6) C(10) 112.7(2) yes . . . C(3) C(8) C(6) 129.3(2) yes . . . C(3) C(8) C(9) 119.0(2) yes . . . C(6) C(8) C(9) 111.7(2) yes . . . S(1) C(9) C(4) 125.11(18) yes . . 3_666 S(1) C(9) C(8) 111.81(17) yes . . . C(4) C(9) C(8) 123.1(2) yes 3_666 . . S(1) C(10) C(6) 112.9(2) yes . . . N(2) C(11) C(4) 121.6(2) yes . . 3_666 N(2) C(11) C(5) 120.2(2) yes . . . C(4) C(11) C(5) 118.2(2) yes 3_666 . . S(2) C(1) H(1) 118.8(18) no . . . C(2) C(1) H(1) 127.9(19) no . . . C(1) C(2) H(2) 122.2(18) no . . . C(3) C(2) H(2) 125.5(18) no . . . C(8) C(6) H(3) 125.6(16) no . . . C(10) C(6) H(3) 121.7(16) no . . . S(1) C(10) H(4) 118.7(18) no . . . C(6) C(10) H(4) 128.3(19) no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(9) S(1) C(10) C(6) -0.02(17) ? . . . . C(10) S(1) C(9) C(8) -0.23(19) ? . . . . C(10) S(1) C(9) C(4) 179.2(2) ? . . . 3_666 C(1) S(2) C(5) C(3) 0.2(2) ? . . . . C(1) S(2) C(5) C(11) -178.6(2) ? . . . . C(5) S(2) C(1) C(2) 0.2(2) ? . . . . C(4) N(2) C(11) C(5) 179.99(18) ? . . . . C(4) N(2) C(11) C(4) 0.2(3) ? . . . 3_666 C(11) N(2) C(4) C(9) 179.6(2) ? . . . 3_666 C(11) N(2) C(4) C(11) -0.2(3) ? . . . 3_666 S(2) C(1) C(2) C(3) -0.6(3) ? . . . . C(1) C(2) C(3) C(5) 0.7(3) ? . . . . C(1) C(2) C(3) C(8) -178.8(2) ? . . . . C(2) C(3) C(5) S(2) -0.5(2) ? . . . . C(2) C(3) C(5) C(11) 178.2(2) ? . . . . C(2) C(3) C(8) C(6) 0.6(4) ? . . . . C(2) C(3) C(8) C(9) 179.7(2) ? . . . . C(5) C(3) C(8) C(6) -178.9(2) ? . . . . C(5) C(3) C(8) C(9) 0.2(3) ? . . . . C(8) C(3) C(5) S(2) 179.03(18) ? . . . . C(8) C(3) C(5) C(11) -2.2(3) ? . . . . N(2) C(4) C(9) S(1) 1.3(3) ? . . 3_666 3_666 N(2) C(4) C(9) C(8) -178.1(2) ? . . 3_666 3_666 N(2) C(4) C(11) N(2) 0.2(3) ? . . 3_666 3_666 N(2) C(4) C(11) C(5) -179.99(19) ? . . 3_666 3_666 C(9) C(4) C(11) N(2) -179.6(2) ? 3_666 . 3_666 3_666 C(9) C(4) C(11) C(5) 0.2(3) ? 3_666 . 3_666 3_666 C(11) C(4) C(9) S(1) -178.90(17) ? 3_666 . 3_666 3_666 C(11) C(4) C(9) C(8) 1.8(3) ? 3_666 . 3_666 3_666 S(2) C(5) C(11) N(2) 0.9(3) ? . . . . S(2) C(5) C(11) C(4) -179.23(17) ? . . . 3_666 C(3) C(5) C(11) N(2) -177.6(2) ? . . . . C(3) C(5) C(11) C(4) 2.2(3) ? . . . 3_666 C(8) C(6) C(10) S(1) 0.3(3) ? . . . . C(10) C(6) C(8) C(3) 178.7(2) ? . . . . C(10) C(6) C(8) C(9) -0.4(3) ? . . . . C(3) C(8) C(9) S(1) -178.82(18) ? . . . . C(3) C(8) C(9) C(4) 1.8(3) ? . . . 3_666 C(6) C(8) C(9) S(1) 0.4(2) ? . . . . C(6) C(8) C(9) C(4) -179.0(2) ? . . . 3_666 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(2) C(1) 3.596(2) ? . 2_546 N(2) C(2) 3.562(3) ? . 1_545 N(2) C(3) 3.407(3) ? . 1_545 N(2) C(6) 3.535(3) ? . 3_676 N(2) C(8) 3.538(3) ? . 3_676 C(1) S(2) 3.596(2) ? . 2_556 C(2) N(2) 3.562(3) ? . 1_565 C(2) C(6) 3.525(3) ? . 2_646 C(2) C(11) 3.574(3) ? . 1_565 C(3) N(2) 3.407(3) ? . 1_565 C(3) C(4) 3.577(3) ? . 1_565 C(3) C(11) 3.593(3) ? . 1_565 C(4) C(3) 3.577(3) ? . 1_545 C(4) C(5) 3.573(3) ? . 1_545 C(4) C(6) 3.413(3) ? . 3_676 C(4) C(8) 3.592(3) ? . 3_676 C(5) C(4) 3.573(3) ? . 1_565 C(6) N(2) 3.535(3) ? . 3_676 C(6) C(2) 3.525(3) ? . 2_656 C(6) C(4) 3.413(3) ? . 3_676 C(8) N(2) 3.538(3) ? . 3_676 C(8) C(4) 3.592(3) ? . 3_676 C(8) C(11) 3.580(3) ? . 3_676 C(9) C(11) 3.443(3) ? . 3_676 C(11) C(2) 3.574(3) ? . 1_545 C(11) C(3) 3.593(3) ? . 1_545 C(11) C(8) 3.580(3) ? . 3_676 C(11) C(9) 3.443(3) ? . 3_676 S(1) H(1) 3.02(3) ? . 4_574 S(1) H(2) 3.51(2) ? . 2_646 S(1) H(3) 3.50(2) ? . . S(1) H(4) 2.28(2) ? . . S(1) H(4) 3.26(2) ? . 3_776 S(2) H(1) 2.34(3) ? . . S(2) H(1) 3.26(3) ? . 2_546 S(2) H(2) 3.44(2) ? . . C(1) H(1) 0.97(3) ? . . C(1) H(2) 1.99(2) ? . . C(1) H(3) 3.47(2) ? . 2_646 C(1) H(4) 3.17(2) ? . 2_646 C(2) H(1) 2.09(3) ? . . C(2) H(2) 0.90(2) ? . . C(2) H(3) 3.14(2) ? . . C(2) H(3) 2.76(2) ? . 2_646 C(2) H(4) 3.41(2) ? . 2_646 C(3) H(1) 3.25(3) ? . . C(3) H(2) 2.09(2) ? . . C(3) H(3) 2.92(2) ? . . C(3) H(3) 2.81(2) ? . 2_646 C(4) H(3) 3.43(2) ? . 3_676 C(5) H(1) 3.39(3) ? . . C(5) H(2) 3.36(2) ? . 1_545 C(5) H(2) 3.19(2) ? . . C(5) H(3) 3.57(2) ? . 2_646 C(6) H(2) 3.14(2) ? . . C(6) H(2) 2.91(2) ? . 2_646 C(6) H(3) 0.97(2) ? . . C(6) H(3) 3.38(2) ? . 2_646 C(6) H(4) 2.01(2) ? . . C(8) H(2) 2.89(2) ? . . C(8) H(2) 3.31(2) ? . 2_646 C(8) H(3) 2.14(2) ? . . C(8) H(3) 3.10(2) ? . 2_646 C(8) H(4) 3.15(2) ? . . C(9) H(3) 3.34(2) ? . 1_545 C(9) H(3) 3.25(2) ? . . C(9) H(4) 3.31(2) ? . . C(10) H(1) 3.16(3) ? . 4_574 C(10) H(2) 2.93(2) ? . 2_646 C(10) H(3) 2.03(2) ? . . C(10) H(4) 0.87(2) ? . . C(11) H(2) 3.56(2) ? . 1_545 H(1) S(1) 3.02(3) ? . 4_475 H(1) S(2) 2.34(3) ? . . H(1) S(2) 3.26(3) ? . 2_556 H(1) C(1) 0.97(3) ? . . H(1) C(2) 2.09(3) ? . . H(1) C(3) 3.25(3) ? . . H(1) C(5) 3.39(3) ? . . H(1) C(10) 3.16(3) ? . 4_475 H(1) H(2) 2.43(4) ? . . H(1) H(4) 3.22(4) ? . 2_646 H(1) H(4) 2.93(4) ? . 4_475 H(2) S(1) 3.51(2) ? . 2_656 H(2) S(2) 3.44(2) ? . . H(2) C(1) 1.99(2) ? . . H(2) C(2) 0.90(2) ? . . H(2) C(3) 2.09(2) ? . . H(2) C(5) 3.19(2) ? . . H(2) C(5) 3.36(2) ? . 1_565 H(2) C(6) 3.14(2) ? . . H(2) C(6) 2.91(2) ? . 2_656 H(2) C(8) 2.89(2) ? . . H(2) C(8) 3.31(2) ? . 2_656 H(2) C(10) 2.93(2) ? . 2_656 H(2) C(11) 3.56(2) ? . 1_565 H(2) H(1) 2.43(4) ? . . H(2) H(3) 2.76(3) ? . . H(2) H(3) 2.82(3) ? . 2_646 H(2) H(3) 3.22(4) ? . 2_656 H(2) H(4) 3.18(4) ? . 2_656 H(3) S(1) 3.50(2) ? . . H(3) C(1) 3.47(2) ? . 2_656 H(3) C(2) 3.14(2) ? . . H(3) C(2) 2.76(2) ? . 2_656 H(3) C(3) 2.92(2) ? . . H(3) C(3) 2.81(2) ? . 2_656 H(3) C(4) 3.43(2) ? . 3_676 H(3) C(5) 3.57(2) ? . 2_656 H(3) C(6) 0.97(2) ? . . H(3) C(6) 3.38(2) ? . 2_656 H(3) C(8) 2.14(2) ? . . H(3) C(8) 3.10(2) ? . 2_656 H(3) C(9) 3.25(2) ? . . H(3) C(9) 3.34(2) ? . 1_565 H(3) C(10) 2.03(2) ? . . H(3) H(2) 2.76(3) ? . . H(3) H(2) 3.22(4) ? . 2_646 H(3) H(2) 2.82(3) ? . 2_656 H(3) H(3) 3.37(3) ? . 2_646 H(3) H(3) 3.37(3) ? . 2_656 H(3) H(4) 2.40(3) ? . . H(4) S(1) 2.28(2) ? . . H(4) S(1) 3.26(2) ? . 3_776 H(4) C(1) 3.17(2) ? . 2_656 H(4) C(2) 3.41(2) ? . 2_656 H(4) C(6) 2.01(2) ? . . H(4) C(8) 3.15(2) ? . . H(4) C(9) 3.31(2) ? . . H(4) C(10) 0.87(2) ? . . H(4) H(1) 3.22(4) ? . 2_656 H(4) H(1) 2.93(4) ? . 4_574 H(4) H(2) 3.18(4) ? . 2_646 H(4) H(3) 2.40(3) ? . . H(4) H(4) 3.51(4) ? . 3_776 H(4) H(4) 3.51(4) ? . 3_786 data___l-HTTP _database_code_depnum_ccdc_archive 'CCDC 924750' #TrackingRef 'web_deposit_cif_file_2_YongfaXie_1361091424.l-HTTP.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C44 H56 N2 S4 ' _chemical_formula_moiety 'C44 H56 N2 S4 ' _chemical_formula_weight 741.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 4.8942(14) _cell_length_b 12.751(3) _cell_length_c 17.057(5) _cell_angle_alpha 76.147(11) _cell_angle_beta 84.810(13) _cell_angle_gamma 72.178(10) _cell_volume 983.7(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 2450 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 31.3 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 398.00 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.946 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9314 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 31.30 _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.956 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_ambient_temperature 123.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4556 _reflns_number_gt 2631 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0718 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2671 _refine_ls_number_parameters 254 _refine_ls_goodness_of_fit_ref 1.427 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.46 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; N N 0.006 0.003 ; 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 THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 1.3351(2) 0.75171(9) 0.71321(6) 0.0207(3) Uani 1.00 1 d . . . S(2) S 1.2419(2) 0.15183(9) 0.44770(6) 0.0201(3) Uani 1.00 1 d . . . N(1) N 1.3261(7) 0.4611(2) 0.56522(18) 0.0163(9) Uani 1.00 1 d . . . C(1) C 1.1491(8) 0.6518(3) 0.7510(2) 0.0191(11) Uani 1.00 1 d . . . C(2) C 1.1789(8) 0.5818(3) 0.7007(2) 0.0188(11) Uani 1.00 1 d . . . C(3) C 1.3564(8) 0.6033(3) 0.6310(2) 0.0170(11) Uani 1.00 1 d . . . C(4) C 1.4558(8) 0.6960(3) 0.6296(2) 0.0151(10) Uani 1.00 1 d . . . C(5) C 1.0781(8) 0.1751(3) 0.5405(2) 0.0160(11) Uani 1.00 1 d . . . C(6) C 1.1250(8) 0.2656(3) 0.5582(2) 0.0172(11) Uani 1.00 1 d . . . C(7) C 1.2945(8) 0.3183(3) 0.4997(2) 0.0149(10) Uani 1.00 1 d . . . C(8) C 1.3730(8) 0.2663(3) 0.4343(2) 0.0161(11) Uani 1.00 1 d . . . C(9) C 1.4310(8) 0.5480(3) 0.5641(2) 0.0138(10) Uani 1.00 1 d . . . C(10) C 1.3957(8) 0.4132(3) 0.5011(2) 0.0145(10) Uani 1.00 1 d . . . C(11) C 0.9804(8) 0.6572(3) 0.8280(2) 0.0203(11) Uani 1.00 1 d . . . C(12) C 1.1474(8) 0.6548(3) 0.8998(2) 0.0234(12) Uani 1.00 1 d . . . C(13) C 0.9623(8) 0.6659(3) 0.9762(2) 0.0224(12) Uani 1.00 1 d . . . C(14) C 1.1355(9) 0.6576(3) 1.0488(2) 0.0268(12) Uani 1.00 1 d . . . C(15) C 0.9521(9) 0.6702(3) 1.1256(2) 0.0264(12) Uani 1.00 1 d . . . C(16) C 1.1298(10) 0.6590(3) 1.1980(2) 0.0348(14) Uani 1.00 1 d . . . C(17) C 0.9192(8) 0.0950(3) 0.5855(2) 0.0195(11) Uani 1.00 1 d . . . C(18) C 0.7846(8) 0.1220(3) 0.6653(2) 0.0208(12) Uani 1.00 1 d . . . C(19) C 0.6358(8) 0.0338(3) 0.7097(2) 0.0194(11) Uani 1.00 1 d . . . C(20) C 0.4950(8) 0.0562(3) 0.7904(2) 0.0232(12) Uani 1.00 1 d . . . C(21) C 0.3578(9) -0.0333(3) 0.8346(2) 0.0265(12) Uani 1.00 1 d . . . C(22) C 0.2072(10) -0.0101(3) 0.9142(2) 0.0428(16) Uani 1.00 1 d . . . H(1) H 1.0908 0.5229 0.7106 0.022 Uiso 1.00 1 c R . . H(2) H 1.0508 0.2915 0.6058 0.020 Uiso 1.00 1 c R . . H(3) H 0.8987 0.5928 0.8416 0.024 Uiso 1.00 1 c R . . H(4) H 0.8180 0.7276 0.8190 0.024 Uiso 1.00 1 c R . . H(5) H 1.3023 0.5822 0.9114 0.028 Uiso 1.00 1 c R . . H(6) H 1.2388 0.7164 0.8854 0.027 Uiso 1.00 1 c R . . H(7) H 0.8645 0.6062 0.9894 0.027 Uiso 1.00 1 c R . . H(8) H 0.8124 0.7399 0.9654 0.027 Uiso 1.00 1 c R . . H(9) H 1.2347 0.7168 1.0353 0.032 Uiso 1.00 1 c R . . H(10) H 1.2844 0.5834 1.0597 0.032 Uiso 1.00 1 c R . . H(11) H 0.8055 0.7450 1.1153 0.032 Uiso 1.00 1 c R . . H(12) H 0.8505 0.6117 1.1389 0.032 Uiso 1.00 1 c R . . H(13) H 1.0522 0.0173 0.5966 0.023 Uiso 1.00 1 c R . . H(14) H 0.7658 0.0967 0.5507 0.023 Uiso 1.00 1 c R . . H(15) H 0.9351 0.1234 0.6997 0.026 Uiso 1.00 1 c R . . H(16) H 0.6421 0.1978 0.6546 0.026 Uiso 1.00 1 c R . . H(17) H 0.4874 0.0325 0.6745 0.024 Uiso 1.00 1 c R . . H(18) H 0.7796 -0.0417 0.7196 0.024 Uiso 1.00 1 c R . . H(19) H 0.6419 0.0595 0.8253 0.029 Uiso 1.00 1 c R . . H(20) H 0.3468 0.1307 0.7805 0.029 Uiso 1.00 1 c R . . H(21) H 0.5067 -0.1076 0.8449 0.031 Uiso 1.00 1 c R . . H(22) H 0.2129 -0.0372 0.7993 0.031 Uiso 1.00 1 c R . . H(23) H 1.2835 0.5871 1.2064 0.042 Uiso 1.00 1 c R . . H(24) H 1.0056 0.6613 1.2463 0.042 Uiso 0.96 1 c R . . H(25) H 1.2140 0.7217 1.1876 0.042 Uiso 0.98 1 c R . . H(26) H 0.3465 -0.0457 0.9576 0.054 Uiso 1.00 1 c R . . H(27) H 0.0462 -0.0424 0.9253 0.054 Uiso 1.00 1 c R . . H(28) H 0.1360 0.0715 0.9110 0.054 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0255(7) 0.0205(5) 0.0195(5) -0.0089(5) 0.0020(4) -0.0092(4) S(2) 0.0266(7) 0.0176(5) 0.0200(6) -0.0106(5) 0.0006(5) -0.0065(4) N(1) 0.019(2) 0.0129(16) 0.0185(18) -0.0059(16) -0.0016(15) -0.0049(14) C(1) 0.018(2) 0.019(2) 0.021(2) -0.006(2) 0.0011(19) -0.0056(18) C(2) 0.017(2) 0.016(2) 0.022(2) -0.0010(19) -0.0007(18) -0.0064(18) C(3) 0.020(2) 0.015(2) 0.017(2) -0.006(2) -0.0006(18) -0.0046(16) C(4) 0.014(2) 0.017(2) 0.015(2) -0.0015(19) 0.0007(17) -0.0083(17) C(5) 0.015(2) 0.019(2) 0.015(2) -0.006(2) -0.0010(17) -0.0045(17) C(6) 0.019(2) 0.017(2) 0.014(2) -0.004(2) -0.0007(17) -0.0014(16) C(7) 0.016(2) 0.013(2) 0.015(2) -0.0024(19) -0.0024(17) -0.0048(17) C(8) 0.016(2) 0.013(2) 0.019(2) -0.0034(19) -0.0066(18) -0.0018(17) C(9) 0.018(2) 0.0108(19) 0.014(2) -0.0041(19) -0.0015(17) -0.0044(16) C(10) 0.017(2) 0.0098(18) 0.016(2) -0.0017(18) 0.0006(17) -0.0038(16) C(11) 0.023(2) 0.019(2) 0.020(2) -0.006(2) 0.0005(18) -0.0052(17) C(12) 0.021(2) 0.031(2) 0.017(2) -0.007(2) 0.0044(18) -0.0054(18) C(13) 0.026(2) 0.026(2) 0.016(2) -0.008(2) 0.0016(18) -0.0076(18) C(14) 0.033(2) 0.028(2) 0.018(2) -0.009(2) 0.003(2) -0.0041(18) C(15) 0.034(2) 0.026(2) 0.020(2) -0.011(2) 0.004(2) -0.0067(19) C(16) 0.043(3) 0.034(2) 0.028(2) -0.011(2) 0.004(2) -0.009(2) C(17) 0.024(2) 0.015(2) 0.018(2) -0.005(2) -0.0014(18) -0.0014(17) C(18) 0.020(2) 0.022(2) 0.023(2) -0.009(2) 0.0015(19) -0.0061(18) C(19) 0.021(2) 0.020(2) 0.018(2) -0.006(2) 0.0003(19) -0.0057(18) C(20) 0.022(2) 0.026(2) 0.024(2) -0.009(2) 0.004(2) -0.0087(19) C(21) 0.029(2) 0.025(2) 0.022(2) -0.009(2) 0.009(2) -0.0021(19) C(22) 0.059(3) 0.052(3) 0.024(2) -0.028(3) 0.010(2) -0.010(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S(1) C(1) 1.754(4) yes . . S(1) C(4) 1.721(3) yes . . S(2) C(5) 1.756(3) yes . . S(2) C(8) 1.726(4) yes . . N(1) C(9) 1.352(5) yes . . N(1) C(10) 1.346(5) yes . . C(1) C(2) 1.349(6) yes . . C(1) C(11) 1.490(5) yes . . C(2) C(3) 1.430(5) yes . . C(3) C(4) 1.403(6) yes . . C(3) C(9) 1.445(5) yes . . C(4) C(8) 1.397(5) yes . 2_866 C(5) C(6) 1.347(6) yes . . C(5) C(17) 1.497(5) yes . . C(6) C(7) 1.417(5) yes . . C(7) C(8) 1.397(5) yes . . C(7) C(10) 1.446(6) yes . . C(9) C(10) 1.423(5) yes . 2_866 C(11) C(12) 1.523(5) yes . . C(12) C(13) 1.528(5) yes . . C(13) C(14) 1.527(6) yes . . C(14) C(15) 1.533(5) yes . . C(15) C(16) 1.528(6) yes . . C(17) C(18) 1.526(5) yes . . C(18) C(19) 1.538(6) yes . . C(19) C(20) 1.531(5) yes . . C(20) C(21) 1.513(6) yes . . C(21) C(22) 1.533(5) yes . . C(2) H(1) 0.950 no . . C(6) H(2) 0.950 no . . C(11) H(3) 0.990 no . . C(11) H(4) 0.990 no . . C(12) H(5) 0.990 no . . C(12) H(6) 0.990 no . . C(13) H(7) 0.990 no . . C(13) H(8) 0.990 no . . C(14) H(9) 0.990 no . . C(14) H(10) 0.990 no . . C(15) H(11) 0.990 no . . C(15) H(12) 0.990 no . . C(16) H(23) 0.980 no . . C(16) H(24) 0.980 no . . C(16) H(25) 0.980 no . . C(17) H(13) 0.990 no . . C(17) H(14) 0.990 no . . C(18) H(15) 0.990 no . . C(18) H(16) 0.990 no . . C(19) H(17) 0.990 no . . C(19) H(18) 0.990 no . . C(20) H(19) 0.990 no . . C(20) H(20) 0.990 no . . C(21) H(21) 0.990 no . . C(21) H(22) 0.990 no . . C(22) H(26) 0.980 no . . C(22) H(27) 0.980 no . . C(22) H(28) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(1) S(1) C(4) 92.1(2) yes . . . C(5) S(2) C(8) 91.8(2) yes . . . C(9) N(1) C(10) 116.1(3) yes . . . S(1) C(1) C(2) 110.9(2) yes . . . S(1) C(1) C(11) 119.0(3) yes . . . C(2) C(1) C(11) 130.0(4) yes . . . C(1) C(2) C(3) 114.2(4) yes . . . C(2) C(3) C(4) 111.6(3) yes . . . C(2) C(3) C(9) 129.7(4) yes . . . C(4) C(3) C(9) 118.7(3) yes . . . S(1) C(4) C(3) 111.2(2) yes . . . S(1) C(4) C(8) 127.6(3) yes . . 2_866 C(3) C(4) C(8) 121.2(3) yes . . 2_866 S(2) C(5) C(6) 110.9(2) yes . . . S(2) C(5) C(17) 117.5(3) yes . . . C(6) C(5) C(17) 131.6(3) yes . . . C(5) C(6) C(7) 114.1(3) yes . . . C(6) C(7) C(8) 112.5(3) yes . . . C(6) C(7) C(10) 128.7(3) yes . . . C(8) C(7) C(10) 118.8(3) yes . . . S(2) C(8) C(4) 127.5(3) yes . . 2_866 S(2) C(8) C(7) 110.7(2) yes . . . C(4) C(8) C(7) 121.8(4) yes 2_866 . . N(1) C(9) C(3) 117.9(3) yes . . . N(1) C(9) C(10) 122.1(3) yes . . 2_866 C(3) C(9) C(10) 120.0(3) yes . . 2_866 N(1) C(10) C(7) 118.6(3) yes . . . N(1) C(10) C(9) 121.8(3) yes . . 2_866 C(7) C(10) C(9) 119.6(3) yes . . 2_866 C(1) C(11) C(12) 115.4(3) yes . . . C(11) C(12) C(13) 113.4(3) yes . . . C(12) C(13) C(14) 112.7(3) yes . . . C(13) C(14) C(15) 113.4(3) yes . . . C(14) C(15) C(16) 112.7(3) yes . . . C(5) C(17) C(18) 113.7(3) yes . . . C(17) C(18) C(19) 110.9(3) yes . . . C(18) C(19) C(20) 113.6(3) yes . . . C(19) C(20) C(21) 112.9(3) yes . . . C(20) C(21) C(22) 113.6(3) yes . . . C(1) C(2) H(1) 123.1 no . . . C(3) C(2) H(1) 122.7 no . . . C(5) C(6) H(2) 122.8 no . . . C(7) C(6) H(2) 123.1 no . . . C(1) C(11) H(3) 108.1 no . . . C(1) C(11) H(4) 108.6 no . . . C(12) C(11) H(3) 108.9 no . . . C(12) C(11) H(4) 108.0 no . . . H(3) C(11) H(4) 107.5 no . . . C(11) C(12) H(5) 108.4 no . . . C(11) C(12) H(6) 109.2 no . . . C(13) C(12) H(5) 108.5 no . . . C(13) C(12) H(6) 109.4 no . . . H(5) C(12) H(6) 107.7 no . . . C(12) C(13) H(7) 109.4 no . . . C(12) C(13) H(8) 108.5 no . . . C(14) C(13) H(7) 109.2 no . . . C(14) C(13) H(8) 109.1 no . . . H(7) C(13) H(8) 107.8 no . . . C(13) C(14) H(9) 109.1 no . . . C(13) C(14) H(10) 108.9 no . . . C(15) C(14) H(9) 109.1 no . . . C(15) C(14) H(10) 108.6 no . . . H(9) C(14) H(10) 107.7 no . . . C(14) C(15) H(11) 108.8 no . . . C(14) C(15) H(12) 109.3 no . . . C(16) C(15) H(11) 109.3 no . . . C(16) C(15) H(12) 108.9 no . . . H(11) C(15) H(12) 107.8 no . . . C(15) C(16) H(23) 109.7 no . . . C(15) C(16) H(24) 109.4 no . . . C(15) C(16) H(25) 109.3 no . . . H(23) C(16) H(24) 109.5 no . . . H(23) C(16) H(25) 109.5 no . . . H(24) C(16) H(25) 109.5 no . . . C(5) C(17) H(13) 109.2 no . . . C(5) C(17) H(14) 108.7 no . . . C(18) C(17) H(13) 108.6 no . . . C(18) C(17) H(14) 108.8 no . . . H(13) C(17) H(14) 107.6 no . . . C(17) C(18) H(15) 109.6 no . . . C(17) C(18) H(16) 109.4 no . . . C(19) C(18) H(15) 109.6 no . . . C(19) C(18) H(16) 109.3 no . . . H(15) C(18) H(16) 108.0 no . . . C(18) C(19) H(17) 108.9 no . . . C(18) C(19) H(18) 108.6 no . . . C(20) C(19) H(17) 108.9 no . . . C(20) C(19) H(18) 109.0 no . . . H(17) C(19) H(18) 107.6 no . . . C(19) C(20) H(19) 109.1 no . . . C(19) C(20) H(20) 109.2 no . . . C(21) C(20) H(19) 108.8 no . . . C(21) C(20) H(20) 109.0 no . . . H(19) C(20) H(20) 107.7 no . . . C(20) C(21) H(21) 108.9 no . . . C(20) C(21) H(22) 108.7 no . . . C(22) C(21) H(21) 109.9 no . . . C(22) C(21) H(22) 108.0 no . . . H(21) C(21) H(22) 107.7 no . . . C(21) C(22) H(26) 108.3 no . . . C(21) C(22) H(27) 109.8 no . . . C(21) C(22) H(28) 110.3 no . . . H(26) C(22) H(27) 109.5 no . . . H(26) C(22) H(28) 109.5 no . . . H(27) C(22) H(28) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(4) C(3) -0.2(2) ? . . . . C(1) S(1) C(4) C(8) 179.1(3) ? . . . 2_866 C(4) S(1) C(1) C(2) -0.7(2) ? . . . . C(4) S(1) C(1) C(11) -178.6(2) ? . . . . C(5) S(2) C(8) C(7) 0.7(2) ? . . . . C(5) S(2) C(8) C(4) 178.3(3) ? . . . 2_866 C(8) S(2) C(5) C(6) 0.0(2) ? . . . . C(8) S(2) C(5) C(17) -179.4(2) ? . . . . C(9) N(1) C(10) C(7) 178.7(3) ? . . . . C(9) N(1) C(10) C(9) -0.2(4) ? . . . 2_866 C(10) N(1) C(9) C(3) 178.7(3) ? . . . . C(10) N(1) C(9) C(10) 0.2(4) ? . . . 2_866 S(1) C(1) C(2) C(3) 1.4(4) ? . . . . S(1) C(1) C(11) C(12) -55.0(3) ? . . . . C(2) C(1) C(11) C(12) 127.6(4) ? . . . . C(11) C(1) C(2) C(3) 179.0(3) ? . . . . C(1) C(2) C(3) C(4) -1.5(4) ? . . . . C(1) C(2) C(3) C(9) -178.6(3) ? . . . . C(2) C(3) C(4) S(1) 0.9(3) ? . . . . C(2) C(3) C(4) C(8) -178.3(3) ? . . . 2_866 C(2) C(3) C(9) N(1) -1.1(5) ? . . . . C(2) C(3) C(9) C(10) 177.5(3) ? . . . 2_866 C(4) C(3) C(9) N(1) -178.0(3) ? . . . . C(4) C(3) C(9) C(10) 0.6(5) ? . . . 2_866 C(9) C(3) C(4) S(1) 178.3(2) ? . . . . C(9) C(3) C(4) C(8) -0.9(5) ? . . . 2_866 S(1) C(4) C(8) S(2) -1.4(5) ? . . 2_866 2_866 S(1) C(4) C(8) C(7) -178.7(2) ? . . 2_866 2_866 C(3) C(4) C(8) S(2) 177.7(2) ? . . 2_866 2_866 C(3) C(4) C(8) C(7) 0.4(5) ? . . 2_866 2_866 S(2) C(5) C(6) C(7) -0.7(3) ? . . . . S(2) C(5) C(17) C(18) 179.95(17) ? . . . . C(6) C(5) C(17) C(18) 0.7(5) ? . . . . C(17) C(5) C(6) C(7) 178.6(3) ? . . . . C(5) C(6) C(7) C(8) 1.3(4) ? . . . . C(5) C(6) C(7) C(10) -177.1(3) ? . . . . C(6) C(7) C(8) S(2) -1.2(3) ? . . . . C(6) C(7) C(8) C(4) -179.0(3) ? . . . 2_866 C(6) C(7) C(10) N(1) 0.1(4) ? . . . . C(6) C(7) C(10) C(9) 179.0(3) ? . . . 2_866 C(8) C(7) C(10) N(1) -178.2(3) ? . . . . C(8) C(7) C(10) C(9) 0.7(4) ? . . . 2_866 C(10) C(7) C(8) S(2) 177.3(2) ? . . . . C(10) C(7) C(8) C(4) -0.5(5) ? . . . 2_866 N(1) C(9) C(10) N(1) -0.2(4) ? . . 2_866 2_866 N(1) C(9) C(10) C(7) 178.7(3) ? . . 2_866 2_866 C(3) C(9) C(10) N(1) -178.7(3) ? . . 2_866 2_866 C(3) C(9) C(10) C(7) 0.2(4) ? . . 2_866 2_866 C(1) C(11) C(12) C(13) 177.4(3) ? . . . . C(11) C(12) C(13) C(14) 177.2(3) ? . . . . C(12) C(13) C(14) C(15) 179.2(3) ? . . . . C(13) C(14) C(15) C(16) 178.7(3) ? . . . . C(5) C(17) C(18) C(19) -177.7(2) ? . . . . C(17) C(18) C(19) C(20) -179.8(2) ? . . . . C(18) C(19) C(20) C(21) -178.2(3) ? . . . . C(19) C(20) C(21) C(22) -178.1(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(1) C(11) 3.594(4) ? . 1_655 S(2) C(4) 3.563(3) ? . 2_766 N(1) C(7) 3.500(4) ? . 2_766 N(1) C(10) 3.566(4) ? . 2_766 C(2) C(4) 3.590(5) ? . 1_455 C(2) C(8) 3.484(5) ? . 2_766 C(3) C(8) 3.599(5) ? . 2_766 C(4) S(2) 3.563(3) ? . 2_766 C(4) C(2) 3.590(5) ? . 1_655 C(6) C(9) 3.479(4) ? . 2_766 C(6) C(10) 3.588(5) ? . 1_455 C(6) C(18) 3.599(5) ? . 1_655 C(7) N(1) 3.500(4) ? . 2_766 C(7) C(9) 3.578(5) ? . 2_766 C(8) C(2) 3.484(5) ? . 2_766 C(8) C(3) 3.599(5) ? . 2_766 C(9) C(6) 3.479(4) ? . 2_766 C(9) C(7) 3.578(5) ? . 2_766 C(10) N(1) 3.566(4) ? . 2_766 C(10) C(6) 3.588(5) ? . 1_655 C(11) S(1) 3.594(4) ? . 1_455 C(18) C(6) 3.599(5) ? . 1_455 C(22) C(22) 3.423(5) ? . 2_557 S(1) H(3) 3.472 ? . 1_655 S(1) H(4) 3.000 ? . 1_655 S(1) H(13) 3.427 ? . 1_565 S(1) H(18) 3.169 ? . 1_565 S(1) H(21) 3.487 ? . 1_665 S(1) H(22) 3.242 ? . 1_665 S(2) H(13) 3.188 ? . 2_756 S(2) H(13) 3.592 ? . 2_856 S(2) H(14) 3.046 ? . 1_655 S(2) H(14) 3.175 ? . 2_756 S(2) H(17) 3.401 ? . 2_756 S(2) H(18) 3.491 ? . 2_756 N(1) H(2) 3.573 ? . 1_655 N(1) H(16) 3.283 ? . 1_655 C(1) H(12) 3.434 ? . 2_767 C(1) H(23) 3.413 ? . 2_867 C(2) H(12) 3.242 ? . 2_767 C(2) H(23) 3.118 ? . 2_867 C(2) H(24) 3.386 ? . 2_767 C(3) H(23) 3.425 ? . 2_867 C(4) H(1) 3.400 ? . 1_655 C(4) H(14) 3.547 ? . 2_766 C(5) H(14) 3.213 ? . 1_655 C(5) H(17) 3.026 ? . 1_655 C(6) H(14) 3.227 ? . 1_655 C(6) H(16) 2.930 ? . 1_655 C(6) H(17) 3.240 ? . 1_655 C(7) H(14) 3.043 ? . 1_655 C(7) H(16) 3.083 ? . 1_655 C(8) H(1) 3.548 ? . 2_766 C(8) H(14) 2.899 ? . 1_655 C(10) H(2) 3.542 ? . 1_655 C(10) H(16) 3.309 ? . 1_655 C(11) H(6) 3.569 ? . 1_455 C(11) H(12) 3.191 ? . 2_767 C(11) H(21) 3.239 ? . 1_565 C(12) H(7) 3.426 ? . 2_767 C(12) H(10) 3.407 ? . 2_867 C(13) H(7) 3.228 ? . 2_767 C(13) H(9) 3.516 ? . 1_455 C(13) H(21) 3.492 ? . 1_565 C(14) H(3) 3.337 ? . 2_767 C(14) H(5) 3.403 ? . 2_867 C(14) H(7) 3.524 ? . 1_655 C(14) H(7) 3.576 ? . 2_767 C(14) H(28) 3.511 ? . 2_667 C(15) H(1) 3.290 ? . 2_767 C(15) H(3) 3.126 ? . 2_767 C(15) H(20) 3.225 ? . 2_667 C(15) H(25) 3.576 ? . 1_455 C(15) H(28) 3.102 ? . 2_667 C(16) H(1) 2.911 ? . 2_767 C(16) H(2) 3.537 ? . 2_767 C(16) H(3) 3.481 ? . 2_767 C(16) H(12) 3.488 ? . 1_655 C(16) H(15) 3.538 ? . 2_767 C(16) H(20) 3.042 ? . 2_667 C(16) H(28) 3.406 ? . 2_667 C(17) H(17) 3.082 ? . 1_655 C(18) H(17) 3.281 ? . 1_655 C(18) H(20) 3.566 ? . 1_655 C(18) H(22) 3.128 ? . 1_655 C(18) H(25) 3.560 ? . 2_767 C(19) H(15) 3.272 ? . 1_455 C(19) H(22) 3.112 ? . 1_655 C(20) H(11) 3.228 ? . 2_667 C(20) H(15) 3.054 ? . 1_455 C(20) H(22) 3.352 ? . 1_655 C(20) H(27) 3.438 ? . 1_655 C(21) H(4) 3.243 ? . 1_545 C(21) H(6) 3.316 ? . 1_445 C(21) H(8) 3.487 ? . 1_545 C(21) H(15) 3.113 ? . 1_455 C(21) H(19) 3.343 ? . 1_455 C(22) H(6) 3.592 ? . 1_445 C(22) H(9) 3.568 ? . 1_445 C(22) H(11) 3.278 ? . 2_667 C(22) H(19) 3.059 ? . 1_455 C(22) H(26) 3.335 ? . 2_557 C(22) H(26) 3.552 ? . 2_657 C(22) H(27) 3.039 ? . 2_557 C(22) H(28) 3.332 ? . 2_557 H(1) C(4) 3.400 ? . 1_455 H(1) C(8) 3.548 ? . 2_766 H(1) C(15) 3.290 ? . 2_767 H(1) C(16) 2.911 ? . 2_767 H(1) H(12) 2.709 ? . 2_767 H(1) H(23) 2.735 ? . 2_767 H(1) H(23) 3.248 ? . 2_867 H(1) H(24) 2.464 ? . 2_767 H(2) N(1) 3.573 ? . 1_455 H(2) C(10) 3.542 ? . 1_455 H(2) C(16) 3.537 ? . 2_767 H(2) H(16) 2.887 ? . 1_655 H(2) H(17) 3.335 ? . 1_655 H(2) H(20) 3.349 ? . 1_655 H(2) H(24) 2.701 ? . 2_767 H(3) S(1) 3.472 ? . 1_455 H(3) C(14) 3.337 ? . 2_767 H(3) C(15) 3.126 ? . 2_767 H(3) C(16) 3.481 ? . 2_767 H(3) H(5) 3.081 ? . 1_455 H(3) H(6) 3.238 ? . 1_455 H(3) H(7) 3.376 ? . 2_767 H(3) H(10) 2.799 ? . 2_767 H(3) H(12) 2.474 ? . 2_767 H(3) H(23) 3.003 ? . 2_767 H(4) S(1) 3.000 ? . 1_455 H(4) C(21) 3.243 ? . 1_565 H(4) H(6) 2.988 ? . 1_455 H(4) H(18) 2.983 ? . 1_565 H(4) H(21) 2.301 ? . 1_565 H(4) H(22) 3.484 ? . 1_565 H(5) C(14) 3.403 ? . 2_867 H(5) H(3) 3.081 ? . 1_655 H(5) H(5) 3.581 ? . 2_867 H(5) H(7) 3.288 ? . 1_655 H(5) H(7) 2.882 ? . 2_767 H(5) H(10) 2.421 ? . 2_867 H(5) H(12) 3.109 ? . 2_767 H(5) H(23) 3.387 ? . 2_867 H(6) C(11) 3.569 ? . 1_655 H(6) C(21) 3.316 ? . 1_665 H(6) C(22) 3.592 ? . 1_665 H(6) H(3) 3.238 ? . 1_655 H(6) H(4) 2.988 ? . 1_655 H(6) H(7) 3.414 ? . 1_655 H(6) H(8) 3.352 ? . 1_655 H(6) H(21) 2.851 ? . 1_665 H(6) H(22) 3.103 ? . 1_665 H(6) H(27) 3.150 ? . 1_665 H(7) C(12) 3.426 ? . 2_767 H(7) C(13) 3.228 ? . 2_767 H(7) C(14) 3.524 ? . 1_455 H(7) C(14) 3.576 ? . 2_767 H(7) H(3) 3.376 ? . 2_767 H(7) H(5) 3.288 ? . 1_455 H(7) H(5) 2.882 ? . 2_767 H(7) H(6) 3.414 ? . 1_455 H(7) H(7) 2.578 ? . 2_767 H(7) H(9) 3.088 ? . 1_455 H(7) H(10) 3.051 ? . 1_455 H(7) H(10) 3.038 ? . 2_767 H(8) C(21) 3.487 ? . 1_565 H(8) H(6) 3.352 ? . 1_455 H(8) H(9) 3.039 ? . 1_455 H(8) H(21) 2.666 ? . 1_565 H(8) H(26) 2.959 ? . 1_565 H(8) H(27) 3.221 ? . 1_665 H(9) C(13) 3.516 ? . 1_655 H(9) C(22) 3.568 ? . 1_665 H(9) H(7) 3.088 ? . 1_655 H(9) H(8) 3.039 ? . 1_655 H(9) H(11) 3.366 ? . 1_655 H(9) H(12) 3.370 ? . 1_655 H(9) H(26) 3.191 ? . 1_665 H(9) H(27) 3.101 ? . 1_665 H(9) H(28) 3.050 ? . 2_667 H(10) C(12) 3.407 ? . 2_867 H(10) H(3) 2.799 ? . 2_767 H(10) H(5) 2.421 ? . 2_867 H(10) H(7) 3.051 ? . 1_655 H(10) H(7) 3.038 ? . 2_767 H(10) H(10) 3.416 ? . 2_867 H(10) H(12) 3.340 ? . 1_655 H(11) C(20) 3.228 ? . 2_667 H(11) C(22) 3.278 ? . 2_667 H(11) H(9) 3.366 ? . 1_455 H(11) H(19) 3.083 ? . 2_667 H(11) H(20) 2.572 ? . 2_667 H(11) H(25) 3.114 ? . 1_455 H(11) H(26) 3.597 ? . 2_667 H(11) H(28) 2.376 ? . 2_667 H(12) C(1) 3.434 ? . 2_767 H(12) C(2) 3.242 ? . 2_767 H(12) C(11) 3.191 ? . 2_767 H(12) C(16) 3.488 ? . 1_455 H(12) H(1) 2.709 ? . 2_767 H(12) H(3) 2.474 ? . 2_767 H(12) H(5) 3.109 ? . 2_767 H(12) H(9) 3.370 ? . 1_455 H(12) H(10) 3.340 ? . 1_455 H(12) H(23) 2.985 ? . 1_455 H(12) H(25) 3.127 ? . 1_455 H(13) S(1) 3.427 ? . 1_545 H(13) S(2) 3.188 ? . 2_756 H(13) S(2) 3.592 ? . 2_856 H(13) H(13) 3.528 ? . 2_756 H(13) H(14) 3.125 ? . 2_756 H(13) H(17) 2.689 ? . 1_655 H(13) H(22) 3.474 ? . 1_655 H(14) S(2) 3.046 ? . 1_455 H(14) S(2) 3.175 ? . 2_756 H(14) C(4) 3.547 ? . 2_766 H(14) C(5) 3.213 ? . 1_455 H(14) C(6) 3.227 ? . 1_455 H(14) C(7) 3.043 ? . 1_455 H(14) C(8) 2.899 ? . 1_455 H(14) H(13) 3.125 ? . 2_756 H(14) H(14) 3.493 ? . 2_756 H(15) C(16) 3.538 ? . 2_767 H(15) C(19) 3.272 ? . 1_655 H(15) C(20) 3.054 ? . 1_655 H(15) C(21) 3.113 ? . 1_655 H(15) H(17) 2.635 ? . 1_655 H(15) H(20) 2.578 ? . 1_655 H(15) H(22) 2.444 ? . 1_655 H(15) H(24) 3.195 ? . 2_767 H(15) H(25) 2.967 ? . 2_767 H(16) N(1) 3.283 ? . 1_455 H(16) C(6) 2.930 ? . 1_455 H(16) C(7) 3.083 ? . 1_455 H(16) C(10) 3.309 ? . 1_455 H(16) H(2) 2.887 ? . 1_455 H(16) H(24) 3.596 ? . 2_767 H(16) H(25) 3.302 ? . 2_767 H(17) S(2) 3.401 ? . 2_756 H(17) C(5) 3.026 ? . 1_455 H(17) C(6) 3.240 ? . 1_455 H(17) C(17) 3.082 ? . 1_455 H(17) C(18) 3.281 ? . 1_455 H(17) H(2) 3.335 ? . 1_455 H(17) H(13) 2.689 ? . 1_455 H(17) H(15) 2.635 ? . 1_455 H(18) S(1) 3.169 ? . 1_545 H(18) S(2) 3.491 ? . 2_756 H(18) H(4) 2.983 ? . 1_545 H(18) H(22) 2.642 ? . 1_655 H(19) C(21) 3.343 ? . 1_655 H(19) C(22) 3.059 ? . 1_655 H(19) H(11) 3.083 ? . 2_667 H(19) H(22) 2.730 ? . 1_655 H(19) H(25) 3.036 ? . 2_767 H(19) H(27) 2.548 ? . 1_655 H(19) H(28) 2.998 ? . 1_655 H(20) C(15) 3.225 ? . 2_667 H(20) C(16) 3.042 ? . 2_667 H(20) C(18) 3.566 ? . 1_455 H(20) H(2) 3.349 ? . 1_455 H(20) H(11) 2.572 ? . 2_667 H(20) H(15) 2.578 ? . 1_455 H(20) H(24) 2.642 ? . 2_667 H(20) H(25) 2.903 ? . 2_667 H(20) H(25) 3.411 ? . 2_767 H(21) S(1) 3.487 ? . 1_445 H(21) C(11) 3.239 ? . 1_545 H(21) C(13) 3.492 ? . 1_545 H(21) H(4) 2.301 ? . 1_545 H(21) H(6) 2.851 ? . 1_445 H(21) H(8) 2.666 ? . 1_545 H(21) H(27) 3.478 ? . 1_655 H(22) S(1) 3.242 ? . 1_445 H(22) C(18) 3.128 ? . 1_455 H(22) C(19) 3.112 ? . 1_455 H(22) C(20) 3.352 ? . 1_455 H(22) H(4) 3.484 ? . 1_545 H(22) H(6) 3.103 ? . 1_445 H(22) H(13) 3.474 ? . 1_455 H(22) H(15) 2.444 ? . 1_455 H(22) H(18) 2.642 ? . 1_455 H(22) H(19) 2.730 ? . 1_455 H(23) C(1) 3.413 ? . 2_867 H(23) C(2) 3.118 ? . 2_867 H(23) C(3) 3.425 ? . 2_867 H(23) H(1) 2.735 ? . 2_767 H(23) H(1) 3.248 ? . 2_867 H(23) H(3) 3.003 ? . 2_767 H(23) H(5) 3.387 ? . 2_867 H(23) H(12) 2.985 ? . 1_655 H(24) C(2) 3.386 ? . 2_767 H(24) H(1) 2.464 ? . 2_767 H(24) H(2) 2.701 ? . 2_767 H(24) H(15) 3.195 ? . 2_767 H(24) H(16) 3.596 ? . 2_767 H(24) H(20) 2.642 ? . 2_667 H(25) C(15) 3.576 ? . 1_655 H(25) C(18) 3.560 ? . 2_767 H(25) H(11) 3.114 ? . 1_655 H(25) H(12) 3.127 ? . 1_655 H(25) H(15) 2.967 ? . 2_767 H(25) H(16) 3.302 ? . 2_767 H(25) H(19) 3.036 ? . 2_767 H(25) H(20) 2.903 ? . 2_667 H(25) H(20) 3.411 ? . 2_767 H(25) H(28) 2.890 ? . 2_667 H(26) C(22) 3.335 ? . 2_557 H(26) C(22) 3.552 ? . 2_657 H(26) H(8) 2.959 ? . 1_545 H(26) H(9) 3.191 ? . 1_445 H(26) H(11) 3.597 ? . 2_667 H(26) H(26) 3.529 ? . 2_557 H(26) H(26) 2.824 ? . 2_657 H(26) H(27) 3.431 ? . 1_655 H(26) H(27) 2.828 ? . 2_557 H(26) H(28) 3.142 ? . 2_557 H(26) H(28) 3.421 ? . 2_657 H(27) C(20) 3.438 ? . 1_455 H(27) C(22) 3.039 ? . 2_557 H(27) H(6) 3.150 ? . 1_445 H(27) H(8) 3.221 ? . 1_445 H(27) H(9) 3.101 ? . 1_445 H(27) H(19) 2.548 ? . 1_455 H(27) H(21) 3.478 ? . 1_455 H(27) H(26) 3.431 ? . 1_455 H(27) H(26) 2.828 ? . 2_557 H(27) H(27) 2.944 ? . 2_557 H(27) H(28) 2.825 ? . 2_557 H(28) C(14) 3.511 ? . 2_667 H(28) C(15) 3.102 ? . 2_667 H(28) C(16) 3.406 ? . 2_667 H(28) C(22) 3.332 ? . 2_557 H(28) H(9) 3.050 ? . 2_667 H(28) H(11) 2.376 ? . 2_667 H(28) H(19) 2.998 ? . 1_455 H(28) H(25) 2.890 ? . 2_667 H(28) H(26) 3.142 ? . 2_557 H(28) H(26) 3.421 ? . 2_657 H(28) H(27) 2.825 ? . 2_557 H(28) H(28) 3.523 ? . 2_557 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================