Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global #------------------------------------------------------------------------------ _publ_requested_journal 'Journal of Materials Chemistry' _journal_coden_Cambridge 1145 _publ_contact_author_name 'Shuichi Sekizaki,Gunzi Saito' _publ_contact_author_address ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; _publ_contact_author_email 'sekizaki@kuchem.kyoto-u.ac.jp' #------------------------------------------------------------------------------ _publ_section_title ; Structural aspects of a series of cation radical salts of tetrathiotetracene (TTT) with 2-alkoxy-1,1,3,3-tetracyanoallylide anions (RO-TCA; R=Me,Et,Pr,Bu) ; loop_ _publ_author_name _publ_author_address 'Sekizaki, Shuichi' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Tada, Chiyoko' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Yamochi, Hideki' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; 'Saito, Gunzi' ; Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto, 606-8502, Japan ; #------------------------------------------------------------------------------ data_(TTT)(MeO-TCA) _database_code_CSD 165346 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _chemical_formula_moiety 'C18 H8 S4 1+,C7 H3 N4 O1 1-' _chemical_formula_sum 'C25 H11 N4 O1 S4 ' _chemical_formula_weight 511.65 _cell_length_a 12.351(2) _cell_length_b 23.632(4) _cell_length_c 7.603(1) _cell_angle_alpha 90.000000(0) _cell_angle_beta 101.47(1) _cell_angle_gamma 90.000000(0) _cell_volume 2174.9(6) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '?' _cell_measurement_theta_max '?' _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_meas 1.575 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.465 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3-chi' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 5661 _reflns_number_total ? _reflns_number_observed 2992 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _refine_ls_structure_factor_coef ? _refine_ls_R_factor_obs 0.041 _refine_ls_wR_factor_obs 0.046 _refine_ls_hydrogen_treatment 'refall' _refine_ls_number_reflns 2992 _refine_ls_number_parameters 360 _refine_ls_goodness_of_fit_obs 2.303 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0817 _refine_ls_shift/esd_mean 0.0034 _refine_diff_density_min -0.33 _refine_diff_density_max 0.29 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+0.5,+Y+0.5,-Z+0.5 +X+0.5,-Y+0.5,+Z+0.5 _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_cell_setting 'Monoclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.12247(8) -0.12375(4) 0.49050(14) 0.0333(5) 1.000 Uij S2 -0.03717(9) -0.15186(4) 0.39062(14) 0.0338(5) 1.000 Uij S3 -0.15160(8) 0.08235(4) 0.01486(14) 0.0334(5) 1.000 Uij S4 0.00796(8) 0.11020(4) 0.11315(14) 0.0329(5) 1.000 Uij O21 0.3135(3) 0.2187(1) 0.4212(4) 0.046(2) 1.000 Uij N21 0.4149(3) 0.2553(2) 0.8572(6) 0.051(2) 1.000 Uij N22 0.1201(3) 0.3542(2) 0.7035(6) 0.056(2) 1.000 Uij N23 0.0996(4) 0.3852(2) 0.2446(6) 0.057(3) 1.000 Uij N24 0.1367(4) 0.2220(2) -0.0077(6) 0.063(3) 1.000 Uij C1 0.1048(3) -0.0569(2) 0.3951(5) 0.028(2) 1.000 Uij C2 -0.0016(3) -0.0470(2) 0.2952(5) 0.026(2) 1.000 Uij C3 -0.0813(3) -0.0897(2) 0.2772(5) 0.028(2) 1.000 Uij C4 -0.1900(3) -0.0805(2) 0.1761(5) 0.027(2) 1.000 Uij C5 -0.2732(3) -0.1225(2) 0.1588(6) 0.034(2) 1.000 Uij C6 -0.3770(4) -0.1124(2) 0.0617(6) 0.040(2) 1.000 Uij C7 -0.4024(3) -0.0600(2) -0.0228(6) 0.038(2) 1.000 Uij C8 -0.3248(3) -0.0181(2) -0.0099(6) 0.034(2) 1.000 Uij C9 -0.2166(3) -0.0269(2) 0.0890(5) 0.028(2) 1.000 Uij C10 -0.1334(3) 0.0154(2) 0.1073(5) 0.028(2) 1.000 Uij C11 -0.0279(3) 0.0059(2) 0.2097(5) 0.026(2) 1.000 Uij C12 0.0525(3) 0.0480(2) 0.2269(5) 0.028(2) 1.000 Uij C13 0.1605(3) 0.0399(2) 0.3332(5) 0.029(2) 1.000 Uij C14 0.2412(3) 0.0830(2) 0.3598(6) 0.035(2) 1.000 Uij C15 0.3429(4) 0.0734(2) 0.4653(6) 0.043(2) 1.000 Uij C16 0.3687(4) 0.0210(2) 0.5482(6) 0.041(2) 1.000 Uij C17 0.2938(3) -0.0219(2) 0.5244(6) 0.036(2) 1.000 Uij C18 0.1867(3) -0.0142(2) 0.4174(5) 0.029(2) 1.000 Uij C21 0.3442(4) 0.2672(2) 0.7420(6) 0.037(2) 1.000 Uij C22 0.1781(4) 0.3227(2) 0.6557(6) 0.039(2) 1.000 Uij C23 0.1343(4) 0.3402(2) 0.2595(6) 0.041(2) 1.000 Uij C24 0.1575(4) 0.2509(2) 0.1169(7) 0.046(2) 1.000 Uij C25 0.2550(3) 0.2850(2) 0.6027(6) 0.036(2) 1.000 Uij C26 0.2490(3) 0.2649(2) 0.4287(6) 0.036(2) 1.000 Uij C27 0.1821(3) 0.2857(2) 0.2725(6) 0.038(2) 1.000 Uij C28 0.3861(5) 0.2188(3) 0.2948(9) 0.060(3) 1.000 Uij H5 -0.259(3) -0.156(2) 0.219(5) 0.02(1) 1.000 Uiso H6 -0.428(4) -0.138(2) 0.068(6) 0.03(1) 1.000 Uiso H7 -0.475(4) -0.052(2) -0.082(7) 0.07(2) 1.000 Uiso H8 -0.345(3) 0.017(2) -0.065(5) 0.03(1) 1.000 Uiso H14 0.225(4) 0.120(2) 0.305(6) 0.05(1) 1.000 Uiso H15 0.395(4) 0.103(2) 0.475(6) 0.05(1) 1.000 Uiso H16 0.429(4) 0.016(2) 0.602(7) 0.05(2) 1.000 Uiso H17 0.317(3) -0.057(2) 0.563(6) 0.04(1) 1.000 Uiso H28A 0.354(6) 0.199(3) 0.176(11) 0.13(3) 1.000 Uiso H28B 0.400(6) 0.251(4) 0.247(11) 0.13(3) 1.000 Uiso H28C 0.443(5) 0.191(3) 0.332(8) 0.09(2) 1.000 Uiso 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 S1 0.0317(5) 0.0322(5) 0.0330(5) 0.0030(4) -0.0017(4) 0.0061(4) S2 0.0351(5) 0.0273(5) 0.0357(6) -0.0014(4) -0.0013(4) 0.0041(4) S3 0.0317(5) 0.0287(5) 0.0375(6) 0.0054(4) 0.0033(4) 0.0038(4) S4 0.0362(5) 0.0253(5) 0.0355(6) -0.0009(4) 0.0060(4) 0.0020(4) O21 0.058(2) 0.036(2) 0.042(2) 0.008(1) 0.013(2) -0.001(1) N21 0.055(3) 0.045(2) 0.046(2) 0.004(2) -0.006(2) 0.001(2) N22 0.045(2) 0.064(3) 0.053(3) 0.010(2) 0.002(2) -0.010(2) N23 0.060(3) 0.047(3) 0.061(3) 0.008(2) 0.003(2) 0.006(2) N24 0.063(3) 0.067(3) 0.053(3) 0.001(2) -0.005(2) -0.018(2) C1 0.032(2) 0.028(2) 0.022(2) 0.002(2) 0.002(2) -0.001(2) C2 0.024(2) 0.031(2) 0.021(2) 0.001(1) 0.003(1) -0.001(2) C3 0.030(2) 0.025(2) 0.027(2) 0.004(1) 0.005(2) 0.000(2) C4 0.024(2) 0.032(2) 0.026(2) -0.001(2) 0.004(1) -0.003(2) C5 0.034(2) 0.031(2) 0.036(2) -0.004(2) 0.006(2) -0.002(2) C6 0.032(2) 0.043(3) 0.043(2) -0.007(2) 0.008(2) -0.006(2) C7 0.021(2) 0.047(3) 0.044(3) 0.001(2) 0.001(2) -0.005(2) C8 0.029(2) 0.037(2) 0.036(2) 0.004(2) 0.002(2) 0.001(2) C9 0.028(2) 0.030(2) 0.024(2) 0.001(2) 0.005(1) -0.001(2) C10 0.029(2) 0.026(2) 0.028(2) 0.003(2) 0.007(2) 0.000(2) C11 0.025(2) 0.027(2) 0.024(2) 0.002(1) 0.005(1) 0.000(1) C12 0.030(2) 0.027(2) 0.027(2) 0.001(2) 0.007(2) -0.002(2) C13 0.028(2) 0.031(2) 0.027(2) -0.003(2) 0.007(2) -0.005(2) C14 0.036(2) 0.032(2) 0.037(2) -0.007(2) 0.005(2) -0.004(2) C15 0.036(2) 0.048(3) 0.042(3) -0.015(2) 0.006(2) -0.010(2) C16 0.025(2) 0.059(3) 0.037(2) -0.003(2) 0.000(2) -0.005(2) C17 0.030(2) 0.043(3) 0.031(2) 0.005(2) 0.002(2) -0.002(2) C18 0.027(2) 0.035(2) 0.024(2) 0.002(2) 0.004(1) -0.006(2) C21 0.041(2) 0.030(2) 0.039(2) -0.003(2) 0.008(2) -0.004(2) C22 0.039(2) 0.039(2) 0.036(2) -0.002(2) 0.001(2) -0.002(2) C23 0.036(2) 0.048(3) 0.037(2) -0.003(2) 0.002(2) 0.002(2) C24 0.041(2) 0.045(3) 0.047(3) 0.001(2) -0.004(2) 0.002(2) C25 0.037(2) 0.032(2) 0.038(2) -0.003(2) 0.002(2) -0.001(2) C26 0.036(2) 0.031(2) 0.040(2) -0.005(2) 0.008(2) -0.001(2) C27 0.038(2) 0.036(2) 0.038(2) -0.004(2) 0.005(2) -0.004(2) C28 0.050(3) 0.059(4) 0.072(4) 0.007(3) 0.020(3) 0.004(3) 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 S1 S2 2.076(2) . . ? S1 C1 1.733(4) . . ? S2 C3 1.735(4) . . ? S3 S4 2.071(2) . . ? S3 C10 1.728(4) . . ? S4 C12 1.738(4) . . ? O21 C26 1.358(6) . . ? O21 C28 1.439(8) . . ? N21 C21 1.142(6) . . ? N22 C22 1.142(7) . . ? N23 C23 1.144(7) . . ? N24 C24 1.155(7) . . ? C1 C2 1.401(6) . . ? C1 C18 1.415(6) . . ? C2 C3 1.398(6) . . ? C2 C11 1.417(6) . . ? C3 C4 1.424(6) . . ? C4 C5 1.416(6) . . ? C4 C9 1.437(6) . . ? C5 C6 1.367(7) . . ? C6 C7 1.401(7) . . ? C7 C8 1.368(7) . . ? C8 C9 1.413(6) . . ? C9 C10 1.420(6) . . ? C10 C11 1.397(6) . . ? C11 C12 1.393(6) . . ? C12 C13 1.428(6) . . ? C13 C14 1.412(6) . . ? C13 C18 1.438(6) . . ? C14 C15 1.368(7) . . ? C15 C16 1.398(8) . . ? C16 C17 1.360(7) . . ? C17 C18 1.419(6) . . ? C21 C25 1.431(7) . . ? C22 C25 1.418(7) . . ? C23 C27 1.413(7) . . ? C24 C27 1.423(7) . . ? C25 C26 1.394(6) . . ? C26 C27 1.394(6) . . ? C5 H5 0.92(4) . . ? C6 H6 0.88(5) . . ? C7 H7 0.94(6) . . ? C8 H8 0.95(5) . . ? C14 H14 0.96(5) . . ? C15 H15 0.94(5) . . ? C16 H16 0.79(5) . . ? C17 H17 0.91(5) . . ? C28 H28A 1.03(8) . . ? C28 H28B 0.88(9) . . ? C28 H28C 0.97(7) . . ? 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 S2 S1 C1 96.2(2) . . . ? S1 S2 C3 95.3(2) . . . ? S4 S3 C10 96.1(2) . . . ? S3 S4 C12 95.5(2) . . . ? C26 O21 C28 118.4(4) . . . ? S1 C1 C2 113.9(3) . . . ? S1 C1 C18 124.9(3) . . . ? C2 C1 C18 121.1(4) . . . ? C1 C2 C3 119.9(4) . . . ? C1 C2 C11 120.1(4) . . . ? C3 C2 C11 120.0(4) . . . ? S2 C3 C2 114.6(3) . . . ? S2 C3 C4 124.5(3) . . . ? C2 C3 C4 120.8(4) . . . ? C3 C4 C5 122.2(4) . . . ? C3 C4 C9 119.2(4) . . . ? C5 C4 C9 118.7(4) . . . ? C4 C5 C6 120.9(5) . . . ? C5 C6 C7 120.2(5) . . . ? C6 C7 C8 121.1(4) . . . ? C7 C8 C9 120.5(4) . . . ? C4 C9 C8 118.7(4) . . . ? C4 C9 C10 118.7(4) . . . ? C8 C9 C10 122.6(4) . . . ? S3 C10 C9 124.8(3) . . . ? S3 C10 C11 113.9(3) . . . ? C9 C10 C11 121.3(4) . . . ? C2 C11 C10 120.0(4) . . . ? C2 C11 C12 119.6(4) . . . ? C10 C11 C12 120.5(4) . . . ? S4 C12 C11 114.1(3) . . . ? S4 C12 C13 124.3(3) . . . ? C11 C12 C13 121.6(4) . . . ? C12 C13 C14 122.4(4) . . . ? C12 C13 C18 118.3(4) . . . ? C14 C13 C18 119.3(4) . . . ? C13 C14 C15 120.2(5) . . . ? C14 C15 C16 120.8(5) . . . ? C15 C16 C17 120.8(5) . . . ? C16 C17 C18 120.8(5) . . . ? C1 C18 C13 119.2(4) . . . ? C1 C18 C17 122.7(4) . . . ? C13 C18 C17 118.1(4) . . . ? N21 C21 C25 176.9(5) . . . ? N22 C22 C25 176.8(5) . . . ? N23 C23 C27 176.6(5) . . . ? N24 C24 C27 178.8(6) . . . ? C21 C25 C22 115.8(4) . . . ? C21 C25 C26 119.3(4) . . . ? C22 C25 C26 124.9(4) . . . ? O21 C26 C25 113.1(4) . . . ? O21 C26 C27 120.0(4) . . . ? C25 C26 C27 126.8(4) . . . ? C23 C27 C24 116.8(4) . . . ? C23 C27 C26 123.4(4) . . . ? C24 C27 C26 119.8(4) . . . ? C4 C5 H5 119.7(25) . . . ? C6 C5 H5 119.3(25) . . . ? C5 C6 H6 117.1(29) . . . ? C7 C6 H6 122.1(29) . . . ? C6 C7 H7 120.4(33) . . . ? C8 C7 H7 118.3(33) . . . ? C7 C8 H8 119.5(24) . . . ? C9 C8 H8 120.0(24) . . . ? C13 C14 H14 120.8(28) . . . ? C15 C14 H14 119.0(28) . . . ? C14 C15 H15 116.9(29) . . . ? C16 C15 H15 122.3(29) . . . ? C15 C16 H16 118.9(37) . . . ? C17 C16 H16 120.0(37) . . . ? C16 C17 H17 118.8(27) . . . ? C18 C17 H17 119.7(27) . . . ? O21 C28 H28A 114.2(43) . . . ? O21 C28 H28B 118.1(53) . . . ? O21 C28 H28C 108.4(37) . . . ? H28A C28 H28B 96.0(69) . . . ? H28A C28 H28C 94.5(57) . . . ? H28B C28 H28C 122.2(64) . . . ? 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 S1 N21 3.153(4) 1_555 3_546 ? S1 C21 3.257(4) 1_555 3_546 ? S2 N21 3.102(4) 1_555 3_546 ? S3 C1 3.336(4) 1_555 2_555 ? S3 C2 3.408(4) 1_555 2_555 ? S3 C22 3.392(5) 1_555 4_565 ? S3 C23 3.474(5) 1_555 4_565 ? S3 C25 3.450(4) 1_555 4_565 ? S4 C2 3.432(4) 1_555 2_555 ? S4 C3 3.306(4) 1_555 2_555 ? N24 C5 3.235(6) 1_555 2_555 ? C5 C15 3.351(6) 1_555 2_556 ? C6 H28A 2.78(8) 1_555 2_555 ? C10 C12 3.273(5) 1_555 2_555 ? C21 H5 2.86(4) 1_555 2_556 ? S4 N24 3.306(5) 1_555 1_555 ? O21 H14 2.66(5) 1_555 1_555 ? N23 H8 2.74(4) 1_555 4_565 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)(EtO-TCA)(THF)0.25 _database_code_CSD 165347 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _chemical_formula_moiety 'C18 H8 S4 1+,C8 H5 N4 O1 1-,0.25(C4 H8 O1)' _chemical_formula_sum 'C27 H15 O1.25 N4 S4 ' _chemical_formula_weight 543.71 _cell_length_a 7.573(1) _cell_length_b 14.909(1) _cell_length_c 23.061(2) _cell_angle_alpha 74.423(4) _cell_angle_beta 88.636(5) _cell_angle_gamma 83.511(5) _cell_volume 2491.3(1) _cell_measurement_reflns_used '?' _cell_measurement_theta_min '?' _cell_measurement_theta_max '?' _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_meas 1.460 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.948 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science DIP2000' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 9024 _reflns_number_total 9024 _reflns_number_observed 6515 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 26.10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _refine_ls_structure_factor_coef ? _refine_ls_R_factor_obs 0.039 _refine_ls_wR_factor_obs 0.042 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 6515 _refine_ls_number_parameters 770 _refine_ls_goodness_of_fit_obs 1.289 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.2735 _refine_ls_shift/esd_mean 0.0055 _refine_diff_density_min -0.27 _refine_diff_density_max 0.23 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.00659(11) 0.18667(6) 0.88627(3) 0.0404(4) 1.000 Uij S2 0.02744(11) 0.25147(6) 0.95455(4) 0.0398(4) 1.000 Uij S3 0.45097(11) -0.11556(6) 1.11278(3) 0.0379(4) 1.000 Uij S4 0.43074(11) -0.17985(6) 1.04415(4) 0.0380(4) 1.000 Uij S21 0.34009(13) 0.27935(6) 0.53936(4) 0.0495(5) 1.000 Uij S22 0.40336(14) 0.33318(6) 0.44979(4) 0.0514(5) 1.000 Uij S23 0.14062(12) 0.73903(6) 0.46550(4) 0.0458(4) 1.000 Uij S24 0.07333(13) 0.68674(7) 0.55486(4) 0.0491(5) 1.000 Uij O41 0.3873(3) 0.6527(2) 0.7932(1) 0.048(1) 1.000 Uij O51 0.5291(3) 0.9548(2) 0.6517(1) 0.059(1) 1.000 Uij O61 0.489(3) 0.599(1) 0.980(1) 0.24(1) 0.500 Uij N41 0.8003(5) 0.6513(3) 0.7309(2) 0.068(2) 1.000 Uij N42 0.7970(4) 0.3774(2) 0.8564(2) 0.063(2) 1.000 Uij N43 0.3710(5) 0.3213(2) 0.8571(2) 0.059(2) 1.000 Uij N44 0.0242(5) 0.5636(3) 0.8832(2) 0.085(3) 1.000 Uij N51 0.4439(6) 1.1085(3) 0.7424(2) 0.083(2) 1.000 Uij N52 -0.0527(5) 1.1029(3) 0.6633(2) 0.082(3) 1.000 Uij N53 0.0578(5) 1.1012(3) 0.5116(2) 0.069(2) 1.000 Uij N54 0.4384(5) 0.8575(3) 0.5283(2) 0.072(2) 1.000 Uij C1 0.1248(4) 0.0808(2) 0.9236(1) 0.035(1) 1.000 Uij C2 0.1836(4) 0.0781(2) 0.9810(1) 0.032(1) 1.000 Uij C3 0.1507(4) 0.1569(2) 1.0028(1) 0.033(1) 1.000 Uij C4 0.2113(4) 0.1558(2) 1.0612(1) 0.036(1) 1.000 Uij C5 0.1797(5) 0.2344(3) 1.0845(2) 0.046(2) 1.000 Uij C6 0.2375(5) 0.2310(3) 1.1413(2) 0.056(2) 1.000 Uij C7 0.3282(5) 0.1487(3) 1.1769(2) 0.055(2) 1.000 Uij C8 0.3617(5) 0.0709(3) 1.1559(2) 0.045(2) 1.000 Uij C9 0.3060(4) 0.0712(2) 1.0978(1) 0.036(1) 1.000 Uij C10 0.3393(4) -0.0081(2) 1.0743(1) 0.034(1) 1.000 Uij C11 0.2796(4) -0.0054(2) 1.0171(1) 0.032(1) 1.000 Uij C12 0.3136(4) -0.0839(2) 0.9948(1) 0.034(1) 1.000 Uij C13 0.2516(4) -0.0830(2) 0.9369(1) 0.036(1) 1.000 Uij C14 0.2815(5) -0.1626(3) 0.9139(2) 0.048(2) 1.000 Uij C15 0.2187(6) -0.1592(3) 0.8582(2) 0.059(2) 1.000 Uij C16 0.1247(5) -0.0773(3) 0.8225(2) 0.057(2) 1.000 Uij C17 0.0940(5) 0.0010(3) 0.8427(2) 0.047(2) 1.000 Uij C18 0.1556(4) 0.0014(2) 0.9002(1) 0.038(2) 1.000 Uij C21 0.2558(4) 0.3866(2) 0.5509(1) 0.040(2) 1.000 Uij C22 0.2656(4) 0.4633(2) 0.5010(1) 0.037(1) 1.000 Uij C23 0.3369(4) 0.4489(2) 0.4474(1) 0.039(2) 1.000 Uij C24 0.3549(4) 0.5258(2) 0.3962(1) 0.041(2) 1.000 Uij C25 0.4352(5) 0.5134(3) 0.3422(2) 0.051(2) 1.000 Uij C26 0.4555(6) 0.5898(3) 0.2946(2) 0.060(2) 1.000 Uij C27 0.3973(6) 0.6801(3) 0.2978(2) 0.057(2) 1.000 Uij C28 0.3178(5) 0.6956(3) 0.3491(2) 0.049(2) 1.000 Uij C29 0.2956(4) 0.6188(2) 0.3997(1) 0.040(2) 1.000 Uij C30 0.2189(4) 0.6317(2) 0.4546(1) 0.038(2) 1.000 Uij C31 0.2063(4) 0.5552(2) 0.5045(1) 0.036(1) 1.000 Uij C32 0.1359(4) 0.5700(2) 0.5582(1) 0.039(2) 1.000 Uij C33 0.1227(4) 0.4929(3) 0.6097(1) 0.042(2) 1.000 Uij C34 0.0533(5) 0.5058(3) 0.6650(2) 0.054(2) 1.000 Uij C35 0.0461(6) 0.4295(4) 0.7138(2) 0.067(3) 1.000 Uij C36 0.1049(6) 0.3393(4) 0.7106(2) 0.066(3) 1.000 Uij C37 0.1714(5) 0.3236(3) 0.6579(2) 0.055(2) 1.000 Uij C38 0.1832(4) 0.4000(2) 0.6059(1) 0.042(2) 1.000 Uij C41 0.7199(5) 0.6010(3) 0.7648(2) 0.047(2) 1.000 Uij C42 0.7160(5) 0.4476(3) 0.8349(2) 0.046(2) 1.000 Uij C43 0.3493(5) 0.4002(3) 0.8519(1) 0.046(2) 1.000 Uij C44 0.1544(5) 0.5346(3) 0.8647(2) 0.056(2) 1.000 Uij C45 0.6208(4) 0.5357(2) 0.8059(1) 0.041(2) 1.000 Uij C46 0.4409(4) 0.5596(2) 0.8146(1) 0.039(2) 1.000 Uij C47 0.3179(4) 0.4986(2) 0.8429(1) 0.044(2) 1.000 Uij C48 0.2367(6) 0.6808(3) 0.7519(2) 0.066(2) 1.000 Uij C49 0.2757(9) 0.7551(6) 0.7009(3) 0.116(5) 1.000 Uij C51 0.3771(6) 1.0819(3) 0.7072(2) 0.058(2) 1.000 Uij C52 0.0971(6) 1.0805(3) 0.6617(2) 0.058(2) 1.000 Uij C53 0.1654(5) 1.0503(3) 0.5413(2) 0.053(2) 1.000 Uij C54 0.3788(5) 0.9145(3) 0.5501(2) 0.053(2) 1.000 Uij C55 0.2822(5) 1.0537(3) 0.6638(2) 0.051(2) 1.000 Uij C56 0.3702(5) 0.9995(2) 0.6286(2) 0.047(2) 1.000 Uij C57 0.3048(5) 0.9871(3) 0.5754(2) 0.048(2) 1.000 Uij C58 0.6866(6) 0.9621(4) 0.6134(2) 0.071(3) 1.000 Uij C59 0.8268(9) 0.8916(5) 0.6432(3) 0.099(4) 1.000 Uij C61 0.6255(11) 0.5402(7) 0.9810(3) 0.123(6) 1.000 Uij C62 0.6248(16) 0.4405(7) 0.9987(4) 0.160(7) 1.000 Uij H5 0.116(4) 0.291(2) 1.061(1) 0.05(1) 1.000 Uiso H6 0.216(5) 0.289(3) 1.159(2) 0.07(1) 1.000 Uiso H7 0.370(5) 0.148(3) 1.217(2) 0.07(1) 1.000 Uiso H8 0.417(4) 0.013(2) 1.178(1) 0.037(9) 1.000 Uiso H14 0.347(5) -0.219(3) 0.939(2) 0.05(1) 1.000 Uiso H15 0.239(5) -0.211(3) 0.843(2) 0.06(1) 1.000 Uiso H16 0.074(5) -0.077(3) 0.782(2) 0.07(1) 1.000 Uiso H17 0.036(5) 0.061(3) 0.819(2) 0.05(1) 1.000 Uiso H25 0.474(5) 0.448(3) 0.341(2) 0.07(1) 1.000 Uiso H26 0.521(5) 0.578(3) 0.261(2) 0.07(1) 1.000 Uiso H27 0.409(5) 0.734(3) 0.264(2) 0.06(1) 1.000 Uiso H28 0.281(5) 0.761(3) 0.352(1) 0.06(1) 1.000 Uiso H34 0.010(5) 0.572(3) 0.668(2) 0.06(1) 1.000 Uiso H35 -0.006(5) 0.443(3) 0.750(2) 0.07(1) 1.000 Uiso H36 0.100(6) 0.284(3) 0.745(2) 0.10(2) 1.000 Uiso H37 0.207(5) 0.262(3) 0.655(1) 0.05(1) 1.000 Uiso H48A 0.208(5) 0.627(3) 0.739(1) 0.050 1.000 Uiso H48B 0.135(5) 0.703(3) 0.775(2) 0.050 1.000 Uiso H49A 0.174(5) 0.780(3) 0.676(2) 0.050 1.000 Uiso H49B 0.384(5) 0.749(3) 0.684(2) 0.050 1.000 Uiso H49C 0.334(6) 0.798(3) 0.711(2) 0.050 1.000 Uiso H58A 0.657(4) 0.958(2) 0.570(2) 0.050 1.000 Uiso H58B 0.736(5) 1.030(3) 0.611(1) 0.050 1.000 Uiso H59A 0.776(5) 0.831(3) 0.639(2) 0.050 1.000 Uiso H59B 0.843(5) 0.886(3) 0.681(2) 0.050 1.000 Uiso H59C 0.930(5) 0.889(2) 0.617(2) 0.050 1.000 Uiso 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 S1 0.0388(5) 0.0383(5) 0.0377(4) 0.0012(4) -0.0030(3) -0.0020(3) S2 0.0391(5) 0.0298(4) 0.0445(5) 0.0041(3) -0.0004(3) -0.0039(3) S3 0.0395(5) 0.0317(4) 0.0371(4) 0.0011(3) -0.0013(3) -0.0034(3) S4 0.0378(5) 0.0273(4) 0.0445(4) 0.0007(3) 0.0015(3) -0.0072(3) S21 0.0581(6) 0.0298(5) 0.0560(5) 0.0011(4) -0.0077(4) -0.0106(4) S22 0.0611(6) 0.0345(5) 0.0559(5) 0.0032(4) -0.0014(4) -0.0205(4) S23 0.0513(6) 0.0305(5) 0.0519(5) 0.0016(4) 0.0005(4) -0.0135(3) S24 0.0521(6) 0.0407(5) 0.0517(5) 0.0030(4) 0.0035(4) -0.0211(4) O41 0.045(1) 0.034(1) 0.060(2) 0.005(1) -0.013(1) -0.011(1) O51 0.050(2) 0.061(2) 0.056(2) 0.010(1) -0.006(1) -0.005(1) O61 0.28(2) 0.06(1) 0.34(2) -0.03(1) 0.14(2) -0.02(1) N41 0.063(2) 0.054(2) 0.078(2) -0.007(2) 0.011(2) -0.005(2) N42 0.056(2) 0.050(2) 0.070(2) 0.011(2) -0.002(2) 0.000(2) N43 0.060(2) 0.038(2) 0.071(2) -0.003(2) 0.005(2) -0.002(1) N44 0.064(3) 0.080(3) 0.100(3) 0.011(2) 0.022(2) -0.025(2) N51 0.119(4) 0.057(2) 0.064(2) -0.004(2) -0.032(2) -0.009(2) N52 0.064(3) 0.076(3) 0.099(3) 0.008(2) 0.003(2) -0.034(2) N53 0.073(2) 0.056(2) 0.073(2) 0.020(2) -0.020(2) -0.032(2) N54 0.079(3) 0.046(2) 0.084(3) 0.013(2) -0.007(2) -0.025(2) C1 0.029(2) 0.035(2) 0.035(2) -0.004(1) 0.002(1) -0.002(1) C2 0.028(2) 0.029(2) 0.033(2) -0.004(1) 0.004(1) -0.005(1) C3 0.030(2) 0.028(2) 0.038(2) -0.002(1) 0.003(1) -0.005(1) C4 0.034(2) 0.031(2) 0.039(2) -0.003(1) 0.005(1) -0.010(1) C5 0.044(2) 0.037(2) 0.054(2) 0.002(2) 0.002(1) -0.017(2) C6 0.055(2) 0.052(3) 0.060(2) -0.002(2) 0.004(2) -0.031(2) C7 0.054(2) 0.061(3) 0.047(2) -0.003(2) -0.001(2) -0.027(2) C8 0.044(2) 0.048(2) 0.039(2) 0.001(2) -0.002(1) -0.011(1) C9 0.030(2) 0.036(2) 0.037(2) -0.004(1) 0.003(1) -0.010(1) C10 0.030(2) 0.032(2) 0.034(2) -0.002(1) 0.002(1) -0.005(1) C11 0.029(2) 0.029(2) 0.036(2) -0.003(1) 0.002(1) -0.007(1) C12 0.030(2) 0.028(2) 0.040(2) -0.003(1) 0.004(1) -0.007(1) C13 0.034(2) 0.034(2) 0.037(2) -0.006(1) 0.005(1) -0.011(1) C14 0.047(2) 0.040(2) 0.053(2) -0.006(2) 0.007(2) -0.018(2) C15 0.060(3) 0.057(3) 0.061(2) -0.012(2) 0.008(2) -0.035(2) C16 0.058(3) 0.065(3) 0.044(2) -0.013(2) 0.004(2) -0.024(2) C17 0.045(2) 0.053(2) 0.039(2) -0.009(2) 0.001(1) -0.012(2) C18 0.031(2) 0.041(2) 0.038(2) -0.007(1) 0.005(1) -0.010(1) C21 0.039(2) 0.030(2) 0.048(2) -0.002(1) -0.006(1) -0.011(1) C22 0.034(2) 0.032(2) 0.041(2) -0.003(1) -0.003(1) -0.012(1) C23 0.041(2) 0.029(2) 0.046(2) -0.001(1) -0.005(1) -0.016(1) C24 0.038(2) 0.040(2) 0.042(2) -0.004(1) -0.002(1) -0.017(1) C25 0.055(2) 0.049(2) 0.049(2) -0.006(2) 0.003(2) -0.025(2) C26 0.065(3) 0.071(3) 0.042(2) -0.021(2) 0.008(2) -0.024(2) C27 0.067(3) 0.055(3) 0.044(2) -0.018(2) 0.002(2) -0.008(2) C28 0.054(2) 0.038(2) 0.049(2) -0.005(2) 0.000(2) -0.009(1) C29 0.039(2) 0.036(2) 0.040(2) -0.004(1) -0.002(1) -0.012(1) C30 0.038(2) 0.027(2) 0.044(2) 0.000(1) -0.004(1) -0.013(1) C31 0.032(2) 0.033(2) 0.041(2) -0.002(1) -0.003(1) -0.013(1) C32 0.036(2) 0.034(2) 0.045(2) 0.000(1) -0.002(1) -0.017(1) C33 0.034(2) 0.049(2) 0.038(2) -0.007(2) -0.001(1) -0.013(1) C34 0.046(2) 0.062(3) 0.048(2) -0.004(2) 0.005(2) -0.018(2) C35 0.061(3) 0.088(4) 0.045(2) -0.009(2) 0.012(2) -0.013(2) C36 0.068(3) 0.072(3) 0.048(2) -0.013(2) 0.006(2) 0.003(2) C37 0.058(3) 0.044(2) 0.055(2) -0.005(2) -0.001(2) -0.003(2) C38 0.038(2) 0.040(2) 0.043(2) -0.006(1) -0.004(1) -0.007(1) C41 0.047(2) 0.039(2) 0.050(2) 0.000(2) -0.003(2) -0.012(1) C42 0.042(2) 0.046(2) 0.043(2) 0.002(2) 0.001(1) -0.009(1) C43 0.042(2) 0.047(2) 0.041(2) -0.002(2) 0.006(1) -0.003(1) C44 0.051(2) 0.050(2) 0.061(2) 0.002(2) 0.005(2) -0.013(2) C45 0.045(2) 0.033(2) 0.040(2) 0.003(1) -0.003(1) -0.010(1) C46 0.042(2) 0.033(2) 0.039(2) 0.005(1) -0.007(1) -0.011(1) C47 0.038(2) 0.041(2) 0.048(2) 0.001(2) 0.002(1) -0.010(1) C48 0.066(3) 0.047(3) 0.076(3) 0.011(2) -0.031(2) -0.010(2) C49 0.085(5) 0.136(6) 0.096(5) -0.018(4) -0.029(3) 0.041(4) C51 0.075(3) 0.041(2) 0.050(2) -0.001(2) -0.012(2) -0.002(2) C52 0.070(3) 0.044(2) 0.055(2) 0.000(2) -0.001(2) -0.015(2) C53 0.058(2) 0.040(2) 0.057(2) 0.002(2) -0.003(2) -0.023(2) C54 0.055(2) 0.036(2) 0.062(2) 0.003(2) -0.005(2) -0.011(2) C55 0.056(2) 0.039(2) 0.051(2) -0.002(2) -0.006(2) -0.010(1) C56 0.050(2) 0.033(2) 0.053(2) -0.001(2) -0.003(2) -0.004(1) C57 0.051(2) 0.036(2) 0.052(2) 0.003(2) -0.002(2) -0.012(1) C58 0.046(3) 0.085(4) 0.071(3) -0.005(2) -0.003(2) -0.007(2) C59 0.080(4) 0.082(4) 0.112(5) 0.024(3) 0.025(4) 0.009(4) C61 0.136(7) 0.119(7) 0.103(5) -0.035(5) 0.018(4) -0.020(4) C62 0.23(1) 0.12(1) 0.12(1) -0.03(1) 0.01(1) -0.03(1) 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 S1 S2 2.074(2) . . ? S1 C1 1.737(4) . . ? S2 C3 1.734(4) . . ? S3 S4 2.075(2) . . ? S3 C10 1.742(4) . . ? S4 C12 1.736(4) . . ? S21 S22 2.071(2) . . ? S21 C21 1.739(4) . . ? S22 C23 1.728(4) . . ? S23 S24 2.071(2) . . ? S23 C30 1.723(4) . . ? S24 C32 1.733(4) . . ? O41 C46 1.360(4) . . ? O41 C48 1.453(6) . . ? O51 C56 1.354(5) . . ? O51 C58 1.463(6) . . ? O61 C61 1.28(3) . . ? O61 C62 1.13(3) . 2_657 ? N41 C41 1.144(6) . . ? N42 C42 1.144(5) . . ? N43 C43 1.144(6) . . ? N44 C44 1.151(6) . . ? N51 C51 1.143(6) . . ? N52 C52 1.148(7) . . ? N53 C53 1.148(6) . . ? N54 C54 1.145(6) . . ? C1 C2 1.396(4) . . ? C1 C18 1.422(5) . . ? C2 C3 1.394(5) . . ? C2 C11 1.428(5) . . ? C3 C4 1.428(5) . . ? C4 C5 1.411(5) . . ? C4 C9 1.439(5) . . ? C5 C6 1.376(6) . . ? C6 C7 1.396(6) . . ? C7 C8 1.368(6) . . ? C8 C9 1.413(5) . . ? C9 C10 1.423(5) . . ? C10 C11 1.395(4) . . ? C11 C12 1.395(5) . . ? C12 C13 1.423(5) . . ? C13 C14 1.419(5) . . ? C13 C18 1.442(5) . . ? C14 C15 1.366(6) . . ? C15 C16 1.402(6) . . ? C16 C17 1.364(6) . . ? C17 C18 1.418(5) . . ? C21 C22 1.395(5) . . ? C21 C38 1.425(5) . . ? C22 C23 1.396(5) . . ? C22 C31 1.416(5) . . ? C23 C24 1.423(5) . . ? C24 C25 1.420(5) . . ? C24 C29 1.430(5) . . ? C25 C26 1.373(6) . . ? C26 C27 1.389(7) . . ? C27 C28 1.377(6) . . ? C28 C29 1.420(5) . . ? C29 C30 1.431(5) . . ? C30 C31 1.397(5) . . ? C31 C32 1.398(5) . . ? C32 C33 1.424(5) . . ? C33 C34 1.421(5) . . ? C33 C38 1.434(5) . . ? C34 C35 1.373(7) . . ? C35 C36 1.390(8) . . ? C36 C37 1.371(6) . . ? C37 C38 1.424(6) . . ? C41 C45 1.430(5) . . ? C42 C45 1.425(5) . . ? C43 C47 1.418(6) . . ? C44 C47 1.428(6) . . ? C45 C46 1.393(5) . . ? C46 C47 1.401(5) . . ? C48 C49 1.434(9) . . ? C51 C55 1.423(6) . . ? C52 C55 1.412(7) . . ? C53 C57 1.428(6) . . ? C54 C57 1.418(6) . . ? C55 C56 1.401(6) . . ? C56 C57 1.398(5) . . ? C58 C59 1.448(9) . . ? C61 C62 1.432(15) . . ? C5 H5 0.96(4) . . ? C6 H6 1.04(4) . . ? C7 H7 0.98(4) . . ? C8 H8 0.93(4) . . ? C14 H14 0.98(4) . . ? C15 H15 0.93(4) . . ? C16 H16 1.02(4) . . ? C17 H17 0.97(4) . . ? C25 H25 0.99(5) . . ? C26 H26 0.97(4) . . ? C27 H27 0.97(4) . . ? C28 H28 1.00(4) . . ? C34 H34 1.02(4) . . ? C35 H35 0.96(5) . . ? C36 H36 0.98(5) . . ? C37 H37 0.95(4) . . ? C48 H48A 0.98(4) . . ? C48 H48B 1.01(4) . . ? C49 H49A 0.96(4) . . ? C49 H49B 0.91(4) . . ? C49 H49C 0.90(5) . . ? C58 H58A 1.06(4) . . ? C58 H58B 1.10(4) . . ? C59 H59A 1.05(4) . . ? C59 H59B 0.86(4) . . ? C59 H59C 0.98(4) . . ? 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 S2 S1 C1 95.8(2) . . . ? S1 S2 C3 95.5(2) . . . ? S4 S3 C10 95.7(2) . . . ? S3 S4 C12 95.7(2) . . . ? S22 S21 C21 95.4(2) . . . ? S21 S22 C23 95.8(2) . . . ? S24 S23 C30 95.4(2) . . . ? S23 S24 C32 96.0(2) . . . ? C46 O41 C48 118.0(3) . . . ? C56 O51 C58 119.6(3) . . . ? C61 O61 C62 108.3(13) . . 2_657 ? S1 C1 C2 114.0(3) . . . ? S1 C1 C18 124.5(3) . . . ? C2 C1 C18 121.4(3) . . . ? C1 C2 C3 120.2(3) . . . ? C1 C2 C11 119.8(3) . . . ? C3 C2 C11 120.0(3) . . . ? S2 C3 C2 114.4(3) . . . ? S2 C3 C4 124.5(3) . . . ? C2 C3 C4 121.0(3) . . . ? C3 C4 C5 122.3(3) . . . ? C3 C4 C9 118.9(3) . . . ? C5 C4 C9 118.8(3) . . . ? C4 C5 C6 121.0(4) . . . ? C5 C6 C7 120.0(4) . . . ? C6 C7 C8 120.7(4) . . . ? C7 C8 C9 121.3(4) . . . ? C4 C9 C8 118.0(3) . . . ? C4 C9 C10 119.0(3) . . . ? C8 C9 C10 122.9(3) . . . ? S3 C10 C9 124.8(3) . . . ? S3 C10 C11 114.0(3) . . . ? C9 C10 C11 121.2(3) . . . ? C2 C11 C10 119.9(3) . . . ? C2 C11 C12 119.8(3) . . . ? C10 C11 C12 120.3(3) . . . ? S4 C12 C11 114.3(3) . . . ? S4 C12 C13 124.6(3) . . . ? C11 C12 C13 121.1(3) . . . ? C12 C13 C14 122.1(3) . . . ? C12 C13 C18 119.2(3) . . . ? C14 C13 C18 118.8(3) . . . ? C13 C14 C15 120.3(4) . . . ? C14 C15 C16 121.1(4) . . . ? C15 C16 C17 120.6(4) . . . ? C16 C17 C18 120.8(4) . . . ? C1 C18 C13 118.6(3) . . . ? C1 C18 C17 122.9(3) . . . ? C13 C18 C17 118.5(3) . . . ? S21 C21 C22 114.6(3) . . . ? S21 C21 C38 125.2(3) . . . ? C22 C21 C38 120.2(3) . . . ? C21 C22 C23 119.4(3) . . . ? C21 C22 C31 120.6(3) . . . ? C23 C22 C31 120.0(3) . . . ? S22 C23 C22 114.8(3) . . . ? S22 C23 C24 124.3(3) . . . ? C22 C23 C24 120.9(3) . . . ? C23 C24 C25 122.0(4) . . . ? C23 C24 C29 119.3(3) . . . ? C25 C24 C29 118.7(4) . . . ? C24 C25 C26 120.1(4) . . . ? C25 C26 C27 121.2(4) . . . ? C26 C27 C28 120.8(4) . . . ? C27 C28 C29 120.0(4) . . . ? C24 C29 C28 119.2(3) . . . ? C24 C29 C30 118.9(3) . . . ? C28 C29 C30 121.9(4) . . . ? S23 C30 C29 124.3(3) . . . ? S23 C30 C31 115.0(3) . . . ? C29 C30 C31 120.6(3) . . . ? C22 C31 C30 120.3(3) . . . ? C22 C31 C32 120.2(3) . . . ? C30 C31 C32 119.6(3) . . . ? S24 C32 C31 114.0(3) . . . ? S24 C32 C33 125.6(3) . . . ? C31 C32 C33 120.4(3) . . . ? C32 C33 C34 121.7(4) . . . ? C32 C33 C38 119.2(3) . . . ? C34 C33 C38 119.1(4) . . . ? C33 C34 C35 119.6(5) . . . ? C34 C35 C36 121.6(4) . . . ? C35 C36 C37 120.7(5) . . . ? C36 C37 C38 120.3(4) . . . ? C21 C38 C33 119.4(3) . . . ? C21 C38 C37 121.9(4) . . . ? C33 C38 C37 118.7(3) . . . ? N41 C41 C45 177.9(4) . . . ? N42 C42 C45 177.3(4) . . . ? N43 C43 C47 177.2(4) . . . ? N44 C44 C47 178.9(5) . . . ? C41 C45 C42 116.2(3) . . . ? C41 C45 C46 119.8(3) . . . ? C42 C45 C46 124.0(3) . . . ? O41 C46 C45 113.6(3) . . . ? O41 C46 C47 119.7(3) . . . ? C45 C46 C47 126.7(3) . . . ? C43 C47 C44 117.2(4) . . . ? C43 C47 C46 122.6(4) . . . ? C44 C47 C46 120.2(4) . . . ? O41 C48 C49 110.4(5) . . . ? N51 C51 C55 175.5(5) . . . ? N52 C52 C55 176.2(5) . . . ? N53 C53 C57 176.8(4) . . . ? N54 C54 C57 178.3(5) . . . ? C51 C55 C52 115.1(4) . . . ? C51 C55 C56 120.6(4) . . . ? C52 C55 C56 124.2(4) . . . ? O51 C56 C55 113.7(4) . . . ? O51 C56 C57 120.5(4) . . . ? C55 C56 C57 125.7(4) . . . ? C53 C57 C54 115.7(4) . . . ? C53 C57 C56 121.8(4) . . . ? C54 C57 C56 122.4(4) . . . ? O51 C58 C59 108.8(5) . . . ? O61 C61 C62 124.8(12) . . . ? O61 C62 C61 126.4(13) 2_657 . . ? C4 C5 H5 120.3(21) . . . ? C6 C5 H5 118.6(21) . . . ? C5 C6 H6 121.8(22) . . . ? C7 C6 H6 118.1(22) . . . ? C6 C7 H7 119.1(24) . . . ? C8 C7 H7 120.2(24) . . . ? C7 C8 H8 124.7(20) . . . ? C9 C8 H8 113.9(20) . . . ? C13 C14 H14 117.5(21) . . . ? C15 C14 H14 122.2(21) . . . ? C14 C15 H15 120.2(23) . . . ? C16 C15 H15 118.7(23) . . . ? C15 C16 H16 119.8(22) . . . ? C17 C16 H16 119.5(22) . . . ? C16 C17 H17 124.0(21) . . . ? C18 C17 H17 115.1(21) . . . ? C24 C25 H25 116.4(22) . . . ? C26 C25 H25 123.5(22) . . . ? C25 C26 H26 116.7(24) . . . ? C27 C26 H26 121.9(24) . . . ? C26 C27 H27 122.0(23) . . . ? C28 C27 H27 117.2(23) . . . ? C27 C28 H28 120.2(20) . . . ? C29 C28 H28 119.8(20) . . . ? C33 C34 H34 119.2(20) . . . ? C35 C34 H34 121.2(20) . . . ? C34 C35 H35 115.6(25) . . . ? C36 C35 H35 122.7(25) . . . ? C35 C36 H36 122.7(29) . . . ? C37 C36 H36 116.6(29) . . . ? C36 C37 H37 121.2(21) . . . ? C38 C37 H37 118.5(21) . . . ? O41 C48 H48A 109.4(21) . . . ? O41 C48 H48B 105.9(20) . . . ? C49 C48 H48A 110.2(20) . . . ? C49 C48 H48B 110.4(21) . . . ? H48A C48 H48B 110.4(30) . . . ? C48 C49 H49A 111.8(23) . . . ? C48 C49 H49B 117.2(26) . . . ? C48 C49 H49C 112.4(26) . . . ? H49A C49 H49B 118.9(33) . . . ? H49A C49 H49C 115.5(35) . . . ? H49B C49 H49C 76.6(37) . . . ? O51 C58 H58A 111.3(19) . . . ? O51 C58 H58B 108.3(19) . . . ? C59 C58 H58A 113.3(19) . . . ? C59 C58 H58B 105.2(19) . . . ? H58A C58 H58B 109.6(26) . . . ? C58 C59 H59A 100.1(21) . . . ? C58 C59 H59B 116.4(27) . . . ? C58 C59 H59C 111.7(22) . . . ? H59A C59 H59B 107.5(33) . . . ? H59A C59 H59C 97.4(30) . . . ? H59B C59 H59C 119.6(34) . . . ? 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 S1 N42 3.010(3) 1_555 1_455 ? S2 N42 2.976(3) 1_555 1_455 ? S3 N43 3.110(3) 1_555 2_657 ? S3 C1 3.363(3) 1_555 2_657 ? S3 C2 3.473(3) 1_555 2_657 ? S4 N43 2.959(3) 1_555 2_657 ? S4 C2 3.409(3) 1_555 2_657 ? S4 C3 3.350(3) 1_555 2_657 ? S21 N54 3.198(4) 1_555 2_666 ? S22 N54 2.874(4) 1_555 2_666 ? S23 N52 3.286(4) 1_555 2_576 ? S23 N53 2.836(4) 1_555 2_576 ? S24 N53 3.177(4) 1_555 2_576 ? N41 H34 2.54(4) 1_555 1_655 ? N44 H6 2.67(4) 1_555 2_567 ? N51 H8 2.37(3) 1_555 2_667 ? N51 H27 2.67(4) 1_555 2_676 ? N52 H28 2.47(4) 1_555 2_576 ? N52 H58B 2.54(3) 1_555 1_455 ? C8 C14 3.348(5) 1_555 2_657 ? C10 C12 3.283(4) 1_555 2_657 ? C41 H6 2.80(4) 1_555 2_667 ? C42 H35 2.86(4) 1_555 1_655 ? C43 H26 2.70(4) 1_555 2_666 ? C45 H26 2.87(4) 1_555 2_666 ? C51 H37 2.81(4) 1_555 1_565 ? C52 H37 2.88(4) 1_555 1_565 ? C53 H58A 2.89(4) 1_555 2_676 ? C54 H58A 2.90(3) 1_555 2_676 ? O41 H15 2.71(4) 1_555 1_545 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)(BuO-TCA) _database_code_CSD 165348 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _chemical_formula_moiety 'C18 H8 S4 1+,C11 H9 N4 O1 1-' _chemical_formula_sum 'C29 H17 N4 O1 S4 ' _chemical_formula_weight 565.74 _cell_length_a 20.971(7) _cell_length_b 21.949(8) _cell_length_c 14.078(5) _cell_angle_alpha 90.000000(0) _cell_angle_beta 128.70(2) _cell_angle_gamma 90.000000(0) _cell_volume 5057(3) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '??' _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas 1.484 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.914 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science DIP2000' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 4429 _reflns_number_total 4049 _reflns_number_observed 2956 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 24.39 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.048 _refine_ls_wR_factor_obs 0.047 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 2956 _refine_ls_number_parameters 375 _refine_ls_goodness_of_fit_obs 2.742 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0663 _refine_ls_shift/esd_mean 0.0040 _refine_diff_density_min -0.57 _refine_diff_density_max 0.46 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.02303 _diffrn_orient_matrix_UB_12 -0.04148 _diffrn_orient_matrix_UB_13 0.01223 _diffrn_orient_matrix_UB_21 0.01005 _diffrn_orient_matrix_UB_22 -0.00329 _diffrn_orient_matrix_UB_23 0.07903 _diffrn_orient_matrix_UB_31 -0.05502 _diffrn_orient_matrix_UB_32 -0.01796 _diffrn_orient_matrix_UB_33 -0.04275 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+0.5,-Y+0.5,-Z +X+0.5,+Y+0.5,+Z -X,+Y,-Z+0.5 +X,-Y,+Z+0.5 +X+0.5,-Y+0.5,+Z+0.5 -X+0.5,+Y+0.5,-Z+0.5 _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_cell_setting 'Monoclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.22360(6) 0.11020(5) 0.06670(10) 0.0573(6) 1.000 Uij S2 0.22950(6) 0.01650(5) 0.07760(10) 0.0553(5) 1.000 Uij S3 0.60860(6) 0.03040(5) 0.48810(10) 0.0547(6) 1.000 Uij S4 0.60220(6) 0.12470(5) 0.48030(10) 0.0593(6) 1.000 Uij O21 -0.00520(17) 0.08520(14) 0.07630(27) 0.065(2) 1.000 Uij N21 -0.0540(2) -0.0576(2) 0.0931(4) 0.077(2) 1.000 Uij N22 0.2086(2) -0.0601(2) 0.2954(4) 0.081(2) 1.000 Uij N23 0.2813(3) 0.0840(2) 0.4134(4) 0.095(3) 1.000 Uij N24 0.1300(3) 0.2133(2) 0.1378(4) 0.090(3) 1.000 Uij C1 0.3269(2) 0.1220(2) 0.1791(4) 0.051(2) 1.000 Uij C2 0.3726(2) 0.0693(2) 0.2304(3) 0.046(2) 1.000 Uij C3 0.3343(2) 0.0128(2) 0.1888(3) 0.047(2) 1.000 Uij C4 0.3794(2) -0.0422(2) 0.2395(3) 0.048(2) 1.000 Uij C5 0.3421(3) -0.0997(2) 0.2023(4) 0.060(2) 1.000 Uij C6 0.3862(3) -0.1519(2) 0.2544(5) 0.073(3) 1.000 Uij C7 0.4708(3) -0.1488(2) 0.3457(5) 0.071(3) 1.000 Uij C8 0.5102(3) -0.0944(2) 0.3845(4) 0.060(2) 1.000 Uij C9 0.4665(2) -0.0391(2) 0.3344(3) 0.048(2) 1.000 Uij C10 0.5043(2) 0.0191(2) 0.3736(3) 0.046(2) 1.000 Uij C11 0.4592(2) 0.0724(2) 0.3242(3) 0.047(2) 1.000 Uij C12 0.4971(2) 0.1290(2) 0.3645(4) 0.052(2) 1.000 Uij C13 0.4521(3) 0.1842(2) 0.3153(4) 0.057(2) 1.000 Uij C14 0.4884(3) 0.2420(2) 0.3545(5) 0.073(3) 1.000 Uij C15 0.4421(4) 0.2936(2) 0.3031(5) 0.093(4) 1.000 Uij C16 0.3574(4) 0.2903(3) 0.2107(5) 0.085(3) 1.000 Uij C17 0.3193(3) 0.2352(2) 0.1702(5) 0.070(3) 1.000 Uij C18 0.3644(3) 0.1807(2) 0.2195(4) 0.055(2) 1.000 Uij C21 0.0043(3) -0.0303(2) 0.1331(4) 0.061(3) 1.000 Uij C22 0.1509(3) -0.0309(2) 0.2470(4) 0.060(2) 1.000 Uij C23 0.2171(3) 0.0922(2) 0.3256(4) 0.063(2) 1.000 Uij C24 0.1312(3) 0.1658(2) 0.1725(4) 0.063(2) 1.000 Uij C25 0.0774(2) 0.0033(2) 0.1837(4) 0.055(2) 1.000 Uij C26 0.0726(2) 0.0658(2) 0.1633(4) 0.054(2) 1.000 Uij C27 0.1379(2) 0.1067(2) 0.2199(4) 0.053(2) 1.000 Uij C28 -0.0328(3) 0.1433(3) 0.0840(6) 0.114(4) 1.000 Uij C29 -0.1161(3) 0.1449(3) 0.0240(6) 0.107(4) 1.000 Uij C30 -0.1473(4) 0.2041(3) 0.0374(6) 0.113(4) 1.000 Uij C31 -0.1697(4) 0.2498(3) -0.0523(7) 0.117(4) 1.000 Uij H5 0.283(2) -0.101(2) 0.138(4) 0.05(1) 1.000 Uiso H6 0.357(2) -0.191(2) 0.225(4) 0.05(1) 1.000 Uiso H7 0.502(2) -0.186(2) 0.384(4) 0.05(1) 1.000 Uiso H8 0.567(3) -0.093(2) 0.448(4) 0.05(1) 1.000 Uiso H14 0.550(3) 0.244(2) 0.424(4) 0.06(1) 1.000 Uiso H15 0.470(3) 0.330(2) 0.328(4) 0.07(1) 1.000 Uiso H16 0.324(3) 0.325(2) 0.171(4) 0.08(2) 1.000 Uiso H17 0.257(3) 0.232(2) 0.104(4) 0.06(1) 1.000 Uiso H28A -0.02250 0.17260 0.04440 0.050 1.000 Uiso H28B -0.00330 0.15500 0.16750 0.050 1.000 Uiso H29A -0.12650 0.11220 0.05800 0.050 1.000 Uiso H29B -0.14550 0.13740 -0.06120 0.050 1.000 Uiso H30A -0.10440 0.22020 0.11660 0.050 1.000 Uiso H30B -0.19440 0.19620 0.03230 0.050 1.000 Uiso H31A -0.18790 0.28750 -0.04190 0.050 1.000 Uiso H31B -0.21260 0.23370 -0.13150 0.050 1.000 Uiso H31C -0.12260 0.25770 -0.04730 0.050 1.000 Uiso 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 S1 0.0339(5) 0.0516(7) 0.0530(7) 0.0051(5) 0.0218(5) 0.0016(5) S2 0.0294(5) 0.0514(7) 0.0520(7) -0.0012(5) 0.0186(5) -0.0006(5) S3 0.0304(5) 0.0635(7) 0.0418(6) -0.0005(5) 0.0174(5) 0.0026(5) S4 0.0368(6) 0.0621(7) 0.0467(6) -0.0109(5) 0.0207(5) -0.0101(5) O21 0.038(2) 0.059(2) 0.056(2) 0.011(1) 0.018(1) -0.006(2) N21 0.044(2) 0.070(3) 0.069(3) -0.008(2) 0.025(2) -0.006(2) N22 0.047(2) 0.051(2) 0.091(3) 0.004(2) 0.034(2) 0.007(2) N23 0.049(3) 0.062(3) 0.086(3) 0.002(2) -0.002(2) 0.003(2) N24 0.077(3) 0.052(3) 0.074(3) 0.005(2) 0.029(2) 0.004(2) C1 0.034(2) 0.049(3) 0.044(2) 0.001(2) 0.024(2) -0.002(2) C2 0.030(2) 0.047(2) 0.038(2) 0.002(2) 0.021(2) 0.000(2) C3 0.031(2) 0.047(2) 0.040(2) -0.002(2) 0.021(2) -0.001(2) C4 0.034(2) 0.046(2) 0.039(2) 0.002(2) 0.021(2) 0.004(2) C5 0.038(2) 0.052(3) 0.054(3) -0.005(2) 0.023(2) 0.001(2) C6 0.056(3) 0.045(3) 0.072(3) -0.005(2) 0.036(3) 0.002(2) C7 0.051(3) 0.051(3) 0.066(3) 0.010(2) 0.031(3) 0.015(2) C8 0.039(2) 0.059(3) 0.051(3) 0.009(2) 0.026(2) 0.010(2) C9 0.032(2) 0.051(2) 0.039(2) -0.001(2) 0.022(2) 0.001(2) C10 0.029(2) 0.055(3) 0.033(2) -0.001(2) 0.017(2) -0.001(2) C11 0.034(2) 0.047(2) 0.038(2) -0.003(2) 0.023(2) -0.004(2) C12 0.038(2) 0.054(3) 0.041(2) -0.005(2) 0.025(2) -0.006(2) C13 0.050(2) 0.047(2) 0.046(2) -0.004(2) 0.033(2) -0.009(2) C14 0.063(3) 0.053(3) 0.064(3) -0.013(3) 0.041(3) -0.017(2) C15 0.097(5) 0.046(3) 0.086(4) -0.014(3) 0.064(4) -0.016(3) C16 0.084(4) 0.051(3) 0.072(4) 0.007(3) 0.050(3) 0.001(3) C17 0.059(3) 0.051(3) 0.061(3) 0.005(2) 0.037(3) -0.002(2) C18 0.045(2) 0.049(3) 0.044(2) 0.003(2) 0.028(2) -0.002(2) C21 0.042(2) 0.056(3) 0.050(3) 0.003(2) 0.024(2) -0.001(2) C22 0.043(2) 0.045(3) 0.056(3) -0.004(2) 0.027(2) -0.001(2) C23 0.044(2) 0.041(2) 0.059(3) 0.002(2) 0.020(2) 0.002(2) C24 0.045(2) 0.049(3) 0.054(3) 0.006(2) 0.022(2) -0.002(2) C25 0.035(2) 0.054(3) 0.047(2) 0.000(2) 0.022(2) -0.001(2) C26 0.037(2) 0.059(3) 0.039(2) 0.007(2) 0.020(2) -0.004(2) C27 0.036(2) 0.048(2) 0.044(2) 0.006(2) 0.021(2) 0.002(2) C28 0.057(3) 0.125(6) 0.096(5) 0.017(3) 0.033(3) -0.044(4) C29 0.060(3) 0.091(4) 0.101(5) 0.021(3) 0.034(3) -0.012(4) C30 0.075(4) 0.096(5) 0.105(5) 0.026(4) 0.050(4) 0.007(4) C31 0.070(4) 0.099(5) 0.113(5) 0.018(4) 0.045(4) 0.018(4) 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 S1 S2 2.060(2) . . ? S1 C1 1.725(4) . . ? S2 C3 1.728(4) . . ? S3 S4 2.073(2) . . ? S3 C10 1.742(4) . . ? S4 C12 1.741(4) . . ? O21 C26 1.358(5) . . ? O21 C28 1.432(8) . . ? N21 C21 1.145(6) . . ? N22 C22 1.144(6) . . ? N23 C23 1.137(7) . . ? N24 C24 1.145(7) . . ? C1 C2 1.383(6) . . ? C1 C18 1.429(6) . . ? C2 C3 1.392(6) . . ? C2 C11 1.431(6) . . ? C3 C4 1.420(6) . . ? C4 C5 1.402(7) . . ? C4 C9 1.440(6) . . ? C5 C6 1.363(7) . . ? C6 C7 1.397(7) . . ? C7 C8 1.357(7) . . ? C8 C9 1.415(7) . . ? C9 C10 1.420(6) . . ? C10 C11 1.387(6) . . ? C11 C12 1.390(6) . . ? C12 C13 1.422(6) . . ? C13 C14 1.403(7) . . ? C13 C18 1.451(6) . . ? C14 C15 1.368(8) . . ? C15 C16 1.401(9) . . ? C16 C17 1.363(8) . . ? C17 C18 1.409(7) . . ? C21 C25 1.427(6) . . ? C22 C25 1.420(6) . . ? C23 C27 1.408(6) . . ? C24 C27 1.425(7) . . ? C25 C26 1.392(7) . . ? C26 C27 1.397(6) . . ? C28 C29 1.386(8) . . ? C29 C30 1.519(10) . . ? C30 C31 1.442(10) . . ? C5 H5 0.97(4) . . ? C6 H6 0.98(5) . . ? C7 H7 0.97(5) . . ? C8 H8 0.95(5) . . ? C14 H14 1.03(5) . . ? C15 H15 0.93(5) . . ? C16 H16 0.94(6) . . ? C17 H17 1.02(5) . . ? C28 H28A 0.960 . . ? C28 H28B 0.960 . . ? C29 H29A 0.960 . . ? C29 H29B 0.960 . . ? C30 H30A 0.960 . . ? C30 H30B 0.960 . . ? C31 H31A 0.960 . . ? C31 H31B 0.960 . . ? C31 H31C 0.960 . . ? 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 S2 S1 C1 95.7(2) . . . ? S1 S2 C3 95.6(2) . . . ? S4 S3 C10 95.2(2) . . . ? S3 S4 C12 96.1(2) . . . ? C26 O21 C28 121.7(4) . . . ? S1 C1 C2 114.6(4) . . . ? S1 C1 C18 124.3(4) . . . ? C2 C1 C18 121.1(4) . . . ? C1 C2 C3 119.8(4) . . . ? C1 C2 C11 120.5(4) . . . ? C3 C2 C11 119.7(4) . . . ? S2 C3 C2 114.3(3) . . . ? S2 C3 C4 124.4(3) . . . ? C2 C3 C4 121.2(4) . . . ? C3 C4 C5 122.5(4) . . . ? C3 C4 C9 119.1(4) . . . ? C5 C4 C9 118.5(4) . . . ? C4 C5 C6 121.5(5) . . . ? C5 C6 C7 119.9(5) . . . ? C6 C7 C8 121.1(5) . . . ? C7 C8 C9 120.8(5) . . . ? C4 C9 C8 118.2(4) . . . ? C4 C9 C10 118.6(4) . . . ? C8 C9 C10 123.2(4) . . . ? S3 C10 C9 124.1(4) . . . ? S3 C10 C11 114.3(3) . . . ? C9 C10 C11 121.6(4) . . . ? C2 C11 C10 119.8(4) . . . ? C2 C11 C12 119.4(4) . . . ? C10 C11 C12 120.8(4) . . . ? S4 C12 C11 113.6(3) . . . ? S4 C12 C13 124.6(4) . . . ? C11 C12 C13 121.8(4) . . . ? C12 C13 C14 123.2(4) . . . ? C12 C13 C18 118.5(4) . . . ? C14 C13 C18 118.3(4) . . . ? C13 C14 C15 120.6(5) . . . ? C14 C15 C16 121.1(6) . . . ? C15 C16 C17 120.4(6) . . . ? C16 C17 C18 120.7(5) . . . ? C1 C18 C13 118.7(4) . . . ? C1 C18 C17 122.4(4) . . . ? C13 C18 C17 118.9(4) . . . ? N21 C21 C25 179.5(5) . . . ? N22 C22 C25 177.7(5) . . . ? N23 C23 C27 175.8(5) . . . ? N24 C24 C27 176.6(5) . . . ? C21 C25 C22 116.5(4) . . . ? C21 C25 C26 119.3(4) . . . ? C22 C25 C26 124.1(4) . . . ? O21 C26 C25 112.7(4) . . . ? O21 C26 C27 120.6(4) . . . ? C25 C26 C27 126.6(4) . . . ? C23 C27 C24 114.0(4) . . . ? C23 C27 C26 123.0(4) . . . ? C24 C27 C26 122.9(4) . . . ? O21 C28 C29 113.0(6) . . . ? C28 C29 C30 115.0(6) . . . ? C29 C30 C31 114.6(6) . . . ? C4 C5 H5 116.8(23) . . . ? C6 C5 H5 121.7(23) . . . ? C5 C6 H6 118.5(25) . . . ? C7 C6 H6 121.6(25) . . . ? C6 C7 H7 119.9(25) . . . ? C8 C7 H7 119.0(25) . . . ? C7 C8 H8 119.9(25) . . . ? C9 C8 H8 119.2(25) . . . ? C13 C14 H14 117.5(24) . . . ? C15 C14 H14 121.9(24) . . . ? C14 C15 H15 116.4(30) . . . ? C16 C15 H15 122.3(29) . . . ? C15 C16 H16 123.5(31) . . . ? C17 C16 H16 116.1(31) . . . ? C16 C17 H17 121.4(24) . . . ? C18 C17 H17 118.0(24) . . . ? O21 C28 H28A 107.7(5) . . . ? O21 C28 H28B 110.5(6) . . . ? C29 C28 H28A 106.5(6) . . . ? C29 C28 H28B 110.0(6) . . . ? H28A C28 H28B 109.0(7) . . . ? C28 C29 H29A 105.7(6) . . . ? C28 C29 H29B 109.7(6) . . . ? C30 C29 H29A 109.1(6) . . . ? C30 C29 H29B 108.2(6) . . . ? H29A C29 H29B 109.0(7) . . . ? C29 C30 H30A 107.2(6) . . . ? C29 C30 H30B 109.8(6) . . . ? C31 C30 H30A 108.4(7) . . . ? C31 C30 H30B 107.7(6) . . . ? H30A C30 H30B 109.0(7) . . . ? C30 C31 H31A 114.1(7) . . . ? C30 C31 H31B 108.4(7) . . . ? C30 C31 H31C 107.7(7) . . . ? H31A C31 H31B 108.7(7) . . . ? H31A C31 H31C 108.8(7) . . . ? H31B C31 H31C 109.0(7) . . . ? 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 S1 N21 3.006(4) 1_555 2_555 ? S1 C24 3.327(5) 1_555 1_555 ? S2 N21 3.012(4) 1_555 2_555 ? S3 N22 3.130(4) 1_555 2_656 ? S3 N23 3.091(4) 1_555 2_656 ? S3 C2 3.444(4) 1_555 5_655 ? S3 C3 3.393(4) 1_555 5_655 ? S4 C1 3.380(4) 1_555 5_655 ? O21 C21 3.196(5) 1_555 2_555 ? N23 H8 2.48(4) 1_555 2_656 ? N24 H14 2.54(4) 1_555 7_455 ? C10 C10 3.370(5) 1_555 5_655 ? C12 C12 3.301(6) 1_555 5_655 ? C14 C14 3.269(7) 1_555 5_655 ? H28B H28B 2.2389 1_555 5_555 ? N22 H16 2.75(5) 1_555 8_555 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)(PrO-TCA)(THF)0.5 _database_code_CSD 165349 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _chemical_formula_moiety 'C18 H8 S4 1+,C10 H7 N4 O1 1-, 0.5(C4 H8 O1)' _chemical_formula_sum 'C30 H19 N4 O1.5 S4 ' _chemical_formula_weight 587.77 _cell_length_a 11.969(2) _cell_length_b 12.060(2) _cell_length_c 11.166(2) _cell_angle_alpha 73.67(1) _cell_angle_beta 84.16(1) _cell_angle_gamma 59.910(8) _cell_volume 1336.8(5) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '??' _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas 1.450 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.742 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science DIP2020K' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 5012 _reflns_number_total 4305 _reflns_number_observed 2829 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.083 _refine_ls_wR_factor_obs 0.080 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 2829 _refine_ls_number_parameters 414 _refine_ls_goodness_of_fit_obs 1.767 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.4478 _refine_ls_shift/esd_mean 0.0419 _refine_diff_density_min -0.36 _refine_diff_density_max 0.34 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.04177 _diffrn_orient_matrix_UB_12 0.07404 _diffrn_orient_matrix_UB_13 -0.00696 _diffrn_orient_matrix_UB_21 -0.02765 _diffrn_orient_matrix_UB_22 0.06064 _diffrn_orient_matrix_UB_23 -0.08149 _diffrn_orient_matrix_UB_31 -0.07881 _diffrn_orient_matrix_UB_32 0.01237 _diffrn_orient_matrix_UB_33 0.05638 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.6301(2) 0.5075(2) 0.1624(2) 0.064(1) 1.000 Uij S2 0.5622(2) 0.3774(2) 0.1766(2) 0.070(2) 1.000 Uij S3 0.1562(2) 0.6393(2) 0.5511(2) 0.065(1) 1.000 Uij S4 0.2262(2) 0.7674(2) 0.5412(2) 0.066(1) 1.000 Uij O21 0.1999(5) 0.8940(6) 0.1604(6) 0.061(3) 1.000 Uij O31 -0.091(4) 0.608(4) -0.048(3) 0.24(3) 0.500 Uij N21 0.0570(9) 1.1223(9) 0.3410(9) 0.109(7) 1.000 Uij N22 -0.2187(8) 0.9994(10) 0.3233(9) 0.102(7) 1.000 Uij N23 -0.0620(9) 0.6901(9) 0.2655(10) 0.106(7) 1.000 Uij N24 0.2444(9) 0.6625(10) 0.0163(9) 0.110(7) 1.000 Uij C1 0.5287(7) 0.5844(8) 0.2720(7) 0.052(5) 1.000 Uij C2 0.4417(7) 0.5406(8) 0.3183(8) 0.049(4) 1.000 Uij C3 0.4448(8) 0.4395(8) 0.2797(8) 0.055(5) 1.000 Uij C4 0.3586(8) 0.3903(8) 0.3288(8) 0.056(5) 1.000 Uij C5 0.3581(10) 0.2877(10) 0.2924(10) 0.074(6) 1.000 Uij C6 0.2732(10) 0.2446(10) 0.3399(11) 0.078(6) 1.000 Uij C7 0.1856(10) 0.2981(10) 0.4288(10) 0.075(6) 1.000 Uij C8 0.1825(8) 0.3977(9) 0.4654(9) 0.059(5) 1.000 Uij C9 0.2673(7) 0.4482(7) 0.4161(7) 0.045(4) 1.000 Uij C10 0.2644(7) 0.5531(7) 0.4520(7) 0.043(4) 1.000 Uij C11 0.3499(7) 0.5998(8) 0.4047(7) 0.043(4) 1.000 Uij C12 0.3460(7) 0.7047(8) 0.4386(7) 0.049(4) 1.000 Uij C13 0.4339(7) 0.7522(8) 0.3925(8) 0.047(4) 1.000 Uij C14 0.4316(9) 0.8570(9) 0.4253(8) 0.060(5) 1.000 Uij C15 0.5188(9) 0.8984(9) 0.3774(9) 0.067(6) 1.000 Uij C16 0.6130(9) 0.8356(9) 0.2997(9) 0.065(6) 1.000 Uij C17 0.6174(9) 0.7336(9) 0.2634(9) 0.059(5) 1.000 Uij C18 0.5285(8) 0.6901(8) 0.3074(7) 0.047(4) 1.000 Uij C21 0.0347(9) 1.0551(10) 0.3057(9) 0.076(6) 1.000 Uij C22 -0.1187(9) 0.9829(9) 0.2980(9) 0.069(6) 1.000 Uij C23 0.0043(8) 0.7312(9) 0.2241(9) 0.064(5) 1.000 Uij C24 0.1766(9) 0.7160(10) 0.0848(9) 0.072(6) 1.000 Uij C25 0.0046(8) 0.9718(9) 0.2648(8) 0.062(5) 1.000 Uij C26 0.0930(8) 0.8841(8) 0.1973(8) 0.051(5) 1.000 Uij C27 0.0893(8) 0.7797(8) 0.1708(7) 0.050(5) 1.000 Uij C28 0.1832(11) 1.0110(11) 0.0658(11) 0.084(7) 1.000 Uij C29 0.3096(13) 1.0026(13) 0.0326(13) 0.110(9) 1.000 Uij C30 0.4006(12) 0.8953(13) -0.0196(12) 0.089(8) 1.000 Uij C31 -0.128(2) 0.571(2) 0.041(3) 0.20(2) 1.000 Uij C32 -0.018(2) 0.447(2) 0.102(2) 0.15(1) 1.000 Uij H5 0.412(6) 0.248(6) 0.231(6) 0.02(2) 1.000 Uiso H6 0.273(8) 0.177(8) 0.318(8) 0.06(3) 1.000 Uiso H7 0.135(9) 0.265(10) 0.455(9) 0.08(3) 1.000 Uiso H8 0.126(7) 0.431(8) 0.529(7) 0.05(2) 1.000 Uiso H14 0.374(7) 0.900(7) 0.479(7) 0.03(2) 1.000 Uiso H15 0.515(6) 0.968(7) 0.404(6) 0.03(2) 1.000 Uiso H16 0.678(6) 0.857(6) 0.275(6) 0.02(2) 1.000 Uiso H17 0.677(8) 0.696(8) 0.213(7) 0.05(3) 1.000 Uiso H28A 0.141(7) 1.009(8) -0.020(8) 0.050 1.000 Uiso H28B 0.114(8) 1.087(8) 0.090(7) 0.050 1.000 Uiso H29A 0.317(8) 1.006(8) 0.123(8) 0.050 1.000 Uiso H29B 0.294(7) 1.093(8) -0.015(7) 0.050 1.000 Uiso H30A 0.415(7) 0.809(8) 0.032(8) 0.050 1.000 Uiso H30B 0.494(8) 0.871(8) -0.018(7) 0.050 1.000 Uiso H30C 0.368(8) 0.913(8) -0.106(8) 0.050 1.000 Uiso 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 S1 0.060(1) 0.057(1) 0.058(1) -0.037(1) 0.027(1) -0.028(1) S2 0.065(2) 0.059(1) 0.069(2) -0.042(1) 0.028(1) -0.034(1) S3 0.043(1) 0.062(1) 0.070(2) -0.032(1) 0.021(1) -0.026(1) S4 0.052(1) 0.062(2) 0.064(2) -0.033(1) 0.021(1) -0.032(1) O21 0.046(3) 0.054(4) 0.062(4) -0.029(3) 0.004(3) -0.009(3) O31 0.20(4) 0.28(4) 0.11(2) -0.07(3) 0.06(2) -0.04(2) N21 0.098(7) 0.093(7) 0.115(8) -0.069(6) 0.032(6) -0.057(6) N22 0.062(5) 0.104(7) 0.120(8) -0.050(5) 0.031(5) -0.072(7) N23 0.080(6) 0.088(7) 0.129(8) -0.062(6) 0.045(6) -0.053(6) N24 0.098(7) 0.099(8) 0.104(8) -0.059(6) 0.055(6) -0.060(6) C1 0.045(5) 0.053(5) 0.041(5) -0.029(4) 0.014(4) -0.020(4) C2 0.040(4) 0.042(4) 0.048(5) -0.023(4) 0.003(4) -0.012(4) C3 0.047(5) 0.052(5) 0.050(5) -0.032(4) 0.014(4) -0.016(4) C4 0.052(5) 0.044(5) 0.053(5) -0.026(4) 0.008(4) -0.015(4) C5 0.059(6) 0.059(6) 0.085(7) -0.032(5) 0.013(5) -0.037(6) C6 0.060(6) 0.052(6) 0.102(8) -0.036(5) 0.003(6) -0.026(6) C7 0.060(6) 0.060(6) 0.088(8) -0.047(5) 0.008(5) -0.013(5) C8 0.038(5) 0.054(6) 0.063(6) -0.027(4) 0.007(4) -0.006(5) C9 0.031(4) 0.036(4) 0.048(5) -0.016(3) -0.006(4) -0.001(4) C10 0.030(4) 0.038(4) 0.043(5) -0.017(4) 0.000(3) -0.005(4) C11 0.039(4) 0.040(4) 0.035(4) -0.021(4) 0.005(3) -0.010(4) C12 0.029(4) 0.050(5) 0.049(5) -0.018(4) 0.002(4) -0.019(4) C13 0.026(4) 0.043(5) 0.051(5) -0.013(4) -0.005(4) -0.011(4) C14 0.060(6) 0.054(5) 0.046(5) -0.030(5) 0.009(4) -0.019(4) C15 0.070(6) 0.056(6) 0.058(6) -0.039(5) 0.014(5) -0.027(5) C16 0.055(5) 0.063(6) 0.059(6) -0.045(5) -0.001(5) -0.003(5) C17 0.054(5) 0.050(5) 0.050(5) -0.029(5) 0.011(5) -0.010(5) C18 0.044(4) 0.035(4) 0.043(5) -0.022(4) 0.008(4) -0.003(4) C21 0.065(6) 0.075(7) 0.070(6) -0.047(6) 0.019(5) -0.034(5) C22 0.055(6) 0.055(6) 0.079(7) -0.028(5) 0.011(5) -0.036(5) C23 0.050(5) 0.055(5) 0.066(6) -0.029(5) 0.012(5) -0.022(5) C24 0.064(6) 0.063(6) 0.066(6) -0.035(5) 0.017(5) -0.028(5) C25 0.057(5) 0.066(6) 0.045(5) -0.043(5) 0.015(4) -0.020(4) C26 0.041(4) 0.049(5) 0.047(5) -0.028(4) 0.001(4) -0.006(4) C27 0.042(4) 0.052(5) 0.036(4) -0.021(4) -0.005(4) -0.011(4) C28 0.075(8) 0.055(6) 0.076(8) -0.022(6) 0.018(6) 0.008(6) C29 0.12(1) 0.09(1) 0.10(1) -0.07(1) 0.06(1) -0.03(1) C30 0.071(8) 0.086(9) 0.068(7) -0.040(7) 0.007(7) 0.001(7) C31 0.12(2) 0.15(2) 0.26(3) -0.07(2) -0.02(2) -0.03(2) C32 0.13(1) 0.13(1) 0.12(1) -0.04(1) 0.01(1) -0.01(1) 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 S1 S2 2.065(4) . . ? S1 C1 1.743(9) . . ? S2 C3 1.721(9) . . ? S3 S4 2.070(4) . . ? S3 C10 1.728(9) . . ? S4 C12 1.733(9) . . ? O21 C26 1.356(10) . . ? O21 C28 1.438(14) . . ? O31 C31 1.11(5) . . ? O31 C32 1.30(5) . 2_555 ? N21 C21 1.141(13) . . ? N22 C22 1.130(14) . . ? N23 C23 1.131(14) . . ? N24 C24 1.134(15) . . ? C1 C2 1.386(12) . . ? C1 C18 1.435(11) . . ? C2 C3 1.386(11) . . ? C2 C11 1.425(12) . . ? C3 C4 1.425(12) . . ? C4 C5 1.409(13) . . ? C4 C9 1.426(13) . . ? C5 C6 1.360(15) . . ? C6 C7 1.404(17) . . ? C7 C8 1.356(13) . . ? C8 C9 1.422(12) . . ? C9 C10 1.415(11) . . ? C10 C11 1.395(11) . . ? C11 C12 1.398(11) . . ? C12 C13 1.425(11) . . ? C13 C14 1.398(12) . . ? C13 C18 1.441(12) . . ? C14 C15 1.372(14) . . ? C15 C16 1.382(14) . . ? C16 C17 1.376(13) . . ? C17 C18 1.399(13) . . ? C21 C25 1.414(13) . . ? C22 C25 1.433(14) . . ? C23 C27 1.417(13) . . ? C24 C27 1.418(14) . . ? C25 C26 1.404(13) . . ? C26 C27 1.394(11) . . ? C28 C29 1.480(19) . . ? C29 C30 1.44(2) . . ? C31 C32 1.44(4) . . ? C5 H5 0.95(7) . . ? C6 H6 0.92(9) . . ? C7 H7 0.87(10) . . ? C8 H8 0.95(9) . . ? C14 H14 0.91(8) . . ? C15 H15 0.94(7) . . ? C16 H16 0.92(7) . . ? C17 H17 0.88(9) . . ? C28 H28A 1.14(8) . . ? C28 H28B 0.97(9) . . ? C29 H29A 1.04(8) . . ? C29 H29B 1.00(9) . . ? C30 H30A 0.97(9) . . ? C30 H30B 1.00(9) . . ? C30 H30C 1.00(8) . . ? 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 S2 S1 C1 95.1(3) . . . ? S1 S2 C3 95.8(3) . . . ? S4 S3 C10 96.2(3) . . . ? S3 S4 C12 95.8(3) . . . ? C26 O21 C28 117.9(7) . . . ? C31 O31 C32 132.8(37) . . 2_555 ? S1 C1 C2 114.5(7) . . . ? S1 C1 C18 123.6(6) . . . ? C2 C1 C18 121.8(8) . . . ? C1 C2 C3 119.5(8) . . . ? C1 C2 C11 119.9(8) . . . ? C3 C2 C11 120.7(7) . . . ? S2 C3 C2 115.0(6) . . . ? S2 C3 C4 124.5(7) . . . ? C2 C3 C4 120.4(8) . . . ? C3 C4 C5 122.5(8) . . . ? C3 C4 C9 119.3(8) . . . ? C5 C4 C9 118.2(8) . . . ? C4 C5 C6 120.9(10) . . . ? C5 C6 C7 121.3(10) . . . ? C6 C7 C8 119.6(10) . . . ? C7 C8 C9 121.2(9) . . . ? C4 C9 C8 118.8(8) . . . ? C4 C9 C10 119.2(7) . . . ? C8 C9 C10 122.0(8) . . . ? S3 C10 C9 125.4(6) . . . ? S3 C10 C11 113.3(6) . . . ? C9 C10 C11 121.3(7) . . . ? C2 C11 C10 119.2(7) . . . ? C2 C11 C12 119.5(7) . . . ? C10 C11 C12 121.3(7) . . . ? S4 C12 C11 113.3(6) . . . ? S4 C12 C13 124.7(7) . . . ? C11 C12 C13 122.0(8) . . . ? C12 C13 C14 122.9(8) . . . ? C12 C13 C18 118.4(7) . . . ? C14 C13 C18 118.7(7) . . . ? C13 C14 C15 120.1(9) . . . ? C14 C15 C16 121.3(9) . . . ? C15 C16 C17 120.4(9) . . . ? C16 C17 C18 120.2(9) . . . ? C1 C18 C13 118.5(7) . . . ? C1 C18 C17 122.4(8) . . . ? C13 C18 C17 119.1(8) . . . ? N21 C21 C25 178.3(11) . . . ? N22 C22 C25 175.9(11) . . . ? N23 C23 C27 178.4(10) . . . ? N24 C24 C27 177.7(11) . . . ? C21 C25 C22 115.7(8) . . . ? C21 C25 C26 120.6(8) . . . ? C22 C25 C26 123.6(8) . . . ? O21 C26 C25 117.4(8) . . . ? O21 C26 C27 114.9(7) . . . ? C25 C26 C27 127.4(8) . . . ? C23 C27 C24 116.8(8) . . . ? C23 C27 C26 124.8(8) . . . ? C24 C27 C26 118.4(8) . . . ? O21 C28 C29 110.8(10) . . . ? C28 C29 C30 117.2(12) . . . ? O31 C31 C32 104.5(28) . . . ? O31 C32 C31 122.3(24) 2_555 . . ? C4 C5 H5 123.2(36) . . . ? C6 C5 H5 115.8(36) . . . ? C5 C6 H6 121.5(53) . . . ? C7 C6 H6 117.1(53) . . . ? C6 C7 H7 116.2(65) . . . ? C8 C7 H7 124.3(65) . . . ? C7 C8 H8 119.6(47) . . . ? C9 C8 H8 119.2(47) . . . ? C13 C14 H14 123.0(44) . . . ? C15 C14 H14 116.9(44) . . . ? C14 C15 H15 116.9(41) . . . ? C16 C15 H15 121.7(42) . . . ? C15 C16 H16 121.2(39) . . . ? C17 C16 H16 118.2(39) . . . ? C16 C17 H17 118.7(52) . . . ? C18 C17 H17 121.0(52) . . . ? O21 C28 H28A 104.8(40) . . . ? O21 C28 H28B 107.2(47) . . . ? C29 C28 H28A 107.3(40) . . . ? C29 C28 H28B 121.5(48) . . . ? H28A C28 H28B 103.8(61) . . . ? C28 C29 H29A 86.5(44) . . . ? C28 C29 H29B 108.2(44) . . . ? C30 C29 H29A 124.3(45) . . . ? C30 C29 H29B 115.9(46) . . . ? H29A C29 H29B 100.2(63) . . . ? C29 C30 H30A 112.2(49) . . . ? C29 C30 H30B 117.6(46) . . . ? C29 C30 H30C 108.5(46) . . . ? H30A C30 H30B 95.4(63) . . . ? H30A C30 H30C 111.0(67) . . . ? H30B C30 H30C 111.7(63) . . . ? 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 S1 N24 3.01(1) 1_555 2_665 ? S1 C31 3.42(3) 1_555 1_655 ? S2 N24 2.95(1) 1_555 2_665 ? S3 N21 3.19(1) 1_555 2_576 ? S4 N21 3.25(1) 1_555 2_576 ? S4 C21 3.39(1) 1_555 2_576 ? N23 H8 2.62(8) 1_555 2_566 ? C8 C16 3.32(1) 1_555 2_666 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)(EtO-TCA)2 _database_code_CSD 165350 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _chemical_formula_moiety 'C18 H8 S4 1+,2(C9 H5 N4 O1 1-)' _chemical_formula_sum 'C36 H18 N8 O2 S4 ' _chemical_formula_weight 722.86 _cell_length_a 7.814(1) _cell_length_b 8.649(2) _cell_length_c 14.448(2) _cell_angle_alpha 105.06(1) _cell_angle_beta 91.61(1) _cell_angle_gamma 116.51(1) _cell_volume 832.0(2) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '??' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_meas 1.448 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.189 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3-chi' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 4198 _reflns_number_total 3821 _reflns_number_observed 2256 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _refine_ls_structure_factor_coef ? _refine_ls_R_factor_obs 0.049 _refine_ls_wR_factor_obs 0.049 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 2256 _refine_ls_number_parameters 242 _refine_ls_goodness_of_fit_obs 0.650 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0011 _refine_ls_shift/esd_mean 0.0002 _refine_diff_density_min -0.26 _refine_diff_density_max 0.39 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P-1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.19698(16) 0.42746(12) 0.50901(7) 0.0438(5) 1.000 Uij S2 0.25248(16) 0.28773(12) 0.38700(7) 0.0461(5) 1.000 Uij O11 0.7933(4) -0.0791(4) 0.1651(2) 0.056(2) 1.000 Uij N11 0.7278(7) 0.1908(5) 0.3599(3) 0.083(3) 1.000 Uij N12 0.4556(6) -0.3337(5) 0.4027(3) 0.062(2) 1.000 Uij N13 0.4161(11) -0.6721(6) 0.1979(4) 0.131(4) 1.000 Uij N14 0.7777(7) -0.4686(7) 0.0017(3) 0.092(3) 1.000 Uij C1 0.0667(5) 0.2434(4) 0.5474(3) 0.035(2) 1.000 Uij C2 0.0498(5) 0.0810(4) 0.4879(3) 0.033(2) 1.000 Uij C3 0.1335(5) 0.0799(5) 0.4042(3) 0.035(2) 1.000 Uij C4 0.1186(6) -0.0857(5) 0.3399(3) 0.035(2) 1.000 Uij C5 0.1968(6) -0.0903(5) 0.2539(3) 0.044(2) 1.000 Uij C6 0.1764(7) -0.2524(5) 0.1942(3) 0.049(2) 1.000 Uij C7 0.0817(7) -0.4107(6) 0.2187(3) 0.052(2) 1.000 Uij C8 0.0026(6) -0.4110(5) 0.3023(3) 0.045(2) 1.000 Uij C9 0.0173(5) -0.2504(5) 0.3645(3) 0.035(2) 1.000 Uij C11 0.6851(6) 0.0402(6) 0.3288(3) 0.051(2) 1.000 Uij C12 0.5344(6) -0.2536(5) 0.3519(3) 0.042(2) 1.000 Uij C13 0.5150(9) -0.5420(6) 0.1821(3) 0.075(3) 1.000 Uij C14 0.7181(7) -0.4302(6) 0.0698(3) 0.059(3) 1.000 Uij C15 0.6334(6) -0.1468(5) 0.2929(3) 0.041(2) 1.000 Uij C16 0.6820(6) -0.2124(5) 0.2034(3) 0.042(2) 1.000 Uij C17 0.6382(7) -0.3898(6) 0.1546(3) 0.050(2) 1.000 Uij C18 0.7156(13) -0.0704(12) 0.0803(6) 0.161(7) 1.000 Uij C19 0.7892(15) 0.0784(11) 0.0544(7) 0.169(7) 1.000 Uij H5 0.265(6) 0.016(5) 0.234(3) 0.04(1) 1.000 Uiso H6 0.223(6) -0.258(6) 0.140(3) 0.05(1) 1.000 Uiso H7 0.068(7) -0.517(6) 0.180(3) 0.07(2) 1.000 Uiso H8 -0.064(6) -0.514(6) 0.319(3) 0.06(1) 1.000 Uiso H18A 0.58250 -0.10006 0.08389 0.050 1.000 Uiso H18B 0.72030 -0.16266 0.02809 0.050 1.000 Uiso H19A 0.73637 0.08657 -0.00381 0.050 1.000 Uiso H19B 0.92087 0.10447 0.04909 0.050 1.000 Uiso H19C 0.78907 0.17237 0.10719 0.050 1.000 Uiso 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 S1 0.0525(6) 0.0225(4) 0.0417(5) 0.0154(4) 0.0167(5) 0.0107(4) S2 0.0561(7) 0.0268(5) 0.0393(5) 0.0152(5) 0.0208(5) 0.0135(4) O11 0.056(2) 0.042(2) 0.048(2) 0.011(1) 0.019(1) 0.018(1) N11 0.114(4) 0.036(2) 0.068(3) 0.029(2) 0.027(3) 0.010(2) N12 0.072(3) 0.040(2) 0.050(2) 0.021(2) 0.021(2) 0.014(2) N13 0.218(7) 0.040(2) 0.079(3) 0.033(4) 0.071(4) 0.019(2) N14 0.094(4) 0.086(3) 0.057(3) 0.048(3) 0.022(3) -0.004(2) C1 0.037(2) 0.021(2) 0.033(2) 0.012(1) 0.007(2) 0.006(1) C2 0.034(2) 0.024(2) 0.030(2) 0.013(1) 0.009(1) 0.007(1) C3 0.035(2) 0.024(2) 0.032(2) 0.009(1) 0.006(2) 0.008(1) C4 0.037(2) 0.026(2) 0.031(2) 0.014(2) 0.010(2) 0.007(1) C5 0.043(2) 0.036(2) 0.037(2) 0.017(2) 0.013(2) 0.010(2) C6 0.052(3) 0.040(2) 0.035(2) 0.021(2) 0.015(2) 0.004(2) C7 0.057(3) 0.039(2) 0.042(2) 0.026(2) 0.011(2) 0.000(2) C8 0.049(2) 0.027(2) 0.043(2) 0.020(2) 0.011(2) 0.005(2) C9 0.034(2) 0.026(2) 0.032(2) 0.013(1) 0.006(2) 0.005(1) C11 0.054(3) 0.039(2) 0.042(2) 0.017(2) 0.013(2) 0.013(2) C12 0.042(2) 0.031(2) 0.038(2) 0.017(2) 0.008(2) 0.007(2) C13 0.110(4) 0.041(2) 0.045(3) 0.033(3) 0.027(3) 0.006(2) C14 0.057(3) 0.051(3) 0.045(2) 0.026(2) 0.004(2) 0.001(2) C15 0.043(2) 0.026(2) 0.038(2) 0.014(2) 0.009(2) 0.009(2) C16 0.037(2) 0.036(2) 0.039(2) 0.015(2) 0.007(2) 0.014(2) C17 0.056(3) 0.040(2) 0.036(2) 0.022(2) 0.011(2) 0.009(2) C18 0.153(8) 0.128(7) 0.121(6) -0.012(6) -0.021(6) 0.092(6) C19 0.21(1) 0.11(1) 0.13(1) 0.05(1) 0.01(1) 0.07(1) 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 S1 S2 2.040(2) . . ? S1 C1 1.709(4) . . ? S2 C3 1.705(4) . . ? O11 C16 1.361(6) . . ? O11 C18 1.387(9) . . ? N11 C11 1.145(6) . . ? N12 C12 1.144(6) . . ? N13 C13 1.132(8) . . ? N14 C14 1.136(7) . . ? C1 C2 1.390(5) . . ? C1 C9 1.448(6) . 2_556 ? C2 C2 1.409(5) . 2_556 ? C2 C3 1.391(6) . . ? C3 C4 1.443(5) . . ? C4 C5 1.399(6) . . ? C4 C9 1.433(5) . . ? C5 C6 1.378(6) . . ? C6 C7 1.382(7) . . ? C7 C8 1.372(7) . . ? C8 C9 1.397(6) . . ? C11 C15 1.420(6) . . ? C12 C15 1.409(6) . . ? C13 C17 1.407(7) . . ? C14 C17 1.424(7) . . ? C15 C16 1.407(6) . . ? C16 C17 1.387(6) . . ? C18 C19 1.314(13) . . ? C5 H5 0.95(5) . . ? C6 H6 0.88(5) . . ? C7 H7 0.90(5) . . ? C8 H8 0.91(5) . . ? C18 H18A 0.960 . . ? C18 H18B 0.960 . . ? C19 H19A 0.960 . . ? C19 H19B 0.960 . . ? C19 H19C 0.960 . . ? 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 S2 S1 C1 95.7(2) . . . ? S1 S2 C3 96.3(2) . . . ? C16 O11 C18 119.1(5) . . . ? S1 C1 C2 114.5(3) . . . ? S1 C1 C9 124.6(3) . . 2_556 ? C2 C1 C9 120.9(4) . . 2_556 ? C1 C2 C2 120.6(4) . . 2_556 ? C1 C2 C3 119.2(4) . . . ? C2 C2 C3 120.2(4) 2_556 . . ? S2 C3 C2 114.2(3) . . . ? S2 C3 C4 124.7(3) . . . ? C2 C3 C4 121.1(4) . . . ? C3 C4 C5 121.9(4) . . . ? C3 C4 C9 118.7(4) . . . ? C5 C4 C9 119.3(4) . . . ? C4 C5 C6 119.8(4) . . . ? C5 C6 C7 120.9(4) . . . ? C6 C7 C8 120.8(4) . . . ? C7 C8 C9 120.5(4) . . . ? C1 C9 C4 118.5(4) 2_556 . . ? C1 C9 C8 122.8(4) 2_556 . . ? C4 C9 C8 118.8(4) . . . ? N11 C11 C15 178.4(5) . . . ? N12 C12 C15 177.1(5) . . . ? N13 C13 C17 175.0(6) . . . ? N14 C14 C17 177.7(6) . . . ? C11 C15 C12 115.8(4) . . . ? C11 C15 C16 119.3(4) . . . ? C12 C15 C16 124.9(4) . . . ? O11 C16 C15 113.4(4) . . . ? O11 C16 C17 118.6(4) . . . ? C15 C16 C17 128.0(4) . . . ? C13 C17 C14 114.6(4) . . . ? C13 C17 C16 124.8(5) . . . ? C14 C17 C16 120.7(4) . . . ? O11 C18 C19 122.0(8) . . . ? C4 C5 H5 122.3(24) . . . ? C6 C5 H5 117.9(24) . . . ? C5 C6 H6 120.8(28) . . . ? C7 C6 H6 118.4(28) . . . ? C6 C7 H7 120.9(31) . . . ? C8 C7 H7 118.3(31) . . . ? C7 C8 H8 122.7(29) . . . ? C9 C8 H8 116.8(29) . . . ? O11 C18 H18A 107.3(8) . . . ? O11 C18 H18B 106.2(8) . . . ? C19 C18 H18A 105.6(9) . . . ? C19 C18 H18B 106.2(9) . . . ? H18A C18 H18B 109.0(9) . . . ? C18 C19 H19A 122.9(10) . . . ? C18 C19 H19B 104.8(9) . . . ? C18 C19 H19C 106.7(9) . . . ? H19A C19 H19B 106.5(9) . . . ? H19A C19 H19C 106.5(10) . . . ? H19B C19 H19C 109.0(9) . . . ? 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 S1 N11 3.129(4) 1_555 2_666 ? S1 N12 2.967(4) 1_555 1_565 ? S2 N12 2.871(4) 1_555 1_565 ? S2 N13 3.085(6) 1_555 1_565 ? N11 H8 2.58(5) 1_555 1_665 ? N12 C1 3.466(6) 1_555 2_656 ? N13 H5 2.62(4) 1_555 1_545 ? N14 C6 3.353(6) 1_555 2_645 ? N14 H6 2.69(4) 1_555 2_645 ? C1 C12 3.358(5) 1_555 2_656 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)(PrO-TCA)2 _database_code_CSD 165351 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _chemical_formula_moiety 'C18 H8 S4 1+,2(C10 H7 N4 O1 1-)' _chemical_formula_sum 'C38 H22 N8 O2 S4 ' _chemical_formula_weight 750.91 _cell_length_a 7.915(2) _cell_length_b 8.923(4) _cell_length_c 14.943(4) _cell_angle_alpha 108.34(2) _cell_angle_beta 90.04(2) _cell_angle_gamma 117.84(2) _cell_volume 872.0(5) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '??' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_meas 1.445 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.070 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3-chi' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 4420 _reflns_number_total 3616 _reflns_number_observed 2584 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.050 _refine_ls_wR_factor_obs 0.052 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 2584 _refine_ls_number_parameters 251 _refine_ls_goodness_of_fit_obs 0.822 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0494 _refine_ls_shift/esd_mean 0.0052 _refine_diff_density_min -0.51 _refine_diff_density_max 0.38 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.01593 _diffrn_orient_matrix_UB_12 0.01046 _diffrn_orient_matrix_UB_13 -0.07091 _diffrn_orient_matrix_UB_21 0.13641 _diffrn_orient_matrix_UB_22 -0.07901 _diffrn_orient_matrix_UB_23 -0.00111 _diffrn_orient_matrix_UB_31 -0.03493 _diffrn_orient_matrix_UB_32 -0.10125 _diffrn_orient_matrix_UB_33 0.01002 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.19356(15) 0.42191(11) 0.51246(7) 0.0447(5) 1.000 Uij S2 0.24920(15) 0.27955(12) 0.39134(7) 0.0473(5) 1.000 Uij O11 0.8002(4) -0.0966(3) 0.1841(2) 0.054(1) 1.000 Uij N11 0.7296(7) 0.1768(5) 0.3716(3) 0.079(3) 1.000 Uij N12 0.4448(6) -0.3447(5) 0.4078(3) 0.066(2) 1.000 Uij N13 0.4046(10) -0.6850(6) 0.2032(4) 0.134(4) 1.000 Uij N14 0.7562(6) -0.4857(5) 0.0086(3) 0.077(3) 1.000 Uij C1 0.0655(5) 0.2424(4) 0.5489(2) 0.035(2) 1.000 Uij C2 0.0503(5) 0.0797(4) 0.4889(2) 0.034(2) 1.000 Uij C3 0.1336(5) 0.0756(4) 0.4071(2) 0.037(2) 1.000 Uij C4 0.1195(5) -0.0903(5) 0.3427(2) 0.037(2) 1.000 Uij C5 0.2001(6) -0.0984(5) 0.2592(3) 0.047(2) 1.000 Uij C6 0.1823(6) -0.2599(6) 0.1997(3) 0.052(2) 1.000 Uij C7 0.0899(7) -0.4139(6) 0.2226(3) 0.054(2) 1.000 Uij C8 0.0075(6) -0.4128(5) 0.3033(3) 0.047(2) 1.000 Uij C9 0.0201(5) -0.2520(4) 0.3654(2) 0.037(2) 1.000 Uij C11 0.6845(6) 0.0267(5) 0.3424(3) 0.052(2) 1.000 Uij C12 0.5253(6) -0.2653(5) 0.3600(3) 0.046(2) 1.000 Uij C13 0.5038(9) -0.5572(6) 0.1885(3) 0.077(3) 1.000 Uij C14 0.7018(6) -0.4478(5) 0.0782(3) 0.054(2) 1.000 Uij C15 0.6298(5) -0.1600(5) 0.3054(3) 0.041(2) 1.000 Uij C16 0.6791(5) -0.2288(5) 0.2170(3) 0.042(2) 1.000 Uij C17 0.6287(6) -0.4055(5) 0.1644(3) 0.048(2) 1.000 Uij C18 0.7252(9) -0.0790(8) 0.1046(4) 0.104(4) 1.000 Uij C19 0.8320(11) 0.0832(9) 0.0920(5) 0.126(5) 1.000 Uij C20 0.7839(10) 0.1202(9) 0.0121(5) 0.119(5) 1.000 Uij H5 0.254(5) -0.005(5) 0.244(3) 0.04(1) 1.000 Uiso H6 0.229(6) -0.266(5) 0.146(3) 0.05(1) 1.000 Uiso H7 0.086(6) -0.515(5) 0.179(3) 0.05(1) 1.000 Uiso H8 -0.055(6) -0.511(5) 0.320(3) 0.04(1) 1.000 Uiso H18A 0.59766 -0.09525 0.11130 0.050 1.000 Uiso H18B 0.71576 -0.17225 0.04750 0.050 1.000 Uiso H19A 0.96111 0.10057 0.09121 0.050 1.000 Uiso H19B 0.83311 0.17337 0.14821 0.050 1.000 Uiso H20A 0.86445 0.23660 0.00715 0.050 1.000 Uiso H20B 0.65485 0.10280 0.01295 0.050 1.000 Uiso H20C 0.78285 0.03000 -0.04405 0.050 1.000 Uiso 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 S1 0.0522(6) 0.0233(4) 0.0407(5) 0.0155(4) 0.0143(4) 0.0134(4) S2 0.0560(7) 0.0286(4) 0.0385(5) 0.0169(4) 0.0193(5) 0.0172(4) O11 0.049(2) 0.040(1) 0.049(2) 0.014(1) 0.009(1) 0.024(1) N11 0.100(4) 0.035(2) 0.069(3) 0.032(2) 0.012(2) 0.010(2) N12 0.077(3) 0.046(2) 0.049(2) 0.026(2) 0.024(2) 0.022(2) N13 0.205(7) 0.038(2) 0.090(4) 0.026(3) 0.081(4) 0.023(2) N14 0.080(3) 0.065(3) 0.053(2) 0.040(2) 0.021(2) 0.008(2) C1 0.034(2) 0.023(2) 0.033(2) 0.011(1) 0.005(1) 0.011(1) C2 0.034(2) 0.024(2) 0.029(2) 0.013(1) 0.006(1) 0.009(1) C3 0.036(2) 0.026(2) 0.033(2) 0.011(1) 0.007(2) 0.012(1) C4 0.037(2) 0.029(2) 0.029(2) 0.016(1) 0.005(1) 0.008(1) C5 0.046(2) 0.042(2) 0.035(2) 0.021(2) 0.014(2) 0.017(2) C6 0.053(3) 0.049(2) 0.032(2) 0.028(2) 0.015(2) 0.009(2) C7 0.058(3) 0.041(2) 0.039(2) 0.029(2) 0.012(2) 0.005(2) C8 0.052(2) 0.028(2) 0.043(2) 0.020(2) 0.010(2) 0.009(2) C9 0.036(2) 0.028(2) 0.032(2) 0.015(1) 0.004(1) 0.007(1) C11 0.055(3) 0.036(2) 0.043(2) 0.019(2) 0.009(2) 0.014(2) C12 0.046(2) 0.035(2) 0.038(2) 0.021(2) 0.007(2) 0.010(2) C13 0.109(4) 0.036(2) 0.048(3) 0.026(3) 0.032(3) 0.009(2) C14 0.056(3) 0.040(2) 0.045(2) 0.025(2) 0.008(2) 0.013(2) C15 0.041(2) 0.027(2) 0.038(2) 0.014(2) 0.004(2) 0.011(1) C16 0.037(2) 0.034(2) 0.039(2) 0.015(2) 0.006(2) 0.018(2) C17 0.052(2) 0.034(2) 0.038(2) 0.019(2) 0.010(2) 0.011(2) C18 0.094(4) 0.075(4) 0.091(4) 0.007(3) -0.015(3) 0.057(3) C19 0.132(6) 0.080(4) 0.113(5) 0.025(4) 0.009(5) 0.066(4) C20 0.109(5) 0.095(4) 0.114(5) 0.039(4) 0.016(4) 0.076(4) 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 S1 S2 2.040(2) . . ? S1 C1 1.710(4) . . ? S2 C3 1.709(4) . . ? O11 C16 1.364(5) . . ? O11 C18 1.412(7) . . ? N11 C11 1.139(6) . . ? N12 C12 1.146(6) . . ? N13 C13 1.135(7) . . ? N14 C14 1.139(7) . . ? C1 C2 1.394(5) . . ? C1 C9 1.446(6) . 2_556 ? C2 C2 1.416(5) . 2_556 ? C2 C3 1.388(6) . . ? C3 C4 1.442(5) . . ? C4 C5 1.398(6) . . ? C4 C9 1.437(5) . . ? C5 C6 1.375(6) . . ? C6 C7 1.377(6) . . ? C7 C8 1.372(7) . . ? C8 C9 1.400(6) . . ? C11 C15 1.420(6) . . ? C12 C15 1.411(6) . . ? C13 C17 1.413(7) . . ? C14 C17 1.426(7) . . ? C15 C16 1.410(6) . . ? C16 C17 1.376(6) . . ? C18 C19 1.368(10) . . ? C19 C20 1.429(10) . . ? C5 H5 0.84(4) . . ? C6 H6 0.88(5) . . ? C7 H7 0.92(5) . . ? C8 H8 0.90(5) . . ? C18 H18A 0.960 . . ? C18 H18B 0.960 . . ? C19 H19A 0.960 . . ? C19 H19B 0.960 . . ? C20 H20A 0.960 . . ? C20 H20B 0.960 . . ? C20 H20C 0.960 . . ? 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 S2 S1 C1 96.0(2) . . . ? S1 S2 C3 96.1(2) . . . ? C16 O11 C18 118.6(4) . . . ? S1 C1 C2 114.2(3) . . . ? S1 C1 C9 124.9(3) . . 2_556 ? C2 C1 C9 120.9(3) . . 2_556 ? C1 C2 C2 120.3(3) . . 2_556 ? C1 C2 C3 119.3(3) . . . ? C2 C2 C3 120.5(3) 2_556 . . ? S2 C3 C2 114.4(3) . . . ? S2 C3 C4 124.6(3) . . . ? C2 C3 C4 121.0(3) . . . ? C3 C4 C5 122.1(4) . . . ? C3 C4 C9 118.8(3) . . . ? C5 C4 C9 119.1(4) . . . ? C4 C5 C6 120.0(4) . . . ? C5 C6 C7 120.7(4) . . . ? C6 C7 C8 121.4(4) . . . ? C7 C8 C9 119.9(4) . . . ? C1 C9 C4 118.6(3) 2_556 . . ? C1 C9 C8 122.6(4) 2_556 . . ? C4 C9 C8 118.9(4) . . . ? N11 C11 C15 179.5(5) . . . ? N12 C12 C15 177.1(5) . . . ? N13 C13 C17 176.2(6) . . . ? N14 C14 C17 178.3(5) . . . ? C11 C15 C12 116.8(4) . . . ? C11 C15 C16 118.8(4) . . . ? C12 C15 C16 124.4(4) . . . ? O11 C16 C15 113.1(4) . . . ? O11 C16 C17 118.0(4) . . . ? C15 C16 C17 128.8(4) . . . ? C13 C17 C14 114.6(4) . . . ? C13 C17 C16 124.7(4) . . . ? C14 C17 C16 120.7(4) . . . ? O11 C18 C19 115.7(6) . . . ? C18 C19 C20 123.2(7) . . . ? C4 C5 H5 119.7(26) . . . ? C6 C5 H5 120.2(26) . . . ? C5 C6 H6 119.8(26) . . . ? C7 C6 H6 119.6(26) . . . ? C6 C7 H7 114.8(26) . . . ? C8 C7 H7 123.8(26) . . . ? C7 C8 H8 123.6(25) . . . ? C9 C8 H8 116.5(25) . . . ? O11 C18 H18A 108.5(6) . . . ? O11 C18 H18B 108.6(6) . . . ? C19 C18 H18A 107.6(7) . . . ? C19 C18 H18B 107.2(6) . . . ? H18A C18 H18B 109.0(6) . . . ? C18 C19 H19A 105.6(7) . . . ? C18 C19 H19B 105.7(7) . . . ? C20 C19 H19A 106.6(7) . . . ? C20 C19 H19B 106.2(7) . . . ? H19A C19 H19B 109.0(7) . . . ? C19 C20 H20A 119.5(7) . . . ? C19 C20 H20B 106.6(7) . . . ? C19 C20 H20C 106.2(7) . . . ? H20A C20 H20B 107.6(7) . . . ? H20A C20 H20C 107.6(7) . . . ? H20B C20 H20C 109.0(7) . . . ? 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 S1 N11 3.202(4) 1_555 2_666 ? S1 N12 2.988(4) 1_555 1_565 ? S2 N12 2.886(4) 1_555 1_565 ? S2 N13 3.117(6) 1_555 1_565 ? C2 C11 3.385(5) 1_555 1_455 ? C2 C12 3.400(5) 1_555 2_656 ? H20B H20B 2.2081 1_555 2_655 ? H6 N14 2.70(4) 1_555 2_645 ? #=================================================== #===END #------------------------------------------------------------------------------ data_(TTT)3(PrO-TCA)2 _database_code_CSD 165352 #------------------------------------------------------------------------------ _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _chemical_formula_moiety '2(C18 H8 S4 1+),C18 H8 S4,2(C10 H7 N4 O1 1-)' _chemical_formula_sum 'C74 H38 N8 O2 S12 ' _chemical_formula_weight 1455.96 _cell_length_a 10.357(3) _cell_length_b 12.243(8) _cell_length_c 14.085(9) _cell_angle_alpha 74.74(5) _cell_angle_beta 69.26(4) _cell_angle_gamma 73.11(4) _cell_volume 1573(2) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '??' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_meas 1.557 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.559 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3-chi' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 7908 _reflns_number_total 7220 _reflns_number_observed 3337 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _refine_ls_structure_factor_coef ? _refine_ls_R_factor_obs 0.050 _refine_ls_wR_factor_obs 0.048 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_number_reflns 3337 _refine_ls_number_parameters 489 _refine_ls_goodness_of_fit_obs 2.104 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0111 _refine_ls_shift/esd_mean 0.0017 _refine_diff_density_min -0.47 _refine_diff_density_max 0.54 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P-1' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type S1 0.18837(17) 0.31230(13) 0.15806(11) 0.0405(8) 1.000 Uij S2 0.29604(17) 0.17528(12) 0.07992(11) 0.0401(8) 1.000 Uij S3 0.28836(18) 0.51090(13) -0.33963(11) 0.0439(8) 1.000 Uij S4 0.17673(17) 0.64675(12) -0.26105(12) 0.0424(8) 1.000 Uij S21 0.44847(18) 0.40909(14) 0.25171(11) 0.0453(9) 1.000 Uij S22 0.55811(18) 0.26751(13) 0.17708(12) 0.0437(8) 1.000 Uij O31 0.0919(5) 0.1190(3) 0.5500(3) 0.051(2) 1.000 Uij N31 0.1359(7) 0.0051(5) 0.8121(4) 0.068(4) 1.000 Uij N32 0.4800(7) -0.1844(6) 0.5867(4) 0.077(4) 1.000 Uij N33 0.2515(7) -0.2639(5) 0.4940(5) 0.067(3) 1.000 Uij N34 0.1378(7) 0.0790(5) 0.3052(4) 0.065(3) 1.000 Uij C1 0.1851(6) 0.4183(4) 0.0487(4) 0.032(3) 1.000 Uij C2 0.2466(6) 0.3740(5) -0.0435(4) 0.032(3) 1.000 Uij C3 0.3059(6) 0.2571(5) -0.0425(4) 0.033(3) 1.000 Uij C4 0.3636(6) 0.2099(5) -0.1344(4) 0.035(3) 1.000 Uij C5 0.4236(6) 0.0905(5) -0.1360(5) 0.040(3) 1.000 Uij C6 0.4724(7) 0.0483(6) -0.2244(5) 0.047(3) 1.000 Uij C7 0.4663(7) 0.1217(6) -0.3181(5) 0.048(3) 1.000 Uij C8 0.4115(7) 0.2385(5) -0.3215(5) 0.043(3) 1.000 Uij C9 0.3593(6) 0.2865(5) -0.2309(4) 0.033(3) 1.000 Uij C10 0.2993(6) 0.4074(5) -0.2305(4) 0.034(3) 1.000 Uij C11 0.2441(6) 0.4503(5) -0.1390(4) 0.032(3) 1.000 Uij C12 0.1796(6) 0.5677(5) -0.1400(4) 0.036(3) 1.000 Uij C13 0.1189(6) 0.6143(5) -0.0473(4) 0.034(3) 1.000 Uij C14 0.0576(7) 0.7334(5) -0.0474(6) 0.044(3) 1.000 Uij C15 -0.0003(7) 0.7745(5) 0.0437(5) 0.050(3) 1.000 Uij C16 0.0021(7) 0.7005(6) 0.1376(5) 0.051(4) 1.000 Uij C17 0.0622(6) 0.5856(6) 0.1402(5) 0.043(3) 1.000 Uij C18 0.1231(6) 0.5379(5) 0.0487(5) 0.035(3) 1.000 Uij C21 0.4393(6) 0.5107(5) 0.1385(4) 0.035(3) 1.000 Uij C22 0.5010(6) 0.4632(5) 0.0480(4) 0.032(3) 1.000 Uij C23 0.5646(6) 0.3449(5) 0.0519(4) 0.035(3) 1.000 Uij C24 0.6262(6) 0.2964(5) -0.0373(4) 0.035(3) 1.000 Uij C25 0.6948(7) 0.1775(5) -0.0362(5) 0.044(3) 1.000 Uij C26 0.7546(8) 0.1342(6) -0.1248(6) 0.055(4) 1.000 Uij C27 0.7500(8) 0.2046(6) -0.2202(6) 0.055(4) 1.000 Uij C28 0.6879(7) 0.3189(6) -0.2269(5) 0.048(4) 1.000 Uij C29 0.6238(6) 0.3701(5) -0.1362(4) 0.037(3) 1.000 Uij C31 0.1825(7) -0.0133(5) 0.7303(5) 0.050(3) 1.000 Uij C32 0.3714(7) -0.1217(6) 0.6072(4) 0.052(3) 1.000 Uij C33 0.2252(7) -0.1650(5) 0.4831(4) 0.046(3) 1.000 Uij C34 0.1588(7) 0.0251(5) 0.3799(4) 0.045(3) 1.000 Uij C35 0.2423(6) -0.0399(5) 0.6295(4) 0.047(3) 1.000 Uij C36 0.1760(6) 0.0123(5) 0.5510(4) 0.040(3) 1.000 Uij C37 0.1896(6) -0.0415(5) 0.4721(4) 0.041(3) 1.000 Uij C38 0.1285(13) 0.2080(7) 0.5805(8) 0.078(6) 1.000 Uij C39 0.090(2) 0.316(1) 0.524(1) 0.25(1) 1.000 Uij C40 0.0822(14) 0.3524(9) 0.4333(9) 0.133(9) 1.000 Uij H5 0.422(5) 0.050(4) -0.076(3) 0.01(1) 1.000 Uiso H6 0.508(7) -0.029(6) -0.228(5) 0.07(2) 1.000 Uiso H7 0.496(7) 0.093(6) -0.381(5) 0.06(2) 1.000 Uiso H8 0.416(5) 0.288(4) -0.385(4) 0.02(1) 1.000 Uiso H14 0.058(7) 0.787(5) -0.105(5) 0.06(2) 1.000 Uiso H15 -0.040(5) 0.848(5) 0.043(4) 0.03(1) 1.000 Uiso H16 -0.036(5) 0.727(4) 0.202(4) 0.03(1) 1.000 Uiso H17 0.060(5) 0.536(4) 0.204(4) 0.03(1) 1.000 Uiso H25 0.702(5) 0.127(4) 0.031(4) 0.02(1) 1.000 Uiso H26 0.800(7) 0.061(6) -0.126(5) 0.06(2) 1.000 Uiso H27 0.792(6) 0.177(5) -0.281(4) 0.04(2) 1.000 Uiso H28 0.682(7) 0.373(6) -0.295(5) 0.07(2) 1.000 Uiso H38A 0.224(9) 0.193(7) 0.563(7) 0.09(3) 1.000 Uiso H38B 0.077(12) 0.205(9) 0.651(9) 0.15(5) 1.000 Uiso H39A 0.13825 0.36472 0.53563 0.050 1.000 Uiso H39B -0.00875 0.33502 0.56133 0.050 1.000 Uiso H40A 0.05742 0.42887 0.39546 0.050 1.000 Uiso H40B 0.01512 0.31227 0.43326 0.050 1.000 Uiso H40C 0.17432 0.31957 0.39146 0.050 1.000 Uiso 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 S1 0.043(1) 0.039(1) 0.028(1) -0.003(1) -0.014(1) -0.001(1) S2 0.045(1) 0.030(1) 0.033(1) -0.001(1) -0.016(1) 0.001(1) S3 0.055(1) 0.036(1) 0.027(1) -0.005(1) -0.012(1) 0.001(1) S4 0.048(1) 0.029(1) 0.037(1) -0.002(1) -0.016(1) 0.002(1) S21 0.050(1) 0.042(1) 0.031(1) -0.006(1) -0.014(1) -0.002(1) S22 0.050(1) 0.034(1) 0.036(1) -0.008(1) -0.019(1) 0.002(1) O31 0.054(3) 0.035(2) 0.053(3) -0.001(2) -0.026(2) -0.011(2) N31 0.079(5) 0.065(4) 0.044(3) -0.005(3) -0.022(3) -0.015(3) N32 0.061(4) 0.097(5) 0.043(3) 0.019(4) -0.021(3) -0.004(3) N33 0.082(5) 0.040(3) 0.061(4) -0.006(3) -0.030(3) -0.001(3) N34 0.089(5) 0.047(3) 0.037(3) -0.008(3) -0.021(3) 0.004(2) C1 0.028(3) 0.032(3) 0.028(3) -0.006(2) -0.012(2) -0.002(2) C2 0.031(3) 0.027(3) 0.029(3) -0.007(2) -0.011(2) -0.002(2) C3 0.028(3) 0.030(3) 0.032(3) -0.003(2) -0.012(2) -0.002(2) C4 0.027(3) 0.036(3) 0.035(3) -0.005(2) -0.011(2) -0.004(2) C5 0.036(4) 0.031(3) 0.041(4) -0.004(3) -0.017(3) 0.001(3) C6 0.042(4) 0.038(3) 0.046(4) -0.001(3) -0.007(3) -0.014(3) C7 0.042(4) 0.047(4) 0.045(4) -0.002(3) -0.009(3) -0.023(3) C8 0.042(4) 0.038(3) 0.036(3) -0.004(3) -0.011(3) -0.005(3) C9 0.031(3) 0.032(3) 0.027(3) -0.008(2) -0.008(2) -0.003(2) C10 0.034(3) 0.029(3) 0.031(3) -0.006(2) -0.010(2) 0.001(2) C11 0.027(3) 0.032(3) 0.030(3) -0.008(2) -0.007(2) -0.004(2) C12 0.033(3) 0.029(3) 0.038(3) -0.009(2) -0.015(3) 0.000(2) C13 0.029(3) 0.027(3) 0.038(3) -0.007(2) -0.011(3) -0.004(2) C14 0.038(3) 0.026(3) 0.058(4) -0.007(3) -0.017(3) -0.007(3) C15 0.042(4) 0.031(3) 0.067(4) 0.000(3) -0.019(3) -0.023(3) C16 0.040(4) 0.056(4) 0.049(4) -0.009(3) -0.011(3) -0.026(3) C17 0.030(3) 0.054(4) 0.037(3) -0.011(3) -0.009(3) -0.014(3) C18 0.026(3) 0.034(3) 0.037(3) -0.005(2) -0.010(2) -0.009(2) C21 0.031(3) 0.037(3) 0.029(3) -0.010(3) -0.008(3) -0.004(2) C22 0.028(3) 0.027(3) 0.032(3) -0.006(2) -0.009(2) -0.004(2) C23 0.032(3) 0.031(3) 0.035(3) -0.011(2) -0.019(3) 0.004(2) C24 0.033(3) 0.031(3) 0.035(3) -0.007(3) -0.014(3) -0.003(2) C25 0.039(4) 0.035(3) 0.047(4) -0.012(3) -0.013(3) -0.002(3) C26 0.045(4) 0.034(3) 0.071(5) -0.004(3) -0.015(4) -0.020(3) C27 0.052(4) 0.051(4) 0.051(4) -0.009(3) -0.008(3) -0.026(3) C28 0.045(4) 0.049(4) 0.041(4) -0.008(3) -0.013(3) -0.017(3) C29 0.028(3) 0.036(3) 0.042(3) -0.007(3) -0.011(3) -0.014(3) C31 0.051(4) 0.046(4) 0.039(3) -0.006(3) -0.019(3) -0.002(3) C32 0.051(4) 0.058(4) 0.032(3) -0.002(3) -0.019(3) 0.001(3) C33 0.051(4) 0.043(3) 0.033(3) -0.007(3) -0.016(3) -0.002(3) C34 0.051(4) 0.036(3) 0.033(3) -0.009(3) -0.005(3) -0.005(2) C35 0.044(4) 0.047(3) 0.036(3) 0.000(3) -0.017(3) -0.006(3) C36 0.034(3) 0.037(3) 0.038(3) -0.005(2) -0.010(3) -0.003(2) C37 0.040(3) 0.039(3) 0.033(3) -0.005(3) -0.013(3) -0.002(2) C38 0.103(8) 0.045(4) 0.074(6) -0.017(5) -0.047(6) -0.009(4) C39 0.40(3) 0.06(1) 0.26(2) -0.05(1) -0.28(2) 0.03(1) C40 0.16(1) 0.09(1) 0.10(1) -0.04(1) -0.02(1) 0.02(1) 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 S1 S2 2.070(2) . . ? S1 C1 1.736(6) . . ? S2 C3 1.736(6) . . ? S3 S4 2.067(3) . . ? S3 C10 1.731(6) . . ? S4 C12 1.731(6) . . ? S21 S22 2.090(3) . . ? S21 C21 1.758(6) . . ? S22 C23 1.757(6) . . ? O31 C36 1.342(8) . . ? O31 C38 1.456(9) . . ? N31 C31 1.136(9) . . ? N32 C32 1.150(10) . . ? N33 C33 1.142(9) . . ? N34 C34 1.141(8) . . ? C1 C2 1.404(8) . . ? C1 C18 1.418(8) . . ? C2 C3 1.382(8) . . ? C2 C11 1.425(8) . . ? C3 C4 1.419(8) . . ? C4 C5 1.415(8) . . ? C4 C9 1.441(8) . . ? C5 C6 1.347(9) . . ? C6 C7 1.398(10) . . ? C7 C8 1.372(9) . . ? C8 C9 1.410(8) . . ? C9 C10 1.430(8) . . ? C10 C11 1.386(7) . . ? C11 C12 1.397(8) . . ? C12 C13 1.424(8) . . ? C13 C14 1.411(8) . . ? C13 C18 1.434(9) . . ? C14 C15 1.371(10) . . ? C15 C16 1.396(10) . . ? C16 C17 1.359(10) . . ? C17 C18 1.417(9) . . ? C21 C22 1.403(8) . . ? C21 C29 1.413(8) . 2_655 ? C22 C22 1.416(8) . 2_655 ? C22 C23 1.401(8) . . ? C23 C24 1.394(8) . . ? C24 C25 1.421(9) . . ? C24 C29 1.452(8) . . ? C25 C26 1.353(10) . . ? C26 C27 1.401(11) . . ? C27 C28 1.353(10) . . ? C28 C29 1.429(9) . . ? C31 C35 1.418(9) . . ? C32 C35 1.408(10) . . ? C33 C37 1.428(9) . . ? C34 C37 1.427(8) . . ? C35 C36 1.419(8) . . ? C36 C37 1.382(7) . . ? C38 C39 1.377(17) . . ? C39 C40 1.26(3) . . ? C5 H5 0.86(5) . . ? C6 H6 0.91(7) . . ? C7 H7 0.95(7) . . ? C8 H8 0.94(6) . . ? C14 H14 0.90(7) . . ? C15 H15 0.88(6) . . ? C16 H16 0.95(6) . . ? C17 H17 0.94(6) . . ? C25 H25 1.00(5) . . ? C26 H26 0.88(7) . . ? C27 H27 0.91(6) . . ? C28 H28 1.03(8) . . ? C38 H38A 0.91(9) . . ? C38 H38B 0.94(12) . . ? C39 H39A 0.960 . . ? C39 H39B 0.960 . . ? C40 H40A 0.960 . . ? C40 H40B 0.960 . . ? C40 H40C 0.960 . . ? 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 S2 S1 C1 96.0(2) . . . ? S1 S2 C3 95.7(2) . . . ? S4 S3 C10 95.4(2) . . . ? S3 S4 C12 95.8(2) . . . ? S22 S21 C21 95.5(2) . . . ? S21 S22 C23 95.9(2) . . . ? C36 O31 C38 119.6(6) . . . ? S1 C1 C2 113.3(4) . . . ? S1 C1 C18 125.3(5) . . . ? C2 C1 C18 121.3(5) . . . ? C1 C2 C3 120.8(5) . . . ? C1 C2 C11 119.4(5) . . . ? C3 C2 C11 119.7(5) . . . ? S2 C3 C2 114.1(4) . . . ? S2 C3 C4 124.1(4) . . . ? C2 C3 C4 121.7(5) . . . ? C3 C4 C5 123.2(6) . . . ? C3 C4 C9 118.7(5) . . . ? C5 C4 C9 118.1(5) . . . ? C4 C5 C6 121.4(6) . . . ? C5 C6 C7 120.9(6) . . . ? C6 C7 C8 120.3(6) . . . ? C7 C8 C9 120.8(6) . . . ? C4 C9 C8 118.5(5) . . . ? C4 C9 C10 118.7(5) . . . ? C8 C9 C10 122.8(5) . . . ? S3 C10 C9 124.4(4) . . . ? S3 C10 C11 114.6(4) . . . ? C9 C10 C11 120.9(5) . . . ? C2 C11 C10 120.2(5) . . . ? C2 C11 C12 119.9(5) . . . ? C10 C11 C12 119.8(5) . . . ? S4 C12 C11 114.1(5) . . . ? S4 C12 C13 124.4(5) . . . ? C11 C12 C13 121.4(5) . . . ? C12 C13 C14 122.1(6) . . . ? C12 C13 C18 118.8(5) . . . ? C14 C13 C18 119.2(6) . . . ? C13 C14 C15 120.1(6) . . . ? C14 C15 C16 121.0(6) . . . ? C15 C16 C17 120.4(7) . . . ? C16 C17 C18 121.2(6) . . . ? C1 C18 C13 119.2(6) . . . ? C1 C18 C17 122.7(6) . . . ? C13 C18 C17 118.1(6) . . . ? S21 C21 C22 114.1(5) . . . ? S21 C21 C29 124.3(5) . . 2_655 ? C22 C21 C29 121.7(5) . . 2_655 ? C21 C22 C22 119.1(5) . . 2_655 ? C21 C22 C23 120.7(5) . . . ? C22 C22 C23 120.2(5) 2_655 . . ? S22 C23 C22 113.9(4) . . . ? S22 C23 C24 124.7(5) . . . ? C22 C23 C24 121.5(5) . . . ? C23 C24 C25 122.8(6) . . . ? C23 C24 C29 119.2(5) . . . ? C25 C24 C29 118.0(6) . . . ? C24 C25 C26 120.9(6) . . . ? C25 C26 C27 121.3(7) . . . ? C26 C27 C28 120.9(7) . . . ? C27 C28 C29 120.6(7) . . . ? C21 C29 C24 118.4(5) 2_655 . . ? C21 C29 C28 123.2(6) 2_655 . . ? C24 C29 C28 118.4(5) . . . ? N31 C31 C35 178.2(7) . . . ? N32 C32 C35 176.9(7) . . . ? N33 C33 C37 178.5(7) . . . ? N34 C34 C37 178.1(7) . . . ? C31 C35 C32 118.5(6) . . . ? C31 C35 C36 122.3(6) . . . ? C32 C35 C36 119.1(6) . . . ? O31 C36 C35 121.3(5) . . . ? O31 C36 C37 115.0(5) . . . ? C35 C36 C37 123.7(6) . . . ? C33 C37 C34 118.2(5) . . . ? C33 C37 C36 121.2(5) . . . ? C34 C37 C36 120.5(6) . . . ? O31 C38 C39 111.0(11) . . . ? C38 C39 C40 134.7(13) . . . ? C4 C5 H5 113.1(30) . . . ? C6 C5 H5 125.4(31) . . . ? C5 C6 H6 123.9(43) . . . ? C7 C6 H6 115.1(43) . . . ? C6 C7 H7 122.2(39) . . . ? C8 C7 H7 117.5(39) . . . ? C7 C8 H8 120.2(30) . . . ? C9 C8 H8 118.8(30) . . . ? C13 C14 H14 124.0(40) . . . ? C15 C14 H14 115.8(40) . . . ? C14 C15 H15 119.5(34) . . . ? C16 C15 H15 119.5(34) . . . ? C15 C16 H16 123.0(32) . . . ? C17 C16 H16 116.6(32) . . . ? C16 C17 H17 119.9(31) . . . ? C18 C17 H17 118.8(31) . . . ? C24 C25 H25 118.3(28) . . . ? C26 C25 H25 120.7(28) . . . ? C25 C26 H26 121.9(44) . . . ? C27 C26 H26 116.8(44) . . . ? C26 C27 H27 122.1(36) . . . ? C28 C27 H27 116.9(36) . . . ? C27 C28 H28 123.2(38) . . . ? C29 C28 H28 116.3(38) . . . ? O31 C38 H38A 107.1(52) . . . ? O31 C38 H38B 104.6(65) . . . ? C39 C38 H38A 105.5(54) . . . ? C39 C38 H38B 111.1(66) . . . ? H38A C38 H38B 117.5(84) . . . ? C38 C39 H39A 105.4(16) . . . ? C38 C39 H39B 100.0(14) . . . ? C40 C39 H39A 106.4(14) . . . ? C40 C39 H39B 99.1(16) . . . ? H39A C39 H39B 109.0(13) . . . ? C39 C40 H40A 132.6(12) . . . ? C39 C40 H40B 101.2(13) . . . ? C39 C40 H40C 103.4(13) . . . ? H40A C40 H40B 104.7(12) . . . ? H40A C40 H40C 104.7(11) . . . ? H40B C40 H40C 109.0(11) . . . ? 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 S1 S4 3.472(2) 1_555 2_565 ? S3 N33 3.139(6) 1_555 1_564 ? S4 N33 3.211(6) 1_555 1_564 ? S21 N32 3.164(7) 1_555 2_656 ? S22 N32 3.127(6) 1_555 2_656 ? S22 C32 3.303(6) 1_555 2_656 ? C1 C13 3.293(7) 1_555 2_565 ? C3 C15 3.305(8) 1_555 2_565 ? C7 C33 3.311(9) 1_555 2_655 ? C11 C17 3.333(7) 1_555 2_565 ? C15 C25 3.343(8) 1_555 2_665 ? H16 H38B 2.3(1) 1_555 2_566 ? S1 N34 3.117(6) 1_555 1_555 ? S2 N34 3.102(6) 1_555 1_555 ? #=================================================== #===END