#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/48/2204866.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204866 loop_ _publ_author_name 'Lei Wang' 'Jing-Ping Zhang' 'Bin Zhang' _publ_section_title ; 4,4',5,5'-Tetrakis(methylsulfanyl)tetrathiafulvalene ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o65 _journal_page_last o66 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C10 H12 S8' _chemical_formula_moiety 'C10 H12 S8' _chemical_formula_sum 'C10 H12 S8' _chemical_formula_weight 388.68 _chemical_name_systematic ; 4,4',5,5'-Tetrakis(methylsulfanyl)tetrathiafulvalene ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 106.2130(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.0010(2) _cell_length_b 7.08110(10) _cell_length_c 15.6584(3) _cell_measurement_reflns_used 19853 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 3.395 _cell_volume 1490.67(4) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1997--2000)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) and Scalepack' _computing_molecular_graphics 'XP (Bruker, 1998)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f or \w scans?' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 33274 _diffrn_reflns_theta_full 27.87 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_min 3.46 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_T_max 0.7421 _exptl_absorpt_correction_T_min 0.6199 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _refine_diff_density_max 0.375 _refine_diff_density_min -0.381 _refine_ls_extinction_coef 0.0134(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 3521 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0309 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.2485P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.0793 _reflns_number_gt 2515 _reflns_number_total 3521 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cv6415.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2204866 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S1 0.38160(4) 0.56949(8) 0.17051(4) 0.04475(16) Uani d . 1 S S2 0.49020(4) 0.25570(8) 0.24089(4) 0.04678(16) Uani d . 1 S S3 0.26402(4) 0.54055(9) 0.32811(4) 0.04963(17) Uani d . 1 S S4 0.38388(5) 0.23792(9) 0.39745(4) 0.05367(18) Uani d . 1 S S5 0.52939(5) 0.67385(8) 0.07204(4) 0.04526(16) Uani d . 1 S S6 0.64932(4) 0.31553(8) 0.14828(4) 0.04037(15) Uani d . 1 S S7 0.22441(5) 0.62280(10) 0.50320(5) 0.0624(2) Uani d . 1 S S8 0.36593(6) 0.28489(13) 0.58361(5) 0.0795(3) Uani d . 1 S C1 0.40249(14) 0.4084(3) 0.25144(14) 0.0378(5) Uani d . 1 C C2 0.35611(15) 0.3986(3) 0.31602(14) 0.0401(5) Uani d . 1 C C3 0.49566(14) 0.5341(3) 0.14575(13) 0.0343(4) Uani d . 1 C C4 0.54498(14) 0.3898(3) 0.17754(13) 0.0337(4) Uani d . 1 C C5 0.28543(17) 0.4968(3) 0.44257(16) 0.0471(6) Uani d . 1 C C6 0.34107(18) 0.3592(3) 0.47454(16) 0.0488(6) Uani d . 1 C C7 0.5099(2) 0.8795(3) 0.1168(2) 0.0719(8) Uani d . 1 C H7A 0.5257 0.9816 0.0828 0.108 Uiso calc R 1 H H7B 0.5515 0.8868 0.1769 0.108 Uiso calc R 1 H H7C 0.4414 0.8881 0.1165 0.108 Uiso calc R 1 H C8 0.7274(2) 0.2473(4) 0.25400(17) 0.0679(8) Uani d . 1 C H8A 0.7896 0.2017 0.2475 0.102 Uiso calc R 1 H H8B 0.6956 0.1491 0.2783 0.102 Uiso calc R 1 H H8C 0.7392 0.3542 0.2933 0.102 Uiso calc R 1 H C9 0.2912(2) 0.8203(4) 0.51300(18) 0.0623(7) Uani d . 1 C H9A 0.2666 0.9111 0.5471 0.093 Uiso calc R 1 H H9B 0.2860 0.8707 0.4550 0.093 Uiso calc R 1 H H9C 0.3596 0.7928 0.5425 0.093 Uiso calc R 1 H C10 0.4884(2) 0.2056(5) 0.6073(2) 0.0779(9) Uani d . 1 C H10A 0.5096 0.1598 0.6674 0.117 Uiso calc R 1 H H10B 0.5307 0.3078 0.6004 0.117 Uiso calc R 1 H H10C 0.4925 0.1054 0.5672 0.117 Uiso calc R 1 H 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 0.0437(3) 0.0421(3) 0.0525(3) 0.0093(2) 0.0202(3) 0.0021(2) S2 0.0585(3) 0.0299(3) 0.0651(4) 0.0054(2) 0.0390(3) 0.0040(2) S3 0.0465(3) 0.0511(3) 0.0575(4) 0.0088(3) 0.0248(3) -0.0046(3) S4 0.0653(4) 0.0432(3) 0.0662(4) 0.0076(3) 0.0411(3) 0.0051(3) S5 0.0624(4) 0.0347(3) 0.0429(3) 0.0007(3) 0.0217(3) 0.0032(2) S6 0.0422(3) 0.0404(3) 0.0438(3) 0.0065(2) 0.0208(2) 0.0011(2) S7 0.0638(4) 0.0603(4) 0.0789(5) -0.0079(3) 0.0461(4) -0.0244(3) S8 0.0858(5) 0.1014(6) 0.0674(5) 0.0096(4) 0.0482(4) 0.0213(4) C1 0.0397(11) 0.0308(10) 0.0473(12) -0.0001(8) 0.0191(10) -0.0047(9) C2 0.0407(11) 0.0344(11) 0.0508(13) -0.0006(9) 0.0219(10) -0.0053(9) C3 0.0397(11) 0.0305(10) 0.0351(11) -0.0007(8) 0.0142(9) -0.0025(8) C4 0.0392(10) 0.0292(10) 0.0365(11) -0.0009(8) 0.0170(9) -0.0024(8) C5 0.0480(13) 0.0458(13) 0.0576(14) -0.0058(11) 0.0313(11) -0.0117(11) C6 0.0544(13) 0.0493(14) 0.0538(14) -0.0067(11) 0.0334(11) -0.0038(11) C7 0.094(2) 0.0278(12) 0.107(2) 0.0068(13) 0.0500(18) 0.0045(13) C8 0.0572(16) 0.088(2) 0.0592(16) 0.0287(14) 0.0177(13) 0.0160(15) C9 0.0762(18) 0.0428(14) 0.0710(17) 0.0024(13) 0.0260(15) -0.0058(12) C10 0.084(2) 0.083(2) 0.0621(17) 0.0021(17) 0.0126(16) 0.0018(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 C1 1.669(2) yes S1 C3 1.763(2) yes S2 C1 1.678(2) yes S2 C4 1.703(2) yes S3 C2 1.687(2) yes S3 C5 1.760(2) yes S4 C2 1.672(2) yes S4 C6 1.720(2) yes S5 C7 1.671(2) yes S5 C3 1.6849(19) yes S6 C4 1.7305(19) yes S6 C8 1.777(3) yes S7 C9 1.665(3) yes S7 C5 1.697(2) yes S8 C6 1.727(2) yes S8 C10 1.743(3) yes C1 C2 1.348(3) yes C3 C4 1.255(3) yes C5 C6 1.261(3) yes C7 H7A 0.9600 no C7 H7B 0.9600 no C7 H7C 0.9600 no C8 H8A 0.9600 no C8 H8B 0.9600 no C8 H8C 0.9600 no C9 H9A 0.9600 no C9 H9B 0.9600 no C9 H9C 0.9600 no C10 H10A 0.9600 no C10 H10B 0.9600 no C10 H10C 0.9600 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C1 S1 C3 95.30(9) yes C1 S2 C4 99.15(10) yes C2 S3 C5 95.23(11) yes C2 S4 C6 98.23(11) yes C7 S5 C3 96.58(12) yes C4 S6 C8 100.45(11) yes C9 S7 C5 97.78(12) yes C6 S8 C10 102.90(13) yes C2 C1 S1 125.86(16) yes C2 C1 S2 124.06(17) yes S1 C1 S2 110.09(12) yes C1 C2 S4 123.30(16) yes C1 C2 S3 126.68(17) yes S4 C2 S3 110.02(12) yes C4 C3 S5 121.42(16) yes C4 C3 S1 117.39(16) yes S5 C3 S1 120.75(11) yes C3 C4 S2 113.43(16) yes C3 C4 S6 123.64(16) yes S2 C4 S6 122.38(12) yes C6 C5 S7 122.4(2) yes C6 C5 S3 116.81(18) yes S7 C5 S3 120.52(15) yes C5 C6 S4 113.89(19) yes C5 C6 S8 124.03(19) yes S4 C6 S8 121.91(15) yes S5 C7 H7A 109.5 no S5 C7 H7B 109.5 no H7A C7 H7B 109.5 no S5 C7 H7C 109.5 no H7A C7 H7C 109.5 no H7B C7 H7C 109.5 no S6 C8 H8A 109.5 no S6 C8 H8B 109.5 no H8A C8 H8B 109.5 no S6 C8 H8C 109.5 no H8A C8 H8C 109.5 no H8B C8 H8C 109.5 no S7 C9 H9A 109.5 no S7 C9 H9B 109.5 no H9A C9 H9B 109.5 no S7 C9 H9C 109.5 no H9A C9 H9C 109.5 no H9B C9 H9C 109.5 no S8 C10 H10A 109.5 no S8 C10 H10B 109.5 no H10A C10 H10B 109.5 no S8 C10 H10C 109.5 no H10A C10 H10C 109.5 no H10B C10 H10C 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C7 H7A S6 1_565 0.96 2.94 3.612(3) 128 no C9 H9A S8 1_565 0.96 2.97 3.535(3) 119 no C9 H9B S1 2 0.96 2.96 3.653(3) 130 no C10 H10C S4 3_656 0.96 2.95 3.625(3) 129 no C10 H10B S3 3_666 0.96 2.98 3.783(3) 142 no C10 H10B C2 3_666 0.96 2.72 3.546(4) 145 no _cod_database_fobs_code 2204866 _journal_paper_doi 10.1107/S1600536804031769