#------------------------------------------------------------------------------ #$Date: 2010-01-30 14:59:17 +0100 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003389.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003389 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 690 _journal_page_last 697 _publ_section_title ; Five 3,3'-Bridged 2,2'-Dithiophenes ; _chemical_formula_sum 'C13 H14 O2 S2' _chemical_formula_weight 266.37 _cell_length_a 7.643(2) _cell_length_b 24.604(3) _cell_length_c 7.767(1) _cell_angle_alpha 90.00 _cell_angle_beta 115.29(2) _cell_angle_gamma 90.00 _cell_volume 1320.59(47) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.3398 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.70930 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 16.9 _exptl_absorpt_coefficient_mu 0.3736 _cell_measurement_temperature 'room temperature' _exptl_crystal_description ; Prism ; _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_colour 'yellow--brown' _chemical_compound_source ; chemical synthesis (Sannicol\'o, 1994). ; _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\q/2\q scan' _exptl_absorpt_correction_type '?' _exptl_absorpt_correction_t_min '?' _exptl_absorpt_correction_t_max '?' _diffrn_reflns_number 3017 _reflns_number_total 3017 _reflns_number_observed 2344 _reflns_observed_criterion 'I~o~ > 2\s(I~o~)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 1 _diffrn_standards_interval_time 360 _diffrn_standards_decay_% 'negligible' _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs 0.032 _refine_ls_wR_factor_obs 0.038 _refine_ls_goodness_of_fit_obs 2.097 _refine_ls_number_reflns 2344 _refine_ls_number_parameters 211 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme ;w = 2F~o~Lp/[\s^2^(I~o~) + (0.02I~o~)^2^]^1/2^ ; _refine_ls_shift/esd_max 0.00 _refine_diff_density_max 0.14 _refine_diff_density_min -0.15 _refine_ls_extinction_method 'Stout & Jensen (1968) ' _refine_ls_extinction_coef 1.47(7)x10^-6^ _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag S Sulphur ;International Tables for X-ray Crystallography (1974, Vol. IV, Tables 2.2A, 2.3.1 and 2.2C) ; 0.110 0.124 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv S1 0.10207(5) 0.35739(2) -0.13381(5) 0.0568(1) S7 -0.22889(5) 0.35134(2) 0.15004(6) 0.0619(2) O12 0.3455(1) 0.44319(4) 0.3387(1) 0.0529(3) O16 0.3201(2) 0.32357(4) 0.5110(1) 0.0582(3) C2 0.2629(2) 0.30620(7) -0.1020(2) 0.0608(5) C3 0.3114(2) 0.28112(6) 0.0658(2) 0.0547(5) C4 0.2177(2) 0.30267(5) 0.1744(2) 0.0422(4) C5 0.0981(2) 0.34495(5) 0.0837(2) 0.0410(4) C6 -0.0244(2) 0.37871(6) 0.1425(2) 0.0443(4) C8 -0.2887(2) 0.41224(8) 0.2148(2) 0.0752(7) C9 -0.1592(2) 0.45076(7) 0.2317(2) 0.0697(6) C10 -0.0049(2) 0.43231(6) 0.1908(2) 0.0516(5) C11 0.1666(2) 0.46608(6) 0.2111(2) 0.0604(5) C13 0.3663(2) 0.43828(7) 0.5298(2) 0.0611(5) C14 0.5291(3) 0.39985(8) 0.6358(2) 0.0729(7) C15 0.5037(2) 0.34511(7) 0.5421(2) 0.0615(6) C17 0.2531(2) 0.28245(6) 0.3689(2) 0.0530(5) H2 0.3130(20) 0.3003(6) -0.1930(20) 0.292(20) H3 0.4040(20) 0.2496(7) 0.1160(20) 0.339(23) H8 -0.3970(20) 0.4157(7) 0.2260(20) 0.376(24) H9 -0.1600(20) 0.4858(7) 0.2730(20) 0.336(22) H111 0.1800(20) 0.4697(7) 0.0920(20) 0.324(21) H112 0.1500(20) 0.4997(7) 0.2530(20) 0.317(21) H131 0.3870(20) 0.4738(7) 0.5850(20) 0.295(20) H132 0.2450(20) 0.4252(6) 0.5280(20) 0.245(18) H141 0.6550(20) 0.4144(7) 0.6450(20) 0.343(22) H142 0.5480(30) 0.3944(8) 0.7660(20) 0.432(27) H151 0.5040(20) 0.3480(6) 0.4140(20) 0.245(19) H152 0.6100(20) 0.3196(7) 0.6220(20) 0.312(21) H171 0.3430(20) 0.2533(6) 0.4000(20) 0.269(19) H172 0.1380(20) 0.2711(6) 0.3740(20) 0.234(18) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 S1 0.0562(2) -0.0026(2) 0.0229(1) 0.0754(3) 0.0060(2) 0.0411(1) S7 0.0447(1) -0.0043(2) 0.0324(1) 0.0770(3) 0.0060(2) 0.0719(2) O12 0.0504(4) 0.0004(4) 0.0286(3) 0.0491(6) 0.0024(4) 0.0636(5) O16 0.0727(5) -0.0106(5) 0.0268(3) 0.0592(6) 0.0026(4) 0.0445(4) C2 0.0597(7) -0.0105(7) 0.0367(4) 0.0761(9) -0.0165(7) 0.0586(6) C3 0.0486(6) -0.0022(6) 0.0290(5) 0.0531(9) -0.0102(7) 0.0668(7) C4 0.0415(6) -0.0043(6) 0.0188(4) 0.0402(6) -0.0030(5) 0.0450(5) C5 0.0389(5) -0.0054(5) 0.0181(4) 0.0469(6) -0.0006(5) 0.0388(5) C6 0.0369(5) 0.0026(6) 0.0197(4) 0.0527(6) 0.0081(6) 0.0455(5) C8 0.0578(7) 0.0203(8) 0.0488(5) 0.097(1) 0.0172(9) 0.0891(8) C9 0.0689(7) 0.0208(7) 0.0451(5) 0.0662(9) 0.0047(8) 0.0864(8) C10 0.0478(6) 0.0098(6) 0.0261(4) 0.0503(9) 0.0100(6) 0.0600(6) C11 0.0603(7) 0.0067(6) 0.0346(6) 0.0417(6) 0.0108(7) 0.0833(8) C13 0.0692(8) -0.0112(7) 0.0324(5) 0.0549(9) -0.0144(7) 0.0635(7) C14 0.073(1) -0.0101(9) 0.0112(7) 0.072(1) -0.0047(8) 0.0560(8) C15 0.0551(8) -0.0014(7) 0.0098(7) 0.0564(9) 0.0089(7) 0.0581(8) C17 0.0615(7) -0.0025(6) 0.0248(5) 0.0435(6) 0.0075(6) 0.0541(6) _cod_database_code 2003389