#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003388.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_2003388 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 690 _journal_page_last 697 _publ_section_title ; Five 3,3'-Bridged 2,2'-Dithiophenes ; _chemical_formula_sum 'C10 H8 O S2' _chemical_formula_weight 208.29 _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 14.030(2) _cell_length_b 9.009(2) _cell_length_c 16.306(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.49(2) _cell_angle_gamma 90.00 _cell_volume 1890.22(82) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.4639 _exptl_crystal_density_meas '?' _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 10.7 _cell_measurement_theta_max 17.0 _exptl_absorpt_coefficient_mu 0.4940 _cell_measurement_temperature 'room temperature' _exptl_crystal_description ; Irregular and partially rounded prism ; _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_colour 'yellow' _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 3848 _reflns_number_total 3701 _reflns_number_observed 2466 _reflns_observed_criterion 'I~o~ > 2\s(I~o~)' _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 26 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _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 0.036 _refine_ls_goodness_of_fit_obs 1.841 _refine_ls_number_reflns 2466 _refine_ls_number_parameters 300 _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 0.003 _refine_diff_density_max 0.021 _refine_diff_density_min '>-0.21' _refine_ls_extinction_method 'Stout & Jensen (1968) ' _refine_ls_extinction_coef 5.2(4)x10^-7^ 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 S1a -0.24609(4) 0.35192(7) 0.13717(4) 0.0611(2) S7a -0.29924(5) 0.69592(7) 0.09094(4) 0.0701(2) O12a -0.5328(1) 0.4976(2) 0.19257(8) 0.0591(5) C2a -0.2682(2) 0.1859(3) 0.1767(2) 0.0659(7) C3a -0.3563(2) 0.1883(2) 0.1903(1) 0.0605(8) C4a -0.4092(1) 0.3264(2) 0.1693(1) 0.0467(6) C5a -0.3582(1) 0.4277(2) 0.1394(1) 0.0438(6) C6a -0.3850(1) 0.5808(2) 0.1126(1) 0.0484(7) C8a -0.3855(2) 0.8394(3) 0.0635(2) 0.0838(12) C9a -0.4735(2) 0.8023(3) 0.0722(2) 0.0765(11) C10a -0.4753(2) 0.6542(2) 0.0994(1) 0.0551(7) C11a -0.5646(2) 0.5855(3) 0.1138(1) 0.0652(9) C13a -0.5100(2) 0.3490(3) 0.1797(1) 0.0661(8) S1b 0.08620(5) 0.36056(7) -0.00522(4) 0.0737(2) S7b 0.00317(5) 0.11700(8) -0.16322(4) 0.0805(3) O12b 0.2730(1) -0.0809(2) 0.07309(9) 0.0689(6) C2b 0.1692(2) 0.4134(3) 0.0997(2) 0.0815(10) C3b 0.2308(2) 0.3020(3) 0.1442(2) 0.0717(9) C4b 0.2135(1) 0.1678(2) 0.0947(1) 0.0547(7) C5b 0.1364(1) 0.1817(2) 0.0112(1) 0.0505(7) C6b 0.0907(1) 0.0702(2) -0.0575(1) 0.0514(6) C8b -0.0186(2) -0.0642(3) -0.1944(2) 0.0825(11) C9b 0.0394(2) -0.1557(3) -0.1282(2) 0.0682(8) C10b 0.1024(1) -0.0803(2) -0.0494(1) 0.0523(7) C11b 0.1753(2) -0.1551(2) 0.0335(2) 0.0674(8) C13b 0.2743(2) 0.0302(3) 0.1345(2) 0.0731(10) H2a -0.2240(10) 0.1100(20) 0.1850(10) 0.0925(79) H3a -0.3820(10) 0.1090(20) 0.2110(10) 0.0700(68) H8a -0.3690(20) 0.9290(30) 0.0470(10) 0.1160(93) H9a -0.5230(20) 0.8620(20) 0.0630(10) 0.0962(81) H111a -0.6050(10) 0.5260(20) 0.0630(10) 0.0880(77) H112a -0.6020(10) 0.6640(20) 0.1220(10) 0.0866(78) H131a -0.5660(20) 0.3050(20) 0.1250(10) 0.1022(85) H132a -0.5060(10) 0.2990(20) 0.2320(10) 0.0821(73) H2b 0.1690(20) 0.5110(20) 0.1190(10) 0.1026(87) H3b 0.2810(10) 0.3070(20) 0.2030(10) 0.0809(74) H8b -0.0680(20) -0.0970(30) -0.2530(20) 0.135(11) H9b 0.0380(10) -0.2630(20) -0.1340(10) 0.0800(71) H111b 0.1920(10) -0.2530(20) 0.0220(10) 0.0803(73) H112b 0.1440(20) -0.1620(30) 0.0780(20) 0.1150(95) H131b 0.3390(10) 0.0540(20) 0.1670(10) 0.0926(78) H132b 0.2500(20) -0.0160(30) 0.1780(10) 0.1076(91) 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 S1a 0.0549(3) 0.0046(3) 0.0321(2) 0.0619(3) 0.0047(3) 0.0727(2) S7a 0.0870(3) -0.0159(3) 0.0364(2) 0.0551(3) 0.0028(3) 0.0726(3) O12a 0.0593(7) 0.0099(7) 0.0258(5) 0.0674(9) -0.0012(6) 0.0538(7) C2a 0.070(1) 0.014(1) 0.0344(8) 0.053(1) 0.009(1) 0.079(1) C3a 0.073(1) -0.002(1) 0.0341(8) 0.047(1) 0.005(1) 0.067(1) C4a 0.0501(8) -0.0008(9) 0.0198(6) 0.046(1) -0.0027(9) 0.0451(9) C5a 0.0465(8) -0.0016(9) 0.0145(6) 0.045(1) -0.0043(9) 0.0374(8) C6a 0.059(1) -0.0043(9) 0.0166(7) 0.045(1) -0.0027(9) 0.0382(8) C8a 0.124(2) -0.006(1) 0.033(1) 0.046(1) 0.009(1) 0.075(1) C9a 0.099(2) 0.017(1) 0.023(1) 0.052(1) 0.005(1) 0.069(1) C10a 0.067(1) 0.006(1) 0.0144(8) 0.049(1) -0.0014(9) 0.0426(9) C11a 0.060(1) 0.014(1) 0.0130(9) 0.066(1) -0.004(1) 0.060(1) C13a 0.068(1) 0.002(1) 0.0408(8) 0.063(1) 0.009(1) 0.079(1) S1b 0.0731(3) 0.0157(3) 0.0300(2) 0.0539(3) 0.0110(3) 0.0913(3) S7b 0.0759(3) 0.0239(4) 0.0098(2) 0.0920(5) 0.0110(3) 0.0576(3) O12b 0.0601(8) 0.0194(7) 0.0213(6) 0.0660(9) 0.0139(8) 0.0752(8) C2b 0.076(1) -0.006(1) 0.037(1) 0.060(1) -0.016(1) 0.109(2) C3b 0.062(1) -0.008(1) 0.021(1) 0.073(2) -0.009(1) 0.075(1) C4b 0.0464(9) -0.0002(9) 0.0214(7) 0.059(1) 0.006(1) 0.059(1) C5b 0.0475(8) 0.0067(9) 0.0279(6) 0.049(1) 0.0102(9) 0.0607(9) C6b 0.0457(8) 0.0086(9) 0.0227(6) 0.061(1) 0.010(1) 0.0511(9) C8b 0.063(1) 0.014(1) 0.015(1) 0.108(2) -0.019(1) 0.067(1) C9b 0.060(1) 0.002(1) 0.0327(8) 0.072(1) -0.013(1) 0.078(1) C10b 0.0513(8) 0.0037(9) 0.0293(6) 0.057(1) 0.001(1) 0.0561(9) C11b 0.085(1) 0.005(1) 0.0323(9) 0.049(1) 0.006(1) 0.070(1) C13b 0.064(1) 0.004(1) 0.005(1) 0.071(1) 0.010(1) 0.065(1)