#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003386.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_2003386 _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 'C9 H6 S2' _chemical_formula_weight 178.266 _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 12.653(1) _cell_length_b 11.233(1) _cell_length_c 11.388(1) _cell_angle_alpha 90.00 _cell_angle_beta 98.40(1) _cell_angle_gamma 90.00 _cell_volume 1601.2(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.479 _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 8.1 _cell_measurement_theta_max 14.6 _exptl_absorpt_coefficient_mu 0.562 _cell_measurement_temperature 'room temperature' _exptl_crystal_description ; crystal sealed in Lindemann glass capillary to prevent sublimation ; _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_colour 'colourless: became yellowish' _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 3126 _reflns_number_total 3126 _reflns_number_observed 2274 _reflns_observed_criterion 'I~o~ > 2\s(I~o~)' _diffrn_reflns_av_R_equivalents '?' _diffrn_reflns_theta_max 26 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 1 _diffrn_standards_interval_time 360 _diffrn_standards_decay_% 'negligible' _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs 0.031 _refine_ls_wR_factor_obs 0.035 _refine_ls_goodness_of_fit_obs 1.951 _refine_ls_number_reflns 2274 _refine_ls_number_parameters 248 _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 .04 _refine_diff_density_max 0.22 _refine_diff_density_min >-0.22 _refine_ls_extinction_method 'Stout & Jensen (1968)' _refine_ls_extinction_coef 3.9(2)x10^-6^ 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 0.31929(5) 0.02325(5) 0.45912(5) 0.0561(2) S7a 0.53241(4) 0.29049(5) 0.46326(5) 0.0520(2) C2a 0.2170(2) -0.0230(2) 0.3515(2) 0.0587(7) C3a 0.2103(2) 0.0417(2) 0.2512(2) 0.0527(7) C4a 0.2892(2) 0.1315(2) 0.2590(2) 0.0425(6) C5a 0.3540(2) 0.1320(2) 0.3668(2) 0.0403(6) C6a 0.4322(2) 0.2257(2) 0.3669(2) 0.0392(6) C8a 0.5531(2) 0.3937(2) 0.3575(2) 0.0519(7) C9a 0.4867(2) 0.3789(2) 0.2542(2) 0.0502(7) C10a 0.4160(2) 0.2828(2) 0.2595(2) 0.0417(7) C11a 0.3221(2) 0.2285(2) 0.1806(2) 0.0492(6) S1b 0.06874(4) 0.41533(5) 0.28951(5) 0.0519(2) S7b -0.00778(5) 0.65612(5) 0.02972(5) 0.0533(2) C2b 0.1848(2) 0.3933(2) 0.3878(2) 0.0499(7) C3b 0.2621(2) 0.4730(2) 0.3734(2) 0.0457(7) C4b 0.2282(2) 0.5550(2) 0.2825(2) 0.0412(6) C5b 0.1257(2) 0.5349(2) 0.2285(2) 0.0400(6) C6b 0.0974(2) 0.6221(2) 0.1369(2) 0.0419(6) C8b 0.0634(2) 0.7729(2) -0.0190(2) 0.0556(7) C9b 0.1624(2) 0.7837(2) 0.0435(2) 0.0547(7) C10b 0.1826(2) 0.6968(2) 0.1331(2) 0.0455(6) C11b 0.2741(2) 0.6614(2) 0.2270(2) 0.0504(7) H2a 0.1770(20) -0.0830(20) 0.3720(20) 0.0911(90) H3a 0.1630(20) 0.0300(20) 0.1870(20) 0.0660(74) H8a 0.5980(10) 0.4450(20) 0.3730(20) 0.0708(79) H9a 0.4890(20) 0.4260(20) 0.1900(20) 0.0988(95) H111a 0.3430(20) 0.2010(20) 0.1080(20) 0.0771(81) H112a 0.2650(20) 0.2810(20) 0.1640(20) 0.0734(79) H2b 0.1870(20) 0.3310(20) 0.4340(20) 0.0795(81) H3b 0.3330(10) 0.4710(20) 0.4170(20) 0.0512(64) H8b 0.0330(20) 0.8160(20) -0.0790(20) 0.0789(81) H9b 0.2120(20) 0.8420(20) 0.0240(20) 0.0979(92) H111b 0.3400(20) 0.6340(20) 0.1890(20) 0.0847(86) H112b 0.2910(20) 0.7220(20) 0.2840(20) 0.0702(75) 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 0.0699(3) -0.0063(3) 0.0178(3) 0.0442(3) 0.0071(3) 0.0568(3) S7a 0.0475(2) -0.0068(2) 0.0007(3) 0.0577(3) -0.0025(3) 0.0491(3) C2a 0.064(1) -0.016(1) 0.024(1) 0.044(1) -0.008(1) 0.072(1) C3a 0.050(1) -0.010(1) 0.013(1) 0.053(1) -0.014(1) 0.057(1) C4a 0.046(1) -0.0036(9) 0.0126(8) 0.040(1) -0.0061(9) 0.044(1) C5a 0.047(1) -0.0005(9) 0.0132(8) 0.035(1) -0.0013(9) 0.041(1) C6a 0.040(1) 0.0007(9) 0.0096(8) 0.038(1) -0.0039(9) 0.041(1) C8a 0.043(1) -0.012(1) 0.012(1) 0.049(1) -0.004(1) 0.065(1) C9a 0.055(1) -0.006(1) 0.0163(9) 0.047(1) 0.004(1) 0.051(1) C10a 0.046(1) -0.0022(9) 0.0113(8) 0.041(1) -0.0016(9) 0.039(1) C11a 0.053(1) -0.006(1) 0.0061(9) 0.055(1) -0.002(1) 0.039(1) S1b 0.0470(3) -0.0058(2) 0.0004(3) 0.0531(3) 0.0159(3) 0.0534(3) S7b 0.0561(3) 0.0060(3) -0.0005(3) 0.0479(3) 0.0098(3) 0.0534(3) C2b 0.054(1) 0.005(1) 0.001(1) 0.050(1) 0.010(1) 0.044(1) C3b 0.045(1) 0.006(1) 0.0010(9) 0.051(1) -0.005(1) 0.039(1) C4b 0.045(1) 0.0010(9) 0.0068(8) 0.042(1) -0.0061(9) 0.037(1) C5b 0.044(1) 0.0001(9) 0.0068(8) 0.038(1) 0.0014(9) 0.038(1) C6b 0.048(1) 0.0028(9) 0.0060(9) 0.038(1) -0.0004(9) 0.039(1) C8b 0.079(1) 0.011(1) 0.014(1) 0.041(1) 0.009(1) 0.049(1) C9b 0.070(1) -0.003(1) 0.017(1) 0.042(1) 0.004(1) 0.055(1) C10b 0.056(1) -0.002(1) 0.0135(9) 0.038(1) -0.0006(9) 0.045(1) C11b 0.051(1) -0.010(1) 0.007(1) 0.047(1) -0.004(1) 0.053(1)