#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003387.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_2003387 _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 'C13 H12 S2' _chemical_formula_weight 232.36 _symmetry_space_group_name_H-M 'P -3' _cell_length_a 21.792(4) _cell_length_b 21.792(4) _cell_length_c 12.566(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5168(2) _cell_formula_units_Z 18 _exptl_crystal_density_diffrn 1.3439 _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 9.7 _cell_measurement_theta_max 17.9 _exptl_absorpt_coefficient_mu 0.4079 _cell_measurement_temperature 'room temperature' _exptl_crystal_description ; Irregular prism ; _exptl_crystal_size_max 0.034 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.022 _exptl_crystal_colour 'golden--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 6637 _reflns_number_total 6045 _reflns_number_observed 3498 _reflns_observed_criterion 'I~o~ > 2\s(I~o~)' _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 1 _diffrn_standards_interval_time 360 _diffrn_standards_decay_% 'negligible' _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs 0.034 _refine_ls_wR_factor_obs 0.035 _refine_ls_goodness_of_fit_obs 1.654 _refine_ls_number_reflns 3498 _refine_ls_number_parameters 551 _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 0.15 _refine_diff_density_max 0.21 _refine_diff_density_min '>-0.21' _refine_ls_extinction_method 'Stout & Jensen (1968)' _refine_ls_extinction_coef 7.7(6)x10^-8^ 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 -0.56533 -0.23274 0.40489 0.0487(3) S7a -0.56931(3) -0.34072(3) 0.14458(6) 0.0491(3) C2a -0.4967(1) -0.1702(1) 0.4799(2) 0.0530(10) C3a -0.4324(1) -0.1550(1) 0.4427(2) 0.0477(10) C4a -0.4379(1) -0.1957(1) 0.3511(2) 0.0387(8) C5a -0.5068(1) -0.2395(1) 0.3223(2) 0.0367(9) C6a -0.5081(1) -0.2794(1) 0.2293(2) 0.0375(8) C8a -0.5029(1) -0.3419(1) 0.0719(2) 0.0539(10) C9a -0.4375(1) -0.2970(1) 0.1110(2) 0.0488(11) C10a -0.4396(1) -0.2602(1) 0.2030(2) 0.0397(9) C11a -0.3876(1) -0.2044(1) 0.2793(2) 0.0410(9) C12a -0.3317(1) -0.1363(1) 0.2223(2) 0.0557(12) C13a -0.2742(1) -0.1516(2) 0.1876(3) 0.0734(14) C14a -0.2788(1) -0.2089(2) 0.2606(3) 0.0708(13) C15a -0.3392(1) -0.2269(1) 0.3368(2) 0.0531(11) S1b 0.56049(3) 0.23704(3) 0.09478(6) 0.0486(3) S7b 0.66407(3) 0.23250(3) 0.35527(6) 0.0470(3) C2b 0.4943(1) 0.1710(1) 0.0212(2) 0.0538(11) C3b 0.4737(1) 0.1054(1) 0.0595(2) 0.0473(10) C4b 0.5122(1) 0.1078(1) 0.1509(2) 0.0380(9) C5b 0.5611(1) 0.1757(1) 0.1791(2) 0.0379(8) C6b 0.5990(1) 0.1739(1) 0.2725(2) 0.0364(9) C8b 0.6590(1) 0.1636(1) 0.4286(2) 0.0509(12) C9b 0.6098(1) 0.0992(1) 0.3912(2) 0.0463(10) C10b 0.5742(1) 0.1047(1) 0.3004(2) 0.0370(8) C11b 0.5160(1) 0.0550(1) 0.2253(2) 0.0386(10) C12b 0.5327(1) 0.0021(1) 0.1695(2) 0.0495(10) C13b 0.5128(2) -0.0572(1) 0.2499(3) 0.0634(12) C14b 0.4559(2) -0.0572(1) 0.3205(3) 0.0685(14) C15b 0.4462(1) 0.0040(1) 0.2823(2) 0.0515(11) S1c 0.11542(4) 0.02733(3) 0.62210(6) 0.0549(3) S7c 0.02192(3) -0.08705(3) 0.88315(6) 0.0485(3) C2c 0.1817(1) 0.0323(1) 0.5420(2) 0.0566(13) C3c 0.2061(1) -0.0108(1) 0.5747(2) 0.0479(10) C4c 0.1715(1) -0.0487(1) 0.6676(2) 0.0379(9) C5c 0.1212(1) -0.0333(1) 0.7017(2) 0.0395(10) C6c 0.0868(1) -0.0753(1) 0.7954(2) 0.0383(9) C8c 0.0335(1) -0.1484(1) 0.9515(2) 0.0510(11) C9c 0.0843(1) -0.1595(1) 0.9082(2) 0.0470(10) C10c 0.1157(1) -0.1171(1) 0.8176(2) 0.0372(9) C11c 0.1729(1) -0.1049(1) 0.7368(2) 0.0377(9) C12c 0.2441(1) -0.0861(1) 0.7875(2) 0.0538(11) C13c 0.2377(1) -0.1560(1) 0.8197(3) 0.0642(11) C14c 0.1783(1) -0.2132(1) 0.7505(2) 0.0597(11) C15c 0.1559(1) -0.1731(1) 0.6761(2) 0.0473(10) H2a -0.5070(10) -0.1520(10) 0.5350(20) 0.0307(42) H3a -0.3900(10) -0.1220(10) 0.4700(20) 0.0254(38) H8a -0.5170(10) -0.3720(10) 0.0190(20) 0.0285(40) H9a -0.3980(10) -0.2900(10) 0.0830(20) 0.0249(38) H121a -0.3540(10) -0.1260(10) 0.1690(20) 0.0350(45) H122a -0.3140(10) -0.0960(10) 0.2710(20) 0.0342(44) H131a -0.2840(10) -0.1690(10) 0.1120(20) 0.0415(50) H132a -0.2280(10) -0.1060(10) 0.1910(30) 0.0643(67) H141a -0.2920(10) -0.2520(10) 0.2180(20) 0.0463(53) H142a -0.2350(10) -0.1950(10) 0.2970(20) 0.0533(58) H151a -0.3660(10) -0.2750(10) 0.3610(20) 0.0249(38) H152a -0.3190(10) -0.1960(10) 0.4030(20) 0.0450(52) H2b 0.4770(10) 0.1810(10) -0.0360(20) 0.0382(47) H3b 0.4400(10) 0.0670(10) 0.0320(20) 0.0224(37) H8b 0.6890(10) 0.1730(10) 0.4840(20) 0.0345(44) H9b 0.6010(10) 0.0580(10) 0.4210(20) 0.0215(36) H121b 0.5020(10) -0.0170(10) 0.1070(20) 0.0274(40) H122b 0.5810(10) 0.0250(10) 0.1470(20) 0.0271(40) H131b 0.4960(10) -0.1010(10) 0.2150(20) 0.0430(50) H132b 0.5550(10) -0.0460(10) 0.2880(20) 0.0335(44) H141b 0.4110(10) -0.1020(10) 0.3230(20) 0.0406(50) H142b 0.4730(10) -0.0470(10) 0.3980(20) 0.0473(54) H151b 0.4090(10) -0.0130(10) 0.2330(20) 0.0317(43) H152b 0.4370(10) 0.0270(10) 0.3390(20) 0.0299(41) H2c 0.1950(10) 0.0630(10) 0.4860(20) 0.0332(44) H3c 0.2427(9) -0.0138(9) 0.5420(20) 0.0164(33) H8c 0.0060(10) -0.1700(10) 1.0070(20) 0.0317(42) H9c 0.0982(9) -0.1891(9) 0.9350(20) 0.0191(34) H121c 0.2540(10) -0.0530(10) 0.8440(20) 0.0238(37) H122c 0.2810(10) -0.0640(10) 0.7310(20) 0.0323(43) H131c 0.2240(10) -0.1660(10) 0.9000(20) 0.0398(48) H132c 0.2820(10) -0.1550(10) 0.8150(20) 0.0401(50) H141c 0.1370(10) -0.2450(10) 0.7960(20) 0.0353(44) H142c 0.1950(10) -0.2410(10) 0.7150(20) 0.0327(44) H151c 0.1073(9) -0.1995(9) 0.6580(20) 0.0179(34) H152c 0.1840(10) -0.1600(10) 0.6100(20) 0.0282(41) 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 0.0466(4) 0.0289(2) 0.0073(3) 0.0561(4) 0.0023(3) 0.0476(4) S7a 0.0466(4) 0.0178(3) -0.0090(3) 0.0462(4) -0.0053(3) 0.0475(4) C2a 0.067(1) 0.0401(9) 0.001(1) 0.061(1) -0.006(1) 0.042(2) C3a 0.051(1) 0.0215(9) -0.011(1) 0.046(1) -0.004(1) 0.043(2) C4a 0.042(1) 0.0216(7) 0.000(1) 0.040(1) 0.005(1) 0.036(1) C5a 0.038(1) 0.0198(7) 0.001(1) 0.038(1) 0.005(1) 0.036(1) C6a 0.038(1) 0.0198(7) -0.002(1) 0.039(1) 0.002(1) 0.036(1) C8a 0.074(1) 0.0347(9) -0.005(1) 0.054(1) -0.009(1) 0.038(2) C9a 0.054(1) 0.0334(8) 0.008(1) 0.058(1) 0.007(1) 0.042(2) C10a 0.045(1) 0.0250(7) 0.003(1) 0.043(1) 0.008(1) 0.034(1) C11a 0.035(1) 0.0180(8) -0.002(1) 0.042(1) 0.003(1) 0.043(1) C12a 0.047(1) 0.016(1) 0.001(1) 0.051(1) 0.010(1) 0.058(2) C13a 0.046(1) 0.029(1) 0.016(2) 0.094(2) 0.019(2) 0.071(2) C14a 0.052(1) 0.045(1) 0.004(1) 0.100(2) 0.003(2) 0.071(2) C15a 0.048(1) 0.0338(9) -0.001(1) 0.069(1) 0.006(1) 0.048(2) S1b 0.0570(4) 0.0282(2) 0.0024(3) 0.0447(4) 0.0082(3) 0.0480(4) S7b 0.0429(4) 0.0160(2) -0.0062(3) 0.0417(4) -0.0094(3) 0.0494(4) C2b 0.063(1) 0.0401(9) -0.002(1) 0.067(1) 0.004(1) 0.042(2) C3b 0.047(1) 0.0254(9) -0.008(1) 0.053(1) -0.010(1) 0.042(2) C4b 0.039(1) 0.0199(7) 0.002(1) 0.040(1) -0.003(1) 0.035(1) C5b 0.041(1) 0.0200(7) 0.006(1) 0.037(1) 0.002(1) 0.037(1) C6b 0.036(1) 0.0164(7) 0.002(1) 0.036(1) -0.003(1) 0.036(1) C8b 0.053(1) 0.0292(9) -0.011(1) 0.061(1) -0.006(1) 0.040(2) C9b 0.057(1) 0.0289(8) -0.002(1) 0.046(1) 0.003(1) 0.040(2) C10b 0.040(1) 0.0208(7) 0.004(1) 0.040(1) -0.001(1) 0.032(1) C11b 0.042(1) 0.0163(8) 0.000(1) 0.034(1) -0.003(1) 0.037(1) C12b 0.060(1) 0.0249(9) 0.001(1) 0.040(1) -0.006(1) 0.049(2) C13b 0.083(2) 0.031(1) -0.005(2) 0.041(1) -0.002(1) 0.067(2) C14b 0.079(2) 0.015(1) 0.010(2) 0.041(1) 0.011(1) 0.067(2) C15b 0.047(1) 0.014(1) 0.006(1) 0.043(1) -0.001(1) 0.053(2) S1c 0.0687(4) 0.0377(2) -0.0010(4) 0.0521(4) 0.0086(3) 0.0538(4) S7c 0.0464(4) 0.0282(2) 0.0039(3) 0.0550(4) -0.0047(3) 0.0479(4) C2c 0.068(2) 0.025(1) 0.003(1) 0.049(1) 0.011(1) 0.046(2) C3c 0.047(1) 0.0230(9) 0.007(1) 0.050(1) 0.000(1) 0.045(2) C4c 0.042(1) 0.0183(8) -0.002(1) 0.038(1) -0.003(1) 0.032(1) C5c 0.043(1) 0.0223(7) -0.005(1) 0.040(1) -0.002(1) 0.036(1) C6c 0.040(1) 0.0209(7) -0.003(1) 0.041(1) -0.005(1) 0.035(1) C8c 0.052(1) 0.022(1) 0.009(1) 0.055(1) 0.002(1) 0.040(2) C9c 0.056(1) 0.0287(8) -0.004(1) 0.050(1) 0.003(1) 0.039(1) C10c 0.042(1) 0.0196(7) -0.005(1) 0.038(1) -0.005(1) 0.031(1) C11c 0.038(1) 0.0236(7) -0.003(1) 0.042(1) -0.004(1) 0.037(1) C12c 0.047(1) 0.0305(9) -0.007(1) 0.063(1) -0.004(1) 0.055(2) C13c 0.066(1) 0.0525(9) -0.008(1) 0.081(1) 0.003(1) 0.067(2) C14c 0.077(1) 0.0504(8) 0.007(1) 0.062(1) 0.007(1) 0.061(2) C15c 0.054(1) 0.0296(8) -0.001(1) 0.050(1) -0.005(1) 0.042(2)