#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003390.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_2003390 _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 'C14 H16 O3 S2' _chemical_formula_weight 296.40 _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 7.999(1) _cell_length_b 12.060(2) _cell_length_c 14.930(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.46(1) _cell_angle_gamma 90.00 _cell_volume 1406.34(35) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.3999 _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 9.8 _cell_measurement_theta_max 17.9 _exptl_absorpt_coefficient_mu 0.3629 _cell_measurement_temperature 'room temperature' _exptl_crystal_description ; prism ; _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_colour '?' _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 2842 _reflns_number_total 2842 _reflns_number_observed 2087 _reflns_observed_criterion 'I~o~ > 2\s(I~o~)' _diffrn_reflns_av_R_equivalents '?' _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_time 360 _diffrn_standards_decay_% 'negligible' _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs 0.035 _refine_ls_wR_factor_obs 0.046 _refine_ls_goodness_of_fit_obs 2.024 _refine_ls_number_reflns 2087 _refine_ls_number_parameters 237 _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 0.24 _refine_diff_density_max 0.40 _refine_diff_density_min '>-0.40' _refine_ls_extinction_method 'Stout & Jensen (1968) ' _refine_ls_extinction_coef 1.4(2)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 S1 -0.22770(7) 0.12441(5) 0.20634(4) 0.0477(2) S7 -0.30744(8) 0.12454(5) -0.03069(4) 0.0534(2) O12 0.2434(2) 0.2946(1) 0.01204(9) 0.0523(5) O15 0.3168(2) 0.5138(1) 0.0878(1) 0.0648(5) O18 0.0479(2) 0.4812(1) 0.1920(1) 0.0579(5) C2 -0.2132(3) 0.2227(2) 0.2900(1) 0.0503(7) C3 -0.1534(3) 0.3194(2) 0.2653(1) 0.0437(6) C4 -0.1168(2) 0.3169(2) 0.1752(1) 0.0372(6) C5 -0.1485(2) 0.2147(2) 0.1357(1) 0.0378(6) C6 -0.1302(3) 0.1759(2) 0.0451(1) 0.0397(7) C8 -0.1906(3) 0.0975(2) -0.1113(2) 0.0587(8) C9 -0.0258(3) 0.1249(2) -0.0814(2) 0.0548(8) C10 0.0125(3) 0.1700(2) 0.0089(1) 0.0435(6) C11 0.1884(3) 0.2032(2) 0.0578(1) 0.0535(8) C13 0.4098(3) 0.3358(2) 0.0540(2) 0.0650(9) C14 0.4060(3) 0.4169(3) 0.1267(2) 0.0673(9) C16 0.2793(3) 0.5872(2) 0.1543(2) 0.0544(8) C17 0.0943(3) 0.5850(2) 0.1578(2) 0.0521(7) C19 -0.0651(3) 0.4171(2) 0.1288(1) 0.0470(7) H2 -0.2430(30) 0.2070(20) 0.3460(10) 0.172(19) H3 -0.1350(20) 0.3830(20) 0.3020(10) 0.117(16) H8 -0.2440(30) 0.0680(20) -0.1670(10) 0.192(20) H9 0.0550(30) 0.1150(20) -0.1150(10) 0.206(22) H111 0.1890(20) 0.2230(20) 0.1210(10) 0.174(20) H112 0.2630(30) 0.1460(20) 0.0590(10) 0.210(23) H131 0.4830(30) 0.2730(20) 0.0830(20) 0.265(25) H132 0.4590(40) 0.3960(30) 0.0120(20) 0.424(39) H141 0.3280(30) 0.3710(20) 0.1720(20) 0.331(32) H142 0.5300(30) 0.4380(20) 0.1580(20) 0.264(26) H161 0.3580(30) 0.5710(20) 0.2170(10) 0.208(22) H162 0.3140(30) 0.6630(20) 0.1400(10) 0.223(23) H171 0.0760(30) 0.6420(20) 0.2020(10) 0.208(22) H172 0.0280(30) 0.6010(20) 0.0980(20) 0.221(23) H191 -0.1640(30) 0.4630(20) 0.1000(20) 0.235(23) H192 -0.0040(30) 0.3960(20) 0.0770(20) 0.263(25) 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 0.0494(2) -0.0040(3) 0.0157(2) 0.0453(3) 0.0088(3) 0.0505(2) S7 0.0538(3) -0.0107(3) 0.0060(2) 0.0547(3) -0.0103(3) 0.0492(3) O12 0.0437(7) -0.0051(7) 0.0110(6) 0.059(1) 0.0000(8) 0.0543(8) O15 0.0759(9) 0.0115(9) 0.0264(7) 0.059(1) 0.0058(8) 0.0651(9) O18 0.0602(9) -0.0215(8) -0.0007(7) 0.0597(9) 0.0152(8) 0.0481(8) C2 0.047(1) 0.002(1) 0.0160(8) 0.065(1) 0.006(1) 0.042(1) C3 0.044(1) 0.004(1) 0.0086(8) 0.048(1) -0.003(1) 0.038(1) C4 0.0360(9) 0.0021(9) 0.0067(7) 0.042(1) 0.0019(9) 0.0332(9) C5 0.0350(9) 0.0011(9) 0.0066(7) 0.042(1) 0.0054(9) 0.0361(9) C6 0.045(1) -0.001(1) 0.0068(8) 0.035(1) -0.0001(9) 0.038(1) C8 0.082(2) -0.012(1) 0.011(1) 0.051(1) -0.012(1) 0.042(1) C9 0.073(1) 0.001(1) 0.0249(9) 0.048(1) -0.004(1) 0.048(1) C10 0.050(1) 0.002(1) 0.0134(8) 0.039(1) 0.0028(9) 0.043(1) C11 0.047(1) 0.006(1) 0.0126(9) 0.065(2) 0.007(1) 0.049(1) C13 0.041(1) 0.002(1) 0.012(1) 0.067(2) -0.010(1) 0.087(2) C14 0.050(1) 0.011(1) -0.002(1) 0.067(2) -0.008(1) 0.078(2) C16 0.050(1) -0.004(1) 0.020(1) 0.049(1) 0.003(1) 0.068(1) C17 0.050(1) -0.003(1) 0.014(1) 0.045(1) 0.010(1) 0.061(1) C19 0.059(1) -0.003(1) 0.0051(9) 0.041(1) 0.003(1) 0.039(1)