#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003343.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_2003343 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 772 _journal_page_last 775 _publ_section_title ; 2-(2,6-Difluorophenyl)-1,3-dithiane and 2-(2,6-Difluorophenyl)-1,3-dithiane-1,1,3,3-tetraoxide, The Role of Oxidation in Locking a Molecular Conformation ; _chemical_formula_moiety ' C10 H10 F2 O4 S2 ' _chemical_formula_sum ' C10 H10 F2 O4 S2 ' _chemical_formula_structural ' C10 H10 F2 O4 S2' _chemical_formula_weight 296.30 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _symmetry_space_group_name_H-M 'P -1' _cell_length_a 5.257(2) _cell_length_b 7.332(2) _cell_length_c 15.474(5) _cell_angle_alpha 87.61(3) _cell_angle_beta 85.91(3) _cell_angle_gamma 78.47(3) _cell_volume 582.7(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 16.0 _cell_measurement_theta_max 24.0 _exptl_absorpt_coefficient_mu 0.47 _cell_measurement_temperature 296 _exptl_crystal_description 'rod' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'colourless' _chemical_compound_source 'Synthesized at UMIST' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _diffrn_reflns_number 3306 _reflns_number_total 1810 _reflns_number_observed 1368 _reflns_observed_criterion 'I>3s(I)' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_max 24.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not significant' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0301 _refine_ls_wR_factor_obs 0.0356 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.492 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1368 _refine_ls_number_parameters 203 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'sigma; default TEXSAN' _refine_ls_shift/esd_max 0.035 _refine_diff_density_max 0.30 _refine_diff_density_min -0.24 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables' 0.002 0.002 H 'International Tables' 0.000 0.000 F 'International Tables' 0.014 0.010 O 'International Tables' 0.008 0.006 S 'International Tables' 0.110 0.124 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; ; MSC/AFC Diffractometer Control Software ; ; TEXSAN PROCESS (Molecular Structure Corporation, 1985) ; ; TEXSAN LS (Molecular Structure Corporation, 1985) ; ; TEXSAN FINISH (Molecular Structure Corporation, 1985) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv S1 0.6301(1) 0.49685(9) 0.12698(4) 0.0275(4) C2 0.6571(6) 0.4263(4) 0.2410(2) 0.025(1) S3 0.5489(1) 0.20652(9) 0.26325(4) 0.0275(4) C4 0.7607(7) 0.0585(4) 0.1914(2) 0.034(2) C5 0.7570(7) 0.1246(4) 0.0970(2) 0.037(2) C6 0.8501(7) 0.3078(4) 0.0790(2) 0.034(2) C11 0.5449(5) 0.5662(3) 0.3093(2) 0.026(1) C12 0.6836(6) 0.5729(4) 0.3823(2) 0.031(2) C13 0.5967(7) 0.6898(4) 0.4491(2) 0.040(2) C14 0.3606(7) 0.8101(4) 0.4442(2) 0.040(2) C15 0.2131(7) 0.8109(4) 0.3740(2) 0.038(2) C16 0.3073(6) 0.6893(4) 0.3093(2) 0.033(2) F12 0.9148(3) 0.4545(3) 0.3870(1) 0.045(1) F16 0.1586(4) 0.6860(3) 0.2416(1) 0.052(1) O1A 0.7292(5) 0.6649(3) 0.1145(1) 0.042(1) O1B 0.3761(4) 0.4938(3) 0.0999(1) 0.037(1) O3A 0.6084(4) 0.1511(3) 0.3501(1) 0.040(1) O3B 0.2863(4) 0.2229(3) 0.2395(1) 0.038(1) H2 0.834(6) 0.390(4) 0.242(2) 0.029(8) H4A 0.926(7) 0.047(4) 0.210(2) 0.046(9) H4B 0.713(6) -0.052(4) 0.200(2) 0.038(8) H5A 0.887(6) 0.023(4) 0.062(2) 0.039(8) H5B 0.595(7) 0.135(4) 0.076(2) 0.038(9) H6A 0.847(7) 0.342(4) 0.020(2) 0.050(9) H6B 1.017(6) 0.309(4) 0.102(2) 0.027(7) H13 0.701(7) 0.684(4) 0.491(2) 0.047(9) H14 0.295(6) 0.883(4) 0.487(2) 0.035(8) H15 0.049(7) 0.890(4) 0.367(2) 0.044(9) 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 0.0302(4) -0.0056(3) -0.0049(3) 0.0293(4) 0.0016(3) 0.0231(4) C2 0.023(2) -0.003(1) -0.006(1) 0.028(1) 0.000(1) 0.024(1) S3 0.0298(4) -0.0066(3) -0.0031(3) 0.0262(4) 0.0008(3) 0.0270(4) C4 0.037(2) -0.007(1) -0.002(2) 0.024(2) -0.001(1) 0.043(2) C5 0.040(2) -0.007(2) 0.002(2) 0.039(2) -0.009(1) 0.033(2) C6 0.035(2) -0.007(1) -0.001(1) 0.040(2) -0.001(1) 0.027(2) C11 0.028(2) -0.009(1) -0.001(1) 0.026(1) 0.000(1) 0.025(2) C12 0.032(2) -0.008(1) -0.006(1) 0.037(2) 0.001(1) 0.028(2) C13 0.050(2) -0.017(2) -0.008(2) 0.048(2) -0.004(1) 0.028(2) C14 0.054(2) -0.012(2) 0.004(2) 0.037(2) -0.009(1) 0.031(2) C15 0.042(2) 0.004(1) 0.003(2) 0.031(2) -0.004(1) 0.038(2) C16 0.034(2) -0.005(1) -0.011(1) 0.036(2) -0.001(1) 0.032(2) F12 0.038(1) 0.0002(9) -0.0167(8) 0.057(1) -0.0076(8) 0.039(1) F16 0.044(1) 0.0164(9) -0.0198(9) 0.061(1) -0.0152(9) 0.045(1) O1A 0.057(1) -0.016(1) -0.005(1) 0.033(1) 0.0054(9) 0.039(1) O1B 0.033(1) -0.0039(10) -0.0116(9) 0.051(1) 0.0013(9) 0.027(1) O3A 0.055(1) -0.0114(10) -0.008(1) 0.039(1) 0.0071(9) 0.029(1) O3B 0.028(1) -0.0110(9) -0.0041(10) 0.042(1) -0.0002(10) 0.048(1)