#------------------------------------------------------------------------------ #$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200158.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200158 loop_ _publ_author_name 'Koskimies, Jorma' 'N\"as\"akk\"al\"a, Matti' 'Mutikainen, Ilpo' _publ_section_title ; 1,8-Dioxa-4,11-dithiacyclotetradecane-2,9-dione ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o261 _journal_page_last o263 _journal_paper_doi 10.1107/S1600536801003038 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C10 H16 O4 S2' _chemical_formula_moiety 'C10 H16 O4 S2' _chemical_formula_sum 'C10 H16 O4 S2' _chemical_formula_weight 264.35 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 71.88(4) _cell_angle_beta 74.04(3) _cell_angle_gamma 85.41(4) _cell_formula_units_Z 1 _cell_length_a 5.3920(18) _cell_length_b 6.858(3) _cell_length_c 8.960(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 7.5 _cell_measurement_theta_min 3.5 _cell_volume 302.8(3) _computing_cell_refinement 'TEXSAN (Molecular Structure Corporation, 1993b)' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993a) ; _computing_data_reduction TEXSAN _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full .985 _diffrn_measured_fraction_theta_max .985 _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0763 _diffrn_reflns_av_sigmaI/netI .0705 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2360 _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 25.24 _diffrn_reflns_theta_min 3.13 _diffrn_standards_decay_% -.1 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .436 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min .885 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 140 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .37 _exptl_crystal_size_min .20 _refine_diff_density_max .423 _refine_diff_density_min -.586 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 105 _refine_ls_number_reflns 1082 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all .0501 _refine_ls_R_factor_gt .0484 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0741P)^2^+0.1359P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1294 _reflns_number_gt 1017 _reflns_number_total 1082 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cv6004.cif _cod_data_source_block I _cod_database_code 2200158 _cod_database_fobs_code 2200158 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol S1 .23774(10) .32376(8) .93150(7) .0339(3) Uani d . 1 . . S C2 .3355(4) .1144(3) .8452(3) .0300(5) Uani d . 1 . . C H2A .278(5) -.008(4) .936(4) .031(6) Uiso d . 1 . . H H2B .522(6) .113(4) .805(4) .041(7) Uiso d . 1 . . H C3 .2011(4) .1243(3) .7160(3) .0271(5) Uani d . 1 . . C O4 .3425(3) .2284(3) .5675(2) .0346(4) Uani d . 1 . . O C5 .2336(5) .2514(4) .4309(3) .0342(6) Uani d . 1 . . C H5A .049(6) .254(4) .467(4) .045(8) Uiso d . 1 . . H H5B .287(6) .132(5) .393(4) .045(8) Uiso d . 1 . . H C6 .3355(4) .4494(4) .3022(3) .0330(5) Uani d . 1 . . C H6A .279(5) .561(4) .350(4) .040(7) Uiso d . 1 . . H H6B .252(6) .466(5) .215(5) .059(9) Uiso d . 1 . . H C7 .6307(4) .4529(3) .2375(3) .0319(5) Uani d . 1 . . C H7A .690(6) .338(5) .193(4) .048(8) Uiso d . 1 . . H H7B .708(6) .433(4) .325(4) .044(8) Uiso d . 1 . . H O8 -.0088(3) .0500(3) .7408(2) .0435(5) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 .0345(4) .0308(4) .0321(5) -.0044(3) .0001(3) -.0103(3) C2 .0264(11) .0253(11) .0351(14) .0001(8) -.0058(10) -.0066(10) C3 .0249(10) .0207(10) .0336(13) .0013(8) -.0049(9) -.0082(9) O4 .0284(8) .0408(9) .0310(10) -.0117(7) -.0054(7) -.0052(8) C5 .0317(12) .0387(13) .0337(15) -.0072(10) -.0085(10) -.0112(11) C6 .0295(12) .0326(12) .0352(14) -.0016(9) -.0067(10) -.0090(11) C7 .0307(11) .0266(11) .0350(14) .0004(9) -.0032(10) -.0094(10) O8 .0323(9) .0510(11) .0417(12) -.0162(8) -.0061(8) -.0055(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C7 S1 C2 2_666 . 102.91(12) C3 C2 S1 . . 111.21(14) C3 C2 H2A . . 108.8(15) S1 C2 H2A . . 104.2(15) C3 C2 H2B . . 112.3(18) S1 C2 H2B . . 110.3(16) H2A C2 H2B . . 110(2) O8 C3 O4 . . 123.5(2) O8 C3 C2 . . 125.2(2) O4 C3 C2 . . 111.31(18) C3 O4 C5 . . 117.05(18) O4 C5 C6 . . 107.84(18) O4 C5 H5A . . 109.3(19) C6 C5 H5A . . 110.8(18) O4 C5 H5B . . 106.9(18) C6 C5 H5B . . 112.4(19) H5A C5 H5B . . 109(2) C5 C6 C7 . . 113.0(2) C5 C6 H6A . . 107.6(17) C7 C6 H6A . . 110.0(16) C5 C6 H6B . . 106(2) C7 C6 H6B . . 111(2) H6A C6 H6B . . 108(2) C6 C7 S1 . 2_666 115.03(17) C6 C7 H7A . . 110.8(17) S1 C7 H7A 2_666 . 103.3(19) C6 C7 H7B . . 109.6(19) S1 C7 H7B 2_666 . 111.8(19) H7A C7 H7B . . 106(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C7 2_666 1.812(3) ? S1 C2 . 1.812(2) ? C2 C3 . 1.508(3) ? C2 H2A . .97(3) ? C2 H2B . .97(3) ? C3 O8 . 1.214(3) ? C3 O4 . 1.341(3) ? O4 C5 . 1.459(3) ? C5 C6 . 1.507(4) ? C5 H5A . .96(3) ? C5 H5B . .97(3) ? C6 C7 . 1.536(3) ? C6 H6A . .98(3) ? C6 H6B . .97(4) ? C7 S1 2_666 1.812(3) ? C7 H7A . .99(3) ? C7 H7B . .96(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7 S1 C2 C3 2_666 . -66.99(18) y S1 C2 C3 O8 . . -86.9(2) y S1 C2 C3 O4 . . 92.61(19) y O8 C3 O4 C5 . . .1(3) y C2 C3 O4 C5 . . -179.42(17) y C3 O4 C5 C6 . . 150.67(19) y O4 C5 C6 C7 . . 61.0(3) y C5 C6 C7 S1 . 2_666 174.15(16) y S1 C2 C3 O4 . . 92.61(19) y C3 O4 C5 C6 . . 150.67(19) y