#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/02/2200294.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_2200294 loop_ _publ_author_name 'Naotake Nakamura' 'Kenjiro Uno' 'Yoshihiro Ogawa' _publ_section_title ; Icosane-1,20-dithiol ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o505 _journal_page_last o507 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C20 H42 S2' _chemical_formula_moiety 'C20 H42 S2' _chemical_formula_sum 'C20 H42 S2' _chemical_formula_weight 346.67 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 87.430(10) _cell_angle_beta 86.560(10) _cell_angle_gamma 83.370(10) _cell_formula_units_Z 1 _cell_length_a 4.2261(6) _cell_length_b 5.4283(6) _cell_length_c 23.819(3) _cell_measurement_reflns_used 24 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 17.5 _cell_measurement_theta_min 9.8 _cell_volume 541.39(12) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 2000)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SAPI91 (Fan, 1991)' _diffrn_measured_fraction_theta_full .9675 _diffrn_measured_fraction_theta_max .9675 _diffrn_measurement_device_type 'Rigaku AFC-5R' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents .045 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 3008 _diffrn_reflns_theta_full 70.50 _diffrn_reflns_theta_max 70.50 _diffrn_standards_decay_% 11.83 _diffrn_standards_interval_count 150 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.172 _exptl_absorpt_correction_T_max .996 _exptl_absorpt_correction_T_min .767 _exptl_absorpt_correction_type \y _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description plate _exptl_crystal_size_max .7 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .01 _refine_diff_density_max .15 _refine_diff_density_min -.35 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.769 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 103 _refine_ls_number_reflns 1966 _refine_ls_R_factor_gt .057 _refine_ls_shift/su_max .0009 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + {0.05[Max(Fo^2^,0) + 2Fc^2^]/3}^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .159 _reflns_number_gt 1453 _reflns_number_total 1967 _reflns_threshold_expression F^2^>2\s(F^2^) _[local]_cod_data_source_file ci6026.cif _[local]_cod_data_source_block I _cod_original_cell_volume 541.40(10) _cod_database_code 2200294 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 1.3470(2) -.28020(10) .05060(3) .0784(2) Uani d . 1.00 . . S C1 1.1699(6) .0041(5) .08170(10) .0626(7) Uani d . 1.00 . . C C2 1.0508(6) -.0239(5) .14241(9) .0563(7) Uani d . 1.00 . . C C3 .9202(6) .2219(4) .16753(9) .0534(6) Uani d . 1.00 . . C C4 .7989(6) .1982(4) .22849(9) .0546(7) Uani d . 1.00 . . C C5 .6752(6) .4440(4) .25398(9) .0530(6) Uani d . 1.00 . . C C6 .5533(6) .4242(4) .31487(9) .0531(6) Uani d . 1.00 . . C C7 .4287(6) .6702(4) .34032(9) .0524(6) Uani d . 1.00 . . C C8 .3073(6) .6504(4) .40118(9) .0520(6) Uani d . 1.00 . . C C9 .1840(6) .8966(4) .42645(9) .0523(6) Uani d . 1.00 . . C C10 .0616(6) .8770(4) .48742(9) .0519(6) Uani d . 1.00 . . C H1a 1.3258 .1176 .0796 .0752 Uiso calc . 1.00 . . H H1b .9946 .0700 .0604 .0752 Uiso calc . 1.00 . . H H1s 1.122(8) -.393(6) .0500(10) .0942 Uiso d T 1.00 . . H H2a .8860 -.1296 .1445 .0675 Uiso calc . 1.00 . . H H2b 1.2226 -.0971 .1637 .0675 Uiso calc . 1.00 . . H H3a 1.0856 .3272 .1653 .0641 Uiso calc . 1.00 . . H H3b .7490 .2948 .1460 .0641 Uiso calc . 1.00 . . H H4a .6305 .0959 .2306 .0655 Uiso calc . 1.00 . . H H4b .9689 .1220 .2498 .0655 Uiso calc . 1.00 . . H H5a .8440 .5462 .2517 .0636 Uiso calc . 1.00 . . H H5b .5054 .5199 .2325 .0636 Uiso calc . 1.00 . . H H6a .3849 .3218 .3172 .0638 Uiso calc . 1.00 . . H H6b .7232 .3488 .3363 .0638 Uiso calc . 1.00 . . H H7a .5970 .7728 .3379 .0630 Uiso calc . 1.00 . . H H7b .2586 .7455 .3189 .0630 Uiso calc . 1.00 . . H H8a .1386 .5483 .4036 .0624 Uiso calc . 1.00 . . H H8b .4772 .5748 .4226 .0624 Uiso calc . 1.00 . . H H9a .3529 .9986 .4241 .0628 Uiso calc . 1.00 . . H H9b .0144 .9724 .4049 .0628 Uiso calc . 1.00 . . H H10a -.1111 .7787 .4905 .0624 Uiso calc . 1.00 . . H H10b .2284 .8018 .5097 .0624 Uiso calc . 1.00 . . H 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 .0960(6) .0717(5) .0627(4) .0077(4) .0184(3) -.0224(3) C1 .075(2) .0630(10) .0460(10) .0020(10) .0100(10) -.0090(10) C2 .0650(10) .0590(10) .0410(10) .0040(10) .0060(10) -.0066(10) C3 .0600(10) .0540(10) .0430(10) .0040(10) .0075(10) -.0077(9) C4 .0620(10) .0560(10) .0420(10) .0050(10) .0070(10) -.0079(10) C5 .0600(10) .0550(10) .0410(10) .0040(10) .0071(10) -.0080(9) C6 .0620(10) .0540(10) .0400(10) .0030(10) .0070(10) -.0082(9) C7 .0600(10) .0540(10) .0400(10) .0040(10) .0064(10) -.0079(9) C8 .0600(10) .0520(10) .0400(10) .0050(10) .0066(10) -.0083(9) C9 .0600(10) .0530(10) .0410(10) .0040(10) .0080(10) -.0084(9) C10 .0590(10) .0540(10) .0390(10) .0050(10) .0061(10) -.0071(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C1 . . 1.806(3) no C1 C2 . . 1.509(3) no C2 C3 . . 1.518(3) no C3 C4 . . 1.515(3) no C4 C5 . . 1.515(3) no C5 C6 . . 1.513(3) no C6 C7 . . 1.516(3) no C7 C8 . . 1.512(3) no C8 C9 . . 1.514(3) no C9 C10 . . 1.515(3) no C10 C10 . 2_576 1.512(4) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .018 .009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H .000 .000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S S .333 .557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 C1 C2 . 114.8(2) no C1 C2 C3 . 112.8(2) no C2 C3 C4 . 113.8(2) no C3 C4 C5 . 113.8(2) no C4 C5 C6 . 114.6(2) no C5 C6 C7 . 114.6(2) no C6 C7 C8 . 114.6(2) no C7 C8 C9 . 114.4(2) no C8 C9 C10 . 114.4(2) no C9 C10 C10 2_576 114.3(2) no 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 _geom_torsion_publ_flag C2 C1 S1 H1s 67.0(10) no _journal_paper_doi 10.1107/S1600536801007188