#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/03/2200338.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_2200338 loop_ _publ_author_name 'Fronczek, Frank R.' 'Johnson, Rolanda J.' 'Strongin, Robert M.' _publ_section_title ; Trimethylsulfonium methanesulfonate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o447 _journal_page_last o448 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C3 H9 S 1+, C H3 O3 S 1-' _chemical_formula_moiety 'C3 H9 S 1+, C H3 O3 S 1-' _chemical_formula_sum 'C4 H12 O3 S2' _chemical_formula_weight 172.26 _chemical_name_systematic ; trimethylsulfonium methanesulfonate ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.6157(4) _cell_length_b 8.2419(4) _cell_length_c 7.5397(8) _cell_measurement_reflns_used 7642 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.0 _cell_measurement_theta_min 2.5 _cell_volume 783.96(9) _computing_cell_refinement 'DENZO and SCALEPACK' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_data_reduction 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR (Altomare et al., 1994)' _diffrn_ambient_temperature 120 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'KappaCCD diffractometer (with Oxford Cryosystems Cryostream cooler)' _diffrn_measurement_method '\w scans with \k offsets' _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 .047 _diffrn_reflns_av_sigmaI/netI .062 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7642 _diffrn_reflns_theta_full 30.05 _diffrn_reflns_theta_max 30.1 _diffrn_reflns_theta_min 3.1 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .620 _exptl_absorpt_correction_T_max .988 _exptl_absorpt_correction_T_min .936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL SCALEPACK (Otwinowski & Minor 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 368 _exptl_crystal_size_max .12 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .02 _refine_diff_density_max .40 _refine_diff_density_min -.37 _refine_ls_extinction_coef .0067(18) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 69 _refine_ls_number_reflns 1222 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all .074 _refine_ls_R_factor_gt .039 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.2622P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .089 _reflns_number_gt 838 _reflns_number_total 1222 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file om6021.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200338 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, 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 .67208(5) .2500 .27070(8) .0207(2) Uani d S 1 . . S O1 .57403(15) .2500 .1667(2) .0272(5) Uani d S 1 . . O O2 .68432(11) .10235(18) .37463(18) .0321(4) Uani d . 1 . . O C1 .7765(2) .2500 .1161(4) .0259(6) Uani d S 1 . . C H1A .844(3) .2500 .188(4) .039 Uiso d S 1 . . H H1B .7715(17) .152(3) .050(3) .039 Uiso d . 1 . . H S2 .51948(6) .7500 .30929(8) .0249(2) Uani d S 1 . . S C2 .6201(2) .7500 .1426(4) .0285(7) Uani d S 1 . . C H2A .582(3) .7500 .017(4) .043 Uiso d S 1 . . H H2B .6628(17) .658(3) .165(3) .043 Uiso d . 1 . . H C3 .43915(17) .5829(3) .2433(3) .0288(5) Uani d . 1 . . C H3A .4185(17) .607(3) .123(3) .043 Uiso d . 1 . . H H3B .3798(19) .582(3) .321(3) .043 Uiso d . 1 . . H H3C .480(2) .490(3) .257(3) .043 Uiso d . 1 . . 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 .0226(3) .0211(3) .0183(3) .000 .0001(3) .000 O1 .0232(10) .0323(11) .0260(10) .000 -.0020(8) .000 O2 .0370(9) .0307(8) .0286(7) -.0008(7) -.0002(6) .0120(6) C1 .0271(16) .0258(16) .0246(14) .000 .0044(12) .000 S2 .0235(4) .0318(4) .0196(3) .000 -.0010(3) .000 C2 .0212(14) .0309(17) .0335(16) .000 .0071(13) .000 C3 .0262(11) .0237(10) .0364(12) -.0011(9) .0046(9) .0030(10) 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 O1 . 1.4646(19) y S1 O2 . 1.4556(14) y S1 O2 8_565 1.4556(14) ? S1 C1 . 1.759(3) y C1 H1A . 1.01(3) ? C1 H1B . .95(2) ? S2 C2 . 1.786(3) y S2 C3 . 1.781(2) y S2 C3 8_575 1.781(2) ? C2 H2A . 1.06(3) ? C2 H2B . .95(2) ? C3 H3A . .97(2) ? C3 H3B . .95(2) ? C3 H3C . .92(3) ? 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 _geom_angle_publ_flag O2 S1 O1 8_565 . 112.20(7) ? O2 S1 O1 . . 112.20(7) y O2 S1 O2 8_565 . 113.45(12) y O1 S1 C1 . . 106.11(13) y O2 S1 C1 8_565 . 106.11(8) ? O2 S1 C1 . . 106.11(8) y S1 C1 H1A . . 105.8(18) ? S1 C1 H1B . . 107.2(13) ? H1A C1 H1B . . 109.6(15) ? C3 S2 C3 . 8_575 101.31(15) y C3 S2 C2 . . 102.00(10) y C3 S2 C2 8_575 . 102.00(10) ? S2 C2 H2A . . 107.7(17) ? S2 C2 H2B . . 106.1(13) ? H2A C2 H2B . . 114.7(16) ? S2 C3 H3A . . 105.0(15) ? S2 C3 H3B . . 106.4(15) ? H3A C3 H3B . . 111.8(19) ? S2 C3 H3C . . 107.1(15) ? H3A C3 H3C . . 115(2) ? H3B C3 H3C . . 111(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C1 H1B O2 2_654 .95(2) 2.54(2) 3.463(2) 163.5(18) C2 H2A O1 4_655 1.06(3) 2.41(3) 3.382(4) 152(2) C3 H3A O1 4_655 .97(2) 2.48(2) 3.388(3) 156.0(19) C3 H3B O2 4_656 .95(2) 2.44(2) 3.279(3) 147.3(19) C3 H3C O1 . .92(3) 2.41(3) 3.280(2) 157.1(19)