Structure and Conformational Properties of Diacetyl Sulfide in the Gaseous and Condensed Phases Explored by Gas Electron Diffraction, Single-Crystal X-ray Diffraction, Vibrational Spectroscopy, and Quantum Chemical Calculations
Rosana M. Romano; Carlos O. Della Védova; Anthony J. Downs; Heinz Oberhammer; Simon Parsons; Journal of the American Chemical Society 123 (2001) 12623–12631; doi:10.1021/ja0117884

data_4115853
_publ_section_title
;
 Structure and Conformational Properties of Diacetyl Sulfide in the
 Gaseous and Condensed Phases Explored by Gas Electron Diffraction,
 Single-Crystal X-ray Diffraction, Vibrational Spectroscopy, and Quantum
 Chemical Calculations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12623
_journal_page_last               12631
_journal_paper_doi               10.1021/ja0117884
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         S(COMe)2
_chemical_formula_sum            'C4 H6 O2 S'
_chemical_formula_weight         118.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.544(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.2230(7)
_cell_length_b                   11.2105(17)
_cell_length_c                   12.332(2)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     581.99(16)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3192
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.31
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.445
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    'rotating group'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.1655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                881
_reflns_number_total             1020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0117884.cif
_cod_data_source_block           C4H6O2S
_cod_original_cell_volume        581.98(16)
_cod_database_code               4115853