Synthesis of Isolable Thiirane-2-thione (α-Dithiolactone) from Thioketene S-Oxide
Kentaro Okuma; Toshiyuki Shigetomi; Yoshinori Nibu; Kosei Shioji; Masato Yoshida; Yoshinobu Yokomori; Journal of the American Chemical Society 126 (2004) 9508–9509; doi:10.1021/ja0480320

data_4112824
_publ_contact_author_address
;
Department of Chemistry, Faculty of Science, Fukuoka University, 
Jonan-ku, Fukuoka 814-0180
;
_publ_contact_author_email       kokuma@fukuoka-u.ac.jp
_publ_contact_author_fax         +81-92-865-6030
_publ_contact_author_name        'Kentaro Okuma'
_publ_contact_author_phone       '+81-92-871-6631 (Ext 6210)'
_publ_section_title
;
 Synthesis of Isolable Thiirane-2-thione (\a-Dithiolactone) from
 Thioketene S-Oxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9508
_journal_page_last               9509
_journal_paper_doi               10.1021/ja0480320
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C10 H18 O S2 '
_chemical_formula_sum            'C10 H18 O S2'
_chemical_formula_weight         218.381
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 92.372(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7860(3)
_cell_length_b                   12.0280(4)
_cell_length_c                   11.2040(4)
_cell_measurement_temperature    298
_cell_volume                     1183.00(7)
_computing_cell_refinement       Scalepack(HKL)
_computing_data_collection       'DIP Image plate'
_computing_data_reduction        'maXus (Mackay et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device       'DIP Image plate'
_diffrn_measurement_method       IP
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.03154
_diffrn_orient_matrix_UB_12      0.00771
_diffrn_orient_matrix_UB_13      -0.10915
_diffrn_orient_matrix_UB_21      0.07286
_diffrn_orient_matrix_UB_22      -0.03282
_diffrn_orient_matrix_UB_23      -0.02337
_diffrn_orient_matrix_UB_31      -0.03652
_diffrn_orient_matrix_UB_32      -0.08179
_diffrn_orient_matrix_UB_33      0.00102
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' CuK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3175
_diffrn_reflns_theta_full        70.06
_diffrn_reflns_theta_max         70.06
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       Cube
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+0.3845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2069
_reflns_number_gt                1843
_reflns_number_total             2053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0480320si20040629_014619.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+0.3845P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1448P)^2^+0.3845P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C10 H18 O S2 '
_cod_database_code               4112824
_cod_database_fobs_code          4112824