A New Approach to 4-Alkylthio-1,3-dithiole-2-thione: An Unusual Reaction of a Zinc Complex of 1,3-Dithole-2-thione-4,5-dithiolate
Jia, Chunyang; Zhang, Deqing; Xu, Wei; Zhu, Daoben; Organic Letters 3 (2001) 1941–; doi:10.1021/ol015990n

data_1507515
_publ_section_title
;
 A New Approach to 4-Alkylthio-1,3-dithiole-2-thione:&#x2009; An Unusual
 Reaction of a Zinc Complex of 1,3-Dithole-2-thione-4,5-dithiolate
;
_journal_issue                   12
_journal_name_full               'Organic Letters'
_journal_page_first              1941
_journal_paper_doi               10.1021/ol015990n
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C9 H7 N S4'
_chemical_formula_weight         257.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.996(3)
_cell_length_b                   7.934(2)
_cell_length_c                   22.205(4)
_cell_measurement_reflns_used    2434
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     2156.6(9)
_computing_cell_refinement
'Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381 USA.''
_computing_data_collection
'Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.''
_computing_data_reduction
'Sheldrick, G. M. (1997) SHELXS97, Program for the Solution of Crystal Structure, University of Gottingen, Germany.''
_computing_molecular_graphics
'Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.''
_computing_publication_material
'Sheldrick, G. M. (1997) SHELXL97, Program for the refinement of Crystal Structure, University of Gottingen, Germany.''
_computing_structure_refinement
'Sheldrick, G. M. (1997) SHELXL97, Program for the Refinement of Crystal Structure, University of Gottingen, Germany.''
_computing_structure_solution
'Sheldrick, G. M. (1997) SHELXS97, Program for the Solution of Crystal Structure, University of Gottingen, Germany.''
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS RIPAD IP'
_diffrn_measurement_method       Oscillation
_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  0.02563
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            2434
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  1.0957
_exptl_absorpt_correction_T_min  0.8490
_exptl_absorpt_correction_type   'ABSOR by T. Higashi'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          '0.1 mm'
_exptl_crystal_size_mid          '0.1 mm'
_exptl_crystal_size_min          '0.1 mm'
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+4.0078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2152
_reflns_number_total             2434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol015990n_s1.cif
_cod_data_source_block           compound_3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2156.6(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1507515