Synthesis of 1,3-Dithiin Dithioortho Esters from the Reaction of Fischer Carbenes and 3H-1,2-Dithiole-3-thiones
Alejandro M. Granados; Jeronimo Kreiker; Rita H. de Rossi; Pedro Fuertes; Tomás Torroba; Journal of Organic Chemistry 71 (2006) 808–810; doi:10.1021/jo052168e

data_4021418
_publ_contact_author_address
;Instituto de Investigaciones en Fisico Quimica de Cordoba (INFIQC) 
Departamento de Quimica Organica 
Facultad de Ciencias Quimicas 
Universidad Nacional de Cordoba 
Ciudad Universitaria, 5000 Cordoba, Argentina
;
_publ_contact_author_email       ale@dqo.fcq.unc.edu.ar
_publ_contact_author_name        'Alejandro M. Granados'
_publ_section_title
;
 Synthesis of 1,3-Dithiin Dithioortho Esters from the Reaction
 of Fischer Carbenes and 3H-1,2-Dithiole-3-thiones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              808
_journal_page_last               810
_journal_paper_doi               10.1021/jo052168e
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C21 H20 Cr O7 S4'
_chemical_formula_sum            'C21 H20 Cr O7 S4'
_chemical_formula_weight         564.61
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.452(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3847(13)
_cell_length_b                   12.0263(13)
_cell_length_c                   19.227(2)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.05
_cell_measurement_theta_min      2.47
_cell_volume                     2610.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24994
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (SHELDRICK, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.2736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                3617
_reflns_number_total             4588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo052168esi20051017_043547.cif
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4021418