A General Method for the Synthesis of Alkylenedithio- and Bis(alkylenedithio)tetraselenafulvalenes
Kazuo Takimiya; Yoshiro Kataoka; Naoto Niihara; Yoshio Aso; Tetsuo Otsubo; Journal of Organic Chemistry 68 (2003) 5217–5224; doi:10.1021/jo034145a

data_4022414
_publ_contact_author_email       ' ktakimi@hiroshima-u.ac.jp '
_publ_contact_author_fax         ' +81-824-24-5494 '
_publ_contact_author_name        ' Kazuo Takimiya '
_publ_contact_author_phone       ' +81-824-24-7734'
_publ_section_title
;
 A General Method for the Synthesis of Alkylenedithio- and
 Bis(alkylenedithio)tetraselenafulvalenes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5217
_journal_page_last               5224
_journal_paper_doi               10.1021/jo034145a
_journal_volume                  68
_journal_year                    2003
_chemical_formula_moiety         'C14 H16 O4 S2 Se4 '
_chemical_formula_sum            'C14 H16 O4 S2 Se4'
_chemical_formula_weight         628.24
_chemical_melting_point          328.6(5)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Tue Jan 7 12:08:38 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 92.73(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.502(4)
_cell_length_b                   8.811(1)
_cell_length_c                   10.208(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      15.0
_cell_volume                     2021.6(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5512
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        1.45
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.482
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.59
_refine_ls_extinction_coef       0.0030(9)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.858
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2725
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                2725
_reflns_number_total             4644
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            jo034145asi20030206_100019.cif
_cod_data_source_block           Compound_13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '55-56 C' was changed to '328.6(5)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C14 H16 O4 S2 Se4 '
_cod_database_code               4022414