Adducts of Phenoxathiin and Thianthrene Cation Radicals with Alkenes and Cycloalkenes
Henry J. Shine; Bingjun Zhao; Ding-Quan Qian; John N. Marx; Ilse Y. Guzmán-Jiménez; John H. Thurston; T. Ould-Ely; Kenton H. Whitmire; Journal of Organic Chemistry 68 (2003) 8910–8917; doi:10.1021/jo030173h

data_4022388
_publ_contact_author
;
Henry J. Shine
Department of Chemistry and Biochemistry
Texas Tech University
Lubbock, Texas 79409
;
_publ_contact_author_email       henry.shine@ttu.edu
_publ_contact_author_fax         '806 742 1289'
_publ_contact_author_phone       '806 742 3067'
_publ_section_title
;
 Adducts of Phenoxathiin and Thianthrene Cation Radicals
 with Alkenes and Cycloalkenes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8910
_journal_page_last               8917
_journal_paper_doi               10.1021/jo030173h
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C19 H19 Cl O5 S'
_chemical_formula_weight         394.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.52(3)
_cell_angle_beta                 83.04(3)
_cell_angle_gamma                77.92(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4800(15)
_cell_length_b                   10.651(2)
_cell_length_c                   12.722(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    318(2)
_cell_measurement_theta_max      11.8
_cell_measurement_theta_min      7.6
_cell_volume                     908.2(3)
_computing_cell_refinement       'TEXSAN V5.0 (Mol.Str.Corp.1990)'
_computing_data_collection       'TEXSAN V5.0 (Mol.Str.Corp.1990)'
_computing_data_reduction        'TEXSAN V5.0 (Mol.Str.Corp.1990)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      318(2)
_diffrn_measured_fraction_theta_full 0.596
_diffrn_measured_fraction_theta_max 0.596
_diffrn_measurement_device_type  'Rigaku AFC 5S'
_diffrn_measurement_method       '2 theta-omega'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2650
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin plate'
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    'Riding Model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0717P)^2^+0.5524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                1725
_reflns_number_total             2441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo030173h_10.cif
_cod_data_source_block
"'1-(5-phenoxathiiniumyl)cycloheptene(ClO4)_qp012'"
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi scan' changed to
'psi-scan' 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_database_code               4022388