Preparation, Structure, and Redox Behavior of Bis(diarylmethylene)dihydrothiophene and Its π-Extended Analogues.
Takeda, Takashi; Akutagawa, Tomoyuki; The Journal of organic chemistry 80 (2015) 2455–2461; doi:10.1021/acs.joc.5b00021

data_4030755
_publ_section_title
;
 Preparation, Structure, and Redox Behavior of
 Bis(diarylmethylene)dihydrothiophene and Its \p-Extended Analogues.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2455
_journal_page_last               2461
_journal_paper_doi               10.1021/acs.joc.5b00021
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C34 H30 O4 S'
_chemical_formula_sum            'C34 H30 O4 S'
_chemical_formula_weight         534.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                89.9142(16)
_cell_angle_beta                 70.0107(13)
_cell_angle_gamma                72.5011(13)
_cell_formula_units_Z            2
_cell_length_a                   10.0009(3)
_cell_length_b                   11.5470(3)
_cell_length_c                   13.2679(4)
_cell_measurement_reflns_used    2999
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.09
_cell_measurement_theta_min      3.57
_cell_volume                     1364.45(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14785
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             564.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4867
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0893P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                3021
_reflns_number_total             4867
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo5b00021_si_003.cif
_cod_data_source_block           140314TT
_cod_database_code               4030755