Synthesis of 3,3-disubstituted indoline-2-thiones catalysed by an N-heterocyclic carbene
Hideo Ikota; Takayuki Ishida; Chihiro Tsukano; Yoshiji Takemoto; Chem.Commun. 50 (2014) 8871–; doi:10.1039/C4cc04047C

data_7115397
_publ_section_title
;
 Synthesis of 3,3-disubstituted indoline-2-thiones catalysed by an
 N-heterocyclic carbene
;
_journal_name_full               Chem.Commun.
_journal_page_first              8871
_journal_paper_doi               10.1039/C4cc04047C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C12.33333 H14.33333 Cl N2 O S'
_chemical_formula_weight         274.11
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            18
_cell_length_a                   22.059(5)
_cell_length_b                   22.059(5)
_cell_length_c                   14.679(3)
_cell_measurement_reflns_used    8346
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.15
_cell_volume                     6186(2)
_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      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18848
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2580.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.810
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3138
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1516P)^2^+11.0226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2761
_reflns_number_gt                1949
_reflns_number_total             3138
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc04047c2.cif
_cod_data_source_block           ikota130606
_cod_depositor_comments
;

2018-03-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C37 H43 Cl3 N6 O3 S3'
_cod_original_formula_weight         822.32
_cod_original_formula_moiety         'C37 H43 Cl3 N6 O3 S3'
_cod_original_formula_units_Z            6
_cod_original_cell_volume        6186(3)
_cod_original_sg_symbol_H-M      'R -3:H'
_cod_database_code               7115397