Iron-Catalyzed Intermolecular Hydrothiolation of Internal Alkynes with Thiosalicylic Acids, and Sequential Intramolecular Cyclization Reaction.
Sonehara, Taro; Murakami, Shogo; Yamazaki, Sae; Kawatsura, Motoi; Organic letters 19 (2017) 4299–4302; doi:10.1021/acs.orglett.7b01953

data_1546771
_publ_section_title
;
 Iron-Catalyzed Intermolecular Hydrothiolation of Internal Alkynes with
 Thiosalicylic Acids, and Sequential Intramolecular Cyclization Reaction.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4299
_journal_page_last               4302
_journal_paper_doi               10.1021/acs.orglett.7b01953
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C17 H13 F3 O2 S'
_chemical_formula_sum            'C17 H13 F3 O2 S'
_chemical_formula_weight         338.34
_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                77.035(17)
_cell_angle_beta                 85.51(3)
_cell_angle_gamma                89.77(3)
_cell_formula_units_Z            2
_cell_length_a                   6.1950(19)
_cell_length_b                   9.868(3)
_cell_length_c                   13.376(4)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.30
_cell_volume                     794.3(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17677
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             348.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3573
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                2781
_reflns_number_total             3573
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol7b01953_si_002.cif
_cod_data_source_block           170207-C17H13F3O2S-173K-1
_cod_depositor_comments          'Adding full bibliography for 1546771.cif.'
_cod_database_code               1546771