Regioselective hydrothiolation of alkynes by sulfonyl hydrazides using organic ionic base-Brønsted Acid.
Singh, Rahul; Raghuvanshi, Dushyant Singh; Singh, Krishna Nand; Organic letters 15 (2013) 4202–4205; doi:10.1021/ol401925u

data_1512232
_publ_section_title
;
 Regioselective hydrothiolation of alkynes by sulfonyl hydrazides using
 organic ionic base-Br\/onsted Acid.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4202
_journal_page_last               4205
_journal_paper_doi               10.1021/ol401925u
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C15 H14 S'
_chemical_formula_weight         226.33
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.00(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.335(3)
_cell_length_b                   17.041(4)
_cell_length_c                   8.600(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1229.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.859
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5517
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.0731
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                1149
_reflns_number_total             2828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol401925u_si_002.cif
_cod_data_source_block           ra-3
_cod_original_cell_volume        1229.6(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512232