Palladium Catalyzed Oxidative Coupling of α-Enolic Dithioesters: A New Entry to 3,4,5-Trisubstituted 1,2-Dithiolesviaa Double Activation Strategy
Chowdhury, Sushobhan; Chanda, Tanmoy; Koley, Suvajit; Ramulu, B. Janaki; Jones, Raymond C. F.; Singh, Maya Shankar; Organic Letters 15 (2013) 5386–; doi:10.1021/ol402728y

data_1512595
_publ_section_title
;
 Palladium Catalyzed Oxidative Coupling of \a-Enolic Dithioesters: A New
 Entry to 3,4,5-Trisubstituted 1,2-Dithiolesviaa Double Activation
 Strategy
;
_journal_issue                   20
_journal_name_full               'Organic Letters'
_journal_page_first              5386
_journal_paper_doi               10.1021/ol402728y
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C19 H14 O2 S3'
_chemical_formula_sum            'C19 H14 O2 S3'
_chemical_formula_weight         370.51
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                61.296(11)
_cell_angle_beta                 87.362(9)
_cell_angle_gamma                74.901(9)
_cell_formula_units_Z            2
_cell_length_a                   7.9941(9)
_cell_length_b                   11.2961(11)
_cell_length_c                   11.4612(14)
_cell_measurement_temperature    293(2)
_cell_volume                     872.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6481
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         6481
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangualar
_exptl_crystal_F_000             384.0
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.03
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.3066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                2581
_reflns_number_total             3928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402728y_si_001.cif
_cod_data_source_block           sr-253
_cod_database_code               1512595