Thiopseudourea ligated palladium complexes: synthesis, characterization and application as catalysts for Suzuki‒Miyaura, Sonogashira, Heck and Hiyama reactions
Srinivas, Keesara; Srinivas, Pottabathula; Prathima, Parvathaneni Sai; Balaswamy, Kodicherla; Sridhar, Balsubramanian; Rao, Mandapati Mohan; Catalysis Science & Technology 2 (2012) 1180–; doi:10.1039/c2cy00542e

data_1556313
_publ_section_title
;
 Thiopseudourea ligated palladium complexes: synthesis, characterization
 and application as catalysts for Suzuki--Miyaura, Sonogashira, Heck and
 Hiyama reactions
;
_journal_issue                   6
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1180
_journal_paper_doi               10.1039/c2cy00542e
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C23 H20 Br N3 O3 Pd S, C2 H4 O2'
_chemical_formula_sum            'C25 H24 Br N3 O5 Pd S'
_chemical_formula_weight         664.84
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.935(5)
_cell_angle_beta                 83.939(5)
_cell_angle_gamma                89.447(5)
_cell_formula_units_Z            2
_cell_length_a                   7.724(5)
_cell_length_b                   13.385(5)
_cell_length_c                   14.000(5)
_cell_measurement_reflns_used    5032
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.64
_cell_volume                     1342.5(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12886
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The unit cell contains one acetic acid molecule which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.5153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                4381
_reflns_number_total             4716
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cy00542e.txt
_cod_data_source_block           ai
_cod_database_code               1556313