Role of the Ligand and of the Size and Flexibility of the Palladium−Ancillary Ligand Cycle on the Reactivity of Substituted Alkynes toward Palladium(0) Complexes Bearing Potentially Terdentate Nitrogen−Sulfur−Nitrogen or Nitrogen−Nitrogen−Nitrogen Ligands: Kinetic and Structural Study
Canovese, Luciano; Visentin, Fabiano; Chessa, Gavino; Uguagliati, Paolo; Levi, Carlo; Dolmella, Alessandro; Bandoli, Giuliano; Organometallics 25 (2006) 5355–; doi:10.1021/om0604728

data_4074220
_publ_section_title
;
 Role of the Ligand and of the Size and Flexibility of the
 Palladium&#x2212;Ancillary Ligand Cycle on the Reactivity of Substituted
 Alkynes toward Palladium(0) Complexes Bearing Potentially Terdentate
 Nitrogen&#x2212;Sulfur&#x2212;Nitrogen or
 Nitrogen&#x2212;Nitrogen&#x2212;Nitrogen Ligands:&#x00A0; Kinetic and
 Structural Study
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5355
_journal_paper_doi               10.1021/om0604728
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C33 H33 Cl2 N3 O10 Pd S'
_chemical_formula_weight         840.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'heavy-atom methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.856(2)
_cell_length_b                   20.630(4)
_cell_length_c                   16.833(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      8.1
_cell_volume                     3631.4(13)
_computing_cell_refinement       'FEBO system'
_computing_data_collection       'FEBO system'
_computing_data_reduction        'FEBO system'
_computing_molecular_graphics    'SHELXTL NT ver. 5.10 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL NT ver. 5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT ver. 5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.689
_diffrn_measured_fraction_theta_max 0.689
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       'omega-2 theta'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5140
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        negligible
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0467P)^2^+15.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                4785
_reflns_number_total             4923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0604728si20060529_095245.cif
_cod_data_source_block           sigla
_cod_original_cell_volume        3631(1)
_cod_original_sg_symbol_H-M      'P2(1)/n (No.14)'
_cod_database_code               4074220