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_4074222
_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            'C32 H25 N3 O4 Pd S'
_chemical_formula_weight         654.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                91.17(3)
_cell_angle_beta                 103.84(3)
_cell_angle_gamma                94.12(3)
_cell_formula_units_Z            2
_cell_length_a                   9.291(2)
_cell_length_b                   11.288(2)
_cell_length_c                   13.748(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1395.3(5)
_computing_cell_refinement
'CrysAlis ver. 1.169.9 (Oxford Diffraction, 2002)'
_computing_data_collection
'CrysAlis ver. 1.169.9 (Oxford Diffraction, 2002)'
_computing_data_reduction
'X-RED ver. 1.22 (STOE & Cie GmbH, Darmstadt, 2001)'
_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 0.776
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measurement_device_type  'STADI4 CCD'
_diffrn_measurement_method       omega
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6001
_diffrn_reflns_theta_full        29.45
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.958
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1833P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2397
_reflns_number_gt                2963
_reflns_number_total             6001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0604728si20060529_095245.cif
_cod_data_source_block           nafto
_cod_original_sg_symbol_H-M      'P-1 (No.2)'
_cod_database_code               4074222