Synthesis and Characterization of Imine-Palladacycles Containing Imidate “Pseudohalide” Ligands: Efficient Suzuki‒Miyaura Cross-Coupling Precatalysts and Their Activation To Give Pd0LnSpecies (L = Phosphine)
Serrano, José Luis; García, Luis; Pérez, José; Pérez, Eduardo; García, Joaquín; Sánchez, Gregorio; Sehnal, Petr; De Ornellas, Sara; Williams, Thomas J.; Fairlamb, Ian J. S.; Organometallics 30 (2011) 5095–; doi:10.1021/om2002443

data_4064656
_publ_section_title
;
 Synthesis and Characterization of Imine-Palladacycles Containing Imidate
 &#x201C;Pseudohalide&#x201D; Ligands: Efficient Suzuki--Miyaura
 Cross-Coupling Precatalysts and Their Activation To Give Pd0LnSpecies (L
 = Phosphine)
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5095
_journal_paper_doi               10.1021/om2002443
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C34 H20 Br4 N4 O4 Pd2, 2(C3 H6 O)'
_chemical_formula_sum            'C40 H32 Br4 N4 O6 Pd2'
_chemical_formula_weight         1197.14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8215(8)
_cell_length_b                   11.6601(6)
_cell_length_c                   22.6230(11)
_cell_measurement_temperature    100(2)
_cell_volume                     4137.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.936
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46483
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    4.783
_exptl_absorpt_correction_T_max  0.5976
_exptl_absorpt_correction_T_min  0.3279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+2.6991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                8495
_reflns_number_total             9566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2002443_si_002.cif
_cod_data_source_block           23dibrs(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4064656