A Heteroleptic Palladium(II) Complex Containing a Bidentate Carbene/Amido Ligand and 3-(Trifluoromethyl)-5-(2-pyridyl)pyrazolate: Fast Catalyst Activation in the Heck Coupling Reaction
Sie, Ming-Han; Hsieh, Yuan-Hsin; Tsai, Yi-Hua; Wu, Jia-Rong; Chen, Shih-Jung; Kumar, P. Vijaya; Lii, Jenn-Huei; Lee, Hon Man; Organometallics 29 (2010) 6473–; doi:10.1021/om100819q

data_4067087
_publ_section_title
;
 A Heteroleptic Palladium(II) Complex Containing a Bidentate Carbene/Amido
 Ligand and 3-(Trifluoromethyl)-5-(2-pyridyl)pyrazolate: Fast Catalyst
 Activation in the Heck Coupling Reaction
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6473
_journal_paper_doi               10.1021/om100819q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '4(C31 H23 F3 N6 O Pd), C H2 Cl2'
_chemical_formula_sum            'C125 H94 Cl2 F12 N24 O4 Pd4'
_chemical_formula_weight         2720.74
_space_group_IT_number           2
_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                99.602(4)
_cell_angle_beta                 95.938(4)
_cell_angle_gamma                111.943(4)
_cell_formula_units_Z            1
_cell_length_a                   12.526(2)
_cell_length_b                   12.809(2)
_cell_length_c                   19.525(4)
_cell_measurement_reflns_used    6255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.3
_cell_volume                     2817.6(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29425
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.08
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_correction_T_min  0.8748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1370
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.009
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         10762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+12.7027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                7946
_reflns_number_total             10762
_reflns_threshold_expression     I>2\s
_cod_data_source_file            om100819q_si_002.cif
_cod_data_source_block           3c
_cod_database_code               4067087