Design of Cationic Mixed Phosphine/N-Heterocyclic Carbene Palladium(II) π-Allyl Complexes as Monoligated Phosphine Pd(0) Precatalysts: Synthesis, Structural Studies, Catalysis, and Reactivity
Normand, Adrien T.; Stasch, Andreas; Ooi, Li-Ling; Cavell, Kingsley J.; Organometallics 27 (2008) 6507–; doi:10.1021/om8008052

data_4072380
_publ_section_title
;
 Design of Cationic Mixed Phosphine/N-Heterocyclic Carbene Palladium(II)
 \p-Allyl Complexes as Monoligated Phosphine Pd(0) Precatalysts:
 Synthesis, Structural Studies, Catalysis, and Reactivity
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6507
_journal_paper_doi               10.1021/om8008052
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31 H38 B F4 N2 P Pd'
_chemical_formula_weight         662.81
_chemical_name_common            kjc0722
_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                 101.5560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0190(2)
_cell_length_b                   17.6620(4)
_cell_length_c                   15.6070(3)
_cell_measurement_reflns_used    22525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2975.83(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997'
_computing_molecular_graphics    'Ortep-99 for Windows (Farrugia, 1995)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    ' Dirdiff-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.1404
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35507
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.8393
_exptl_absorpt_correction_T_min  0.7359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6815
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.5569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                5156
_reflns_number_total             6815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008052_si_008.cif
_cod_data_source_block           kjc0722
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072380