A New Tridentate Pincer Phosphine/N-Heterocyclic Carbene Ligand: Palladium Complexes, Their Structures, and Catalytic Activities
Hon Man Lee; Jing Yao Zeng; Ching-Han Hu; Ming-Tsung Lee; Inorganic Chemistry 43 (2004) 6822–6829; doi:10.1021/ic049492x

data_4311779
_publ_contact_author_address
;National Changhua University of Education
Department of Chemistry
Changhua
Taiwan
50058    
;
_publ_contact_author_email       leehm@cc.ncue.edu.tw
_publ_contact_author_fax         886(4)7211190
_publ_contact_author_name        'Hon Man Lee'
_publ_contact_author_phone       886(4)7232105X3523
_publ_section_title
;
 A New Tridentate Pincer Phosphine/N-Heterocyclic Carbene Ligand:
 Palladium Complexes, Their Structures, and Catalytic Activities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6822
_journal_page_last               6829
_journal_paper_doi               10.1021/ic049492x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C33 H33 B2 F8 N3 P2 Pd'
_chemical_formula_weight         813.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.412(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.749(3)
_cell_length_b                   12.538(2)
_cell_length_c                   20.682(4)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.6
_cell_volume                     3543.0(12)
_computing_cell_refinement       'SAINT 6.28a (Bruker, 2001)'
_computing_data_collection       'SMART 5.054 (Bruker, 2001)'
_computing_data_reduction        'SAINT 6.28a'
_computing_molecular_graphics    'SHELXTL 5.1'
_computing_publication_material  'SHELXTL 5.1'
_computing_structure_refinement  'SHELXTL 5.1'
_computing_structure_solution    'SHELXTL 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19387
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8809
_exptl_absorpt_correction_T_min  0.8475
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                4492
_reflns_number_total             6945
_reflns_threshold_expression     I>2\s
_cod_data_source_file            ic049492xsi20040806_112806_3.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        3543.2(12)
_cod_database_code               4311779