Reactivity Studies of Cationic Palladium(II) Phosphine Carboxylate Complexes with Lewis Bases: Substitution versus Cyclometalation
Thirupathi, Natesan; Amoroso, Dino; Bell, Andrew; Protasiewicz, John D.; Organometallics 26 (2007) 3157–; doi:10.1021/om070069g

data_4073099
_publ_section_title
;
 Reactivity Studies of Cationic Palladium(II) Phosphine Carboxylate
 Complexes with Lewis Bases:&#x00A0; Substitution versus Cyclometalation
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3157
_journal_paper_doi               10.1021/om070069g
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C69 H79 B F20 N2 O2 P2 Pd'
_chemical_formula_weight         1527.49
_space_group_IT_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                69.387(10)
_cell_angle_beta                 67.634(12)
_cell_angle_gamma                88.773(12)
_cell_formula_units_Z            2
_cell_length_a                   14.910(3)
_cell_length_b                   15.0468(19)
_cell_length_c                   18.300(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3523.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12135
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.407
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         10751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.950
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+6.9724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                6913
_reflns_number_total             10751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070069g-file001.cif
_cod_data_source_block           pddmpy
_cod_original_cell_volume        3523.5(9)
_cod_database_code               4073099