Using Ligand Bite Angles To Control the Hydricity of Palladium Diphosphine Complexes
James W. Raebiger; Alex Miedaner; Calvin J. Curtis; Susie M. Miller; Oren P. Anderson; Daniel L. DuBois; Journal of the American Chemical Society 126 (2004) 5502–5514; doi:10.1021/ja0395240

data_4112535
_publ_section_title
;
 Using Ligand Bite Angles To Control the Hydricity of Palladium
 Diphosphine Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5502
_journal_page_last               5514
_journal_paper_doi               10.1021/ja0395240
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C24 H58 B2 F8 O P4 Pd'
_chemical_formula_weight         766.60
_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                 111.6720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3790(8)
_cell_length_b                   16.9052(7)
_cell_length_c                   21.5603(8)
_cell_measurement_temperature    173(2)
_cell_volume                     6902.7(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51440
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             3184
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         12146
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.8842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6672
_reflns_number_total             12146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0395240si20031110_043417.cif
_cod_data_source_block           '[Pd(depp)2](BF4)2'
_cod_database_code               4112535