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_4112534
_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            'C46 H64 O2 P4 Pd'
_chemical_formula_weight         879.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                90.503(3)
_cell_angle_beta                 109.192(3)
_cell_angle_gamma                106.287(3)
_cell_formula_units_Z            2
_cell_length_a                   11.087(2)
_cell_length_b                   14.170(3)
_cell_length_c                   15.859(3)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      3.23
_cell_volume                     2244.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14341
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      0
_exptl_crystal_description       plates
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0398(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                5822
_reflns_number_total             6433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0395240si20031110_043402.cif
_cod_data_source_block           Pd(EtXantphos)2
_cod_original_cell_volume        2244.7(7)
_cod_database_code               4112534