Hydrogenolysis of Palladium(II) Hydroxide, Phenoxide, and Alkoxide Complexes
Gregory R. Fulmer; Alexandra N. Herndon; Werner Kaminsky; Richard A. Kemp; Karen I. Goldberg; Journal of the American Chemical Society 133 (2011) 17713–17726; doi:10.1021/ja205824q

data_4107044
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195, USA
;
_publ_contact_author_email       kaminsky@chem.washington.edu
_publ_contact_author_fax         00(206)6858665
_publ_contact_author_name        'Werner Kaminsky'
_publ_contact_author_phone       00(206)5437585
_publ_section_title
;
 Hydrogenolysis of Palladium(II) Hydroxide, Phenoxide, and Alkoxide
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17713
_journal_page_last               17726
_journal_paper_doi               10.1021/ja205824q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C48 H88 P4 Pd2'
_chemical_formula_sum            'C48 H88 P4 Pd2'
_chemical_formula_weight         1001.86
_chemical_name_common            '[(?-tBuPCHP)Pd]2'
_chemical_name_systematic        (6)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.808(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.584(2)
_cell_length_b                   16.5920(16)
_cell_length_c                   12.0690(12)
_cell_measurement_reflns_used    342
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5048.3(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.1696
_diffrn_reflns_av_sigmaI/netI    0.3108
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.7450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.2064
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                1732
_reflns_number_total             4355
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja205824q_si_003_3.cif
_cod_data_source_block           (6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4107044