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_4107046
_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         'C26 H47 F O P2 Pd'
_chemical_formula_sum            'C26 H47 F O P2 Pd'
_chemical_formula_weight         562.98
_chemical_name_common            (tBuPCP)PdOCH2CH2F
_chemical_name_systematic        (10)
_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
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_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2010-11-23T15:14:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.562(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9157(19)
_cell_length_b                   12.4921(11)
_cell_length_c                   10.8131(9)
_cell_measurement_reflns_used    715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2757.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            104443
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.61
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+11.3398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                7202
_reflns_number_total             8322
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja205824q_si_003_5.cif
_cod_data_source_block           (10)
_cod_database_code               4107046