Pd(I) Phosphine Carbonyl and Hydride Complexes Implicated in the Palladium-Catalyzed Oxo Process
Miguel Baya; Jennifer Houghton; Denes Konya; Yohan Champouret; Jean-Claude Daran; Karina Q. Almeida Leñero; Lodewijk Schoon; Wilhelmus P. Mul; A. Bart van Oort; Nicolaas Meijboom; Eite Drent; A. Guy Orpen; Rinaldo Poli; Journal of the American Chemical Society 130 (2008) 10612–10624; doi:10.1021/ja8012903

data_4108166
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_name        'Daran, Jean-Claude'
_publ_contact_author_phone       ' (33) 5 61 33 31 74 '
_publ_section_title
;
 Pd(I) Phosphine Carbonyl and Hydride Complexes Implicated in the
 Palladium-Catalyzed Oxo Process
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10612
_journal_page_last               10624
_journal_paper_doi               10.1021/ja8012903
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H64 O2 P4 Pd2, 2(C F3 O3 S) '
_chemical_formula_sum            'C40 H64 F6 O8 P4 Pd2 S2'
_chemical_formula_weight         1187.71
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.834(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3241(6)
_cell_length_b                   13.0746(6)
_cell_length_c                   21.2901(8)
_cell_measurement_reflns_used    17091
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      2.7
_cell_volume                     4736.4(3)
_computing_cell_refinement
;
CrysAlis RED, Version 1.170.32 (Oxford Diffraction, 2003)

;
_computing_data_collection
;
CrysAlis CCD, Version 1.170.32 (Oxford Diffraction, 2003)
;
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000    0.0000    0.0000    0.0000 115

  2 omega  -54.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000   90.0000    0.0000    0.0000 115

  3 omega  -54.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  180.0000    0.0000    0.0000 115

  4 omega  -54.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  270.0000    0.0000    0.0000 89

;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_diffrn_orient_matrix_UB_11      -0.0308154265
_diffrn_orient_matrix_UB_12      -0.0124057781
_diffrn_orient_matrix_UB_13      0.0163930744
_diffrn_orient_matrix_UB_21      -0.0279738425
_diffrn_orient_matrix_UB_22      0.0178216973
_diffrn_orient_matrix_UB_23      -0.0264112851
_diffrn_orient_matrix_UB_31      -0.0023656697
_diffrn_orient_matrix_UB_32      -0.0497146889
_diffrn_orient_matrix_UB_33      -0.0135761919
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33348
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK (Oxford-Diffraction, 2005)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       box
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.040
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9655
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+22.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                8374
_reflns_number_total             9655
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja8012903-file003_1.cif
_cod_data_source_block           Pd~2~(BCOPE)~2~(CO)~2~](OTf)~2~
_cod_database_code               4108166