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_4108167
_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         'C54 H96 P6 Pd3, C2 F6 O6 S2'
_chemical_formula_sum            'C56 H96 F6 O6 P6 Pd3 S2'
_chemical_formula_weight         1548.47
_space_group_IT_number           173
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   23.452(3)
_cell_length_b                   23.452(3)
_cell_length_c                   10.6808(15)
_cell_measurement_reflns_used    8680
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      2.1
_cell_volume                     5087.4(12)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart 1000'
_diffrn_measurement_method       '\f and \w'
_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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26852
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.862090
_exptl_absorpt_correction_T_min  0.411857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       needle
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+64.3170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                4832
_reflns_number_total             5829
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja8012903-file003_2.cif
_cod_data_source_block           '[Pd3(BCOPE)3H2](OTF)2'
_cod_original_cell_volume        5087.4(11)
_cod_database_code               4108167