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_4108168
_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_formula_moiety         '2(C18 H32 O2 P2 Pd), 4(C F3 O3 S), H2 O '
_chemical_formula_sum            'C20 H33 F6 O8.5 P2 Pd S2'
_chemical_formula_weight         755.96
_chemical_name_systematic
;
 ?
;
_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                90.0
_cell_angle_beta                 100.165(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            16
_cell_length_a                   44.5742(18)
_cell_length_b                   11.3560(7)
_cell_length_c                   23.1131(12)
_cell_measurement_reflns_used    7975
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      2.9
_cell_volume                     11515.9(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43903
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.8313
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       box
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         11769
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                8619
_reflns_number_total             11769
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja8012903-file003_3.cif
_cod_data_source_block           Pd(BCOPE)(OTf)~2~
_cod_original_cell_volume        11515.8(10)
_cod_database_code               4108168