Kinetic and Electrochemical Studies of the Oxidative Addition of Demanding Organic Halides to Pd(0): the Efficiency of Polyphosphane Ligands in Low Palladium Loading Cross-Couplings Decrypted
Veronika A. Zinovyeva; Sophal Mom; Sophie Fournier; Charles H. Devillers; Hélène Cattey; Henri Doucet; Jean-Cyrille Hierso; Dominique Lucas; Inorganic Chemistry 52 (2013) 11923–11933; doi:10.1021/ic401613w

data_4336431
_publ_contact_author_address
;
ICMUB UMR 6302
Universit\'e de Bourgogne
Facult\'e des Sciences
9 Avenue Alain Savary
21000 DIJON
France
;
_publ_contact_author_email       hcattey@u-bourgogne.fr
_publ_contact_author_fax         +33-0380393835
_publ_contact_author_name        'Cattey, H\'el\`ene'
_publ_contact_author_phone       +33-0380393665
_publ_section_title
;
 Kinetic and Electrochemical Studies of the Oxidative Addition of
 Demanding Organic Halides to Pd(0): the Efficiency of Polyphosphane
 Ligands in Low Palladium Loading Cross-Couplings Decrypted
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11923
_journal_page_last               11933
_journal_paper_doi               10.1021/ic401613w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'0.84(C67 H64 Cl2 Fe P4 Pd), 0.16(C66 H62 Cl2 Fe P4 Pd), C H2 Cl2'
_chemical_formula_sum            'C67.84 H65.68 Cl4 Fe P4 Pd'
_chemical_formula_weight         1308.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             date
_audit_creation_method           'wingx routine cif_update'
_audit_update_record
;
2009-01-09 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 120.253(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3917(4)
_cell_length_b                   20.0428(6)
_cell_length_c                   25.2108(6)
_cell_measurement_reflns_used    70782
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6281.7(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45553
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.0221
_exptl_absorpt_correction_T_min  0.7643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       prism
_exptl_crystal_F_000             2691
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         14200
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0000P)^2^+28.9046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                13262
_reflns_number_total             14200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401613w_si_002.cif
_cod_data_source_block           1112cd24abs
_cod_database_code               4336431