Chelating Assistance of P‒C and P‒H Bond Activation at Palladium and Nickel: Straightforward Access to Diverse Pincer Complexes from a Diphosphine‒Phosphine Oxide
Derrah, Eric J.; Martin, Carmen; Mallet-Ladeira, Sonia; Miqueu, Karinne; Bouhadir, Ghenwa; Bourissou, Didier; Organometallics 32 (2013) 1121–; doi:10.1021/om400042v

data_4080107
_publ_section_title
;
 Chelating Assistance of P--C and P--H Bond Activation at Palladium and
 Nickel: Straightforward Access to Diverse Pincer Complexes from a
 Diphosphine--Phosphine Oxide
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1121
_journal_paper_doi               10.1021/om400042v
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H45 O7 P3 Pd2, C H2 Cl2 '
_chemical_formula_sum            'C39 H47 Cl2 O7 P3 Pd2'
_chemical_formula_weight         1004.38
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.647(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3667(5)
_cell_length_b                   10.5128(4)
_cell_length_c                   27.3848(9)
_cell_measurement_reflns_used    7954
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     4108.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28880
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8277
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+2.7157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                6113
_reflns_number_total             8277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400042v_si_002.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080107