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_4080108
_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         'C30 H42 O P3 Pd, C F3 O3 S'
_chemical_formula_sum            'C31 H42 F3 O4 P3 Pd S'
_chemical_formula_weight         767.03
_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                 107.043(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9837(2)
_cell_length_b                   18.4157(5)
_cell_length_c                   21.5909(5)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.26
_cell_measurement_wavelength     0.71073
_cell_volume                     3415.16(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APRXII'
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61108
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         10265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                7186
_reflns_number_total             10265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400042v_si_002.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080108