Palladium Complexes of the Heterodiphosphineo-C6H4(CH2PtBu2)(CH2PPh2) Are Highly Selective and Robust Catalysts for the Hydromethoxycarbonylation of Ethene
Fanjul, Tamara; Eastham, Graham; Fey, Natalie; Hamilton, Alex; Orpen, A. Guy; Pringle, Paul G.; Waugh, Mark; Organometallics 29 (2010) 2292–; doi:10.1021/om100049n

data_4065653
_publ_section_title
;
 Palladium Complexes of the Heterodiphosphineo-C6H4(CH2PtBu2)(CH2PPh2) Are
 Highly Selective and Robust Catalysts for the Hydromethoxycarbonylation
 of Ethene
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2292
_journal_paper_doi               10.1021/om100049n
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C29 H39 Cl P2 Pd'
_chemical_formula_sum            'C29 H39 Cl P2 Pd'
_chemical_formula_weight         591.39
_chemical_name_systematic
; 
 ? 
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.777(3)
_cell_length_b                   12.854(3)
_cell_length_c                   17.241(3)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4495
_cell_measurement_theta_min      2.289
_cell_volume                     2731.9(11)
_computing_cell_refinement       'SMART v5.628 (Bruker-AXS, 1997-2002)'
_computing_data_collection       'SMART v5.628 (Bruker-AXS, 1997-2002)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28362
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.874676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADBABS V2.05'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6291
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0261P)^2^+0.5231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                5013
_reflns_number_total             6291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100049n_si_001.cif
_cod_data_source_block           Structure_14a_[PtClMe(L3)]
_cod_original_cell_volume        2731.7(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4065653