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_4065655
_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         '2(C28 H34 Cl2 P2 Pt), 2(C H2 Cl2)'
_chemical_formula_sum            'C29 H37 Cl4 P2 Pt'
_chemical_formula_weight         784.40
_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                 100.803(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.8721(7)
_cell_length_b                   14.8743(4)
_cell_length_c                   17.4941(5)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.60
_cell_volume                     6612.9(3)
_computing_cell_refinement       'Apex II (Bruker-AXS, 2007)'
_computing_data_collection       'Apex II (Bruker-AXS, 2007)'
_computing_data_reduction
; 
 SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) 
;
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            146657
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    4.680
_exptl_absorpt_correction_T_max  0.4309
_exptl_absorpt_correction_T_min  0.3776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs - bruker 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
Disordered solvent squeeze from unit cell.
;
_refine_diff_density_max         8.377
_refine_diff_density_min         -3.772
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         20311
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0007P)^2^+189.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                14525
_reflns_number_total             20311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100049n_si_001.cif
_cod_data_source_block           Structure_16_[PtCl2(L4)]
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4065655