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_4065654
_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         'C46 H70 P3 Pd, B F4'
_chemical_formula_sum            'C46 H70 B F4 P3 Pd'
_chemical_formula_weight         909.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.7840(10)
_cell_angle_beta                 88.4170(10)
_cell_angle_gamma                76.8790(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6758(2)
_cell_length_b                   12.9640(4)
_cell_length_c                   15.5027(3)
_cell_measurement_reflns_used    28457
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2284.16(9)
_computing_cell_refinement
; 
DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) 
;
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
; 
DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) 
;
_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 9.091
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
; 
Bruker-Nonius Roper CCD camera on \k-goniostat' 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_sigmaI/netI    0.0978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38349
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.866895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.001
_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^+15.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                7841
_reflns_number_total             10447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100049n_si_001.cif
_cod_data_source_block           Structure_15b_[PdH(PCy3)(L3)][BF4]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065654