Regioselective Hydromethoxycarbonylation of Terminal Alkynes Catalyzed by Palladium(II)‒Tetraphos Complexes
Oberhauser, Werner; Ienco, Andrea; Vizza, Francesco; Trettenbrein, Barbara; Oberhuber, Dennis; Strabler, Christof; Ortner, Teresa; Brüggeller, Peter; Organometallics 31 (2012) 4832–; doi:10.1021/om3003812

data_4078737
_publ_section_title
;
 Regioselective Hydromethoxycarbonylation of Terminal Alkynes Catalyzed by
 Palladium(II)--Tetraphos Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4832
_journal_paper_doi               10.1021/om3003812
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C54 H50 Cl2 P4 Pd2, 4(C3 H7 N O)'
_chemical_formula_sum            'C66 H78 Cl2 N4 O4 P4 Pd2'
_chemical_formula_weight         1398.90
_chemical_name_systematic        '[Pd2(CH3)2Cl2(dppcb)]'
_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                73.181(3)
_cell_angle_beta                 84.086(3)
_cell_angle_gamma                76.133(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4567(4)
_cell_length_b                   12.3501(4)
_cell_length_c                   12.3652(5)
_cell_measurement_temperature    170(2)
_cell_volume                     1624.85(11)
_computing_molecular_graphics    'SHELXTL-NT V6.1'
_computing_publication_material  'SHELXTL-NT V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22640
_diffrn_reflns_theta_full        72.42
_diffrn_reflns_theta_max         72.42
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.542
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.141
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0905P)^2^+2.5791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                5900
_reflns_number_total             6430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003812_si_008.cif
_cod_data_source_block           2
_cod_database_code               4078737