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_4078736
_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         'C26 H28 O2 P2 Pd, 2(C7 H7 O3 S)'
_chemical_formula_sum            'C40 H42 O8 P2 Pd S2'
_chemical_formula_weight         883.22
_chemical_name_systematic        '[Pd(dppe)(H2O)2](OTs)2'
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 95.940(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.0836(3)
_cell_length_b                   9.2876(1)
_cell_length_c                   18.8179(2)
_cell_measurement_temperature    150(2)
_cell_volume                     4012.73(8)
_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      150(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8936
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         4.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8936
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0254P)^2^+1.2589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                8696
_reflns_number_total             8936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003812_si_008.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4078736