Palladium(0) Complexes with Unsymmetric Bidentate Nitrogen Ligands for the Stereoselective Hydrogenation of 1-Phenyl-1-propyne to (Z)-1-Phenyl-1-propene
van Laren, Martijn W.; Duin, Marcel A.; Klerk, Chantal; Naglia, Michele; Rogolino, Dominga; Pelagatti, Paolo; Bacchi, Alessia; Pelizzi, Corrado; Elsevier, Cornelis J.; Organometallics 21 (2002) 1546–; doi:10.1021/om0108346

data_4076646
_publ_section_title
;
 Palladium(0) Complexes with Unsymmetric Bidentate Nitrogen Ligands for
 the Stereoselective Hydrogenation of 1-Phenyl-1-propyne to
 (Z)-1-Phenyl-1-propene
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1546
_journal_paper_doi               10.1021/om0108346
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C16.5 H23 Cl N2 O4 Pd'
_chemical_formula_weight         455.22
_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                 93.369(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.629(2)
_cell_length_b                   20.363(2)
_cell_length_c                   14.169(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3925.5(9)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS CCD diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40678
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856734
_exptl_absorpt_correction_type   'symmetry-related measurements'
_exptl_absorpt_process_details
'according to procedures implemented in the SADABS package'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                5907
_reflns_number_total             8001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0108346.cif
_cod_data_source_block           pdl7nik
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C16.50 H23 Cl N2 O4 Pd'
_cod_database_code               4076646