Palladium(II) 3-Iminophosphine Complexes as Intermolecular Hydroamination Catalysts for the Formation of Imines and Enamines
Shaffer, Andrew R.; Schmidt, Joseph A. R.; Organometallics 27 (2008) 1259–; doi:10.1021/om701106q

data_4070889
_publ_section_title
;
 Palladium(II) 3-Iminophosphine Complexes as Intermolecular Hydroamination
 Catalysts for the Formation of Imines and Enamines
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1259
_journal_paper_doi               10.1021/om701106q
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C22 H26 N P'
_chemical_formula_weight         335.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                114.074(3)
_cell_angle_beta                 91.190(3)
_cell_angle_gamma                102.036(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6727(18)
_cell_length_b                   10.3984(19)
_cell_length_c                   10.748(2)
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      2.3
_cell_volume                     958.5(3)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.22'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.632
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6057
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0744P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                2551
_reflns_number_total             3022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701106q.cif
_cod_data_source_block           3IP_Ph2-Pen-tBu
_cod_database_code               4070889