Chemoselective Transfer Hydrogenation of α,β-Unsaturated Ketones Catalyzed by Pincer-Pd Complexes Using Alcohol as a Hydrogen Source
Ding, Boqiang; Zhang, Zhenfeng; Liu, Yangang; Sugiya, Masashi; Imamoto, Tsuneo; Zhang, Wanbin; Organic Letters 15 (2013) 3690–; doi:10.1021/ol401560q

data_1512191
_publ_section_title
;
 Chemoselective Transfer Hydrogenation of \a,\b-Unsaturated Ketones
 Catalyzed by Pincer-Pd Complexes Using Alcohol as a Hydrogen Source
;
_journal_issue                   14
_journal_name_full               'Organic Letters'
_journal_page_first              3690
_journal_paper_doi               10.1021/ol401560q
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C36 H34 O2 P2 Pd, C H Cl3'
_chemical_formula_sum            'C37 H35 Cl3 O2 P2 Pd'
_chemical_formula_weight         786.34
_chemical_name_systematic
; 
 ? 
;
_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                 111.491(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6441(8)
_cell_length_b                   11.9037(4)
_cell_length_c                   20.3524(11)
_cell_measurement_reflns_used    10313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4897
_cell_measurement_theta_min      3.2742
_cell_volume                     3526.6(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21449
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.8042
_exptl_absorpt_correction_T_min  0.7668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+4.4618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                5140
_reflns_number_total             6455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol401560q_si_003.cif
_cod_data_source_block           121127_chcl3_m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512191