The Mechanism of Efficient Asymmetric Transfer Hydrogenation of Acetophenone Using an Iron(II) Complex Containing an (S,S)-Ph2PCH2CH=NCHPhCHPhN=CHCH2PPh2 Ligand: Partial Ligand Reduction Is the Key
Alexandre A. Mikhailine; Mazharul I. Maishan; Alan J. Lough; Robert H. Morris; Journal of the American Chemical Society 134 (2012) 12266–12280; doi:10.1021/ja304814s

data_4118356
_publ_section_title
;
 The Mechanism of Efficient Asymmetric Transfer Hydrogenation of
 Acetophenone Using an Iron(II) Complex Containing an
 (S,S)-Ph2PCH2CH=NCHPhCHPhN=CHCH2PPh2 Ligand: Partial Ligand Reduction Is
 the Key
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12266
_journal_page_last               12280
_journal_paper_doi               10.1021/ja304814s
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H42 Br Fe N2 O P2, C24 H20 B'
_chemical_formula_sum            'C67 H62 B Br Fe N2 O P2'
_chemical_formula_weight         1119.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.522(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2639(3)
_cell_length_b                   16.1292(3)
_cell_length_c                   20.9014(4)
_cell_measurement_reflns_used    66102
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     5809.06(19)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23920
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1341
_refine_ls_number_reflns         23920
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                14662
_reflns_number_total             23920
_reflns_threshold_expression     I.2\s(I)
_cod_data_source_file            ja304814s_si_002.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        5809.06(18)
_cod_database_code               4118356