Highly Selective, Efficient Deoxygenative Hydrogenation of Amides Catalyzed by a Manganese Pincer Complex via Metal-Ligand Cooperation.
Zou, You-Quan; Chakraborty, Subrata; Nerush, Alexander; Oren, Dror; Diskin-Posner, Yael; Ben-David, Yehoshoa; Milstein, David; ACS catalysis 8 (2018) 8014–8019; doi:10.1021/acscatal.8b02902

data_4515719
_publ_section_title
;
 Highly Selective, Efficient Deoxygenative Hydrogenation of Amides
 Catalyzed by a Manganese Pincer Complex via Metal-Ligand Cooperation.
;
_journal_issue                   9
_journal_name_full               'ACS catalysis'
_journal_page_first              8014
_journal_page_last               8019
_journal_paper_doi               10.1021/acscatal.8b02902
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C42 H68 Mn2 N4 O4 P4'
_chemical_formula_sum            'C42 H68 Mn2 N4 O4 P4'
_chemical_formula_weight         926.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 99.2180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6109(2)
_cell_length_b                   18.5885(2)
_cell_length_c                   21.5322(3)
_cell_measurement_reflns_used    39329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.46
_cell_volume                     4587.26(11)
_computing_cell_refinement       APEX2
_computing_data_collection       'Collect package APEX2'
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39322
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         1.455
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.8768
_exptl_absorpt_correction_T_min  0.7350
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+1.5504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8635
_reflns_number_total             10493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02902_si_002.cif
_cod_data_source_block           complex5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515719
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2014/6
_shelx_res_checksum              97971
_shelx_hkl_checksum              4091