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_4515718
_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         'C21 H36 Mn N O2 P2'
_chemical_formula_sum            'C21 H36 Mn N O2 P2'
_chemical_formula_weight         451.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.1920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6272(2)
_cell_length_b                   10.62300(10)
_cell_length_c                   23.1001(3)
_cell_measurement_reflns_used    13714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.6610
_cell_measurement_theta_min      4.8020
_cell_volume                     4484.04(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24184
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.065
_diffrn_reflns_theta_min         4.815
_exptl_absorpt_coefficient_mu    6.254
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+4.0133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4524
_reflns_number_total             4854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02902_si_002.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4515718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              36255
_shelx_hkl_checksum              78870