Selective Hydrogenation of Amides to Amines and Alcohols Catalyzed by Improved Iron Pincer Complexes
Schneck, Felix; Assmann, Maik; Balmer, Markus; Harms, Klaus; Langer, Robert; Organometallics 35 (2016) 1931–; doi:10.1021/acs.organomet.6b00251

data_4088632
_publ_section_title
;
 Selective Hydrogenation of Amides to Amines and Alcohols Catalyzed by
 Improved Iron Pincer Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1931
_journal_paper_doi               10.1021/acs.organomet.6b00251
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C28 H59 B2 N P2'
_chemical_formula_weight         493.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                68.713(18)
_cell_angle_beta                 89.288(16)
_cell_angle_gamma                78.376(15)
_cell_formula_units_Z            2
_cell_length_a                   6.4856(8)
_cell_length_b                   15.051(4)
_cell_length_c                   17.126(4)
_cell_measurement_reflns_used    2198
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      3.24
_cell_volume                     1522.4(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, 2008) XT V2014/1 (Bruker AXS Inc., 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7362
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.279
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.0848
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.588
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.588
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3016
_reflns_number_total             7362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00251_si_006.cif
_cod_data_source_block           hklf5
_cod_database_code               4088632
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              45202
_shelx_hkl_checksum              63523