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_4088631
_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_moiety         'C57 H113 B3 Fe N2 O P4, 1.5(C6 H14)'
_chemical_formula_sum            'C66 H134 B3 Fe N2 O P4'
_chemical_formula_weight         1183.91
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.23(3)
_cell_angle_beta                 93.46(3)
_cell_angle_gamma                98.10(3)
_cell_formula_units_Z            2
_cell_length_a                   14.370(3)
_cell_length_b                   14.854(3)
_cell_length_c                   16.803(3)
_cell_measurement_reflns_used    1398
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.49
_cell_measurement_theta_min      3.61
_cell_volume                     3536.7(12)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2g (Brandenburg 2011) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'STOE IPDS2'
_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  0.0743
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33399
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.751
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         12325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2573
_refine_ls_wR_factor_ref         0.2657
_reflns_number_gt                9942
_reflns_number_total             12325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00251_si_004.cif
_cod_data_source_block           fsma89a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4088631
_plat029_alert_3_a
;
PROBLEM: Low data completeness at high theta angles (93.4%)
RESPONSE: Despite several attempts a strong decay of the scattering power with diffraction angle was observed. 
The resulting low data completeness at high theta angles remained despite several measurements.
The Level A alert for the data completeness of 93.4% reflects the poor quality of the crystals. 
Nonetheless, the quality of the measurement is sufficient to interpret the chemical connectivity in this structure.
;