Hydrosilylative reduction of primary amides to primary amines catalyzed by a terminal [Ni-OH] complex.
Pandey, Pragati; Bera, Jitendra K.; Chemical communications (Cambridge, England) 57 (2021) 9204–9207; doi:10.1039/d1cc03537a

data_7128851
_publ_section_title
;
 Hydrosilylative reduction of primary amides to primary amines catalyzed
 by a terminal [Ni-OH] complex.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9204
_journal_page_last               9207
_journal_paper_doi               10.1039/d1cc03537a
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_sum            'C36 H47 F6 N9 Ni O5 S2'
_chemical_formula_weight         922.65
_space_group_crystal_system      hexagonal
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_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-08 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
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_cell_angle_gamma                120
_cell_formula_units_Z            6
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_cell_length_c                   16.1646(8)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.98
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_cell_volume                     7843.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    DIAMOND
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_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            95940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6119
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(6)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         9299
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.4831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7523
_reflns_number_total             9299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03537a2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7128847--7128851.cif.'
_cod_original_cell_volume        7843.5(8)
_cod_database_code               7128851
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.900
_exptl_absorpt_special_details   SADABS
_shelx_res_checksum              60969
_shelx_fab_checksum              60991