Metal-free nitroxyl radical-mediated β-C(sp(3))-H amination of saturated ketones with heteroaryl halides: multiple roles of TEMPO.
Qian, Ping; Deng, Yu; Mei, Haibo; Han, Jianlin; Pan, Yi; Chemical communications (Cambridge, England) 53 (2017) 2958–2961; doi:10.1039/c7cc00145b

data_7119769
_publ_section_title
;
 Metal-free nitroxyl radical-mediated \b-C(sp(3))-H amination of saturated
 ketones with heteroaryl halides: multiple roles of TEMPO.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2958
_journal_page_last               2961
_journal_paper_doi               10.1039/c7cc00145b
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C25 H20 Br2 N2 O3'
_chemical_formula_weight         556.25
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-25 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0522
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_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_limit_k_max       6
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15632
_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_reflns_theta_max         25.010
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+0.4461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                2822
_reflns_number_total             3928
_reflns_threshold_expression     'I > 2\s(I)'
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