Palladium-Catalyzed Direct Intermolecular Amination of Unactivated Methylene C(sp3)–H Bonds with Azodiformates via Bidentate-Chelation Assistance
Bai, He-Yuan; Ma, Zhi-Gang; Yi, Min; Lin, Jun-Bing; Zhang, Shu-Yu; ACS Catalysis 7 (2017) 2042–; doi:10.1021/acscatal.6b03621

data_4514027
_publ_section_title
;
 Palladium-Catalyzed Direct Intermolecular Amination of Unactivated
 Methylene C(sp3)--H Bonds with Azodiformates via Bidentate-Chelation
 Assistance
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              2042
_journal_paper_doi               10.1021/acscatal.6b03621
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C15 H23 N3 O3'
_chemical_formula_sum            'C15 H23 N3 O3'
_chemical_formula_weight         293.36
_space_group_crystal_system      orthorhombic
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_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
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_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_c                   20.9981(12)
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_cell_measurement_theta_min      4.21
_cell_volume                     3273.3(3)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0194
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_point_group_measured_fraction_max 0.995
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_diffrn_reflns_theta_max         68.294
_diffrn_reflns_theta_min         4.211
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         2983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0465
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_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+0.8340P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                2438
_reflns_number_total             2983
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 4514027.cif.'
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_shelxl_version_number           2014-3
_shelx_res_checksum              90350
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