Direct Carbon–Carbon σ Bond Amination of Unstrained Arylalkylketones
Hu, Xinwei; Shao, Youxiang; Xie, Haisheng; Chen, Xin; Chen, Fengjuan; Ke, Zhuofeng; Jiang, Huanfeng; Zeng, Wei; ACS Catalysis  (2020) 8402–8408; doi:10.1021/acscatal.0c02683

data_4517858
_publ_section_title
;
 Direct Carbon--Carbon \s Bond Amination of Unstrained Arylalkylketones
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              8402
_journal_page_last               8408
_journal_paper_doi               10.1021/acscatal.0c02683
_journal_year                    2020
_chemical_formula_sum            'C26 H21 N3 O2 S'
_chemical_formula_weight         439.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.925(4)
_cell_length_b                   10.806(2)
_cell_length_c                   20.270(4)
_cell_measurement_reflns_used    4388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.8340
_cell_measurement_theta_min      4.3580
_cell_volume                     4360.3(15)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.876
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10055
_diffrn_reflns_point_group_measured_fraction_full 0.876
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.206
_diffrn_reflns_theta_min         2.011
_exptl_absorpt_coefficient_mu    0.178
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0810P)^2^+1.5794P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3024
_reflns_number_total             3458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02683_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4517857--4517858.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4517858
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-2
_shelx_res_checksum              59366
_shelx_hkl_checksum              5888