One-Pot C-H Arylation/Lactamization Cascade Reaction of Free Benzylamines.
Chand-Thakuri, Pratibha; Landge, Vinod G.; Kapoor, Mohit; Young, Michael C.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00542

data_4038315
_publ_section_title
;
 One-Pot C-H Arylation/Lactamization Cascade Reaction of Free
 Benzylamines.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00542
_journal_year                    2020
_chemical_formula_sum            'C17 H15 F2 N O'
_chemical_formula_weight         287.30
_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   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 113.721(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7435(16)
_cell_length_b                   22.987(3)
_cell_length_c                   11.0387(18)
_cell_measurement_reflns_used    8102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8
_cell_measurement_theta_min      3.393
_cell_volume                     2728.1(7)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEXIII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14507
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.897
_diffrn_reflns_theta_min         3.413
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2017)'
_exptl_crystal_colour            'translucent white'
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block-like
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   0.9940
_exptl_transmission_factor_min   0.9700
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3575
_reflns_number_total             4070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c00542_si_002.cif
_cod_data_source_block           PCT_2_207B_0m_a
_cod_original_cell_volume        2728.2(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4038315
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              7189
_shelx_hkl_checksum              58893