Nitrogen atom insertion into arenols to access benzazepines.
He, Yi; Wang, Juanjuan; Zhu, Tongtong; Zheng, Zhaojing; Wei, Hao; Chemical science 15 (2024) 2612–2617; doi:10.1039/d3sc05367a

data_1570782
_publ_section_title
;
 Nitrogen atom insertion into arenols to access benzazepines.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2612
_journal_page_last               2617
_journal_paper_doi               10.1039/d3sc05367a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C17 H10 Br N O3'
_chemical_formula_sum            'C17 H10 Br N O3'
_chemical_formula_weight         356.17
_chemical_name_systematic        29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4496(2)
_cell_length_b                   20.6183(6)
_cell_length_c                   13.2918(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      57.05
_cell_measurement_theta_min      2.94
_cell_volume                     1471.45(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14842
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.048
_diffrn_reflns_theta_min         3.478
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       Block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0519P)^2^+0.6028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2703
_reflns_number_total             2964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05367a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1570782--1570784.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1570782
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.653
_shelx_estimated_absorpt_t_max   0.747
_shelx_res_checksum              96185
_shelx_hkl_checksum              26711