Stereochemistry of N-Benzoyl-5-substituted-1-benzazepines Revisited: Synthesis of the Conformationally Biased Derivatives and Revision of the Reported Structure.
Tabata, Hidetsugu; Yoneda, Tetsuya; Tasaka, Tomohiko; Ito, Shigekazu; Oshitari, Tetsuta; Takahashi, Hideyo; Natsugari, Hideaki; The Journal of organic chemistry 81 (2016) 3136–3148; doi:10.1021/acs.joc.5b02900

data_4036595
_publ_section_title
;
 Stereochemistry of N-Benzoyl-5-substituted-1-benzazepines Revisited:
 Synthesis of the Conformationally Biased Derivatives and Revision of the
 Reported Structure.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3136
_journal_page_last               3148
_journal_paper_doi               10.1021/acs.joc.5b02900
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C18 H18 Cl N O'
_chemical_formula_sum            'C18 H18 Cl N O'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.4167(8)
_cell_angle_beta                 89.6078(9)
_cell_angle_gamma                78.8942(9)
_cell_formula_units_Z            4
_cell_length_a                   9.43615(17)
_cell_length_b                   9.54443(17)
_cell_length_c                   17.4522(4)
_cell_measurement_reflns_used    12429
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      4.75
_cell_volume                     1534.93(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
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_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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'Larson (1970) Crystallographic Computing eq. 22'
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_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3446
_reflns_number_total             5510
_reflns_threshold_expression     F>2.0\s(F)
_cod_data_source_file            jo5b02900_si_002.cif
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