N-Benzoyl- and N-Sulfonyl-1,5-benzodiazepines: Comparison of Their Atropisomeric and Conformational Properties.
Yoneda, Tetsuya; Tabata, Hidetsugu; Nakagomi, Jun; Tasaka, Tomohiko; Oshitari, Tetsuta; Takahashi, Hideyo; Natsugari, Hideaki; The Journal of organic chemistry 79 (2014) 5717–5727; doi:10.1021/jo5008509

data_4029527
_publ_section_title
;
 N-Benzoyl- and N-Sulfonyl-1,5-benzodiazepines: Comparison of Their
 Atropisomeric and Conformational Properties.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5717
_journal_page_last               5727
_journal_paper_doi               10.1021/jo5008509
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C17 H20 N2 O2 S'
_chemical_formula_sum            'C17 H20 N2 O2 S'
_chemical_formula_weight         316.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                80.1484(17)
_cell_angle_beta                 89.0366(19)
_cell_angle_gamma                76.3943(17)
_cell_formula_units_Z            2
_cell_length_a                   7.7090(3)
_cell_length_b                   8.0411(2)
_cell_length_c                   13.5247(4)
_cell_measurement_reflns_used    6344
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      3.32
_cell_volume                     802.60(4)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8522
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.360
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2870
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                2409
_reflns_number_total             2870
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo5008509_si_007.cif
_cod_data_source_block           120712
_cod_depositor_comments
'Adding full bibliography for 4029521--4029530.cif.'
_cod_database_code               4029527