Isolation and Characterization of Atropisomers of Seven-Membered-Ring Benzolactams
Hidetsugu Tabata; Naoya Wada; Yuko Takada; Tetsuta Oshitari; Hideyo Takahashi; Hideaki Natsugari; Journal of Organic Chemistry 76 (2011) 5123–5131; doi:10.1021/jo2008725

data_4026407
_publ_section_title
;
 Isolation and Characterization of Atropisomers of Seven-Membered-Ring
 Benzolactams
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5123
_journal_page_last               5131
_journal_paper_doi               10.1021/jo2008725
_journal_volume                  76
_journal_year                    2011
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C19 H19 Cl N2 O2 S '
_chemical_formula_sum            'C19 H19 Cl N2 O2 S'
_chemical_formula_weight         374.88
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.842(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   8.3785(4)
_cell_length_b                   12.3205(4)
_cell_length_c                   8.5550(3)
_cell_measurement_reflns_used    6693
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      67.7
_cell_measurement_theta_min      3.6
_cell_volume                     883.01(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15903
_diffrn_reflns_theta_full        68.17
_diffrn_reflns_theta_max         68.17
_exptl_absorpt_coefficient_mu    3.145
_exptl_absorpt_correction_T_max  0.284
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             392.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.59
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1508 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       30(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2290
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.0000
_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         0.0906
_reflns_number_gt                2278
_reflns_number_total             3198
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo2008725_si_005.cif
_cod_data_source_block           '_HN2-69-40'
_cod_original_formula_sum        'C19 H19 Cl N2 O2 S '
_cod_database_code               4026407