Facile net cycloaddition approach to optically active 1,5-benzothiazepines.
Fukata, Yukihiro; Asano, Keisuke; Matsubara, Seijiro; Journal of the American Chemical Society 137 (2015) 5320–5323; doi:10.1021/jacs.5b02537

data_4129414
_publ_section_title
;
 Facile net cycloaddition approach to optically active
 1,5-benzothiazepines.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5320
_journal_page_last               5323
_journal_paper_doi               10.1021/jacs.5b02537
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C22 H19 N O3 S2'
_chemical_formula_sum            'C22 H19 N O3 S2'
_chemical_formula_weight         409.52
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.4202(10)
_cell_length_b                   18.5765(15)
_cell_length_c                   8.4080(7)
_cell_measurement_reflns_used    19384
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.13
_cell_volume                     1939.9(3)
_computing_cell_refinement       'CrystalClear-SM Auto 2.0 r15'
_computing_data_collection       'CrystalClear-SM Auto 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Auto 2.0 r15'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19465
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             856.00
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.210
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1905 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.3067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                4374
_reflns_number_total             4431
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5b02537_si_002.cif
_cod_data_source_block           User-defined
_cod_database_code               4129414