One Pot Regioselective Synthesis of a Small Library of Dibenzo[b,f][1,4]thiazepin-11(10H)-ones via Smiles Rearrangement.
Zhao, Yongmei; Dai, Qiaoling; Chen, Zhi; Zhang, Qihui; Bai, Yongcheng; Ma, Chen; ACS combinatorial science 15 (2013) 130–134; doi:10.1021/co300139s

data_4507428
_publ_section_title
;
 One Pot Regioselective Synthesis of a Small Library of
 Dibenzo[b,f][1,4]thiazepin-11(10H)-ones via Smiles Rearrangement.
;
_journal_issue                   2
_journal_name_full               'ACS combinatorial science'
_journal_page_first              130
_journal_page_last               134
_journal_paper_doi               10.1021/co300139s
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C20 H13 Cl N2 O3 S'
_chemical_formula_weight         396.85
_space_group_IT_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.077(11)
_cell_angle_beta                 95.394(11)
_cell_angle_gamma                108.561(12)
_cell_formula_units_Z            2
_cell_length_a                   7.942(5)
_cell_length_b                   9.763(7)
_cell_length_c                   12.245(9)
_cell_measurement_temperature    298(2)
_cell_volume                     892.6(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4397
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.8823
_exptl_absorpt_correction_T_min  0.7832
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             495
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+0.0659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                2205
_reflns_number_total             3097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            co300139s_si_002.cif
_cod_data_source_block           p
_cod_database_code               4507428