BF3•OEt2-mediated one pot synthesis of 10-indolyldibenzo[b,f]azepine derivatives via tandem ring expansion and C-C bond formation
Yao, Ching-Fa; Kotipalli, Trimurtulu; Donala, Janreddy; Kavala, Veerababurao; Kuo, Chun-Wei; Chen, Mei-Ling; Kuo, Ting-Shen; He, Chiu-Hui; RSC Adv.  (2014) –; doi:10.1039/C4RA08723B

data_7218236
_publ_section_title
;
 BF3&#x2022;OEt2-mediated one pot synthesis of
 10-indolyldibenzo[b,f]azepine derivatives via tandem ring expansion and
 C-C bond formation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA08723B
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 Cl2 N2'
_chemical_formula_sum            'C28 H20 Cl2 N2'
_chemical_formula_weight         455.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.242(6)
_cell_length_b                   21.438(12)
_cell_length_c                   14.019(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2161(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.2401
_diffrn_reflns_av_sigmaI/netI    0.4358
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10614
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.9936
_exptl_absorpt_correction_T_min  0.8537
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.3364
_refine_ls_R_factor_gt           0.1027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2902
_reflns_number_gt                1112
_reflns_number_total             3907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra08723b2.cif
_cod_data_source_block           a16134
_cod_original_cell_volume        2161(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7218236