An efficient synthesis of novel dibenzoxdiazepine-fused heterocycles through multicomponent reaction
Qian, Zhiwei; Yang, Anjiang; Yu, Ting; Ma, Lanping; Wang, Xin; Zhang, Yongliang; Shen, Jingkang; Meng, Tao; RSC Adv.  (2014) –; doi:10.1039/C4RA09196E

data_7218387
_publ_section_title
;
 An efficient synthesis of novel dibenzoxdiazepine-fused heterocycles
 through multicomponent reaction
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA09196E
_journal_year                    2014
_chemical_formula_sum            'C22 H14 F3 N3 O2'
_chemical_formula_weight         409.36
_space_group_IT_number           33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.511(14)
_cell_length_b                   8.066(6)
_cell_length_c                   26.88(2)
_cell_measurement_temperature    296(2)
_cell_volume                     3797(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(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  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35922
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9943
_exptl_absorpt_correction_T_min  0.9776
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.1(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8610
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                4398
_reflns_number_total             8610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09196e3.cif
_cod_data_source_block           mo_2013417_0ma
_cod_original_cell_volume        3796(5)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7218387