Efficient [4+3] Cycloaddition Reaction of aza-o-Quinodimethanes with C,N-cyclic Azomethine Imines: Stereoselective Synthesis of 1,2,4-Triazepines
Wang, Jian; chen, lei; yang, gongming; jia, qianfa; wei, jia; Du, Zhiyun; RSC Adv.  (2015) –; doi:10.1039/C5RA15903B

data_7222018
_publ_section_title
;
 Efficient [4+3] Cycloaddition Reaction of aza-o-Quinodimethanes with
 C,N-cyclic Azomethine Imines: Stereoselective Synthesis of
 1,2,4-Triazepines
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA15903B
_journal_year                    2015
_chemical_formula_sum            'C30 H27 N3 O3 S'
_chemical_formula_weight         509.61
_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
_audit_update_record
;
2015-07-27 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.278(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.029(5)
_cell_length_b                   12.960(6)
_cell_length_c                   21.156(8)
_cell_measurement_temperature    100(2)
_cell_volume                     2486(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  bruker-CCD
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12484
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_correction_T_min  0.9654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0574P)^2^+0.3670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                3424
_reflns_number_total             4371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra15903b2.cif
_cod_data_source_block           qq
_cod_original_cell_volume        2486.5(19)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7222018