Substrate-controlled divergent synthesis of polycyclic indoloazepines and indolodiazepines via 1,5-hydride shift/7-cyclization cascades.
Liu, Siyuan; Qu, Jingping; Wang, Baomin; Chemical communications (Cambridge, England) 54 (2018) 7928–7931; doi:10.1039/c8cc03804j

data_7121847
_publ_section_title
;
 Substrate-controlled divergent synthesis of polycyclic indoloazepines and
 indolodiazepines via 1,5-hydride shift/7-cyclization cascades.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7928
_journal_page_last               7931
_journal_paper_doi               10.1039/c8cc03804j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C41 H43 N4'
_chemical_formula_weight         591.79
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
;
2018-05-04 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.124(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.821(3)
_cell_length_b                   9.5022(12)
_cell_length_c                   17.881(2)
_cell_measurement_reflns_used    855
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.12
_cell_measurement_theta_min      2.38
_cell_volume                     3321.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.1556
_diffrn_reflns_av_sigmaI/netI    0.1559
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9801
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.2155
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.2027
_reflns_number_gt                2170
_reflns_number_total             5784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc03804j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7121845--7121847.cif.'
_cod_original_cell_volume        3321.8(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7121847