Cascade [1,5]-Hydride Transfer/Cyclization for Synthesis of [3,4]-Fused Oxindoles.
Zhu, Shuai; Chen, Chunqi; Duan, Kang; Sun, Yun-Ming; Li, Shuai-Shuai; Liu, Qing; Xiao, Jian; The Journal of organic chemistry 84 (2019) 8440–8448; doi:10.1021/acs.joc.9b00489

data_4034119
_publ_section_title
;
 Cascade [1,5]-Hydride Transfer/Cyclization for Synthesis of [3,4]-Fused
 Oxindoles.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8440
_journal_page_last               8448
_journal_paper_doi               10.1021/acs.joc.9b00489
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C56.5 H45 Cl N4 O6'
_chemical_formula_weight         911.41
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/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                 91.672(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   53.283(2)
_cell_length_b                   7.9450(2)
_cell_length_c                   20.8497(7)
_cell_measurement_reflns_used    5244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4750
_cell_measurement_theta_min      4.4870
_cell_volume                     8822.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28658
_diffrn_reflns_theta_full        67.25
_diffrn_reflns_theta_max         67.25
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.334
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         7924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1406P)^2^+13.4394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2434
_reflns_number_gt                5705
_reflns_number_total             7924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9b00489_si_002.cif
_cod_data_source_block           exp_7576
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C56.50 H45 Cl N4 O6'
_cod_database_code               4034119