Facile oxidative cyclization to access C2-quaternary 2-hydroxy-indolin-3-ones: Synthetic studies towards matemone
Wen, Sai-Shuai; Zhou, Zhao-Fang; Xiao, Jun-An; Li, Jun; Xiang, Haoyue; Yang, Hua; New J. Chem. 41 (2017) 11503–11506; doi:10.1039/C7NJ02246H

data_7056576
_publ_section_title
;
 Facile oxidative cyclization to access C2-quaternary
 2-hydroxy-indolin-3-ones: Synthetic studies towards matemone
;
_journal_issue                   20
_journal_name_full               'New J. Chem.'
_journal_page_first              11503
_journal_page_last               11506
_journal_paper_doi               10.1039/C7NJ02246H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C22 H21 N O4'
_chemical_formula_weight         363.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jpcdz
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-26 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                72.080(6)
_cell_angle_beta                 89.811(7)
_cell_angle_gamma                77.711(7)
_cell_formula_units_Z            8
_cell_length_a                   11.0068(12)
_cell_length_b                   18.8343(18)
_cell_length_c                   19.829(2)
_cell_measurement_temperature    296(2)
_cell_volume                     3813.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42562
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9828
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         13430
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0826P)^2^+0.1728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                6887
_reflns_number_total             13430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02246h2.cif
_cod_data_source_block           ja
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7056576