An unprecedented base-promoted domino reaction of methyleneindolinones and N-tosyloxycarbamates for the construction of bispirooxindoles and spiroaziridine oxindoles
Qi-Lin Wang; Tian Cai; Jing Zhou; Fang Tian; Xiao-Ying Xu; Li-Xin Wang; Chem.Commun. 51 (2015) 10726–; doi:10.1039/C5cc03793J

data_7117366
_publ_section_title
;
 An unprecedented base-promoted domino reaction of methyleneindolinones
 and N-tosyloxycarbamates for the construction of bispirooxindoles and
 spiroaziridine oxindoles
;
_journal_name_full               Chem.Commun.
_journal_page_first              10726
_journal_paper_doi               10.1039/C5cc03793J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C24 H24 N2 O7'
_chemical_formula_sum            'C24 H24 N2 O7'
_chemical_formula_weight         452.45
_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_creation_method           SHELXL-97
_audit_update_record
;
2014-01-07 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                87.147(15)
_cell_angle_beta                 79.429(16)
_cell_angle_gamma                89.310(15)
_cell_formula_units_Z            2
_cell_length_a                   6.647(8)
_cell_length_b                   12.469(15)
_cell_length_c                   14.173(16)
_cell_measurement_reflns_used    1919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      3.12
_cell_volume                     1153(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1587
_diffrn_reflns_av_sigmaI/netI    0.2079
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13439
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.8797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             476
_exptl_crystal_size_max          1.36
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.2708
_refine_ls_R_factor_gt           0.1679
_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^)+(0.1847P)^2^+6.0367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4117
_refine_ls_wR_factor_ref         0.4605
_reflns_number_gt                2419
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03793j2.cif
_cod_data_source_block           mo_wlx_wql_1_0m
_cod_database_code               7117366