Construction of dispirocyclohexyl-3,3’-bisoxindole and dispirocyclopentyl-3,3’-bisoxindole via cycloaddition reactions of N-benzylbenzimidazolium salts with 2-(2-oxoindolin-3-ylidene)acetates†
Yan, Chao Guo; Sun, Jing; Shen, Guo-Liang; RSC Adv.  (2014) –; doi:10.1039/C4RA13760D

data_7219034
_publ_section_title
;
 Construction of dispirocyclohexyl-3,3&#x2019;-bisoxindole and
 dispirocyclopentyl-3,3&#x2019;-bisoxindole via cycloaddition reactions of
 N-benzylbenzimidazolium salts with
 2-(2-oxoindolin-3-ylidene)acetates&#x2020;
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA13760D
_journal_year                    2014
_chemical_formula_moiety         'C41 H36 Cl2 N2 O8'
_chemical_formula_sum            'C41 H36 Cl2 N2 O8'
_chemical_formula_weight         755.62
_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/cc13l7tr
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-01 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.481(2)
_cell_angle_beta                 76.954(2)
_cell_angle_gamma                75.004(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8295(16)
_cell_length_b                   12.8333(19)
_cell_length_c                   15.121(2)
_cell_measurement_reflns_used    5412
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.17
_cell_volume                     1977.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13843
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_platon_squeeze_details          ' '
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1064
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2890
_refine_ls_wR_factor_ref         0.3093
_reflns_number_gt                5299
_reflns_number_total             7783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra13760d2.cif
_cod_data_source_block           4d
_cod_database_code               7219034