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_7219032
_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         'C46 H37 Cl3 N2 O7, C3 H7 N O'
_chemical_formula_sum            'C49 H44 Cl3 N3 O8'
_chemical_formula_weight         909.22
_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/cc13k6jd
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-16 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                105.258(3)
_cell_angle_beta                 90.346(3)
_cell_angle_gamma                91.168(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5355(12)
_cell_length_b                   12.0272(13)
_cell_length_c                   16.4726(17)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.19
_cell_volume                     2204.2(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46666
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         10160
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+1.1458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                6729
_reflns_number_total             10202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra13760d2.cif
_cod_data_source_block           3f
_cod_database_code               7219032