Highly stereoselective construction of novel dispirooxindole-imidazolidines via self-1,3-dipolar cyclization of ketimines.
Sun, Yan-Hua; Xiong, Yu; Peng, Chu-Qin; Li, Wu; Xiao, Jun-An; Yang, Hua; Organic & biomolecular chemistry 13 (2015) 7907–7910; doi:10.1039/c5ob00954e

data_7154533
_publ_section_title
;
 Highly stereoselective construction of novel
 dispirooxindole-imidazolidines via self-1,3-dipolar cyclization of
 ketimines.
;
_journal_issue                   29
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7907
_journal_page_last               7910
_journal_paper_doi               10.1039/c5ob00954e
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C32 H28 N4 O2'
_chemical_formula_weight         500.58
_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
;
2014-08-28 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                80.998(3)
_cell_angle_beta                 89.343(3)
_cell_angle_gamma                78.842(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6074(5)
_cell_length_b                   9.9108(5)
_cell_length_c                   15.7203(9)
_cell_measurement_temperature    296(2)
_cell_volume                     1299.24(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16672
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.081
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0725P)^2^+0.3344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4820
_reflns_number_total             5904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob00954e2.cif
_cod_data_source_block           ja_16
_cod_depositor_comments          'Adding full bibliography for 7154533.cif.'
_cod_original_cell_volume        1299.24(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7154533