Stereoselective Synthesis of Five-Membered Spirooxindoles through Tomita Zipper Cyclization.
Ramachary, D. B.; Venkaiah, Chintalapudi; Krishna, Patoju M.; Organic letters 15 (2013) 4714–4717; doi:10.1021/ol4020305

data_1512312
_publ_section_title
;
 Stereoselective Synthesis of Five-Membered Spirooxindoles through Tomita
 Zipper Cyclization.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4714
_journal_page_last               4717
_journal_paper_doi               10.1021/ol4020305
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C29 H30 Br N O6'
_chemical_formula_weight         568.45
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.794(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2030(3)
_cell_length_b                   15.6497(3)
_cell_length_c                   14.7753(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2771.76(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9454
_diffrn_reflns_theta_full        67.07
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    2.370
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.732
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.732
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2390
_reflns_number_gt                4299
_reflns_number_total             4946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4020305_si_003.cif
_cod_data_source_block           test1
_cod_original_cell_volume        2771.75(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1512312