Construction of bridged cyclic N,O-ketal spirooxindoles through a Michael addition/N,O-ketalization sequence.
Zhu, Yanshuo; Guo, Jia; Jin, Shaojing; Guo, Jiaomei; Bai, Xuguan; Wang, Qilin; Bu, Zhanwei; Organic & biomolecular chemistry 16 (2018) 1751–1759; doi:10.1039/c8ob00306h

data_7156126
_publ_section_title
;
 Construction of bridged cyclic N,O-ketal spirooxindoles through a Michael
 addition/N,O-ketalization sequence.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1751
_journal_page_last               1759
_journal_paper_doi               10.1039/c8ob00306h
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C26 H22 N2 O3'
_chemical_formula_sum            'C26 H22 N2 O3'
_chemical_formula_weight         410.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-08 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.398(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4093(12)
_cell_length_b                   6.2017(7)
_cell_length_c                   15.4242(17)
_cell_measurement_reflns_used    6064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.32
_cell_volume                     994.84(19)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11165
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.006
_diffrn_reflns_theta_min         1.321
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          1.360
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.2132
_exptl_transmission_factor_min   0.1799
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2191 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.2514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                5343
_reflns_number_total             5599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob00306h2.cif
_cod_data_source_block           mo_hd_wql18_0m
_cod_depositor_comments          'Adding full bibliography for 7156126.cif.'
_cod_database_code               7156126
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              9550