DBU-promoted [3+2] cycloaddition for the synthesis of trispiro heterocycles from acetylpyrazolyl-substituted oxindoles and substituted isatins
Jia, Yun-Qing; Mu, Ting-ting; Liu, Hong-xian; Xiang, Min; Shen, Li-Wen; New Journal of Chemistry 50 (2026) 3947–3951; doi:10.1039/D5NJ04657B

data_7064273
_publ_section_title
;
 DBU-promoted [3+2] cycloaddition for the synthesis of trispiro
 heterocycles from acetylpyrazolyl-substituted oxindoles and substituted
 isatins
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3947
_journal_page_last               3951
_journal_paper_doi               10.1039/D5NJ04657B
_journal_volume                  50
_journal_year                    2026
_chemical_formula_sum            'C20 H16 N2 O4'
_chemical_formula_weight         348.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-12-14 deposited with the CCDC.	2026-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.177(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1194(4)
_cell_length_b                   12.8734(4)
_cell_length_c                   10.0344(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1668.06(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6201
_diffrn_reflns_point_group_measured_fraction_full 0.700
_diffrn_reflns_point_group_measured_fraction_max 0.683
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.946
_diffrn_reflns_theta_min         4.851
_exptl_absorpt_coefficient_mu    0.808
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.135
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 518 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2199
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+0.2601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.381
_reflns_Friedel_fraction_full    0.399
_reflns_Friedel_fraction_max     0.378
_reflns_number_gt                2054
_reflns_number_total             2199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04657b2.cif
_cod_data_source_block           20250498a_auto
_cod_depositor_comments          'Adding full bibliography for 7064273.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7064273
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              16025