DABCO-catalysed highly diastereoselective synthesis of 1,3-indandione containing fully saturated spirocyclopentanes involving 2-(2′-ketoalkyl)-1,3-indandiones and nitrostyrenes
Mishra, Gitanjali; Bobonga, Missa Saril; Islam, Khadimul; Chakraborty, Arundhuti; Thirupathi, Barla; RSC Advances 15 (2025) 30768–30780; doi:10.1039/D5RA04224K

data_7250818
_publ_section_title
;
 DABCO-catalysed highly diastereoselective synthesis of 1,3-indandione
 containing fully saturated spirocyclopentanes involving
 2-(2&#x2032;-ketoalkyl)-1,3-indandiones and nitrostyrenes
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              30768
_journal_page_last               30780
_journal_paper_doi               10.1039/D5RA04224K
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C25 H18 Cl N O5'
_chemical_formula_sum            'C25 H18 Cl N O5'
_chemical_formula_weight         447.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                101.342(4)
_cell_angle_beta                 99.504(4)
_cell_angle_gamma                103.374(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2235(12)
_cell_length_b                   9.6756(16)
_cell_length_c                   12.758(2)
_cell_measurement_reflns_used    3536
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      0.957
_cell_measurement_theta_min      0.949
_cell_volume                     1059.2(3)
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 quest photon detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29045
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.438
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0408P)^2^+0.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3536
_reflns_number_total             4857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra04224k2.cif
_cod_data_source_block           tb_ac_ocl_0m
_cod_database_code               7250818
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              52276