Multicomponent reaction (MCR) for constructing bis-spirocyclohexane skeletons using β-nitrostyrene derived MBH acetates, 1,3-indanedione and aldehydes via [1 + 1 + 1 + 3] annulation
Gudise, Veera Babu; Anwar, Shaik; RSC Advances 13 (2023) 27456–27460; doi:10.1039/D3RA04996E

data_7247387
_publ_section_title
;
 Multicomponent reaction (MCR) for constructing bis-spirocyclohexane
 skeletons using \b-nitrostyrene derived MBH acetates, 1,3-indanedione and
 aldehydes via [1 + 1 + 1 + 3] annulation
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              27456
_journal_page_last               27460
_journal_paper_doi               10.1039/D3RA04996E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C27 H20 N2 O6'
_chemical_formula_sum            'C27 H20 N2 O6'
_chemical_formula_weight         468.45
_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
;
2022-05-26 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                77.743(3)
_cell_angle_beta                 83.426(4)
_cell_angle_gamma                81.286(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0225(6)
_cell_length_b                   10.0191(6)
_cell_length_c                   14.8134(10)
_cell_measurement_reflns_used    7963
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.035
_cell_measurement_theta_min      2.578
_cell_volume                     1145.92(14)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14297
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.285
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0873P)^2^+0.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3399
_reflns_number_total             4479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra04996e2.cif
_cod_data_source_block           KA984_0m
_cod_database_code               7247387
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              49240