Amberlite-15 promoted an unprecedented aza Michael rearrangement for one pot synthesis of dihydroquinazolinone compounds
Murthy, V. Narayana; Nikumbh, Satish P.; Tadiparthi, Krishnaji; Madhubabu, M. V.; Jammula, Subba Rao; Rao, L. Vaikunta; Raghunadh, Akula; RSC Advances 8 (2018) 22331–; doi:10.1039/C8RA03308K

data_7237100
_publ_section_title
;
 Amberlite-15 promoted an unprecedented aza Michael rearrangement for one
 pot synthesis of dihydroquinazolinone compounds
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              22331
_journal_paper_doi               10.1039/C8RA03308K
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C23 H27 N2 O4'
_chemical_formula_sum            'C23 H27 N2 O4'
_chemical_formula_weight         395.46
_space_group_IT_number           1
_space_group_name_Hall           'C 1'
_space_group_name_H-M_alt        'C 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.852(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7483(19)
_cell_length_b                   9.2050(7)
_cell_length_c                   13.1074(15)
_cell_measurement_reflns_used    6335
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      56.085
_cell_measurement_theta_min      4.510
_cell_volume                     2179.2(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13371
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         1.871
_exptl_absorpt_coefficient_mu    0.083
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2687 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0513
_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^)+(0.1127P)^2^+0.1757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.690
_reflns_Friedel_fraction_full    0.792
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                7250
_reflns_number_total             8631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra03308k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__computing_data_collection' was replaced with
'_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      0
_cod_database_code               7237100
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              38568