Regioselective synthesis of spiro quinazolinones via sequential hydroalkoxylation and intramolecular amide-cyclization of alkynol ureas
Biswas, Subhamoy; Bora, Surjya Kumar; Arandhara, Pallav Jyoti; Saikia, Anil K.; New Journal of Chemistry 48 (2024) 10756–10761; doi:10.1039/D4NJ01745E

data_7063220
_publ_section_title
;
 Regioselective synthesis of spiro quinazolinones via sequential
 hydroalkoxylation and intramolecular amide-cyclization of alkynol ureas
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10756
_journal_page_last               10761
_journal_paper_doi               10.1039/D4NJ01745E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C18 H18 N2 O2'
_chemical_formula_weight         294.34
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.222(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5261(6)
_cell_length_b                   7.3772(4)
_cell_length_c                   16.8208(9)
_cell_measurement_reflns_used    8977
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.18
_cell_volume                     1538.39(14)
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         1.903
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0326P)^2^+1.1298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1849
_reflns_number_total             2718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01745e2.cif
_cod_data_source_block           SB_C_210_0m_a
_cod_depositor_comments          'Adding full bibliography for 7063220.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063220
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              96353