Electrochemical access to benzimidazolone and quinazolinone derivatives <i>via in situ</i> generation of isocyanates.
Saha, Debarshi; Taily, Irshad Maajid; Naik, Sumitra; Banerjee, Prabal; Chemical communications (Cambridge, England) 57 (2021) 631–634; doi:10.1039/d0cc07125k

data_7127576
_publ_section_title
;
 Electrochemical access to benzimidazolone and quinazolinone derivatives
 <i>via in situ</i> generation of isocyanates.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              631
_journal_page_last               634
_journal_paper_doi               10.1039/d0cc07125k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C15 H13 N3 O3'
_chemical_formula_sum            'C15 H13 N3 O3'
_chemical_formula_weight         283.28
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.966(5)
_cell_angle_beta                 96.111(4)
_cell_angle_gamma                90.897(4)
_cell_formula_units_Z            1
_cell_length_a                   5.0971(6)
_cell_length_b                   5.3649(7)
_cell_length_c                   12.3429(16)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      3.4
_cell_volume                     330.34(7)
_computing_cell_refinement       'APEX2 (Bruker, 2014); SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014);XPREP(Sheldrick,2014)'
_computing_molecular_graphics    'ORTEP, Platon, Mercury'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.233
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4129
_diffrn_reflns_point_group_measured_fraction_full 0.852
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.621
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flakes
_exptl_crystal_F_000             148
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_exptl_transmission_factor_max   0.7459
_exptl_transmission_factor_min   0.3660
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Flack x determined using 742 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2817
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.638
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.589
_reflns_number_gt                2328
_reflns_number_total             2817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07125k2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7127575--7127576.cif.'
_cod_database_code               7127576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.120
_shelx_estimated_absorpt_t_max   0.169
_shelx_res_checksum              16000
_shelx_hkl_checksum              9043