The Rh(iii)-catalysed C–H/N–H annulation of 2-thienyl- and 2-phenyl-quinazolin-4(3H)-ones with diphenylacetylene
Moshkina, Tatyana N.; Nosova, Emiliya V.; Lipunova, Galina N.; Zhilina, Ekaterina F.; Slepukhin, Pavel A.; Nikonov, Igor L.; Charushin, Valery N.; New Journal of Chemistry 45 (2021) 8456–8466; doi:10.1039/D1NJ00935D

data_7060513
_publ_section_title
;
 The Rh(iii)-catalysed C--H/N--H annulation of 2-thienyl- and
 2-phenyl-quinazolin-4(3H)-ones with diphenylacetylene
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8456
_journal_page_last               8466
_journal_paper_doi               10.1039/D1NJ00935D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C26 H16 N2 O S'
_chemical_formula_sum            'C26 H16 N2 O S'
_chemical_formula_weight         404.47
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2021-03-23 deposited with the CCDC.	2021-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                98.812(6)
_cell_angle_beta                 91.216(6)
_cell_angle_gamma                97.590(6)
_cell_formula_units_Z            4
_cell_length_a                   8.9557(7)
_cell_length_b                   9.9486(8)
_cell_length_c                   22.5422(17)
_cell_measurement_reflns_used    2090
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.4370
_cell_measurement_theta_min      3.5600
_cell_volume                     1965.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device_type  'Xcalibur 3 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.1413
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17949
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1891
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.2254
_reflns_number_gt                4298
_reflns_number_total             10435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj00935d2.cif
_cod_data_source_block           exp_663
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7060512--7060514.cif.
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7060513