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_7060512
_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         'C45 H28 F6 N2 O2'
_chemical_formula_sum            'C45 H28 F6 N2 O2'
_chemical_formula_weight         742.69
_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                66.069(12)
_cell_angle_beta                 86.317(10)
_cell_angle_gamma                85.015(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8731(13)
_cell_length_b                   12.7566(16)
_cell_length_c                   14.5064(19)
_cell_measurement_reflns_used    1295
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.8820
_cell_measurement_theta_min      3.5650
_cell_volume                     1831.2(4)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Xcalibur 3'
_diffrn_measurement_method       '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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.1393
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_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12914
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73521
_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            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.053
_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     508
_refine_ls_number_reflns         7267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1986
_refine_ls_R_factor_gt           0.0718
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                2594
_reflns_number_total             7267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj00935d2.cif
_cod_data_source_block           exp_704
_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.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7060512