Ru-Catalyzed C-H Annulation: Accessing Quinazolinone-BCP Hybrids from Stable Precursors
Luan, Yu-Yong; Li, Jin-Ye; Liu, Xue-Yuan; Liang, Yong-Min; Chemical Communications  (2026) –; doi:10.1039/D5CC05977A

data_7135285
_publ_section_title
;
 Ru-Catalyzed C-H Annulation: Accessing Quinazolinone-BCP Hybrids from
 Stable Precursors
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC05977A
_journal_year                    2026
_chemical_formula_moiety         '2(C17 H18 N2 O3)'
_chemical_formula_sum            'C34 H36 N4 O6'
_chemical_formula_weight         596.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.3440(10)
_cell_angle_beta                 104.7740(10)
_cell_angle_gamma                102.0290(10)
_cell_formula_units_Z            2
_cell_length_a                   9.05820(10)
_cell_length_b                   11.4917(2)
_cell_length_c                   16.1874(2)
_cell_measurement_reflns_used    15121
_cell_measurement_temperature    295.52(10)
_cell_measurement_theta_max      76.0050
_cell_measurement_theta_min      2.9400
_cell_volume                     1528.74(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.52(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  28.00   0.50    0.05    --  -46.55  19.00 -60.00  106
  2  \w    -25.00  26.00   0.50    0.05    --  -46.55  19.00  30.00  102
  3  \w    -25.00  28.00   0.50    0.05    --  -46.55  19.00  90.00  106
  4  \w     53.00  79.00   0.50    0.05    --   46.55-161.00 165.00   52
  5  \w     95.00 141.00   0.50    0.05    --  104.39-161.00 165.00   92
  6  \w     40.00  89.00   0.50    0.05    --  104.39-161.00 165.00   98
  7  \w     58.00 117.00   0.50    0.05    --  104.39-125.00 150.00  118
  8  \w     27.00  53.00   0.50    0.05    --   46.55-117.00 -43.00   52
  9  \w     82.00 111.00   0.50    0.05    --  104.39-125.00-150.00   58
 10  \w     35.00  67.00   0.50    0.05    --  104.39-125.00-150.00   64
 11  \w     58.00 116.00   0.50    0.05    --  104.39-125.00 -90.00  116
 12  \w     52.00  82.00   0.50    0.05    --  104.39 -94.00 150.00   60
 13  \w     62.00 102.00   0.50    0.05    --  104.39-117.00 -43.00   80
 14  \w     72.00 103.00   0.50    0.05    --  104.39 -94.00 -60.00   62
 15  \w     34.00  60.00   0.50    0.05    --  104.39 -94.00 -60.00   52
 16  \w     33.00  70.00   0.50    0.05    --  104.39 -77.00-180.00   74
 17  \w     47.00  72.00   0.50    0.05    --  104.39 -61.00 -90.00   50
 18  \w     33.00  67.00   0.50    0.05    --  104.39 -61.00 -30.00   68
 19  \w     40.00  72.00   0.50    0.05    --  104.39 -61.00  90.00   64
 20  \w     46.00 107.00   0.50    0.05    --  104.39 -77.00 -30.00  122
 21  \w     32.00  60.00   0.50    0.05    --  104.39 -61.00 -60.00   56
 22  \w     34.00  68.00   0.50    0.05    --  104.39 -61.00-180.00   68
 23  \w     93.00 175.00   0.50    0.05    --  104.39  30.00 -90.00  164
 24  \w     83.00 108.00   0.50    0.05    --  104.39 161.00-164.00   50
 25  \w     76.00 101.00   0.50    0.05    --   46.55 161.00-164.00   50
 26  \w    146.00 171.00   0.50    0.05    --  104.39  45.00  30.00   50
 27  \w    103.00 129.00   0.50    0.05    --  104.39  45.00  30.00   52
 28  \w    103.00 129.00   0.50    0.05    --  104.39 117.00  43.00   52
 29  \w    -84.00 -34.00   0.50    0.05    --  -46.55 117.00  43.00  100
 30  \w    -85.00 -60.00   0.50    0.05    -- -102.00 161.00-164.00   50
 31  \w   -117.00 -70.00   0.50    0.05    --  -46.55 161.00-164.00   94
 32  \w    -85.00 -59.00   0.50    0.05    -- -102.00 117.00  43.00   52
 33  \w    -62.00 -29.00   0.50    0.05    -- -102.00  77.00  60.00   66
 34  \w    -99.00 -68.00   0.50    0.05    -- -102.00  77.00  60.00   62
 35  \w    -79.00 -29.00   0.50    0.05    -- -102.00  77.00 -90.00  100
 36  \w    -66.00 -35.00   0.50    0.05    -- -102.00  61.00-180.00   62
 37  \w   -167.00 -89.00   0.50    0.05    -- -102.00 -15.00-150.00  156
 38  \w   -174.00-120.00   0.50    0.05    -- -102.00 -45.00   0.00  108
 39  \w   -174.00 -91.00   0.50    0.05    -- -102.00 -45.00  30.00  166
 40  \w   -174.00-117.00   0.50    0.05    -- -102.00 -45.00 150.00  114
 41  \w   -143.00-104.00   0.50    0.05    -- -102.00-161.00 165.00   78
 42  \w    -98.00 -72.00   0.50    0.05    --  -46.55-161.00 165.00   52
 43  \w   -103.00 -74.00   0.50    0.05    --  -46.55-125.00 120.00   58
 44  \w   -116.00 -70.00   0.50    0.05    --  -46.55-125.00  30.00   92
 45  \w   -116.00 -71.00   0.50    0.05    --  -46.55-125.00   0.00   90
 46  \w   -139.00-100.00   0.50    0.05    -- -102.00-117.00 -43.00   78
 47  \w   -141.00-107.00   0.50    0.05    -- -102.00 -94.00 -90.00   68
 48  \w   -116.00 -71.00   0.50    0.05    --  -46.55-125.00-180.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0776094000
_diffrn_orient_matrix_UB_12      -0.0329621000
_diffrn_orient_matrix_UB_13      -0.1015517000
_diffrn_orient_matrix_UB_21      -0.0898766000
_diffrn_orient_matrix_UB_22      -0.1298020000
_diffrn_orient_matrix_UB_23      -0.0004893000
_diffrn_orient_matrix_UB_31      -0.1394058000
_diffrn_orient_matrix_UB_32      0.0497913000
_diffrn_orient_matrix_UB_33      0.0145944000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20554
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.186
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0744P)^2^+0.2479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5351
_reflns_number_total             6121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05977a2.cif
_cod_data_source_block           luanyuyong-lym_0603_auto
_cod_database_code               7135285
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C21(H21A,H21B), C25(H25A,H25B), C30(H30A,H30B), C5(H5A,H5B),
 C23(H23A,H23B), C24(H24A,H24B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C32(H32), C7(H7), C9(H9), C19(H19), C27(H27)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              2070
_shelx_hkl_checksum              47310
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.444