BF3·OEt2 catalyzed synthesis of functionalized 9-fluorene-9-ylidene appended quinazolin-4-ones
Athira, Mohanakumaran; Smile, Suresh Snoxma; Shanmugam, Ponnusamy; New Journal of Chemistry 46 (2022) 2952–2961; doi:10.1039/D1NJ05379E

data_7061247
_publ_section_title
;
 BF3&#x00B7;OEt2 catalyzed synthesis of functionalized
 9-fluorene-9-ylidene appended quinazolin-4-ones
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2952
_journal_page_last               2961
_journal_paper_doi               10.1039/D1NJ05379E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C34 H23 I N2 O, C H2 Cl2'
_chemical_formula_sum            'C35 H25 Cl2 I N2 O'
_chemical_formula_weight         687.37
_chemical_name_common            AM3-63
_chemical_name_systematic
2-((9H-fluoren-9-ylidene)methyl)-6-iodo-1,2-diphenyl-2,3-dihydroquinazolin-4(1H)-one
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2022-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                113.666(12)
_cell_angle_beta                 91.973(14)
_cell_angle_gamma                94.252(13)
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_cell_length_a                   11.086(4)
_cell_length_b                   11.540(4)
_cell_length_c                   12.936(4)
_cell_measurement_reflns_used    9186
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      3.07
_cell_volume                     1507.8(9)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48643
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.070
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0203(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+5.7357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4724
_reflns_number_total             6188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05379e2.cif
_cod_data_source_block           AM63
_cod_depositor_comments
'Adding full bibliography for 7061247--7061248.cif.'
_cod_database_code               7061247
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.832
_shelx_res_checksum              7353