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_7061248
_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         'C43 H33 Br N2 O,) 0.5 (C H2 Cl2)'
_chemical_formula_sum            'C43.5 H34 Br Cl N2 O'
_chemical_formula_weight         716.09
_chemical_name_common            AM3-142
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-30 deposited with the CCDC.	2022-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7423(4)
_cell_length_b                   18.5947(6)
_cell_length_c                   15.4410(5)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      68.43
_cell_measurement_theta_min      3.38
_cell_volume                     3749.3(2)
_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-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 VENTURE diffractometer with PHOTON II detector'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72176
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        65.997
_diffrn_reflns_theta_max         65.997
_diffrn_reflns_theta_min         3.765
_exptl_absorpt_coefficient_mu    2.414
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0023(4)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6524
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1336P)^2^+1.4916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4572
_reflns_number_total             6524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05379e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7061247--7061248.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C43.50 H34 Br Cl N2 O'
_cod_database_code               7061248
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.794
_shelx_res_checksum              80815