Base-promoted multicomponent synthesis of 1,2,4-triazole-based hybrids from 1,3-diones, β-nitrostyrenes, and hydrazones.
Sreelekha, Mariswamy K.; Jijin, Robert K.; Nayak, Kalinga H.; Babu, Beneesh P.; Chemical communications (Cambridge, England) 60 (2024) 11718–11721; doi:10.1039/d4cc03709j

data_7133736
_publ_section_title
;
 Base-promoted multicomponent synthesis of 1,2,4-triazole-based hybrids
 from 1,3-diones, &#x3b2;-nitrostyrenes, and hydrazones.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11718
_journal_page_last               11721
_journal_paper_doi               10.1039/d4cc03709j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C30 H20 F N3 O3'
_chemical_formula_sum            'C30 H20 F N3 O3'
_chemical_formula_weight         489.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-06-21 deposited with the CCDC.	2024-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.972(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9993(7)
_cell_length_b                   14.9425(12)
_cell_length_c                   14.7473(10)
_cell_measurement_reflns_used    6005
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      47.651
_cell_measurement_theta_min      5.212
_cell_volume                     2414.7(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altornare et al., 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28442
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.507
_diffrn_reflns_theta_min         1.386
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 2156 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                6179
_reflns_number_total             11861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03709j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7133736.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7133736
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              93756
_shelx_hkl_checksum              28165