Synthesis, structure and biological activity of new picolinohydrazonamide derivatives.
Sukiennik, Jarosław; Olczak, Andrzej; Gobis, Katarzyna; Korona-Głowniak, Izabela; Suśniak, Katarzyna; Fruziński, Andrzej; Szczesio, Małgorzata; Acta crystallographica. Section C, Structural chemistry 81 (2025) –; doi:10.1107/S2053229624011549

data_2312722
_publ_section_title
;
 Synthesis, structure and biological activity of new picolinohydrazonamide
 derivatives.
;
_journal_coeditor_code           WV3017
_journal_issue                   1
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624011549
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C22 H29 N7 S, C3 H7 N O, 0.285H2 O'
_chemical_formula_moiety         'C22 H29 N7 S, C3 H7 N O, 0.285(H2 O)'
_chemical_formula_sum            'C25 H36.57 N8 O1.29 S'
_chemical_formula_weight         501.81
_chemical_name_systematic
'4-(4-Phenylpiperazin-1-yl)-<i>N</i>'-(piperidine-1-carbonothioyl)picolinohydrazonamide--dimethylformamide--water (1/1/0.285)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.5
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.255(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1063(3)
_cell_length_b                   12.8414(2)
_cell_length_c                   15.6327(3)
_cell_measurement_reflns_used    19656
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      78.6360
_cell_measurement_theta_min      4.4250
_cell_volume                     2603.77(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
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SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
olex2.solve (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9503
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a Pilatus 300K detector'
_diffrn_measurement_method       '\w scans'
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33084
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.960
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             1075
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0471P)^2^+1.1183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                4642
_reflns_number_total             5356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wv3017sup1.cif
_cod_data_source_block           2
_cod_database_code               2312722
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.851
_cod_database_fobs_code 2312722