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_2312721
_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          '2C21 H27 N7 O S, C5 H10 O'
_chemical_formula_moiety         '2(C21 H27 N7 O S), C5 H10 O'
_chemical_formula_sum            'C47 H64 N14 O3 S2'
_chemical_formula_weight         937.24
_chemical_name_systematic
'<i>N</i>'-(Morpholine-4-carbonothioyl)-4-(4-phenylpiperazin-1-yl)picolinohydrazonamide 2-methyltetrahydrofuran hemisolvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.45775(12)
_cell_length_b                   11.96434(9)
_cell_length_c                   23.87725(16)
_cell_measurement_reflns_used    83198
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.2090
_cell_measurement_theta_min      3.6660
_cell_volume                     4701.58(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
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_computing_publication_material
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
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SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.0654
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            139136
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.904
_diffrn_reflns_theta_min         3.694
_diffrn_source                   'micro-focus sealed X-ray tube'
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_exptl_absorpt_correction_T_max  1.000
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;
(CrysAlis PRO; Rigaku OD, 2024)
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_density_diffrn    1.324
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_exptl_crystal_F_000             2000
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_exptl_crystal_size_mid          0.136
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_refine_diff_density_min         -0.248
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;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.677(15)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         9882
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0523P)^2^+1.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                9463
_reflns_number_total             9882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wv3017sup1.cif
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_shelx_estimated_absorpt_t_min   0.440
_shelx_estimated_absorpt_t_max   0.855
_shelx_hkl_checksum              78660
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_cod_database_fobs_code 2312721