Synthesis, structure and biological activity of four new picolinohydrazonamide derivatives
Szczesio, Małgorzata; Gobis, Katarzyna; Korona-Głowniak, Izabela; Mazerant-Politowicz, Ida; Ziembicka, Dagmara; Foks, Henryk; Główka, Marek; Olczak, Andrzej; Acta Crystallographica, Section C 76 (2020) 673–680; doi:10.1107/S2053229620007822

data_2022361
_publ_section_title
;
 Synthesis, structure and biological activity of four new
 picolinohydrazonamide derivatives
;
_journal_coeditor_code           FM3063
_journal_issue                   7
_journal_name_full               'Acta Crystallographica, Section C'
_journal_page_first              673
_journal_page_last               680
_journal_paper_doi               10.1107/S2053229620007822
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C17 H19 Cl N6 S [+ solvent]'
_chemical_formula_moiety         'C17 H19 Cl N6 S [+ solvent]'
_chemical_formula_sum            'C17 H19 Cl N6 S'
_chemical_formula_weight         374.89
_chemical_name_common
;
6-Chloro-<i>N</i>'-(4-phenylpiperazine-1-carbonothioyl)picolinohydrazonamide
;
_chemical_name_systematic
6-Chloro-N'-[(4-phenylpiperazin-1-yl)carbothioylamino]pyridine-2-carboximidamide
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2996(3)
_cell_length_b                   9.3870(3)
_cell_length_c                   18.9935(5)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.4095
_cell_measurement_theta_min      3.996
_cell_volume                     1972.05(10)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD '
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14116
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.118
_diffrn_reflns_theta_min         4.212
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.377
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0392P)^2^+1.2462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                3747
_reflns_number_total             3863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3063sup1.cif
_cod_data_source_block           5
_cod_depositor_comments          'Adding Fobs data.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2022361
_cod_database_fobs_code          2022361
_shelx_estimated_absorpt_t_min   0.52
_shelx_estimated_absorpt_t_max   0.75
_shelx_hkl_checksum              76668
_shelx_res_checksum              74183
_shelx_fab_checksum              21149