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_2022362
_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          'C6 H7 Cl N4'
_chemical_formula_moiety         'C6 H7 Cl N4'
_chemical_formula_sum            'C6 H7 Cl N4'
_chemical_formula_weight         170.61
_chemical_name_common
;
6-Chloropicolinohydrazonamide
;
_chemical_name_systematic
;
<i>N</i>'-Amino-6-chloropyridine-2-carboximidamide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   3.77379(4)
_cell_length_b                   5.63483(4)
_cell_length_c                   32.9783(2)
_cell_measurement_reflns_used    16896
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.5140
_cell_measurement_theta_min      4.0280
_cell_volume                     701.273(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9765
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy Dualflex Pilatus 300K'
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            19459
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         78.6751
_diffrn_reflns_theta_min         4.0214
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.264
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.217
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 533 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0336P)^2^+0.1754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                1460
_reflns_number_total             1471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3063sup1.cif
_cod_data_source_block           6
_cod_depositor_comments          'Adding Fobs data.'
_cod_database_code               2022362
_cod_database_fobs_code          2022362
_shelx_hkl_checksum              8498
_shelx_res_checksum              55275
_shelxl_version_number           2.014