Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu and Ni coordination compounds
Lobana, Tarlok Singh; Kaushal, Mani; Bhatia, Robin; Bala, Ritu; Butcher, Ray J.; Jasinksi, Jerry P.; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S205322962101319X

data_2022488
_publ_section_title
;
 Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu
 and Ni coordination compounds
;
_journal_coeditor_code           YD3022
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322962101319X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C15 H16 N4 S'
_chemical_formula_sum            'C15 H16 N4 S'
_chemical_formula_weight         284.38
_chemical_name_common
;
4-Benzoylpyridine 4-ethylthiosemicarbazone
;
_chemical_name_systematic
(<i>E</i>)-<i>N</i>-Ethyl-2-[phenyl(pyridin-4-yl)methylidene]hydrazine-1-carbothioamide
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
OLEX2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8897(3)
_cell_length_b                   10.9845(2)
_cell_length_c                   16.8393(3)
_cell_measurement_reflns_used    10170
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.3650
_cell_measurement_theta_min      3.9800
_cell_volume                     2939.14(9)
_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_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku OD Gemini Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36150
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.845
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0522P)^2^+0.7060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                4133
_reflns_number_total             5181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3022sup1.cif
_cod_data_source_block           2
_cod_database_code               2022488
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              23706
_shelx_res_checksum              52660
_cod_database_fobs_code 2022488