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_2022490
_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_iupac          '[Cu (C9 H11 N4 S)2]'
_chemical_formula_moiety         'C18 H22 N8 Ni S2'
_chemical_formula_sum            'C18 H22 N8 Ni S2'
_chemical_formula_weight         473.26
_chemical_name_common
;
Bis(3-formylpyridine
4-ethylthiosemicarbazonato-\k^2^<i>N</i>^1^,<i>S</i>)nickel(II)
;
_chemical_name_systematic
Bis[(<i>Z</i>)-<i>N</i>-ethyl-2-(pyridin-3-ylmethylidene)hydrazine-1-carbothioamidato-\k^2^<i>N</i>^1^,<i>S</i>]nickel(II)
_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   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                 107.823(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6398(6)
_cell_length_b                   14.3930(8)
_cell_length_c                   9.7339(7)
_cell_measurement_reflns_used    2040
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.7510
_cell_measurement_theta_min      3.5650
_cell_volume                     1018.97(13)
_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 0.890
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6410
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.781
_diffrn_reflns_theta_min         3.585
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       irregular
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0373P)^2^+0.2595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                2679
_reflns_number_total             3361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3022sup1.cif
_cod_data_source_block           4
_cod_database_code               2022490
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.852
_shelx_hkl_checksum              18902
_shelx_res_checksum              44860
_cod_database_fobs_code 2022490