Square planar Ni(II) complexes of acetone N4-phenyl-thiosemicarbazone and in situ generated benzoyl thiosemicarbazide ligand: Synthesis, spectral and structural characterizations, thermal behaviour and electrochemical studies
Bharty, M. K.; Paswan, Santosh; Bharati, P.; Sonkar, Piyush Kumar; Ganesan, Vellaichamy; Butcher, Raymond J.; New Journal of Chemistry 41 (2017) 15466–15474; doi:10.1039/C7NJ01030C

data_7056744
_publ_section_title
;
 Square planar Ni(II) complexes of acetone N4-phenyl-thiosemicarbazone and
 in situ generated benzoyl thiosemicarbazide ligand: Synthesis, spectral
 and structural characterizations, thermal behaviour and electrochemical
 studies
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15466
_journal_page_last               15474
_journal_paper_doi               10.1039/C7NJ01030C
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C20 H24 N6 Ni S2'
_chemical_formula_sum            'C20 H24 N6 Ni S2'
_chemical_formula_weight         471.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.569(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.403(2)
_cell_length_b                   7.6265(5)
_cell_length_c                   12.2279(9)
_cell_measurement_reflns_used    1471
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0810
_cell_measurement_theta_min      3.2152
_cell_volume                     2168.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8292
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+0.2872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                1764
_reflns_number_total             2563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj01030c2.cif
_cod_data_source_block           shelxl-1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7056744