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_7056743
_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         'C4 H6 N6 Ni S2'
_chemical_formula_sum            'C4 H6 N6 Ni S2'
_chemical_formula_weight         260.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.109(4)
_cell_length_b                   14.882(6)
_cell_length_c                   7.304(4)
_cell_measurement_reflns_used    2121
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.152
_cell_measurement_theta_min      4.012
_cell_volume                     881.4(7)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker Apex 2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8833
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0255P)^2^+0.8703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                850
_reflns_number_total             1282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01030c2.cif
_cod_data_source_block           shelx-2
_cod_original_cell_volume        881.3(7)
_cod_database_code               7056743
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              53513