Metal derivatives of N1-substituted thiosemicarbazones: Synthesis, structures and spectroscopy of nickel(II) and cobalt(III) complexes
Tarlok S. Lobana; Poonam Kumari; Geeta Hundal; Ray J. Butcher; A. Castineiras; Takashiro Akitsu; Inorganica Chimica Acta 394 (2013) 605–615; doi:10.1016/j.ica.2012.09.021

data_1512801
_publ_section_title
;
 Metal derivatives of N1-substituted thiosemicarbazones: Synthesis,
 structures and spectroscopy of nickel(II) and cobalt(III) complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              605
_journal_page_last               615
_journal_paper_doi               10.1016/j.ica.2012.09.021
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C18 H20 N6 Ni S2'
_chemical_formula_sum            'C18 H20 N6 Ni S2'
_chemical_formula_weight         443.23
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.480(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.749(5)
_cell_length_b                   7.474(4)
_cell_length_c                   14.628(5)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     2035.6(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'SHELXTL-PC (Sheldrick, 1993)'
_computing_molecular_graphics
'ORTEP,Mercury(Farrugia,1997;Bruno et.al.,2002)'
_computing_publication_material  'WINGX,(Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altamore et. al., 1992)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1946
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         2.19
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et. al., 1968'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                1371
_reflns_number_total             1889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-605-615-1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1512801