| Abstract | Two new dithiolate copper(II) and nickel(II) complexes with the ligand tert-butyl N-(2-mercaptoethyl)- carbamate (Boc-SH) were prepared. Their structures were established to be [(Boc-S)2M], where M = Cu (1) and Ni (2) by using elemental analysis, thermal analysis, molar conductivity, FT-IR, Raman, UV/VIS, and ESR as well as EI-mass spectroscopic methods. The X-ray structure of the ligand Boc-SH was also determined. Spectral data showed that the carbamate ligand act as anioinic bidentate through one immine nitrogen and one thiolate sulfur donor atoms. The spectral techniques suggest that both complexes appear to have square planar geometries. The very low electrical conductance of the two complexes supports their neutral nature. The redox behaviors of the obtained complexes were also investigated by cyclic voltammetry. The monomeric nature of both complexes was assessed from their magnetic susceptibility values. The thermoanalytical data evidence that complex (2) is stable up to 165 _C and undergo complete decomposition, resulting in NiO as a residual product. The TEM image |