Binary complexes of the type [M(S 2 CCN) 2 ] (M=Mn 2 + , Fe 2 + , Co 2 + , Ni 2 + , Cu 2 + and Zn 2 + ) have been synthesised from alcoholic solutions. They have been characterised using elemental analyses, IR, UV-VIS spectroscopy, magnetic susceptibility measurement and solution conductance data. In thermogravimetry (TG) studies, all these complexes exhibit a prominent weight loss step between 100 and 330 o C under a N 2 atmosphere. Besides, a second weight loss step has also been observed beyond 800 o C for the Mn 2 + , Fe 2 + and Co 2 + complexes, between 400 and 600 o C for Zn 2 + complex and beyond 380 o C for Cu 2 + complex. Broad differential thermal analysis (DTA) endotherms are observed corresponding to these weight loss steps. The first weight loss in the TG scan of the complexes follows a deceleratiory α-time curve with D 3 mechanism for all complexes. The activation energy (E a ) for the thermal decomposition varies between 43 and 115kJ/mol and removal of CS 2 and/or CS have been suggested. Various decomposition parameters have been calculated.