The synthesis and characterization of CoLz(NCS)2.2H20, NiL2(NCS)2-2H20, CuL(NCS)2. 3H20 (L=4,4'-bipyridyt, 4-bipy) CoX3(NCS)2-H20, NiX3(NCS)2 and CuX2(NCS)2 (X=2,4'-bipyridyl, 2,4'-bipy) are reported. The IR spectra and other physical properties of these compounds are discussed. The thermal properties of the complexes in the solid state were studied under non-isothermal conditions in air atmosphere. The intermediates of dehydration and decomposition at different temperatures were characterized by X-ray diffraction.