Studies on thermal properties of substances have a great importance from both scientific and practical point of view. In industries stability of row materials/ intermediates /final product have become essential criteria. In pharmaceutical industries, as per the requirement of the drug for the receptor site of the body drug stability counts a lot, thus thermal properties play a very significant role in day to day life. Thermal properties of synthesized para - Hydroxy - meta - nitro acetophenone compound 1, and its three novel complexes 4-hydroxy-3-Nitro-acetopnenone Cu (II) di μ - Chloro dichloro copper (II) compound 2, 4-hydroxy-3-Nitro-acetopnenone Ni (II) di μ - Chloro Nickel (II) chloride trihydrate compound 3 and Aqua-Chloro-4-hydroxy-3-Nitro-acetopnenone Co (III) di μ Chloro aqua tri Chloro Cobalt (III) compound 4 were assessed. The thermal kinetic parameters such as order of reaction η’ and energy of activation ‘Ea’ were established from computer programme of rising temperature expression of Coats and Redfern. This study signifies that metal complexes are less stable than ligand. This kinetic study has been performed for the first time.