During the past few decades, considerable attention has been paid to the chemistry of the coordination compounds. Co-ordination compounds in which the central metal ion is bounded to different Ligands exhibit different characteristic properties. The characteristics of such compounds are based on nature of metal as well as the type of ligands and their structures. In the present book, series of Copper(II), Nickel(II) and Cobalt(II) complexes derived from 4,6-diacetylresorcinol have been prepared. The ligands and their metal complexes have been characterized by FT-IR, Mass, 1H NMR, UV–Vis., elemental analysis, ESR and Thermal gravimetric analysis. The Schiff base and their metal complexes were tested for antimicrobial activity against Gram positive bacteria Staphylococcus Aureus, Streptococcus Pyogenes and Gram negative bacteria Escherichia Coli, Pseudomonas Aeruginosa and fungus Candida Albicans, Aspergillus Niger and Aspergillus Clavatus.