Four new Macrocyclic Hydrazone Schiff bases were synthesized by condensation of intermediate compounds: 1,6- bis (2-formyl-phenyl) hexane, 1,6-bis (2-acetyl-phenyl)hexane(V), α,α’-bis(2-carboxyaldehyde phenoxy) xylene(VI), and 1,7-bis (2-formyl-phenyl)-1,4,7-trioxaheptane(VII) with 1,3-Dithio-carbohydrazide(III) in the molar ratio (2:2) in DMF. Identification of these macrocyclic Schiff bases ligands (VIII, IX, X, XI). The Schiff bases were checked by different spectral technique (LC-MS, 1H-NMR, IR, elemental analyses). These compounds were tested to determine their ability to inhibit corrosion of mild steel in 1M H2SO4 by Electrochemical measurements. The new Macrocyclic Hydrazone Schiff Bases were studied for antibacterial activities against Gram positive (Bacillus subtilis and Staphylococcus aureus) and Gram negative (Salmonella typhi and Escherichia coli). The compound ligands exhibited a variable activity of inhibition on the growth of the bacteria.