The ligation behavior of 5-hydroxy-2-nitrobenzaldehydethiosemicarbazone (L) and its Mn(II), Co(II) and Ni(II) complexes has been synthesized and characterized by Elemental analysis, Electronic, FT-IR, Raman, EPR spectral techniques and Cyclic voltammetric study. The ligand (L) belongs to triclinic system with P1 space group. The IR spectral data of ligand indicate the taking part of sulphur and azomethine nitrogen in coordination to the central metal ion. The electronic, FT-IR and EPR spectral studies reveals all the complexes are distorted octahedral geometry. The synthesized ligand and its metal(II) complexes were tested for their antioxidant activity by 2, 2-diphenyl-1-picrylhydrazyl (DPPH) method and antibacterial activity against E.coli, Staphylococcus aureus, Bacillus subtilis, Salmonella typhi and Klebsiella pneumonia. The antibacterial and antioxidant activities of the ligand and its metal complexes had shown moderate to good activity, among all the compounds Ni(II) complex had shown more activity.