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The ligand 5-methyl-2-phenyl-4-[(E)-1,3-thiazol-2-yl-diazenyl]-2,4-dihydro-3Hpyrazol-3-one (Dy) has been synthesized by diazo coupling reactions of 5-methyl-2-phenyl-2,4dihydro-3H-pyrazol-3-one with 2-aminothiazole and ferric hydrogen sulfate (FHS), as a catalyst, under solvent-free conditions. A series of complexes of the ligand with Co(II), Ni(II), Cu(II), and Zn(II) ions are synthesized and structurally characterized by 1H NMR, FTIR, and UV-Visible spectral techniques. The cytotoxic activity of the complexes and the uncoordinated ligand against human breast cancer (MCF-7) and chronic myelogenous leukemia cell line (human erythroleukemia) (K-562) cell lines exhibits good viability in the range of 50.16-55.16% at a concentration of >100-110 µg/mL as compared to the inhibition in the untreated cells. Further, the metal complexes and ligand were screened against antibacterial strains of S. typhi, S. aureus, and E. coli. Both the cytotoxicity and antioxidant studies are correlated with computational docking analysis and powder XRD studies reviles that all complexes are in crystalline nature.