The new complexes of xipamide (XPD) with Ti(III), Ni(II), Pd(II), Zr(IV), Ce(IV), and U(VI) have been synthesized. Elemental analysis, magnetic properties, molar conductivities, thermal analysis, and UV-Vis, IR and 1H NMR spectra, elucidated the structures of complexes. According to spectral data, xipamide behaved in the obtained complexes as a bidentate chelating anion with the charge (–1) and coordinated via oxygen atoms of the deprotonated phenolic and carbonyl groups. Kinetic parameters of thermogravimetric analysys and its differential have been evaluated by using the Coats–Redfern and Horowitz–Metzeger methods. Thermodynamic data indicated thermal stability of all complexes. The ligand and its metal complexes were screened for their antifungal activity against A. fumigatus,G. candidum, syncephalastrum, and C. albicans, and antibacterial activities against two Gram-positive bacteria species, such as S. aureus and B. subtilis, two Gramnegative such as E. coli and P. aeruginosa.