In current study, zirconia (ZrO2) nanoparticles have been synthesized through the decomposition of a nano-structured Zr(IV) supramolecular compound, (pydaH)2[Zr(pydc)3].5H2O (1), where [pyda.H]+ = 2,6-diaminopyridinium, and [pydc]2- = 2,6-pyridinedicarboxylate, as a new precursor. The compound 1 has been synthesized by sonochemical method and characterized by field emission scanning electron microscope (FESEM), X-ray powder diffraction (XRD) and elemental analyses. The morphology, structure, and composition of the as-synthesized nanostructures have been confirmed by XRD and FESEM analyses. The XRD pattern of the residue obtained from calcination of compound 1 at 700 °C under air atmosphere provides that crystal system was mixture of monoclinic (m) and tetragonal (t) with particle size about 28 nm.