In the current study, synthesis and characterization of a new nano-structured zirconium(IV)-minoxidil complex (1), where minoxidil, (C₉H₁₅N₅O; 6-(1-Piperidinyl)-2,4-pyrimidinediamine 3-oxide), have been investigated in two different solvents. The compound 1 has been synthesized by sonochemical method in the presence of methanol and monoethylene glycol (MEG) as solvents and characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and elemental analysis. The thermal stability of the compound 1 has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Pure monoclinic (m) zirconia (ZrO₂) nanoparticles were readily synthesized from thermal decomposition of the compound 1 as a new precursor in both solvents. The products were characterized by FT-IR, XRD, and SEM to exhibit the phase and morphology. The results showed that, pure zirconia was produced with particles size of 53 nm and the crystal system was monoclinic when methanol was used as solvent in complexation process. While the particles size of zirconia with the same structure were significantly reduced to 25 nm, using MEG as solvent. This study demonstrates that the coordination compounds may be suitable precursors for the simple one-pot preparation of nano-scale metal oxides with different morphologies.