The nonaqueous preparation of nanocrystalline indium and zinc oxide involving the solvothermal reaction of metalacetylacetonates with acetonitrile is presented. The synthesis approach is characterized by a particularly moderate reaction temperatureof 100
C and by the use of an oxygen-free solvent. The oxygen for the metal oxide formation is supplied by the acetylacetonateligand of the precursor molecules. In the case of In
2O
3, the product consists of crystalline nanoparticles with a spherical morphologyand a narrow size distribution in the range of 3-6 nm. According to transmission electron microscopy (TEM), the ZnO nanoparticlesare in the size range of 15-85 nm, sometimes with well-faceted hexagonal morphology. Powder X-ray diffraction (XRD) data aswell as high-resolution TEM point to mesocrystal formation, i.e., the ZnO nanoparticles are composed of a highly oriented arrangementof smaller nanocrystallites that scatter like a single crystal.