The reactions of ethylene glycol with iron and cobalt oxalates upon heating in air are reported. Heat treatment of mixtures of oxalate powders with ethylene glycol yields new compounds (solvates) via the replacement of the water molecules in the oxalate structure by ethylene glycol molecules: MC 2 O 4 · 2H 2 O + HOCH 2 CH 2 OH = MC 2 O 4 (HOCH 2 CH 2 OH)+2H 2 O↑. The crystals resulting from this reaction are elongated, and their shape is inherited by their thermolysis products. Thermolysis in air yields microwhiskers and nanowhiskers of Fe 2 O 3 and Co 3 O 4 , and thermolysis in an inert atmosphere affords Fe 3 O 4 and Co whiskers. The thermolysis of FeC 2 O 4 (HOCH 2 CH 2 OH) in helium yields a new structural modification of FeC 2 O 4 as an intermediate product. The resulting compounds and their thermolysis products were characterized by X-ray powder diffraction, microscopy, IR spectroscopy, and thermogravimetric and chemical analyses. The particle shape and size were determined by scanning electron microscopy.