The thermochemical behavior of the coordination compound [Fe(urea)(6)](NO3)(3) was studied by simultaneous CG-TG-DTG-DTA and mass spectrometry methods non-isothermal conditions. The compound decomposes at -200 degreesC into a mixture of spinel-type oxides and hematite. The nature and particle size of the final decomposition products are strongly associated with the conditions during the thermal treatments, in particular the heating rate and the calcination temperature. A certain fraction of the products are formed as nanometric particles; they show superparamagnetic behavior at room temperature. The comparably low temperature of the calcination treatments of this compound is a promising perspective to attain small sized magnetic powders.