A study has been made of the catalytic activity of iron-aluminium oxides FexAl2-xO3 obtained by alkoxosynthesis in the liquid-phase oxidation of hexadecane and cumene (343-433 K). The interrelation between the structure of iron-aluminium oxides, studied by means of Mossbauer spectroscopy, static magnetic susceptibility and EXAFS, and their catalytic activity has been established. The role of electron-excited terminal oxygen in surface superparamagnetic clusters of gamma-Fe2O3 as an active oxidation initiation centre is discussed. By the kinetic method of combined initiation it has been shown that iron-aluminium oxides take part only in the stage of initiation of oxidation with subsequent development of the reaction within the liquid phase by a homogeneous mechanism. The kinetic parameters of low-temperature oxidation of cumene in the presence of the systems synthesized have been determined. It has been established that the rate of heterogeneous initiation of the reaction in their presence amounts to (5-7) x 10(-7) mole/l-sec (343 K), which is three orders of magnitude higher than the corresponding values for a number of simple oxides.