A mixture of iron carbides and fullerene C 60 formed by electric arc synthesis has been hydroxylated by adding OH groups to the fullerene surface, which made it possible, according to the EXAFS data, to obtain almost pure fullerenol Fe@C 60 (OH) 30 . Powder samples of the fullerenol and the product obtained after its dehydroxylation have been examined using Mössbauer spectroscopy. The Mössbauer spectra have been processed under the assumption of superposition of three partial doublets of spectral lines. It is established that two doublets due to Fe 3+ dominate in the fullerenol spectrum. For the reduced fullerene Fe@C 60 sample, two doublets are due to Fe 3+ and the Fe 2+ doublet dominates. Thus, attachment of OH groups from the outer side of the fullerene carbon frame increases the oxidation state of iron, which shows that the iron atom is located inside the frame.