Decomposition of Fe(CO)(5) on prereduced Rh/NaY under flowing 5% H-2/Ar has been used to prepare zeolite-encaged RhFex clusters free of Fe2+ or Fe3+ ions or Fe oxides. XPS and TPR results indicate the absence of significant amounts of iron other than Fe-0; some carbon is detected as methane by TPR in flowing H-2. Mossbauer spectroscopy shows a singlet that is assigned to Fe-0 alloyed with Rh but no significant amounts of Fe2+, which is abundant in samples prepared by conventional Fe2+ ion exchange, followed by reduction. A doublet with an isomer shift of 0.39 mm/s (relative to alpha-Fe) and a quadrupole splitting of 0.90 mm/s strongly contributes to the Mossbauer spectra of both the Fe2+-free and the conventional samples. The present results suggest that this signal is caused by some Fe-0 species, not by an irreducible Fe3+ oxide.