The photochemical reaction of C-60 and excess Fe2S2(CO)(6) produces C-60[S2Fe2(CO)(6)](n) (n = 1-3). Chromatographic workup of the reaction mixture afforded pure C60S2-Fe-2(CO)(6) in high yields. This species was characterized by C-13 NMR and IR spectroscopies, as well as mass spectrometry and cyclic voltammetry. These experiments suggest that a variety of M-S-fullerene compounds could be prepared by the additions of metal sulfides to fullerenes.