Reaction of (NH4)2MoS4 and FeCl3 with HOCH2CH2ONa in ethylene glycol (L) solution followed by treatment with Bu4NBr gave a Mo-Fe-S cluster, [Bu4N]3[Mo2FeS8O].L, which was characterized by single crystal x-ray diffraction anal., IR, UV-visible, Moessbauer spectra and electrochem. properties. The complex showed catalytic activity in the reduction of C2H2 with KBH4. The complex is monoclinic, space group P21/c, with a 16.889(6), b 16.671(8), c 24.527(9) ? b 99.66(3)? Z = 4, R = 0.066, Rw = 0.06. The anion consists of a Fe atom bonding to a MoS4 unit via 2 S2- bridges and a MoOS2(S2) unit via 2 S2- bridges and contains 2 Mo-Fe bonds.

Key words: CRYSTAL STRUCTURE DETERMINATION, SODIUM COMPOUNDS, X-RAY DIFFRACTION ANALYSIS, ETHANEDIOL, IRON COMPLEX, MOLYBDENUM COMPLEX, CLUSTER COMPOUND, SULFIDE COMPLEX