Reaction of Fe(DMF)6[(FeCl2)2MoS4] and Et2NCS2Na in DMF results in conversion of the linear trinuclear cluster into the single cubane-like cluster, MoFe3S4(S2CNEt2)5 (I), the structure of which was determine The influence of the ligand-related redox process and the ligation mode on the conversion reaction and the product are discussed. The various structural features of MoFe3S4 core skeleton with different oxidation states are compared. I is triclinic, space group P1, with a 15.711(3), b 16.637(4), c 21.842(3) ? a 86.93(1), b 70.84(1), g 82.61(2)? Z = 4, d.(calcd.) = 1.458 g cm-3, R = 0.082, Rw = 0.096.

Key words: CRYSTAL STRUCTURE DETERMINATION, SODIUM COMPOUNDS, DMF, NITROGENASE, MOLYBDENUM COMPLEX, CLUSTER COMPOUND, TITANIUM COMPLEX, POLYNUCLEAR COMPLEX, DIETHYLAMINE P, SULFIDE COMPLEX