Abstract: In this cxpcrbocnt, the Mossbauer speCtra and crystal structures or the newMo(W)-Fo-S Cluster compounds (1) (Et₄N)MeoFe₂(μ₃-S)₂(CO)₈(S₂CNEt₂ and (2)(Et₄N)WFe₂(μ₃-S)₂(CO)₈(S₂CNEt₂ have been measured. There are only a symmetricquadrupole doublet for each compounds, because the two iron atoms in the molecule of eachcompounds arc equivalent. This is consistent with that of single crystal structural analysis. TheMossbauer data (77 K) obtained by computer fitted, showed:δ=0.008±0.004mm/s,△E_Q=0.965 ±0.004mm/s, line width Г=0.320 ±0.004mm/s; and δ=0.007 ±0.004mm/s,△E_Q=0.834 ±0.004mm/s, Г=0.371 ±0.004mm/s; for (1) and (2), respectively. The isomershift δ is relative to α-Fe. Their Crystal structures have been determined by X-ray diffraction.cluster compounds (1) and (2) crystallizes in triclinic space group P1. From Mossbauer data, itcan be considered that the iron atoms in cluster compounds (1) and (2) are in low spin state andoxidation state of+2.