The new chiral cluster [NiRuMo(CO)5(μ3-S)(η5-C5H5(5-C5H4COCH3)] 3 was synthesized by the reaction of precursor [CoRuMo(CO)8(μ3-S(η5-C5H4COCH3)] 1 with NiCp2 2 in refluxing THF. It was characterized by C/H elemental analysis, IR and 1H NMR. Molecular structure of cluster 3 was determined by single-crystal X-ray analyses. Crystal data: triclinic, space group Pī with the following crystallographic parameters: a = 7.9606(8), b = 8.5604(9), c = 14.779(2)A, = 93.908(2), = 105.057(2), = 101.463(2)°, C17H12O6MoNiRuS, Mr = 600.0(5), Z = 2, V = 945.5(2)A3, Dc = 2.108 g/cm3, = 2.568 mm-1, 2 max 2.00σ(I).