Through isolobal displacement reaction of (η5-RC5H4)MCoFeS(CO)8 (1a:M=Mo, R=H; 1b:M=Mo,R=MeO2C; 1c:M=Mo, R=Me; 1d:M=Mo, R=EtO2C:1e:M=W,R=H) with Cp2Ni, a series of MNiFeS clusters have been synthesized. Further isolobal displacement reactions of 2a,b with Co2(CO)8 and 2c,d with Fe2(CO)9 produce MoFeCoS clusters (η5-RC5H4)MoCoFeS(CO)8 (1a:R H; 1b:R=MeO2C) and MoNiFe2S clusters (η5-C5H5)(η5-RC5H4)MoNiFe2S(CO)10 (3a:R=Me; 3b:R=EtO2C), respectively. New cluster complexes 2c-e and 3a,b have been characterized by elemental analysis, IR, 1H NMR spectroscopy. In addition, the crystal structure of the previously reported analog of 3a,b (η5-C5H5)(η5-MeO2CC5H4)MoNiFe2S(CO)10 (3c) has been determined by X-ray diffraction techniques. 3c belongs to monoclinic system, space group Cc(#9), cell parameters a=1.0051(3) nm, b=1,5311(5) nm, c=1.7437 nm,β=105.5(3)°, Z=4. Final agreement factors R=0.025,Rw=0.033.