AbstractReduction ofn‐C5H11N3by Na2S2O4was performed in the presence of (n‐Bu4N)3[Mo2Fe6S8(OMe)3(SC6H4‐p‐n‐C8H17)6] ((n‐Bu4N)3[Mo‐Fe]) as a catalyst in aqueous Triton X‐100 micellar solutions. The rate of the reduction is enhanced efficiently by the addition of methyl viologen (MV2+). The methyl viologen radical cation (MV+) produced by the reaction of MV2+with Na2S2O4undergoes a disproportionation reaction to afford MV2+and MV° in the micellar solution. The resultant MV° formed in the micelle transfers two electrons to [Mo‐Fe]3−effectively to give [Mo‐Fe]5−, which reducesn‐C5H11N3with two electrons