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The new chiral clusters [η5-C5H4C(NR)CH3]RuNiM(CO)5(μ3-S) (R = NH-C6H3-2,4-(NO2)2, M = Mo, 3; M = W, 4) were synthesized and the structure of cluster 3 was determined by single-crystal X-ray analysis. Crystal data: C23H16O9N4MoNiRuS, Mr = 780.18, orthorho