A series of new Schiff base-containing triosmium alkylidyne carbonyl clusters [Os3 (μ-H) 2 (CO) 9 (μ3-CNC5H4CH NC6H4R)](R= H, NMe2, SMe, CMe3, NH2, Br, Cl, OCnH2n+ 1, n= 1, 6, 7 or 9) have been prepared by reaction of [Os3 (μ-H) 3 (CO) 9 (μ3-CCl)] with one equivalent of 1, 8-diazabicyclo [5.4. 0] undec-7-ene in the presence of a ten-fold excess of the Schiff base ligands NC5H4CH NC6H4R at room temperature. Analogous triosmium ...