The heteroleptic tris(zinc) complex 5 was prepared by a two-step procedure via 4 as an intermediate (Scheme 2). 4 was isolated from the reaction of two equiv. of 3a with [Pd(Me)2(k 2 -TMEDA)] (TMEDA = N,N,N',N'-tetramethylethylenediamine). DOSY experiments, titration experiments, and VT NMR analysis suggest that the TMEDA ligand of 4 is labile and can reversibly dissociate in solution. Although reaction of 4 with further equivalents of 3a did not lead to a homoleptic tris(zinc) complex, addition of the less sterically demanding 3b to 4 resulted in formation of the heteroleptic analogue 5 in low yield. C6D6 solutions containing 5 demonstrated a single resonance at d = -1.27 ppm consistent with a fast-exchanging hydride resonance. 5 is unstable in solution and rapidly decomposes in less than 2h at 25 °C. The purification of this compound was extremely challenging, single crystals could only be isolated on one occasion.