The β-ketoiminato complex [Pd(OAc)L] (3) can be synthesized by the reaction of bis(benzoylacetone)diethylenetriamine (1, = LH) with [Pd(OAc)2] (2). The structure of 3 in the solid state has been determined by single X-ray diffraction analysis. Complex 3 crystallizes as a dimer (32), which is formed by hydrogen bonds between NH and OOAc functionalities of two adjacent ligands. Each of the Pd atoms is complexed by one ON2 donor unit of the polydentate ligand L- and an acetate group. Pd-Pd interactions and hydrogen bond formation between a NH and the C=O acetate moiety lead to a [4 + 2] coordination at Pd. The non-coordinated part of L exists in its β-keto-enamine form. The thermal decomposition behavior of 32 was studied by TG (thermogravimetry) and TG-MS showing that 32 decomposes between 200 and 500°C independent of the applied atmosphere. Under oxygen PdO is produced, while under argon Pd is formed as confirmed by PXRD measurements. Complex 32 was applied as a spin-coating precursor (conc. 0.1 mol L-1, volume 1.5 mL, 3000 rpm, deposition time 6 min, heating rate 50 K min-1, holding time 60 min (Ar) and 120 min (air) at T = 800°C). The as-obtained samples are characterized by granulated particles of Pd/PdO on the substrate surface. EDX (energy-dispersive X-ray spectroscopy) and XPS (X-ray photoelectron spectroscopy) measurements confirmed the formation of Pd (Ar) or PdO (O2) with up to 12 mol% C impurity.
|Number of pages||12|
|Journal||Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences|
|Publication status||Published - 4 Dec 2019|