Synthesis of novel volatile niobium precursors containing carboxamide for Nb2O5 thin films

A series of novel Nb(V) tBu-imido/N-alkoxy carboxamide complexes, NbCl2(NtBu)(pyridine)(edpa) (1), NbCl2(NtBu)(pyridine)(mdpa) (2), and Nb(NtBu)(mdpa)3 (3), were successfully synthesized by metathesis reaction between Nb(NtBu)Cl3(py)2 and several equivalents of Na(edpa) (edpaH = Nethoxy-2,2-dimethylpropanamide) and Na(mdpa) (mdpaH = N-methoxy-2,2-dimethylpropanamide). These complexes could potentially serve as precursors for Nb-containing thin films. Compounds 1–3 were characterized by FT-IR and 1H and 13C NMR spectroscopies, elemental analysis, and thermogravimetric analysis (TGA). Single crystal X-ray diffraction analysis suggested that complex 3 has a distorted pentagonal bipyramidal geometry around the central Nb atom, with three bidentate mdpa ligands and one tBu imido group saturating the coordination. TGA analysis revealed that the thermal characteristics of 3 were superior to those of 1 and 2. All prepared complexes were able to be distilled or sublimed and expected potential precursors for the fabrication of thin films.