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The Au(I) complexes CF3AuCNMe (1a) andCF3AuCNtBu (1b) were investigated as Au(I) precursors forfocused electron beam-induced deposition (FEBID) ofmetallic gold. Both1aand1bare sufficiently volatile forsublimation at 125±1 mTorr in the temperature range ofroughly 40?50°C. Electron impact mass spectra of1a?bshow gold-containing ions resulting from fragmenting the CF3group and the CNR ligand, whereas in negative chemicalionization of1a?b, the major fragment results fromdealkylation of the CNR ligand. Steady-state depositionsfrom1ain an Auger spectrometer produce deposits with asimilar gold content to the commercial precursor Me2Au-(acac) (3) deposited under the same conditions, while the gold content from1bis less. These results enable us to suggest thelikely fate of the CF3and CNR ligands during FEBID