| Summary: | Five trifluoroacetylacetonate (<i>tfaa</i><sup>−</sup>) complexes [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)]<sub>2</sub>, [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>] · <i>diglyme</i>, [Tm(<i>tfaa</i>)<sub>3</sub>(DME)] (DME = 1,2-dimethoxyethane) and [TmCl<sub>2</sub>(<i>tfaa</i>)(<i>diglyme</i>)] (<i>diglyme</i> = bis(2-methoxyethyl) ether) of thulium have been synthesized and characterized by X-ray single-crystal structure analysis and spectroscopic techniques. Thermoanalytical studies at elevated temperatures provide information about their volatility. The results are compared with the hexafluoroacetylacetonate (<i>hfaa</i><sup>−</sup>) complexes of thulium known in the literature, which were reported as volatile precursors for CVD application. The reported high volatility of [Tm(<i>hfaa</i>)<sub>3</sub>(DME)] was confirmed and compared with those of the aqueous complexes which show a lower transport rate. In addition, the new crystal structures of the hexafluoroacetylacetonate complexes [Tm(<i>hfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>hfaa</i>)<sub>2</sub>(<i>tfa</i>)(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub> (<i>tfa</i><sup>−</sup> = trifluoroacetate), [Tm(<i>hfaa</i>)<sub>3</sub>(DME)NaCl]<sub>2</sub> and Na[Tm(<i>hfaa</i>)<sub>4</sub>] are presented.
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