Thermal dehydration of Y(TFA)3(H2O)3: Synthesis and molecular structures of [Y(μ,η1:η1-TFA)3(THF)(H2O)]1∞ · THF and [Y4(μ3-OH)4(μ,η1:η1-TFA)6(η1-TFA)(η2-TFA)(THF)3(DMSO)(H2O)] · 6THF (TFA = trifluoroacetate)

In order to obtain a better anhydrous precursor for various applications in materials science and catalysis, thermal dehydration reactions of Y(TFA)3(H2O)3 (TFA = trifluoroacetate) (A) were investigated. Thermal treatment of A at different temperatures under vacuum (5 × 10−2 mm) for several hours failed to give totally anhydrous yttrium trifluoroacetate (as indicated by IR). Two different complexes, a partially dehydrated [Y(μ,η1:η1-TFA)3(THF)(H2O)]1∞·THF (1) and a partially hydrolyzed [Y4(μ3-OH)4(μ,η1:η1-TFA)6(η1-TFA)(η2-TFA)(THF)3(DMSO)(H2O)] · 6THF (2), were obtained with good and moderate yield, respectively, by crystallization of two different thermally treated batches of A from THF (or THF + DMSO) at room temperature. More efficient dehydration of A could be achieved at 200 °C in a furnace, the obtained anhydrous yttrium tris-trifluoroacetate giving Y(TFA)3(THF)2 (3) on crystallization from THF. All the products were characterized by elemental analyses, FT-IR and 1H NMR spectroscopy as well as thermo-gravimetric analysis. In addition, single crystal X-ray structures are reported for 1 and 2, which show either a terminal (η1 and η2) or bridging (μ,η1:η1) bonding behavior of the TFA ligand.

Graphical abstractThermal dehydration reactions of Y(TFA)3(H2O)3 (A) were investigated to obtain a better anhydrous precursor for various applications in materials science and catalysis. A partially dehydrated [Y(μ-TFA)3(THF)(H2O)] · THF (1), a partially hydrolyzed [Y4(μ3-OH)4(μ-TFA)6(TFA)2(THF)3(DMSO)(H2O)] · 6THF (2) and an anhydrous Y(TFA)3(THF)2 (3) were obtained under different thermal conditions and were characterized by elemental analyses, FT-IR and 1H NMR spectroscopy, as well as thermo-gravimetric analysis. In addition, single crystal X-ray structures are reported for 1 and 2.Figure optionsDownload full-size imageDownload as PowerPoint slide