Beta-diketonates are common ligands for organometallic complexes. Since the 1960s, the potential materials applications of various beta-diketonates was explored. During that time, it was recognized that the beta-diketonate, 2-thenoyltrifluoroacetonate (TTA), is an excellent antenna ligand and can be used to enhance the luminescence properties of lanthanides. Although Ln(tta)3 hydrates are extensively used as starting materials for synthesizing Ln coordination complexes, there is surprisingly little on their characterization. In this study, we report the synthesis of Ln(tta)3(H2O)x (x = 2 or 3) (Ln= La-Lu except Pm) using both mechanochemistry and conventional solution synthesis. These compounds were characterized using FT-IR, 1H and 13C NMR, XRD, elemental analysis, DSC and melting points. FTIR was used to identify the trends in spectral changes over the series including the effect of humidity. 1H, 13C and 19F NMR were used to investigate the molecular identity and structure of the La+3 and Lu+3 (diamagnetic) species. Phase purity and chemical composition were determined using X-ray diffraction (XRD), while elemental analysis, melting points and differential scanning calorimeter (DSC) were used to assess the purity of the compounds. The effect of solvent and humidity on the synthesis, purification and yields of these compounds will be discussed in addition to noted trends along the series.

Ln(tta)3 hydrates: Synthesis, characterization and reactivity

ACS Spring 2022

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