Three new lanthanide heterocyclic β-diketonate complexes [Dy(PPI) 3 (EtOH) 2 ] (1), [Dy(PPI) 3 (DPEPO)] (2), and [Tb(PPI) 3 (DPEPO)] (3) [where HPPI = 3-phenyl-4-p r o p a n o y l -5 -i s o x a z o l o n e a n d D P E P O = b i s ( 2 -(diphenylphosphino)phenyl)ether oxide] have been synthesized and fully characterized. Single-crystal X-ray diffraction analyses reveal that these complexes are mononuclear and that the central Ln III ion is coordinated to eight oxygen atoms that are provided by three bidentate β-diketonate ligands and ethanol or bidentate DPEPO in a distorted square antiprismatic geometry. These complexes have high molar absorption coefficients (up to 3 × 10 4 M −1 cm −1 at 285 nm) and display strong visible and, for Dy III , NIR luminescence upon irradiation at the ligand-centered band in the range 250−350 nm. The emission quantum yields and the luminescence lifetimes at room temperature are 3 ± 0.5% and 15 ± 1 μs for 1, 12 ± 2% and 33 ± 1 μs for 2, and 42 ± 6% and 795 ± 1 μs for 3. Moreover, the crystals of 2 and 3 exhibit brilliant triboluminescence, visible in daylight.

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