Synthesis and Characterization of a New Three-Dimensional Lanthanide Carboxyphosphonate: Ln<sub>4</sub>(H<sub>2</sub>O)<sub>7</sub>[O<sub>2</sub>C−C<sub>5</sub>H<sub>10</sub>N−CH<sub>2</sub><sub>-</sub>PO<sub>3</sub>]<sub>4</sub>(H<sub>2</sub>O)<sub>5</sub>
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The first open-framework lanthanide carboxyphosphonate has been obtained under hydrothermal conditions. The three-dimensional structure of MIL-84(Pr) (MIL = Material Institut Lavoisier) or Pr4(H2O)7[O2C−C5H10N−CH2-PO3]4(H2O)5 has been solved from X-ray diffraction single-crystal data (a = 23.481(1) Å, b = 10.159(1) Å, c = 23.006(1) Å, β = 105.63(1)°, V = 5284.6(6) Å3, space group Cc (No. 9)). Its framework is built up from chains of edged-sharing eight or nine-coordinated monocapped square antiprism polyhedra and carboxyphosphonate anions, creating a three-dimensional structure with small pores filled with water molecules. The thermal behavior of MIL-84(Pr) has been investigated using TGA and X-ray thermodiffractometry and indicates that MIL-84(Pr) is stable up to 523 K with a reversible hydration−dehydration process. The optical study of its yttrium analogue doped at 3.4% with europium (MIL-84(Y,Eu)) reveals a significant red-orange emission under UV radiation.
