Eleven new lanthanide oxalatophosphonate hybrids with a 2D layered structures, namely, [Ln(H3L)(C2O4)]·2H2O (Ln = La–Dy, Er and Y, H4L = C6H5CH2N(CH2PO3H2)2), have been synthesized under hydrothermal conditions and structurally characterized by X-ray single-crystal diffraction, X-ray powder diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. Compounds 1–11 are isomorphous and they exhibit a 2D framework structure. Two {LnO8} polyhedra and four {CPO3} tetrahedra are interconnected into a unit via corner-sharing, and the so-built units are bridged by the oxalate anions into a layer. The result of connections in this manner is the formation of a 24-atom window. The thermal stabilities and guest desorption–sorption properties of compounds 1–11 have been investigated. The luminescent properties of compounds 5, 6, 8 and 9 have also been studied.
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