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Layered compound zirconium bis(monohydrogenphosphate)(α -ZrP) intercalated with rare earth complex Eu(DBM)3phen was prepared. The pre-intercalation of p-methoxyaniline into α -ZrP makes the interlayer separation large enough to exchange PMA with europium complex, thus, the luminescent assembly was prepared. This was confirmed by X-ray diffraction, UV-visible spectra and elemental analysis. The fluorescence spectra and lifetime of the assembly were also presented.