The reaction of 2-acetyl-2'-chloroacetanilide (L) with rare earth nitrates in CH3CH2OH followed by recrystallization in CH3CH2OH gave rise to colorless block crystals materials. The complexes and ligand were analyzed by FAB, elemental analysis(C, H, N), FT-IR spectra, TG-DTA, molar conductivity and X-ray single crystal diffraction. The fluorescence properties of ligand and the Eu (Ⅲ) complex also have been investigated. The results of crystal structure and spectral data show that the rare earth ions coordinated with oxygen and nitrogen atoms of the ligand, the nitrate and coordinated water molecules. The Eu (Ⅲ) complex material shows characteristic red emissions.