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The complexation of Ln(Ⅲ)/An(Ⅲ)with N,N,N',N'-tetraalkyl-diglycolamide were investigated with UV-Vis absorption,fluorescence spectroscopy,and crystallography.By building the relevance of structures tooptical spectra,the structure and composition of the extracted complexes of Ln(Ⅲ)/An(Ⅲ)with TRDGA in solvent extraction was illustrated.The similarity of the spectra of the extracted complexes in various organic solvents indicated that the polarity of the diluents does not have significant influence on the formation of the extracted complexes.