In this paper, we place emphasis on the structure and luminescent properties of novel [Ln(isophth)(Hisophth)(H 2O) 4·4H 2O] n (Ln=Sm, Dy; H 2isophth=isophthalic acid) coordination polymers, which was characterized by elementary analysis, IR, UV, and especially the X-rays single-crystal diffraction. The two complexes are an isostructural series which crystallize in the monoclinic system with P2 1 / c space group. The samarium compound, isomorphous with dysprosium one were determined as a one-dimensional (1D) chain-like configuration by one of the two isophthalic acid ligands in bidentate chelated pattern, while the other isophthalic acid ligands only offer a single carboxylic acid group to bond which is abbreviated as ‘Hisophth’. Fluorescence excitation and emission spectra show that the isophthalic acid is suitable for the sensitization on the luminescence of both Sm(III) and Dy(III).