The complex of [Tb(2-IBA) 3(H2O) 2]n(2-IBA=2-iodobenzoate) was prepared by solvent method from TbCl3·6H2O and 2-iodo-benzoic acid. The crystal structure was determined with X-ray single-crystal diffraction. The X-ray diffraction analysis indicated that the title complex crystallized in triclinic crystal system and Pī space group. The Tb3+ ion was coordinated by six oxygen atoms from five 2-IBA ligands and two oxygen atoms from two water molecules,giving a distorted square-antiprism polyhedral geometry. The carboxyl groups were bonded to the Tb3+ ions with bidentate-bridging and bidentate-chelating coordination modes. The adjacent Tb3+ ions were linked by two bidentate-bridging 2-IBA ligands,forming 1-D chain structure. The fluorescence spectrum of the complex showed four main peaks at 489,543,587,and 618 nm,corresponding to 5D4→7FJ(J=6-3) transition emissions of the Tb3+ ion,respectively. The complex of [Tb (2-IBA) 3 (H2O) 2] n (2-IBA = 2-iodobenzoate) was prepared by solvent method from TbCl3-6H2O and 2-iodo-benzoic acid The X-ray diffraction analysis indicated that the title complex crystallized in triclinic crystal system and P space group. The Tb3 + ion was coordinated by six oxygen atoms from five 2-IBA ligands and two oxygen atoms from two water molecules, giving a distorted square-antiprism polyhedral geometry. The carboxyl groups were bonded to the Tb3 + ions with bidentate-bridging and bidentate-chelating coordination modes. The adjacent Tb3 + ions were linked by two bidentate- bridging 2-IBA ligands, D chain structure. The fluorescence spectrum of the complex showed four main peaks at 489,543,587, and 618 nm, corresponding to 5D4 → 7FJ (J = 6-3) transition emissions of the Tb3 + ion, respectively.