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In this paper, the synthesis of a novel polyoxovanadiumborate [Li(H2O)3]3 [V12 B18 O48 (OH)12 (OH)] · (H2 O)s by hydrotherrnal method.FTIR, 2D FTIR and UV-Vis absorption spectroscopy were em ployed to explore the relationships between structure and properties of 3-D compound 1.