2 O (2). They are characterized by single-crystal X-ray diffraction, FT-IR spectra, powder X-ray diffraction (PXRD), thermogravimetric analyses (TGA) and XPS spectra. All compounds represent 2D framework, but the structures possess some distinctions to a certain degree. In compound 1, 1D wave-like chains are formed. The chains and polyanions are stacked each other in an ABAB fashion to yield a 2D network. However, compared with compound 1, compound 2 exhibits the same construction except for the opposite arrangement mode. Moreover, their electrochemical behaviors and fluorescence properties have been investigated. The electrochemical properties show that compounds 1, 2 display good electrocatalytic activities for the reduction of nitrite.