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We have investigated the thermal and photochemical characteristics of silver 4-nitrobenzoate (Ag-4NBA) using various analytical tools, such as, X-ray diffraction (XRD), diffuse reflectance infrared Fourier transform spectroscopy, Raman spectroscopy, thermogravimetric analysis, scanning electron microscopy, and transmission electron microscopy. The XRD pattern was composed of a series of peaks that could be indexed to (0k0) reflections of a layered structure. Upon heating the sample, structural changes took place particularly at two specific temperatures. The binding state of the carboxylate group changed from bridging to unidentate at ∼380 K. A second dramatic structural change occurred at ∼590 K, producing 4NBA-capped Ag nanoparticles. The latter transition temperature for Ag-4NBA is about 80 K higher than that for silver alkanecarboxylates, and such enhanced thermal stability of Ag-4NBA must be associated with the conjugation of the carboxylate group to the aromatic ring. On the other hand, Ag-4NBA was ...