In this study, the Al 13 -oxalate gel synthesized from Al 13 solution was characterized by XRD, FTIR and MAS 27 Al NMR. The results are: 1) the gel shows obvious XRD diffraction peaks, which is different from common Al gels and their oxalate precipitations; 2) the peak of Al-O stretch vibration of Al 13 -oxalate complexes at 810 cm -1 indicates that the gel was formed directly by the complexes, and the characteristic peaks of IR and solid-state NMR respectively occur at 725 cm -1 and ~6.1×10 -5 chemical shift, which are respectively assigned to (Al-O) Td vibration and (Al-O) 4 tetrahedron, suggesting that the gel has a unique Keggin structure; 3) Al 13 polyoxocation can directly form gel with oxalate, even in a high-pH environment (=7.8). This finding provides new evidence for the universality of Al 13 in natural environments. Through chemical analysis, the chemical formula of the gel was determined to be AlO 4 Al 12 (OH) 24 (H 2 O) 12 (C 2 O 4 ) 7/2 .