“…The K-Al 13 solution has the chemical shift of 63 ppm for the tetrahedral AlO 4 -site, and the Al 30 solution has two unique chemical shifts at about 72 ppm and 11 ppm, consistent with the results by Allouche et al 10 and Fu et al 20 K-GaAl 12 was confirmed by 71 Ga NMR with the chemical shift of around 139 ppm, while the K-GeAl 12 solution only shows a small 27 Al NMR peak from the monomeric aluminium, which are in accordance with the results by Stewart et al 1 K-GeAl 12 was confirmed by inductively coupled plasma atomic emission spectroscopy. 16 College of Chemistry and Life Science, Zhejiang Normal University, Jinhua 321004, China. E-mail: qianzhaosheng@zjnu.cn, fenghui@zjnu.cn; Fax: +86-579-82282269; Tel: +86-579-82282269 w Electronic supplementary information (ESI) available: The 27 Al NMR, 71 The luminescence of these aluminium polyoxocations was recorded in the mode of fluorescence.…”