Gallosilicate hydroxy sodalite, Na8[GaSiO4]6(OH)2 was synthesized at low temperature by hydrothermal method (373 K) and further the sodium ions were partially exchanged with silver and cesium. The obtained products were characterized by IR spectroscopy, X-ray powder diffraction, MAS NMR, TGA and SEM. Parent hydroxy sodalite and its silver and cesium derivatives show cubic symmetry with a space group \(P\bar 4\) 3n. The crystal structures were refined by Rietveld method. The unit cell parameter, a = 8.8527 A for parent hydroxy sodalite, 8.8342 A for the silver derivative and 8.9367 A for cesium one. The 29Si MAS NMR of parent hydroxy sodalite confirms the alternating Ga and Si ordering in sodalite framework, while 23Na MAS NMR shows the effect of cation substitution. The SEM pictures are very regular and show sharp growth for parent sodalite, while the crystal morphology remains nearly same for the silver and cesium derivatives.