One pot synthetic aluminosilicate and gallosilicate sodalites containing acetate guest anion have been synthesized successfully under hydrothermal conditions at 100 °C. This paper deals with the comparison of X-ray powder data with single crystal data for Na8[AlSiO4]6(CH3COO)2 and the characterization of a new Na8[GaSiO4]6(CH3COO)2 sodalite. The products obtained were characterized by IR, X-ray powder diffraction, MAS NMR, SEM and thermogravimetry technique. Crystal structures were refined in the space group \(P\bar 43n\) from X-ray powder data using the Rietveld refinement method with the unit cell parameter a = 9.0679 Å, for aluminosilicate and a = 9.2119 Å, for gallosilicate sodalite. The aluminosilicate and gallosilicate framework shows regular bonding with bond angles of Al-O-Si = 146.241°, Ga-O-Si = 141.294°. 29Si MAS NMR chemical shift values verify Al/Si and Ga/Si ordering of the framework constituents.