Two new gallium phosphonates Ga(OH)(O3PC2H4CO2H) . H2O 1 and Ga-3(OH)(3)(O3PC2H4CO2)(2) . 2H(2)O 2 are prepared and characterized, using P-31 MAS and Ga-71 static NMR spectroscopy, showing a good correspondence between the fitted NMR parameters and the crystallographic data.