Bruno Boury, Robert J. P. Corriu, Valérie Le Strat and Rosario Nuñez
The crystalline sodium salt of p-phenylenebis(silanetriolate), (NaO)3SiC6H4Si(ONa)3·14H2O has been prepared in quantitative yield by reaction of the corresponding alkoxysilane with NaOH. Characterization of its structure indicates two different environments for the silicon atoms (X-ray and 13C, 29Si, 1H NMR) in the solid state. Drying of the salt by thermal treatment between 20 and 180 °C (TG analysis) led to a modification of the structure without loss of the organic group. Elimination of C6H6 occurs above 200 °C and formation of the sodium silicate Na2SiO3 can be identified above 400 °C (X-ray diffraction). Quantitative replacement of the sodium cation with Al3+, Zn2+, Ca2+ and Eu3+ has been achieved resulting in the formation of the corresponding silanetriolates (EDX and elemental analyses). X-Ray diffraction analysis suggests the presence of a lamellar structure on very small domains or a short range order.