The hydrothermal formation of sodium hydroxyborate enclathrated sodalite synthesized from an initial ternary mixture of mullite, cristobalite and corundum has been investigated. Depending on temperature and pressure the compound Na7.5[AlSiO4]6[B(OH)4]1.5 · 2H2O could be synthesized in form of polycrystalline powder as well as in form of single crystals. The kinetics of the sodalite growth could be determined at 423 K and 473 K. 29Si-and 27Al MAS NMR was shown to be the preferred method to describe the conversion into sodalite quantitatively. Evidence for the first formation of polycrystalline sodalite has been found after the total dissolution of mullite and cristobalite.
Single crystal X-ray diffraction data were used for the structure determination and refinement. The position and orientation of the hydroxyborate anions within the sodalite's /β-cages could only be found in the course of a "rigid body" refinement with constraints for the B(OH)4 tetrahedron. The boron atoms are located in an off-centre position within the sodalite cages. One out of the four oxygen atoms of the hydroxyborate group is positioned near the centre of a face of the sodium tetrahedron, whereas the three remaining oxygen atoms are near to the middle of its edges.
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