Synthesis and structure of perrhenate sodalite

• Published in: Microporous and mesoporous materials 2006-04, Vol.91 (1), p.139-144
• Main Authors: Mattigod, Shas V., Peter McGrail, B., McCready, David E., Wang, Li-Quong, Parker, Kent E., Young, James S.
• Format: Article
• Language: English
• Subjects: 29Si and 27Al MAS NMR; Chemistry; Colloidal state and disperse state; Exact sciences and technology; General and physical chemistry; Hydrothermal synthesis; Perrhenate sodalite; Porous materials; Raman spectra; Rietveld refinement
• ISSN: 1387-1811; 1873-3093
• DOI: 10.1016/j.micromeso.2005.11.025

Na 8(AlSiO 4) 6(ReO 4) 2 sodalite was synthesized using a hydrothermal method and its crystal structure was determined from Rietveld refinement of experimental X-ray powder diffraction data. The refinement showed that this compound adopts the cubic sodalite structure (space group P 4 ¯ 3 n , #218) with a = 9.1528 (1) Å. Raman spectroscopic measurements confirm the presence of tetrahedral ReO 4 - groups. Broadening of the asymmetric stretching and bending vibrational modes suggests the tetrahedra are slightly distorted from ideal T d symmetry in the sodalite lattice. MAS NMR of 29Si and 27Al nuclei showed single intense peaks at δ iso = −92.4 ppm and δ iso = 57.5 ppm, respectively, confirming the alternating Si, Al tetrahedral ordering in sodalite deduced from the structural data. Chemical shifts for 29Si and 27Al calculated using correlative structural parameters (56.6 ± 0.8 ppm and −92.3 ± 0.9 ppm) showed good agreement with measured data indicating the validity of data derived from the Rietveld structural refinement.