A. Matijasic et al., Structural characterization of the new porous sodium silicate Mu-11 by Si-29 and Na-23 solid-state NMR, PHYS CHEM P, 2(12), 2000, pp. 2807-2813
A variety of solid-state NMR techniques were applied in order to assign res
onances in the Si-29 and Na-23 NMR spectra of a new crystalline silicate to
crystallographically distinct silicon and sodium sites, respectively. Mu-1
1 is a zeolite-like material with a 1D channel system occupied by water and
sodium cations whose framework contains both bridging and non-bridging oxy
gens. The observed Si-29 isotropic chemical shifts did not allow a direct a
ssignment. A preliminary assignment based on the electronegativities calcul
ated for the four ligands around each silicon was supported by correlations
between the extent of the distortion from an ideal tetrahedron and the mea
sured chemical shift anisotropy for the different Si sites. H-1-Si-29 cross
polarization experiments confirmed the assignments. The two crystallograph
ically different sodium atoms were resolved by Na-23 3Q-MAS NMR, and an ass
ignment for these two sites is proposed.