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1D and 2D solid state NMR investigations of the framework structure of As-synthesized AlPO4-14

✍ Scribed by C.A. Fyfe; H.Meyer zu Altenschildesche; K.C. Wong-Moon; H. Grondey; J.M. Chezeau

Publisher
Elsevier Science
Year
1997
Tongue
English
Weight
844 KB
Volume
9
Category
Article
ISSN
0926-2040

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✦ Synopsis

The framework structure of As-synthesized AlPO,-14 has been investigated with a combination of different one-dimensional *'Al and 31P solid state NMR techniques and *'Al/ 3'P double resonance methods. The results are found to be fully consistent with the assumed structural model. *'Al MAS and DOR experiments at three different magnetic field strengths together with simulations show the presence of two tetrahedral sites, one pentacoordinated and one octahedral aluminum site. The *'Al quadrupolar coupling constants and the 31P isotropic chemical shifts of the tetrahedral sites correlate well with tetrahedral shear-strain parameters and mean P-O-Al bond angles, respectively. These correlations allow one to assign all of the NMR resonances to specific T-sites in the proposed framework structure. The assignments are then further confirmed by the application of three different two-dimensional heteronuclear correlation methods (i.e., 27A1 + 3'P TEDOR, CP, and INEPT) which reveal the connectivities between AlO, and PO, polyhedra. The two-dimensional INEPT experiment is applied here for the first time in the solid state.

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