A set of two-dimensional solid-state NMR experiments providing topologicalinformation for structure refinement of TMP-GaPO

A procedure for structural characterization based on X-ray diffraction (XRD ) and on a set of two-dimensional solid-state NMR experiments is proposed. It has been applied to a new gallophosphate oxyfluorinated compound, T(T = amine)-GaPO [Ga-4(PO4)(3) (HPO4)F-3.T]. To complement and validate structur al information obtained by XRD, a set of three solid-state NMR experiments- RFDR for fluorine-19, double quanta for phosphorus-31 and HETCOR between fl uorine and phosphorus-facilitate the analysis of the topology of homoatomic and heteroatomic sub-networks of fluorine and phosphorus included in the i norganic framework of this material. The efficiency of this combination of NMR experiments in assigning all NMR signals to their crystallographically sites is also demonstrated. Copyright (C) 1999 John Wiley & Sons, Ltd.