HIGH-RESOLUTION SOLID-STATE P-31 AND SN-119 MAGIC-ANGLE SPINNING NUCLEAR-MAGNETIC-RESONANCE STUDIES OF AMORPHOUS AND MICROCRYSTALLINE LAYERED METAL(IV) HYDROGENPHOSPHATES

High-resolution solid-state P-31 and Sn-119 magic-angle spinning nuclear magnetic resonance (MAS NMR) and Mossbauer spectroscopies have been used to probe the structure of amorphous and microcrystalline layered hydrogenphosphates and some of their intercalation compounds. A linear relationship between delta(P-31) and the Allred-Rochow electronegativity of the metal atom was observed. In the case of both alpha and gamma forms of titanium and zirconium hydrogenphosphates, a linear relationship was seen between the isotropic chemical shift (delta-iso) and the number of bridging P-O-M oxygens (connectivity) of the phosphate groups. In a further study of the intercalation compounds of tin(IV) hydrogenphosphate monohydrate (SnP), the NMR data indicated there to be more electron transfer in the propylamine intercalation compound than is the case with E-N,N'-diethylbut-2-ene-1,4-diamine (NNBD) and that there is more electron transfer in the case of NNBD than in the ammonium intercalation compound. A linear relationship was observed when delta(Sn-119) was plotted as a function of delta(P-31). The Sn Mossbauer spectrum of the host material was indicative of ionic character around the metal atom and similar to that of SnF4.