Al-27/P-31 solid-state n.m.r. connectivity experiments were used to in
vestigate the structure of the molecular sieve AlPO4-5 hydrated with D
2O. Hydration with D2O resulted in an increased efficiency of coherenc
e transfer from octahedral Al-27 to P-31 compared with hydration with
H2O. The experiments prove directly that both the tetrahedral aluminum
and the octahedral aluminum formed upon hydration are connected to ph
osphorus in the framework. The two-dimensional Al-27 --> P-31 transfer
red-echo double-resonance and cross-polarization experiments show a do
wnfield offset of the octahedral Al-27 correlation from the tetrahedra
l Al-27 correlation, consistent with the growth of a downfield shoulde
r on the P-31 resonance as water is incorporated into the lattice.