The synthesis and characterization of two novel aluminophosphate mater
ials, obtained from the same nonaqueous tetraethylene glycol-cyclopent
ylamine system, is reported. The first material, [Al3P5O20H](5-). 5[C5
H9NH3+], denoted UT-2, has a 1-D chain structure with a P:Al ratio of
5:3, rather than 1:1 as found in the aluminophosphate AlPO4-n molecula
r sieves. The UT-2 chains are hydrogen-bonded together by terminal pho
sphate groups and organized into a layered structure. The second mater
ial, [Al2P3O12H](2-). 2[C5H9NH3+], denoted UT-3, has a 2-D layer struc
ture with a P:Al ratio of 3:2. Both materials have bilayers of charge-
balancing cyclopentylammonium cations interdisposed between anionic al
uminophosphate sheets. Variable-temperature in situ PXRD establishes a
clean solid-state structural transformation, at 200 degrees C, of UT-
2 to UT-3. The discovery of this chain-to-layer conversion suggests a
new paradigm for the templated assembly of 1-D chain, 2-D layer, and 3
-D open-framework aluminophosphates.