Synthesis and structure of Mu-4, the new layered aluminophosphate [(C2H5)(2)NH2](4)[Al8P10O40H2]center dot[H2O](2.5)

The title compound (named Mu-4) is a new layered aluminophosphate with a un usual Al/P ratio for this kind of materials. Mu-4 was obtained from a quasi nonaqueous mixture involving mainly diethylformamide (DEF) as solvent, in addition to limited amounts of water. DEF is decomposed during the synthesi s and the resulting protonated diethylamine is occluded in the as-synthesiz ed material. The crystal structure was determined by single crystal X-ray d iffraction. The symmetry is triclinic, a=8.632(4) Angstrom, b=9.267(7) Angs trom, c= 17.461(10) Angstrom, alpha=86.66(5)degrees, beta=82.20(4)degrees a nd gamma=89.28(5)degrees, space group P-l. The structure consists of anioni c double sheets essentially built from double 4-ring (D4R) units, The inorg anic layers are in strong interaction with wafer and the protonated amine w hich is located in the interlayer spacing. Another type of diethylamine pro trudes into the 8-membered rings (8-MR) present in the layers. The characte rization of this new aluminophosphate by C-13, Al-27 and P-31 solid State N MR spectroscopy is also reported.