A 2D layered aluminophosphate Al 3P 4O 16· [NH 3CH 2 CH(OH)CH 3] 2· [NH 4] containing [NH 3CH 2CH(OH)CH 3]+ and [NH 4]+ cations has been synthesized using racemic isopropanolamine as the template from several different non aqueous solvents. The compound has been characterized by single crystal structure analysis. Its space group is P2 1/m with a=0.899 81(6) nm, b=1.478 80(10) nm, c= 0.973 72(7) nm, β=104.790(2)° and V=1.252 74(15) nm3. The structure consists of [Al 3P 4O 16] 3- macroanionic sheets stacked in an AAAA sequence and two types of cations, racemic [NH 3CH 2CH(OH)CH 3]+ and [NH 4]+, are located between the inorganic layers. The individual macroanionic sheet contains AlO 4 and PO 4 tetrahedral units in the ratio of 3/4 and all the AlO 4 vertices are shared, but each PO 4 has one terminal PO group. Additional characterization of the compound by XRD, FTIR, ICP and TGA is also described.