The first two examples of layered aluminophosphates with molar ratio P:Al=1 have been synthesized hydrothermally, and their structures have been solved from X-ray powder diffraction data. UiO-13 with composition [NH 3 (CH 2 ) 2 NH 3 ] 2 + [Al 2 P 2 O 9 ] 2 - crystallizes in the orthorhombic space group Pbca with a=9.33138(11) 9, b=9.66045(11) 9 and c=21.82869(31) 9. UiO-14 with composition [NH 3 (CH 2 ) 3 NH 3 ] 2 + [Al 2 P 2 O 9 ] 2 - crystallizes in the monoclinic space group P2 1 /c with a=11.65064(15) 9, b=9.27936(11) 9, c=9.69643(11) 9 and β=103.1378(9) o . In both compounds the atomic arrangement of the anionic aluminophosphate layers is identical to a building unit of the open framework aluminophosphate AlPO 4 -12. The two compounds differ in the stacking sequence of these layers. UiO-13 has an AB stacking sequence, whereas in UiO-14 an AA stacking sequence is present. The compounds contain solely five-coordinated aluminium. Both compounds transform into an amorphous material above 300 o C.