A layered aluminofluorophosphate and a cobalt–aluminophosphate material have been prepared using the azamacrocycle meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (Tet-A) as a structure-directing agent (SDA). Both were synthesised using hydrothermal techniques and their structures solved using microcrystal X-ray diffraction. The first material, [F, Tet-A]-AlPO-1, has the molecular formula Al10P10O40F2C16N4H38 and crystallises in the orthorhombic space group Pca21. Its inorganic layered structure is related to the AlPO-41 (AFO) zeolite structure type. The second material, [Co, Tet-A]-AlPO-2, has the formula Al4(PO4)4(HPO4)2·[Co(C16N4H36)]·C16N4H38·2H2O
and crystallises in the triclinic space group P
. This material contains a cobalt–Tet-A complex that is covalently bound to the inorganic framework and an uncoordinated Tet-A molecule that is hydrogen bonded to the framework.
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