| Abstract
| - Two fluorinated gallium phosphates, Ga4(PO4)4F1.33(OH)0.67·1.5NC5H12·0.5H3O·0.5H2O(ULM-16) and Ga9(PO4)8F7.3(OH)0.2·4NC5H12·0.5H3O·3.5H2O (MIL-46), have been hydrothermally synthesized by varying the fluorine amount in the presence of cyclopentylamineas structure-directing agent (at 180 °C for 3 days). Their structures were determined bymeans of single-crystal X-ray diffraction. The first compound (obtained with low fluorineconcentration) is isostructural to the gallium phosphate ULM-16 previously prepared withcyclohexylamine. Its three-dimensional framework is built up from the connection by cornersharing of the hexameric units Ga3(PO4)3F2 together with the tetramer Ga2(PO4)2 and consistsof channels bound by 16 polyhedra inserting the protonated cyclopentylamine. The secondphase (prepared with high fluorine concentration) exhibits a new three-dimensional topologybased on the condensation by corner sharing of the identical hexameric building block Ga3(PO4)3F2 with a pentameric species Ga3(PO4)2F4. The resulting network is composed of large18-ring channels hosting the protonated cyclopentylamine and water molecules. Crystal dataare as follows: Ga4(PO4)4F1.33(OH)0.67·1.5NC5H12·0.5H3O·0.5H2O (ULM-16), orthorhombic,Pbcn (no. 60), a = 27.316(5) Å, b = 17.472(3) Å, c = 10.1970(14) Å, V = 4866.7(14) Å3 andZ = 8; Ga9(PO4)8F7.3(OH)0.2·4NC5H12·0.5H3O·3.5H2O (MIL-46), orthorhombic, Pnnm (no. 58),a = 10.2735(2) Å, b = 18.5962(3) Å, c = 29.6279(2) Å, V = 5660.4(2) Å3, Z = 4.
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