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A new one-dimensional(1D) fluoroaluminophosphate chain(C4H15N3)[AlPO4F2](denoted AlPO-CJ28) was synthesized in the concentrated fluoride synthetic medium with a gel composition of 1.0Al(OPri)3:1.0H3PO4: 5.4DETA:1.3HF:2.0H2O(DETA=diethylenetriamine). The reagents were mixed directly without introducing additional water solvent. The 1D chain is constructed by alternating AlO2F2 and doubly bridging PO4 tetrahedra to form the simplest serrate chain. AlPO-CJ28 can be transformed to another 1D aluminophosphate chain AlPO-CSC upon further crystallization at 230 °C.