Volker Gramlich

Synthesis and characterization of Mu-19, a new zincophosphate with a three-dimensional 12-membered ring channel system

Abstract A new three-dimensional open-framework zincophosphate [C 5 H 12 NO][ZnP 2 O 5 (OH) 3 ]·H 2 O, named Mu-19, was synthesized at room temperature from a ZnO/P 2 O 5 / N -methylmorpholine/H 2 O system. The crystal structure was determined by single crystal X-ray diffraction. The zincophosphate crystallizes in the orthorhombic space group P2 1 2 1 2 1 (no. 19) with a =9.976(4), b =10.359(6), c =12.980(10) A, V =1341.4(14) A 3 and Z =4. The structure consists of ZnO 4 , PO 2 O(OH) and PO 2 (OH) 2 tetrahedra linked to form an open structure with a three-dimensional channel system delimited by 12-membered ring openings. The organic structure-directing amine is hydrogen bonding to the inorganic framework via water molecules. The zincophosphate Mu-19 is further characterized by 13 C CP MAS/ 31 P MAS NMR with high power decoupling and 1 H CRAMPS NMR spectroscopy, SEM and thermal analyses.