OXYFLUORINATED MICROPOROUS COMPOUNDS .5. SYNTHESIS AND X-RAY STRUCTURAL DETERMINATION OF ULM-3, A NEW FLUORINATED GALLOPHOSPHATE GA3P3O12F2, H3N(CH2)3NH3, H2O

Ga3P3O12F2, H3N(CH2)3NH3, H2O was obtained by hydrothermal synthesis ( 453 K, 24 hr, autogeneous pressure) from a mixture of Ga2O3, P2O5, HF, 1,3-diaminopropane, and H2O in the ratio 1:1:2:1.3:80. It is orthorho mbic (space group Pbca (No. 61) with a = 10.154(1) angstrom, b = 18.39 3(2) angstrom, c = 15.773(2) angstrom, V = 2945.8(9) angstrom3, Z = 8. The three-dimensional network is built up from corner-linked [Ga3(PO4 )3F2] units composed of three PO4 tetrahedra, two GaO4F trigonal bipyr amids, and one GaO4F2 octahedron. Fluorine atoms are shared between th e octahedron and the bipyramid. The framework delimits 10-membered rin g channels along [100] and 8-membered ones along [101] and [10-1]. The amine and the water molecule are inserted in the 10-membered ring cha nnels. The hydrogen bonding scheme is discussed and shows that the wat er is principally linked to the amine within the tunnel and that the t emplate might be the amine monohydrate. The thermal behavior of the ti tle compound is studied by TGA and X-ray thermodiffractometry. (C) 199 4 Academic Press, Inc.