title: The dehydration of SrTeO3(H2O)--a topotactic reaction for preparation of the new metastable strontium oxotellurate(IV) phase ε-SrTeO3.
abstract: Microcrystalline single-phase strontium oxotellurate(IV) monohydrate, SrTeO(3)(H(2)O), was obtained by microwave-assisted hydrothermal synthesis under alkaline conditions at 180 °C for 30 min. A temperature of 220 °C and longer reaction times led to single crystal growth of this material. The crystal structure of SrTeO(3)(H(2)O) was determined from single crystal X-ray diffraction data: P2(1)/c, Z = 4, a = 7.7669(5), b = 7.1739(4), c = 8.3311(5) Å, β = 107.210(1)°, V = 443.42(5) Å(3), 1403 structure factors, 63 parameters, R[F(2)>2σ(F(2))] = 0.0208, wR(F(2) all) = 0.0516, S = 1.031. SrTeO(3)(H(2)O) is isotypic with the homologous BaTeO(3)(H(2)O) and is characterised by a layered assembly parallel to (100) of edge-sharing [SrO(6)(H(2)O)] polyhedra capped on each side of the layer by trigonal-prismatic [TeO(3)] units. The cohesion of the structure is accomplished by moderate O-H···O hydrogen bonding interactions between donor water molecules and acceptor O atoms of adjacent layers. In a topochemical reaction, SrTeO(3)(H(2)O) condensates above 150 °C to the metastable phase ε-SrTeO(3) and transforms upon further heating to δ-SrTeO(3). The crystal structure of ε-SrTeO(3), the fifth known polymorph of this composition, was determined from combined electron microscopy and laboratory X-ray powder diffraction studies: P2(1)/c, Z = 4, a = 6.7759(1), b = 7.2188(1), c = 8.6773(2) Å, β = 126.4980(7)°, V = 341.20(18) Å(3), R(Fobs) = 0.0166, R(Bobs) = 0.0318, Rwp = 0.0733, Goof = 1.38. The structure of ε-SrTeO(3) shows the same basic set-up as SrTeO(3)(H(2)O), but the layered arrangement of the hydrous phase transforms into a framework structure after elimination of water. The structural studies of SrTeO(3)(H(2)O) and ε-SrTeO(3) are complemented by thermal analysis and vibrational spectroscopic measurements.
authors.affiliation: Institute for Chemical Technologies and Analytics, Division of Structural Chemistry, Vienna University of Technology, Getreidemarkt 9/164-SC, A-1060, Vienna, Austria.
authors.forename: Berthold
authors.initials: B
authors.lastname: Stöger
authors.forename: Matthias
authors.initials: M
authors.lastname: Weil
authors.forename: Enrique J
authors.initials: EJ
authors.lastname: Baran
authors.forename: Ana C
authors.initials: AC
authors.lastname: González-Baró
authors.forename: Sylvie
authors.initials: S
authors.lastname: Malo
authors.forename: Jean Michel
authors.initials: JM
authors.lastname: Rueff
authors.forename: Sebastien
authors.initials: S
authors.lastname: Petit
authors.forename: Marie Bernadette
authors.initials: MB
authors.lastname: Lepetit
authors.forename: Bernard
authors.initials: B
authors.lastname: Raveau
authors.forename: Nicolas
authors.initials: N
authors.lastname: Barrier