Synthesis of heterobimetallic tungsten acetylacetonate/alkoxide complexes and their application as molecular precursors to metal tungstates

H. Choujaa, A.L. Johnson, Gabriele Kociok-Kohn, K.C. Molloy

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3 Citations (Scopus)

Abstract

A series of MW2(O)2(acac)2 (OMe)10 [M = Co (1), Ni (2), Mg (3), Zn (4)] have been synthesised and structurally characterised by X-ray crystallography. All the compounds share common structural features which are identical to the analogous molybdenum species, with four edge-sharing octahedra situated in the same plane, and incorporating two μ3-bridging and four μ2- bridging methoxide groups. The divalent metal M and tungsten have both octahedral coordination environments with six oxygen atoms. The structure of Na[Zn(acac)3] (6), a by-product of a failed synthesis of 4, is also reported, and is a linear polymer in which [Zn(acac)3] anions use all six oxygen atoms to link sodium cations either side of the anion.

Thermal decomposition of representative samples (1, 3) shows them to be single-source precursors for metal tungstates MWO4. When the decomposition is carried out under an autogenerated pressure (RAPET) at 700 °C 1 forms CoWO4 nanoparticles, along with WOx-filled carbon nanotubes and amorphous carbon, while 3 forms MgWO4 nanoparticles and rods, though the latter lack a carbon shell and are much shorter in length.

LanguageEnglish
Pages85-90
Number of pages6
JournalPolyhedron
Volume59
DOIs
StatusPublished - 1 Aug 2013

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Tungsten
tungstates
alkoxides
Anions
oxygen atoms
tungsten
Negative ions
Metals
Oxygen
Nanoparticles
anions
Atoms
nanoparticles
Carbon Nanotubes
Molybdenum
carbon
X ray crystallography
Amorphous carbon
synthesis
metals

Cite this

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title = "Synthesis of heterobimetallic tungsten acetylacetonate/alkoxide complexes and their application as molecular precursors to metal tungstates",
abstract = "A series of MW2(O)2(acac)2 (OMe)10 [M = Co (1), Ni (2), Mg (3), Zn (4)] have been synthesised and structurally characterised by X-ray crystallography. All the compounds share common structural features which are identical to the analogous molybdenum species, with four edge-sharing octahedra situated in the same plane, and incorporating two μ3-bridging and four μ2- bridging methoxide groups. The divalent metal M and tungsten have both octahedral coordination environments with six oxygen atoms. The structure of Na[Zn(acac)3] (6), a by-product of a failed synthesis of 4, is also reported, and is a linear polymer in which [Zn(acac)3]− anions use all six oxygen atoms to link sodium cations either side of the anion. Thermal decomposition of representative samples (1, 3) shows them to be single-source precursors for metal tungstates MWO4. When the decomposition is carried out under an autogenerated pressure (RAPET) at 700 °C 1 forms CoWO4 nanoparticles, along with WOx-filled carbon nanotubes and amorphous carbon, while 3 forms MgWO4 nanoparticles and rods, though the latter lack a carbon shell and are much shorter in length.",
author = "H. Choujaa and A.L. Johnson and Gabriele Kociok-Kohn and K.C. Molloy",
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AU - Johnson, A.L.

AU - Kociok-Kohn, Gabriele

AU - Molloy, K.C.

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AB - A series of MW2(O)2(acac)2 (OMe)10 [M = Co (1), Ni (2), Mg (3), Zn (4)] have been synthesised and structurally characterised by X-ray crystallography. All the compounds share common structural features which are identical to the analogous molybdenum species, with four edge-sharing octahedra situated in the same plane, and incorporating two μ3-bridging and four μ2- bridging methoxide groups. The divalent metal M and tungsten have both octahedral coordination environments with six oxygen atoms. The structure of Na[Zn(acac)3] (6), a by-product of a failed synthesis of 4, is also reported, and is a linear polymer in which [Zn(acac)3]− anions use all six oxygen atoms to link sodium cations either side of the anion. Thermal decomposition of representative samples (1, 3) shows them to be single-source precursors for metal tungstates MWO4. When the decomposition is carried out under an autogenerated pressure (RAPET) at 700 °C 1 forms CoWO4 nanoparticles, along with WOx-filled carbon nanotubes and amorphous carbon, while 3 forms MgWO4 nanoparticles and rods, though the latter lack a carbon shell and are much shorter in length.

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