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Ruthenium nanoparticles inside porous Zn4O(bdC)(3) by hydrogenolysis of adsorbed Ru(cod)(cot): A solid-state reference system for surfactant-stabilized ruthenium colloids

Schroeder, F. and Esken, D. and Cokoja, M. and van den Berg, M. W. E. and Lebedev, O. I. and van Tendeloo, G. and Walaszek, B. and Buntkowsky, G. and Limbach, H. H. and Chaudret, B. and Fischer, R. A. (2008):
Ruthenium nanoparticles inside porous Zn4O(bdC)(3) by hydrogenolysis of adsorbed Ru(cod)(cot): A solid-state reference system for surfactant-stabilized ruthenium colloids.
130, In: Journal of the American Chemical Society, (19), pp. 6119-6130, [Online-Edition: http://apps.webofknowledge.com/full_record.do?product=WOS&se...],
[Article]

Abstract

The gas-phase loading of Zn4O(bdc)(3) (MOF-5; bdc = 1,4-benzenedicarboxylate) with the volatile compound Ru(cod)(cot) (cod = 1,5-cyclooctadiene, cot = 1,3,5-cyclooctatriene) was followed by solid-state C-13 magic angle spinning (MAS) NMR spectroscopy. Subsequent hydrogenolysis of the adsorbed complex inside the porous structure of MOF-5 at 3 bar and 150 degrees C was performed, yielding ruthenium nanoparticles in a typical size range of 1.5-1.7 nm, embedded in the intact MOF-5 matrix, as confirmed by transmission electron microscopy (TEM), selected area electron diffraction (SAED), powder X-ray diffraction (PXRD), and X-ray absorption spectroscopy (XAS). The adsorption of CO molecules on the obtained Ru@MOF-5 nanocomposite was followed by IR spectroscopy. Solid-state 2 H NMR measurements indicated that MOF-5 was a stabilizing support with only weak interactions with the embedded particles, as deduced from the surprisingly high mobility of the surface Ru-D species in comparison to surfactant-stabilized colloidal Ru nanoparticles of similar sizes. Surprisingly, hydrogenolysis of the Ru(cod)(cot)(3.5)@MOF-5 inclusion compound at the milder condition of 25 degrees C does not lead to the quantitative formation of Ru nanoparticles. Instead, formation of a ruthenium-cyclooctadiene complex with the arene moiety of the bdc linkers of the framework takes place, as revealed by 13C MAS NMR, PXRD, and TEM.

Item Type: Article
Erschienen: 2008
Creators: Schroeder, F. and Esken, D. and Cokoja, M. and van den Berg, M. W. E. and Lebedev, O. I. and van Tendeloo, G. and Walaszek, B. and Buntkowsky, G. and Limbach, H. H. and Chaudret, B. and Fischer, R. A.
Title: Ruthenium nanoparticles inside porous Zn4O(bdC)(3) by hydrogenolysis of adsorbed Ru(cod)(cot): A solid-state reference system for surfactant-stabilized ruthenium colloids
Language: English
Abstract:

The gas-phase loading of Zn4O(bdc)(3) (MOF-5; bdc = 1,4-benzenedicarboxylate) with the volatile compound Ru(cod)(cot) (cod = 1,5-cyclooctadiene, cot = 1,3,5-cyclooctatriene) was followed by solid-state C-13 magic angle spinning (MAS) NMR spectroscopy. Subsequent hydrogenolysis of the adsorbed complex inside the porous structure of MOF-5 at 3 bar and 150 degrees C was performed, yielding ruthenium nanoparticles in a typical size range of 1.5-1.7 nm, embedded in the intact MOF-5 matrix, as confirmed by transmission electron microscopy (TEM), selected area electron diffraction (SAED), powder X-ray diffraction (PXRD), and X-ray absorption spectroscopy (XAS). The adsorption of CO molecules on the obtained Ru@MOF-5 nanocomposite was followed by IR spectroscopy. Solid-state 2 H NMR measurements indicated that MOF-5 was a stabilizing support with only weak interactions with the embedded particles, as deduced from the surprisingly high mobility of the surface Ru-D species in comparison to surfactant-stabilized colloidal Ru nanoparticles of similar sizes. Surprisingly, hydrogenolysis of the Ru(cod)(cot)(3.5)@MOF-5 inclusion compound at the milder condition of 25 degrees C does not lead to the quantitative formation of Ru nanoparticles. Instead, formation of a ruthenium-cyclooctadiene complex with the arene moiety of the bdc linkers of the framework takes place, as revealed by 13C MAS NMR, PXRD, and TEM.

Journal or Publication Title: Journal of the American Chemical Society
Volume: 130
Number: 19
Uncontrolled Keywords: metal-organic framework nanoporous alumina membranes self-assembled monolayers coordination polymers structural-characterization catalytic-properties supported ruthenium molecular-dynamics ru catalysts giant pores
Divisions: 07 Department of Chemistry
07 Department of Chemistry > Physical Chemistry
Date Deposited: 27 Oct 2014 20:49
Official URL: http://apps.webofknowledge.com/full_record.do?product=WOS&se...
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297MG Times Cited:154 Cited References Count:80

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