High-field pulsed EPR spectroscopy for the speciation of the reduced [PV(2)Mo(10)O(40)](6-) polyoxometalate catalyst used in electron-transfer oxidations

Chemistry : a European Journal
Ilia KaminkerD Goldfarb

Abstract

An in-depth spectroscopic EPR investigation of a key intermediate, formally notated as [PV(IV)V(V)Mo(10)O(40)](6-) and formed in known electron-transfer and electron-transfer/oxygen-transfer reactions catalyzed by H(5)PV(2)Mo(10)O(40), has been carried out. Pulsed EPR spectroscopy have been utilized: specifically, W-band electron-electron double resonance (ELDOR)-detected NMR and two-dimensional (2D) hyperfine sub-level correlation (HYSCORE) measurements, which resolved (95)Mo and (17)O hyperfine interactions, and electron-nuclear double resonance (ENDOR), which gave the weak (51)V and (31)P interactions. In this way, two paramagnetic species related to [PV(IV)V(V)Mo(10)O(40)](6-) were identified. The first species (30-35 %) has a vanadyl (VO(2+))-like EPR spectrum and is not situated within the polyoxometalate cluster. Here the VO(2+) was suggested to be supported on the Keggin cluster and can be represented as an ion pair, [PV(V)Mo(10)O(39)](8-)[V(IV)O(2+)]. This species originates from the parent H(5)PV(2)Mo(10)O(40) in which the vanadium atoms are nearest neighbors and it is suggested that this isomer is more likely to be reactive in electron-transfer/oxygen-transfer reaction oxidation reactions. In the second (70-65 %) spe...Continue Reading

References

Jul 2, 1999·Journal of Magnetic Resonance·I GromovD Goldfarb
Sep 29, 2005·Journal of Magnetic Resonance·Stefan Stoll, Arthur Schweiger
Jun 17, 2006·Chemical Communications : Chem Comm·Ronny Neumann, Alexander M Khenkin
Jul 13, 2006·The Journal of Physical Chemistry. a·Debbie Baute, Daniella Goldfarb
Jun 24, 2008·Journal of Magnetic Resonance·Daniella GoldfarbIlia Kaminker

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Citations

Oct 15, 2013·Journal of Magnetic Resonance·F Mentink-VigierD Goldfarb
Mar 22, 2012·Inorganic Chemistry·Alexey PotapovDaniella Goldfarb
Jul 31, 2010·Journal of the American Chemical Society·Alexander M KhenkinRonny Neumann
Mar 2, 2018·Physical Chemistry Chemical Physics : PCCP·Alexander M KhenkinRonny Neumann
Jan 10, 2018·Chemistry : a European Journal·Harikleia SartziHaralampos N Miras
Aug 1, 2021·Nature Communications·Paolo Cleto BruzzeseMario Chiesa
Dec 10, 2013·Journal of the American Chemical Society·Alexander M KhenkinRonny Neumann
May 17, 2017·Inorganic Chemistry·Marie Ramirez CohenDaniella Goldfarb
Dec 2, 2017·Chemical Reviews·Ira A WeinstockRonny Neumann
Apr 22, 2011·The Journal of Physical Chemistry. a·Irena Efremenko, Ronny Neumann

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