NDLI: 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

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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

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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

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Neumann, Ronny Kaminker, Ilia Goldberg, Hila Goldfarb, Daniella
Description	Author Affiliation: Kaminker I ( Department of Chemical Physics, Weizmann Institute of Science, Rehovot, 76100 Israel.)
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 %) species, the $V^{IV}$ remains embedded within the polyoxometalate framework and originates from reduction of distal $H_{5}PV_{2}Mo_{10}O_{40}$ isomers to yield an intact cluster, $[PV^{IV}V^{V}Mo_{10}O_{40}]^{6−}.$
ISSN	09476539
e-ISSN	15213765
Journal	Chemistry - A European Journal
Issue Number	33
Volume Number	16
Language	English
Publisher	Wiley-VCH;ChemPubSoc Europe
Publisher Date	2010-09-03
Publisher Place	Germany
Access Restriction	Open
Subject Keyword	Electron Spin Resonance Spectroscopy Oxygen Chemistry Tungsten Compounds Catalysis Electron Transport Magnetic Resonance Spectroscopy Oxidation-Reduction Research Support, Non-U.S. Gov't Research Support, U.S. Gov't, Non-P.H.S.
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Catalysis

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