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The polyoxometalates studied were [PW<jats:sub>12<\/jats:sub>O<jats:sub>40<\/jats:sub>]<jats:sup>3\u2013<\/jats:sup> (the parent Keggin anion), [PW<jats:sub>11<\/jats:sub>O<jats:sub>39<\/jats:sub>]<jats:sup>7\u2013<\/jats:sup> (a lacunary anion), [PW<jats:sub>11<\/jats:sub>M(H<jats:sub>2<\/jats:sub>O)O<jats:sub>39<\/jats:sub>]<jats:sup>4\u2013<\/jats:sup>, M = Fe, Ru, and [XW<jats:sub>11<\/jats:sub>Mn<jats:sup>III<\/jats:sup>(H<jats:sub>2<\/jats:sub>O)O<jats:sub>39<\/jats:sub>]<jats:sup><jats:italic>n<\/jats:italic>\u2013<\/jats:sup>, X = P, Si, B (transition\u2010metal\u2010substituted anions). The role of multiple\u2010scattering contributions was evaluated for [PW<jats:sub>12<\/jats:sub>O<jats:sub>40<\/jats:sub>]<jats:sup>3\u2013<\/jats:sup> for which an accurate structure determination was available. The results from the multiple\u2010scattering analyses were compared with the single\u2010scattering method. The average W\u2010shell inter\u2010atomic distances were determined in relation to a selected tungsten atom (W<jats:sub>c<\/jats:sub>) by W <jats:italic>L<\/jats:italic><jats:sub>III<\/jats:sub> edge transmission analysis. Several shells of up to 3.8\u20134.0 \u00c5 were identified. For the anion [PW<jats:sub>12<\/jats:sub>O<jats:sub>40<\/jats:sub>]<jats:sup>3\u2013<\/jats:sup>, the obtained inter\u2010atomic distances in the solid sample and in acetonitrile were identical but for the lacunary anion the EXAFS spectrum of the solid was different from that in solution (the number of atoms coordinated to W<jats:sub>c<\/jats:sub> in [PW<jats:sub>11<\/jats:sub>O<jats:sub>39<\/jats:sub>]<jats:sup>7\u2013<\/jats:sup> was the same in both cases, but the calculated distances for the shells were slightly different). Metal\u2010substituted anions were studied by W <jats:italic>L<\/jats:italic><jats:sub>III<\/jats:sub> edge transmission and by Fe, Mn, or Ru <jats:italic>K<\/jats:italic> edge fluorescence analysis. The average coordination sphere of tungsten was affected by the replacement of a W=O by a M\u2013OH<jats:sub>2<\/jats:sub> group. The EXAFS results indicate that on average the MnO<jats:sub>6<\/jats:sub> octahedron is larger than FeO<jats:sub>6<\/jats:sub> or RuO<jats:sub>6<\/jats:sub> and also larger than the average of all WO<jats:sub>6<\/jats:sub> octahedra in [PW<jats:sub>11<\/jats:sub>M(H<jats:sub>2<\/jats:sub>O)O<jats:sub>39<\/jats:sub>]<jats:sup>4\u2013<\/jats:sup>. This was attributed to the occurrence of the Jahn\u2013Teller effect in the coordination sphere of Mn<jats:sup>III<\/jats:sup>. A comparison of the W <jats:italic>L<\/jats:italic><jats:sub>III<\/jats:sub> edge analysis EXAFS data for three Mn<jats:sup>III<\/jats:sup>\u2010substituted anions (X = P, Si, B) suggested that the average size of the W<jats:sub>3<\/jats:sub>O<jats:sub>13<\/jats:sub> groups did not depend on X. (\u00a9 Wiley\u2010VCH Verlag GmbH &amp; Co. KGaA, 69451 Weinheim, Germany, 2007)<\/jats:p>","DOI":"10.1002\/ejic.200500681","type":"journal-article","created":{"date-parts":[[2007,2,3]],"date-time":"2007-02-03T04:16:38Z","timestamp":1170476198000},"page":"1027-1038","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":31,"title":["Structural Studies of Keggin\u2010Type Polyoxotungstates by Extended X\u2010ray Absorption Fine Structure Spectroscopy"],"prefix":"10.1002","volume":"2007","author":[{"given":"M. Salete S.","family":"Balula","sequence":"first","affiliation":[]},{"given":"Isabel C. M. 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