NDLI: Stabilising pentavalent actinides—visible–near infrared and X-ray absorption spectroscopic studies of the utility of the $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(MW_{9}O_{33})_{3}]^{18−}$ (M = Sb, Bi) structural type

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Stabilising pentavalent actinides—visible–near infrared and X-ray absorption spectroscopic studies of the utility of the $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(MW_{9}O_{33})_{3}]^{18−}$ (M = Sb, Bi) structural type

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Stabilising pentavalent actinides—visible–near infrared and X-ray absorption spectroscopic studies of the utility of the $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(MW_{9}O_{33})_{3}]^{18−}$ (M = Sb, Bi) structural type

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	May, Iain Conradson, Steven D. Boland, Kevin S. Costello, Alison L. Kozimor, Stosh A. Schnaars, David D. Gaunt, Andrew J. Reilly, Sean D.
Description	Author Affiliation: Boland KS ( Los Alamos National Laboratory, Los Alamos, NM 87545, USA.)
Abstract	We report the interaction between B-type tri-lacunary heteropolyoxotungstate anions and actinyl(V) cations in aqueous solution, yielding a greater understanding of the stability of the $O\&\#8801;An\&\#8801;O^{1+}$ linear dioxo actinide moiety. Previously we reported that $B-α-[BiW_{9}O_{33}]^{9−}$ and $B-α-[SbW_{9}O_{33}]^{9−}$ will react with $NpO_{2}^{1+}$ to yield $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(MW_{9}O_{33})_{3}]^{18−}$ (M = Bi, or Sb). Single crystal structural characterisation of salts of these complexes revealed a core in which three $Np^{V}$ atoms interact with a central $W^{VI}$ atom through bridging oxo groups. These bridging oxygen atoms come from one of the two axial oxygens in $O\&\#8801;Np\&\#8801;O^{1+}$ and represent a highly unusual interaction for a discrete molecular species. In this study visible/near infra-red spectroscopy indicates that $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(BiW_{9}O_{33})_{3}]^{18−}$ could be readily stabilized in solution at near neutral pH for several months, with $(NH_{4})_{14}Na_{4}[(Np_{3}W_{4}O_{15})(H_{2}O)_{39}BiW_{9}O_{33})_{3}]·62H_{2}O$ crystallising from solution in high yield. At lower pH and $[BiW_{9}O_{33}]^{9−}:NpO_{2}^{1+}$ ratios additional $Np^{V}$ species could be observed in solution. Stabilization of $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(SbW_{9}O_{33})_{3}]^{18−}$ in solution proved more challenging, with several distinctive $Np^{V}$ near infra-red transitions observed in solution. Slow complexation kinetics and reduction to $Np^{IV}$ was also observed. High $[SbW_{9}O_{33}]^{9−}:NpO_{2}^{1+}$ molar ratios and careful control of solution pH was required to prepare solutions in which $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(SbW_{9}O_{33})_{3}]^{18−}$ was the only neptunium containing species. In stark contrast to the $NpO_{2}^{1+}$ chemistry, $[BiW_{9}O_{33}]^{9−}$ readily oxidizes $PuO_{2}^{1+}$ to $PuO_{2}^{2+}$ yielding further evidence of the decreased stability of $Pu^{V}vs.Np^{V}.$ Np $L_{II}-edge$ XAFS measurement revealed very good agreement with single crystal diffraction data for the Np structural environment for $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(MW_{9}O_{33})_{3}]^{18−}$ (M = Bi, or Sb) in the solid state. There was also good agreement between coordination shells for $[(Np_{3}W_{4}O_{15})(H_{2}O)_{3}(BiW_{9}O_{33})_{3}]^{18−}$ in the solid state and in solution, yielding further confirmation of the high stability of this particular cluster.
ISSN	14779226
Issue Number	7
Journal	Dalton Trans.
Volume Number	41
e-ISSN	13645447
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2012-02-21
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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