Unexpected Actinyl Cation-Directed Structural Variation in Neptunyl(VI) A-Type Tri-lacunary Heteropolyoxotungstate Complexes

Berg, John M.; Gaunt, Andrew J.; May, Iain; Pugmire, Alison L.; Reilly, Sean D.; Scott, Brian L.; Wilkerson, Marianne P.

doi:10.1021/ic5024345

Unexpected Actinyl Cation-Directed Structural Variation in Neptunyl(VI) A-Type Tri-lacunary Heteropolyoxotungstate Complexes

Journal Article · Wed Apr 22 00:00:00 EDT 2015 · Inorganic Chemistry

DOI:https://doi.org/10.1021/ic5024345· OSTI ID:1239107

Berg, John M. ^[1]; Gaunt, Andrew J. ^[1]; May, Iain ^[1]; Pugmire, Alison L. ^[1]; Reilly, Sean D. ^[1]; Scott, Brian L. ^[1]; Wilkerson, Marianne P. ^[1]

Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

A-type tri-lacunary heteropolyoxotungstate anions (e.g., [PW₉O₃₄]^9-, [AsW₉O₃₄]^9-, [SiW₉O₃₄]^10- and [GeW₉O₃₄]^10-) are multi-dentate oxygen donor ligands that readily form sandwich complexes with actinyl cations ({UO₂}²⁺, {NpO₂}⁺, {NpO₂}²⁺ & {PuO₂}²⁺) in near neutral/slightly alkaline aqueous solutions. Two or three actinyl cations are sandwiched between two trilacunary anions, with additional cations (Na⁺, K⁺ or NH₄⁺) also often held within the cluster. Studies thus far have indicated that it is these additional +I cations, rather than the specific actinyl cation, that direct the structural variation in the complexes formed. We now report the structural characterization of the neptunyl (VI) cluster complex (NH⁴)₁₃ [Na(NpO₂)₂(A-α- PW₉O₃₄)₂]·12H₂O. The anion in this complex, [Na(NpO₂)₂(PW₉O₃₄)₂]^13-, contains one Na⁺ cation and two {NpO₂}²⁺ cations held between two [PW₉O₃₄]^9- anions – with an additional partial occupancy NH₄ ⁺ or {NpO₂}²⁺ cation also present. In the analogous uranium (VI) system, under similar reaction conditions that includes an excess of NH₄Cl in the parent solution, it was previously shown that [(NH₄)₂(U^VIO₂)₂(A-PW₉O₃₄)₂]^12- is the dominant species in both solution and the crystallized salt. Spectroscopic studies provide further proof of differences in the observed chemistry for the {NpO₂}²⁺/[PW₉O₃₄]^9- and {UO₂}²⁺/[PW₉O₃₄]^9- systems, both in solution and in solid state complexes crystallized from comparable salt solutions. The work revealed that varying the actinide element (Np vs. U) can indeed measurably impact structure and complex stability in the cluster chemistry of actinyl (VI) cations with A-type tri-lacunary heteropolyoxotungstate anions.

View Accepted Manuscript (DOE)

Research Organization:: Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: AC52-06NA25396

OSTI ID:: 1239107

Report Number(s):: LA-UR--14-27690

Journal Information:: Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 9 Vol. 54; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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