Fast Microwave-Assisted Synthesis of Wells-Dawson-Type 18-Tungsto-2-Phosphate [P₂W₁₈O₆₂]⁶⁻

We report on a fast microwave-assisted synthetic procedure of the Wells-Dawson-type 18-tungsto-2-phosphate [P2W18O62]6− with a 35% yield in 24 h, rather than a week using conventional heating

15-Copper(ii)-containing 36-tungsto-4-silicates(iv) [Cu15O2(OH)(10)X(A--SiW9O34)(4)](25-) (X = Cl, Br): synthesis, structure, magnetic properties, and electrocatalytic CO2 reduction

The 15-copper(ii)-containing 36-tungsto-4-silicates [Cu15O2(OH)(10)X(A--SiW9O34)(4)](25-) (X = Cl, 1; Br, 2) have been prepared in 70% yield by reaction of the trilacunary 9-tungstosilicate precursor [A--SiW9O34](10-) with Cu2+ ions in aqueous pH 8 medium. Both polyanions 1 and 2 were isolated as hydrated mixed potassium/sodium salts and characterized in the solid state by FT-IR, TGA, single-crystal XRD, and elemental analysis. DC magnetic susceptibility measurements from 1.8-300 K established the ground state to be paramagnetic with a magnetic moment corresponding to 15 uncoupled Cu2+ (S = 1/2) ions. EPR measurements and simulations were consistent with this analysis. Electrochemical studies were performed for polyanions 1 and 2 dissolved in solution to elucidate the electroactivity of both copper and tungstate sites. Using 2 as a representative example, the electrocatalytic activity towards CO2 reduction upon deposition on a glassy carbon electrode surface, while retaining selectivity relative to hydrogen evolution, was demonstrated.</p

Dithallium(III)-Containing 30-Tungsto-4-phosphate, [Tl2Na2(H2O)2(P2W15O56)2]16-: Synthesis, Structural Characterization, and Biological Studies

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Dithallium(III)-Containing 30-Tungsto-4-phosphate, [Tl Na (H O) (P W O ) ] : Synthesis, Structural Characterization, and Biological Studies

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Dithallium(III)-Containing 30-Tungsto-4-phosphate, [Tl₂Na₂(H₂O)₂(P₂W₁₅O₅₆)₂]^16–: Synthesis, Structural Characterization, and Biological Studies

Here we report on the synthesis and structural characterization of the dithallium­(III)-containing 30-tungsto<i>-</i>4-phosphate [Tl₂Na₂(H₂O)₂­{P₂W₁₅O₅₆}₂]^16– (<b>1</b>) by a multitude of solid-state and solution techniques. Polyanion <b>1</b> comprises two octahedrally coordinated Tl³⁺ ions sandwiched between two trilacunary {P₂W₁₅} Wells–Dawson fragments and represents only the second structurally characterized, discrete thallium-containing polyoxometalate to date. The two outer positions of the central rhombus are occupied by sodium ions. The title polyanion is solution-stable as shown by ³¹P and ^203/205Tl NMR. This was also supported by Tl NMR spectra simulations including several spin systems of isotopologues with half-spin nuclei (²⁰³Tl, ²⁰⁵Tl, ³¹P, ¹⁸³W). ²³Na NMR showed a time-averaged signal of the Na⁺ counter cations and the structurally bonded Na⁺ ions. ^203/205Tl NMR spectra also showed a minor signal tentatively attributed to the trithallium-containing derivative [Tl₃Na­(H₂O)₂­(P₂W₁₅O₅₆)₂]^14–, which could also be identified in the solid state by single-crystal X-ray diffraction. The bioactivity of polyanion <b>1</b> was also tested against bacteria and <i>Leishmania</i>