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15-Copper(II)-Containing 36-Tungsto-4-silicates(IV) [Cu15O2(OH)10X(A-α-SiW9O34)4]25- (X = Cl, Br): Synthesis, Structure, Magnetic Properties, and Electrocatalytic CO2 Reduction

Abstract

The 15-copper(II)-containing 36-tungsto-4-silicates [Cu15O2(OH)10X(A-α-SiW9O34)4]25- (X = Cl, 1; Br, 2) have been prepared in 70% yield by reaction of the trilacunary 9-tungstosilicate precursor [A-α-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 – 295 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 eletroactivity 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.

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Publication details

The article was received on 11 May 2018, accepted on 01 Aug 2018 and first published on 01 Aug 2018


Article type: Paper
DOI: 10.1039/C8DT01896K
Citation: Dalton Trans., 2018, Accepted Manuscript
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    15-Copper(II)-Containing 36-Tungsto-4-silicates(IV) [Cu15O2(OH)10X(A-α-SiW9O34)4]25- (X = Cl, Br): Synthesis, Structure, Magnetic Properties, and Electrocatalytic CO2 Reduction

    B. Basil, A. Haider, M. Ibrahim, A. S. Mougharbel, S. Bhattacharya, J. Christian, J. Bindra, N. Dalal, M. Wang, G. Zhang, B. Keita, I. A. Rutkowska, P. Kulesza and U. Kortz, Dalton Trans., 2018, Accepted Manuscript , DOI: 10.1039/C8DT01896K

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