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Issue 35, 2018
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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

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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 1.8–300 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.

Graphical abstract: 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

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Supplementary files

Article information


Submitted
11 May 2018
Accepted
01 Aug 2018
First published
01 Aug 2018

Dalton Trans., 2018,47, 12439-12448
Article type
Paper

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. S. Bassil, A. Haider, M. Ibrahim, A. S. Mougharbel, S. Bhattacharya, J. H. Christian, J. K. Bindra, N. S. Dalal, M. Wang, G. Zhang, B. Keita, I. A. Rutkowska, P. J. Kulesza and U. Kortz, Dalton Trans., 2018, 47, 12439
DOI: 10.1039/C8DT01896K

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