A chemically induced, room temperature, single source precursor to CuS (covellite) nanomaterials: synthesis and reactivity of [Cu(S2CNHBz)]n

Siqiao Huang; Xiang Xu; Jagodish C. Sarker; David Pugh; Graeme Hogarth

doi:10.1039/d4dt02366h

A chemically induced, room temperature, single source precursor to CuS (covellite) nanomaterials: synthesis and reactivity of [Cu(S₂CNHBz)]_n

Siqiao Huang, Xiang Xu, Jagodish C. Sarker, David Pugh, Graeme Hogarth^*

^*Corresponding author for this work

King's College London

Research output: Contribution to journal › Article › peer-review

Abstract

Addition of two equivalents of NaS₂CNHBz to CuSO₄ affords the yellow diamagnetic coordination polymer [Cu(S₂CNHBz)]_n (1), resulting from intramolecular electron-transfer and concomitant formation of the thiourea, (BzNH)₂C 00000000 00000000 00000000 00000000 11111111 00000000 11111111 00000000 00000000 00000000 S. 1 reacts with PPh₃ and 1,1′-bis(diphenylphosphino)ferrocene (dppf) in CH₂Cl₂ to give monomeric [Cu(κ²-S₂CNHBz)(PPh₃)₂] (2) and [Cu(κ²-S₂CNHBz)(κ²-dppf)] (3), respectively, both of which have been crystallographically characterised. While 1 is thermally stable in dimethylsulfoxide (DMSO) up to ca. 70 °C, addition of ⁿBuNH₂ to 1 leads to its rapid decomposition to afford CuS (covellite) nanomaterials; indeed in neat ⁿBuNH₂, covellite formation is rapid at room temperature. Thus, 1 serves as an effective low-temperature base-induced single source precursor to covellite nanomaterials.

Original language	English
Pages (from-to)	17140-17145
Number of pages	6
Journal	Dalton Transactions
Volume	53
Issue number	42
DOIs	https://doi.org/10.1039/d4dt02366h
Publication status	Published - 8 Oct 2024

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title = "A chemically induced, room temperature, single source precursor to CuS (covellite) nanomaterials: synthesis and reactivity of [Cu(S2CNHBz)]n",

abstract = "Addition of two equivalents of NaS2CNHBz to CuSO4 affords the yellow diamagnetic coordination polymer [Cu(S2CNHBz)]n (1), resulting from intramolecular electron-transfer and concomitant formation of the thiourea, (BzNH)2C 00000000 00000000 00000000 00000000 11111111 00000000 11111111 00000000 00000000 00000000 S. 1 reacts with PPh3 and 1,1′-bis(diphenylphosphino)ferrocene (dppf) in CH2Cl2 to give monomeric [Cu(κ2-S2CNHBz)(PPh3)2] (2) and [Cu(κ2-S2CNHBz)(κ2-dppf)] (3), respectively, both of which have been crystallographically characterised. While 1 is thermally stable in dimethylsulfoxide (DMSO) up to ca. 70 °C, addition of nBuNH2 to 1 leads to its rapid decomposition to afford CuS (covellite) nanomaterials; indeed in neat nBuNH2, covellite formation is rapid at room temperature. Thus, 1 serves as an effective low-temperature base-induced single source precursor to covellite nanomaterials.",

author = "Siqiao Huang and Xiang Xu and Sarker, {Jagodish C.} and David Pugh and Graeme Hogarth",

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AU - Xu, Xiang

AU - Sarker, Jagodish C.

AU - Pugh, David

AU - Hogarth, Graeme

PY - 2024/10/8

Y1 - 2024/10/8

N2 - Addition of two equivalents of NaS2CNHBz to CuSO4 affords the yellow diamagnetic coordination polymer [Cu(S2CNHBz)]n (1), resulting from intramolecular electron-transfer and concomitant formation of the thiourea, (BzNH)2C 00000000 00000000 00000000 00000000 11111111 00000000 11111111 00000000 00000000 00000000 S. 1 reacts with PPh3 and 1,1′-bis(diphenylphosphino)ferrocene (dppf) in CH2Cl2 to give monomeric [Cu(κ2-S2CNHBz)(PPh3)2] (2) and [Cu(κ2-S2CNHBz)(κ2-dppf)] (3), respectively, both of which have been crystallographically characterised. While 1 is thermally stable in dimethylsulfoxide (DMSO) up to ca. 70 °C, addition of nBuNH2 to 1 leads to its rapid decomposition to afford CuS (covellite) nanomaterials; indeed in neat nBuNH2, covellite formation is rapid at room temperature. Thus, 1 serves as an effective low-temperature base-induced single source precursor to covellite nanomaterials.

AB - Addition of two equivalents of NaS2CNHBz to CuSO4 affords the yellow diamagnetic coordination polymer [Cu(S2CNHBz)]n (1), resulting from intramolecular electron-transfer and concomitant formation of the thiourea, (BzNH)2C 00000000 00000000 00000000 00000000 11111111 00000000 11111111 00000000 00000000 00000000 S. 1 reacts with PPh3 and 1,1′-bis(diphenylphosphino)ferrocene (dppf) in CH2Cl2 to give monomeric [Cu(κ2-S2CNHBz)(PPh3)2] (2) and [Cu(κ2-S2CNHBz)(κ2-dppf)] (3), respectively, both of which have been crystallographically characterised. While 1 is thermally stable in dimethylsulfoxide (DMSO) up to ca. 70 °C, addition of nBuNH2 to 1 leads to its rapid decomposition to afford CuS (covellite) nanomaterials; indeed in neat nBuNH2, covellite formation is rapid at room temperature. Thus, 1 serves as an effective low-temperature base-induced single source precursor to covellite nanomaterials.

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ER -

A chemically induced, room temperature, single source precursor to CuS (covellite) nanomaterials: synthesis and reactivity of [Cu(S₂CNHBz)]_n

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