Oxidative Addition to Sn(II) Guanidinate Complexes: Precursors to Tin(II) Chalcogenide Nanocrystals

Andrew Johnson; Ibbi Ahmet; Joseph Thompson

doi:10.1002/ejic.201800071

Oxidative Addition to Sn(II) Guanidinate Complexes: Precursors to Tin(II) Chalcogenide Nanocrystals

Andrew Johnson, Ibbi Ahmet, Joseph Thompson

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Abstract

SnS, SnSe and SnTe are potentially important semiconductor materials. Here, we describe the application of chalcogen containing Sn ^IV guanidinate precursors for the production of tin(II) chalcogenide nanocrystals. Reaction of the stannylene(II) guanidinate complex [{Me ₂NC(NCy) ₂} ₂Sn] (1) with Ph ₂E ₂ (E = S, Se, Te), and CBr ₄ forms the Sn ^IV complexes [{Me ₂NC(NCy) ₂} ₂Sn(Ch-Ph) ₂] (2–4) and [{Me ₂NC(NCy) ₂} ₂SnBr ₂] (5), respectively. Complex 5 has been subsequently used for the synthesis of the corresponding Sn ^IV mono chalcogenide complexes, [{Me ₂NC(NCy) ₂} ₂Sn = E] (6–8) by the reaction of 5 with Li ₂E systems. Isolated tin complexes have characterized by elemental analysis, NMR spectroscopy, and the molecular structures of complexes 2–5 determined by single-crystal X-ray diffraction. TG analysis showed that complexes 2–4 and 6–8 all have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 6–8 were assessed for their utility in the formation of nanocrystalline materials. The materials obtained were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX). Analysis showed formation of SnSe and SnTe from complexes 7 and 8, respectively.

Original language	English
Pages (from-to)	1670-1678
Number of pages	9
Journal	European Journal of Inorganic Chemistry
Volume	2018
Issue number	15
Early online date	28 Feb 2018
DOIs	https://doi.org/10.1002/ejic.201800071
Publication status	Published - 23 Apr 2018

Keywords

Guanidinate
Precursors
Selenium
Sulfur
Tellurium
Tin(II)

ASJC Scopus subject areas

Inorganic Chemistry

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10.1002/ejic.201800071

ejic.201800071R1-1 (PDF)
This is the peer reviewed version of the following article: Johnson, A., Ahmet, I., & Thompson, J. (2018). Oxidative Addition to Sn(II) Guanidinate Complexes: Precursors to Tin(II) Chalcogenide Nanocrystals. European Journal of Inorganic Chemistry, [ejic.201800071]. , which has been published in final form at https://doi.org/10.1002/ejic.201800071. This article may be used for non-commercial purposes in accordance with Wiley Terms and Conditions for Self-Archiving.
Accepted author manuscript, 1.77 MB
ejic.201800071R1_ESI-1-supplementary information (PDF)Accepted author manuscript, 942 KB

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title = "Oxidative Addition to Sn(II) Guanidinate Complexes: Precursors to Tin(II) Chalcogenide Nanocrystals",

abstract = "SnS, SnSe and SnTe are potentially important semiconductor materials. Here, we describe the application of chalcogen containing Sn IV guanidinate precursors for the production of tin(II) chalcogenide nanocrystals. Reaction of the stannylene(II) guanidinate complex [{Me 2NC(NCy) 2} 2Sn] (1) with Ph 2E 2 (E = S, Se, Te), and CBr 4 forms the Sn IV complexes [{Me 2NC(NCy) 2} 2Sn(Ch-Ph) 2] (2–4) and [{Me 2NC(NCy) 2} 2SnBr 2] (5), respectively. Complex 5 has been subsequently used for the synthesis of the corresponding Sn IV mono chalcogenide complexes, [{Me 2NC(NCy) 2} 2Sn = E] (6–8) by the reaction of 5 with Li 2E systems. Isolated tin complexes have characterized by elemental analysis, NMR spectroscopy, and the molecular structures of complexes 2–5 determined by single-crystal X-ray diffraction. TG analysis showed that complexes 2–4 and 6–8 all have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 6–8 were assessed for their utility in the formation of nanocrystalline materials. The materials obtained were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX). Analysis showed formation of SnSe and SnTe from complexes 7 and 8, respectively. ",

keywords = "Guanidinate, Precursors, Selenium, Sulfur, Tellurium, Tin(II)",

author = "Andrew Johnson and Ibbi Ahmet and Joseph Thompson",

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AU - Johnson, Andrew

AU - Ahmet, Ibbi

AU - Thompson, Joseph

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Y1 - 2018/4/23

N2 - SnS, SnSe and SnTe are potentially important semiconductor materials. Here, we describe the application of chalcogen containing Sn IV guanidinate precursors for the production of tin(II) chalcogenide nanocrystals. Reaction of the stannylene(II) guanidinate complex [{Me 2NC(NCy) 2} 2Sn] (1) with Ph 2E 2 (E = S, Se, Te), and CBr 4 forms the Sn IV complexes [{Me 2NC(NCy) 2} 2Sn(Ch-Ph) 2] (2–4) and [{Me 2NC(NCy) 2} 2SnBr 2] (5), respectively. Complex 5 has been subsequently used for the synthesis of the corresponding Sn IV mono chalcogenide complexes, [{Me 2NC(NCy) 2} 2Sn = E] (6–8) by the reaction of 5 with Li 2E systems. Isolated tin complexes have characterized by elemental analysis, NMR spectroscopy, and the molecular structures of complexes 2–5 determined by single-crystal X-ray diffraction. TG analysis showed that complexes 2–4 and 6–8 all have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 6–8 were assessed for their utility in the formation of nanocrystalline materials. The materials obtained were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX). Analysis showed formation of SnSe and SnTe from complexes 7 and 8, respectively.

AB - SnS, SnSe and SnTe are potentially important semiconductor materials. Here, we describe the application of chalcogen containing Sn IV guanidinate precursors for the production of tin(II) chalcogenide nanocrystals. Reaction of the stannylene(II) guanidinate complex [{Me 2NC(NCy) 2} 2Sn] (1) with Ph 2E 2 (E = S, Se, Te), and CBr 4 forms the Sn IV complexes [{Me 2NC(NCy) 2} 2Sn(Ch-Ph) 2] (2–4) and [{Me 2NC(NCy) 2} 2SnBr 2] (5), respectively. Complex 5 has been subsequently used for the synthesis of the corresponding Sn IV mono chalcogenide complexes, [{Me 2NC(NCy) 2} 2Sn = E] (6–8) by the reaction of 5 with Li 2E systems. Isolated tin complexes have characterized by elemental analysis, NMR spectroscopy, and the molecular structures of complexes 2–5 determined by single-crystal X-ray diffraction. TG analysis showed that complexes 2–4 and 6–8 all have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 6–8 were assessed for their utility in the formation of nanocrystalline materials. The materials obtained were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX). Analysis showed formation of SnSe and SnTe from complexes 7 and 8, respectively.

KW - Guanidinate

KW - Precursors

KW - Selenium

KW - Sulfur

KW - Tellurium

KW - Tin(II)

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JO - European Journal of Inorganic Chemistry

JF - European Journal of Inorganic Chemistry

SN - 1434-1948

IS - 15

ER -

Oxidative Addition to Sn(II) Guanidinate Complexes: Precursors to Tin(II) Chalcogenide Nanocrystals

Abstract

Keywords

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