Tin(IV) chalcogenide complexes: single source precursors for SnS, SnSe and SnTe nanoparticle synthesis

Andrew Johnson, Joseph Thompson, Ibrahim Ahmet, Gabriele Kociok-Kohn

Research output: Contribution to journalArticle

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Abstract

A family of tin(IV) bis(hexamethylsilylamide) complexes 29 have been synthesized by reaction of [Sn{N(SiMe3)2}2] (1) with the diphenyl dichalcogenanes Ph2E2 (E = S, Se, Te), the radical species TEMPO, or the group 16 elements to form the complexes [(PhE)2Sn{N(SiMe3)2}2] (24) and [(TEMPO)2Sn{N(SiMe3)2}2] (5), and [{(Me3Si)2N}2Sn(µ2-E)]2 (69) (E = S, 2 & 6; E = Se 3 & 7; E = Te, 4 & 9, E = O2, 9). The isolated tin complexes were characterized by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction. Thermogravimetric analysis showed complexes 24 and 68 all to have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 24 and 68 were also assessed for their utility in the formation of nanoparticles. 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 34 and 67, respectively.
LanguageEnglish
Pages4711-4720
JournalEuropean Journal of Inorganic Chemistry
Volume2016
Issue number28
Early online date29 Aug 2016
DOIs
StatusPublished - Oct 2016

Fingerprint

Tin
Chalcogens
Nanoparticles
Energy dispersive X ray analysis
Field emission
X ray powder diffraction
Molecular structure
Nuclear magnetic resonance spectroscopy
Thermogravimetric analysis
Single crystals
X ray diffraction
Scanning electron microscopy
Chemical analysis
TEMPO
diphenyl

Keywords

  • Tin Chalcogenides
  • Precursors
  • Nanoparticles
  • Synthesis
  • X ray crystallography
  • materials chemistry

Cite this

Tin(IV) chalcogenide complexes : single source precursors for SnS, SnSe and SnTe nanoparticle synthesis. / Johnson, Andrew; Thompson, Joseph; Ahmet, Ibrahim; Kociok-Kohn, Gabriele.

In: European Journal of Inorganic Chemistry, Vol. 2016, No. 28, 10.2016, p. 4711-4720.

Research output: Contribution to journalArticle

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abstract = "A family of tin(IV) bis(hexamethylsilylamide) complexes 2–9 have been synthesized by reaction of [Sn{N(SiMe3)2}2] (1) with the diphenyl dichalcogenanes Ph2E2 (E = S, Se, Te), the radical species TEMPO, or the group 16 elements to form the complexes [(PhE)2Sn{N(SiMe3)2}2] (2–4) and [(TEMPO)2Sn{N(SiMe3)2}2] (5), and [{(Me3Si)2N}2Sn(µ2-E)]2 (6–9) (E = S, 2 & 6; E = Se 3 & 7; E = Te, 4 & 9, E = O2, 9). The isolated tin complexes were characterized by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction. Thermogravimetric analysis showed complexes 2–4 and 6–8 all to have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 2–4 and 6–8 were also assessed for their utility in the formation of nanoparticles. 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 3–4 and 6–7, respectively.",
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N2 - A family of tin(IV) bis(hexamethylsilylamide) complexes 2–9 have been synthesized by reaction of [Sn{N(SiMe3)2}2] (1) with the diphenyl dichalcogenanes Ph2E2 (E = S, Se, Te), the radical species TEMPO, or the group 16 elements to form the complexes [(PhE)2Sn{N(SiMe3)2}2] (2–4) and [(TEMPO)2Sn{N(SiMe3)2}2] (5), and [{(Me3Si)2N}2Sn(µ2-E)]2 (6–9) (E = S, 2 & 6; E = Se 3 & 7; E = Te, 4 & 9, E = O2, 9). The isolated tin complexes were characterized by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction. Thermogravimetric analysis showed complexes 2–4 and 6–8 all to have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 2–4 and 6–8 were also assessed for their utility in the formation of nanoparticles. 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 3–4 and 6–7, respectively.

AB - A family of tin(IV) bis(hexamethylsilylamide) complexes 2–9 have been synthesized by reaction of [Sn{N(SiMe3)2}2] (1) with the diphenyl dichalcogenanes Ph2E2 (E = S, Se, Te), the radical species TEMPO, or the group 16 elements to form the complexes [(PhE)2Sn{N(SiMe3)2}2] (2–4) and [(TEMPO)2Sn{N(SiMe3)2}2] (5), and [{(Me3Si)2N}2Sn(µ2-E)]2 (6–9) (E = S, 2 & 6; E = Se 3 & 7; E = Te, 4 & 9, E = O2, 9). The isolated tin complexes were characterized by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction. Thermogravimetric analysis showed complexes 2–4 and 6–8 all to have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 2–4 and 6–8 were also assessed for their utility in the formation of nanoparticles. 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 3–4 and 6–7, respectively.

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KW - X ray crystallography

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