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

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

doi:10.1002/ejic.201600790

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

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

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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.

Original language	English
Pages (from-to)	4711-4720
Journal	European Journal of Inorganic Chemistry
Volume	2016
Issue number	28
Early online date	29 Aug 2016
DOIs	https://doi.org/10.1002/ejic.201600790
Publication status	Published - Oct 2016

Keywords

Tin Chalcogenides
Precursors
Nanoparticles
Synthesis
X ray crystallography
materials chemistry

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10.1002/ejic.201600790

ejic_201600790_final
This is the peer reviewed version of the following article: Joseph R. Thompson Ibbi Y. Ahmet Andrew L. Johnson Gabriele Kociok‐Köhn (2016) Tin(IV) Chalcogenide Complexes: Single Source Precursors for SnS, SnSe and SnTe Nanoparticle Synthesis. European Journal of Inorganic Chemistry, 2016(28) which has been published in final form at 10.1002/ejic.201600790. This article may be used for non-commercial purposes in accordance with Wiley Terms and Conditions for Self-Archiving.
Accepted author manuscript, 2.34 MB

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@article{079edc0a3ba44daaba1242e02c2cbf8f,

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

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.",

keywords = "Tin Chalcogenides, Precursors, Nanoparticles, Synthesis, X ray crystallography, materials chemistry",

author = "Andrew Johnson and Joseph Thompson and Ibrahim Ahmet and Gabriele Kociok-Kohn",

year = "2016",

month = oct,

doi = "10.1002/ejic.201600790",

language = "English",

volume = "2016",

pages = "4711--4720",

journal = "European Journal of Inorganic Chemistry",

issn = "1434-1948",

publisher = "Wiley-VCH Verlag",

number = "28",

}

TY - JOUR

T1 - Tin(IV) chalcogenide complexes

T2 - single source precursors for SnS, SnSe and SnTe nanoparticle synthesis

AU - Johnson, Andrew

AU - Thompson, Joseph

AU - Ahmet, Ibrahim

AU - Kociok-Kohn, Gabriele

PY - 2016/10

Y1 - 2016/10

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.

KW - Tin Chalcogenides

KW - Precursors

KW - Nanoparticles

KW - Synthesis

KW - X ray crystallography

KW - materials chemistry

UR - http://dx.doi.org/10.1002/ejic.201600790

U2 - 10.1002/ejic.201600790

DO - 10.1002/ejic.201600790

M3 - Article

SN - 1434-1948

VL - 2016

SP - 4711

EP - 4720

JO - European Journal of Inorganic Chemistry

JF - European Journal of Inorganic Chemistry

IS - 28

ER -

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

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

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MC2- X-ray diffraction (XRD)

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