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.

Isolation of a Diylide‐Stabilized Stannylene and Germylene: Enhanced Donor Strength through Coplanar Lone Pair Alignment

“…To the best of our knowledge,f ormation of such af ive-membered Sn-S cycle has never been observed with any other stannylene. [26] In contrast to the structures of the tetrylenes,nocoordination of the tin and germanium center,r espectively,b yt he sulfonyl group is observed in the molecular structures of 4-5b and only aw eak interaction by one of the sulfonyl groups in 6. This shows that-although important for the stabilization of Y 2 Ge and Y 2 Sn-the sulfonyl coordination is easily opened to facilitate substrate coordination and/or attack.…”

Isolierung eines diylidstabilisierten Stannylens und Germylens: Erhöhte Donorstärke durch coplanare Anordnung freier Elektronenpaare

“…Nach unserem besten Wissen konnte eine Bildung eines derartigen Sn-S-Fünfrings aus einem Stannylen bisher noch nicht beobachtet werden. [26] Im Gegensatz zu den Strukturen der Te trylene weisen die Strukturen von 4-5b keine Wechselwirkungen der Sulfonyleinheiten mit den Zinn-und Germaniumzentren auf und auch in Verbindung 6 liegt nur eine schwache Koordination einer Sulfonylgruppe vor.D ies zeigt, dass,o bgleich die Sulfonylkoordination wichtig fürdie Stabilisierung von Y 2 Ge und Y 2 Sn ist, diese leicht aufgebrochen werden kann um den Angriff oder die Koordination eines Substrats zu ermçglichen.…”

Effect of Temperature and Capping Agents on Structural and Optical Properties of Tin Sulphide Nanocrystals

“…Synthetic routes such as hydrothermal [26], solvothermal [27], hot injection [28], aqueous solution [29], pyrolysis [30], colloidal route [31], single-source approach [32,33], precipitation [34], microwave [35], electrodeposition [36], and so on have been utilized for the synthesis of SnS nanoparticles. e single-source precursor has proven to be a more effective route that forms nanoparticles of high qualities with well-defined size and shape.…”