Thio-, seleno- and telluro-ether complexes of aluminium(iii) halides: Synthesis, structures and properties

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Abstract

The reaction of AlCl3 with Me2E (E = S, Se or Te) or nBu2E (E = Se or Te) in CH2Cl2 under rigorously anhydrous conditions gave the pseudo-tetrahedral complexes [AlCl3(R2E)]. The [AlX3(Me2E)] (X = Br or I, E = S; X = Br, E = Te) were made from toluene solution since attempted syntheses in CH2Cl2 resulted in substantial chloride incorporation. The synthesis of [(AlCl3)2{o-C 6H4(CH2SEt)2}], in which the ligand bridges two tetrahedral aluminium centres, and of the six-coordinate trans-[AlX2{MeE(CH2)2EMe}2][AlX 4] (X = Cl or Br, E = S, and X = Cl, E = Se) and cis-[AlI 2{MeS(CH2)2SMe}2][AlI4] are reported. The tripodal thioether forms [AlCl3{MeC(CH 2SMe)3}], which is a chain polymer with κ2-coordinated ligand and a tbp arrangement at Al(iii). Chalcogenoether macrocycle complexes [AlCl3([9]aneS3)], [AlCl2([14]aneS4)][AlCl4] and [AlCl 2([16]aneSe4)] [AlCl4] are also described. All complexes were characterised by microanalysis, IR and multinuclear NMR ( 1H, 27Al, 77Se or 125Te) spectroscopy as appropriate. In CH2Cl2 solution [AlCl 3(Me2S)] with added Me2S forms [AlCl 3(Me2S)2], and the [AlX2{MeS(CH 2)2SMe}2][AlX4] exist as mixtures of cis and trans isomers which undergo rapid exchange at ambient temperatures. X-Ray crystal structures are reported for [AlCl3(Me2Se], [AlX3(Me2Te)] (X = Cl or Br), trans-[AlCl 2{MeE(CH2)2EMe}2][AlCl4] (E = S or Se), cis-[AlI2{MeS(CH2)2SMe} 2][AlI4], [AlCl3{MeC(CH2SMe) 3}], and for the sulfonium salt [Me2SH][AlCl4]. The aluminium halide chalcogenoether chemistry is compared with the corresponding gallium and indium systems, and the relative Lewis acidities of the metals discussed. Attempts to use [AlCl3(nBu 2E)] (E = Se or Te) as LPCVD reagents to form aluminium chalcogenide films were unsuccessful. © 2014 The Royal Society of Chemistry.

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George, K., Jura, M., Levason, W., Light, M. E., & Reid, G. (2014). Thio-, seleno- and telluro-ether complexes of aluminium(iii) halides: Synthesis, structures and properties. Dalton Transactions, 43(9), 3637–3648. https://doi.org/10.1039/c3dt52991f

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