Low-co-ordination arsenic and antimony compounds: Synthesis and characterisation of 2-arsa- and 2-stiba-1,3-dionatolithium(I) complexes, [Li{OC(R)EC(R)O}L](E = As or Sb; R = But, C6H2Pri3-2,4,6 or C6H2But3-2,4,6; L = Et2O or MeOCH2CH2OMe)

Julie Durkin, David E. Hibbs, Peter B. Hitchcock, Michael B. Hursthouse, Cameron Jones, Joanne Jones, K. M.Abdul Malik, John F. Nixon, Glenn Parry

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Abstract

Reactions of [Li{E(SiMe3)2}(dme)] (E = As or Sb, dme = MeOCH2CH2OMe), with a range of acid chlorides, RCOCl, afforded the novel 2-arsa-1,3-dionatolithium(I) complexes [Li{OC(R)AsC(R)O}L] (R = But, L = 1/2 dme or Et2O; R = C6H2Pri3-2,4,6, L = Et2O; R = C6H2But3-2,4,6, L = dme), and the first example of a 2-stiba-1,3-dionatolithium(I) complex [{[Li{OC(But)SbC(But)O}(dme)0.5] 2}]. X-Ray crystal structural analyses for the complexes with R = But, L = 1/2 dme or Et2O and the antimony compound show them to be dimeric in the solid state with respect to the metal and anionic ligands, the dimeric units being linked in an infinite polymeric chain by bridging dme molecules or solvated with Et2O. A dimeric structure can also be inferred when R = C6H2Pri3-2,4,6, L = Et2O. In solution these four compounds display fluxional behaviour. Treatment with HCl of the monomeric compound having R = C6H2But3-2,4,6, L = dme yields the known diacylarsane [As{C(C6H2But3-2,4,6)0} {C(C6H2But3-2,4,6)OH}] the crystal structure of which reveals the enol form with the alcoholic proton intramolecularly hydrogen bonded to the opposing oxygen centre of the ligand.

Original languageEnglish
Pages (from-to)3277-3282
Number of pages6
JournalDalton
Issue number15
DOIs
Publication statusPublished - 7 Aug 1996
Externally publishedYes

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