Journal of the Chemical Society, Dalton Transactions p. 1381 - 1386 (1993)
Update date:2022-08-05
Topics:
Tian, Zhigang
Tuck, Dennis G.
The oxidation of elemental antimony by the o-quinones Y4C6O2-o (Y = Cl or Br) in diethyl ether gives the unusual antimony(V) products Sb(O2C6Y4)2.5*nEt2O (Y = Cl, n = 1.5; Y = Br, n = 1).The same quinones, and 3,5-di-tert-butyl-1,2-benzoquinone, upon treatment with Sb + 0.5 X2 (X = Br or I) in toluene, give the antimony(III) derivatives Sb(cat)X (cat = substituted catecholate anion).The oxidations are shown by electron spin resonance spectroscopy to proceed via the o-semiquinone intermediates.Adducts of Sb(cat) I with bidentate neutral donors have been prepared.The structure of Sb(dbc)I(bipy) (dbc = 3,5-di-tert-butylcatecholate, bipy = 2,2'-bipyridine) has been shown to be that of a pseudo-octahedral molecule with a stereochemically active lone pair of electrons.Crystal parameters for Sb(dcb)I(bipy)*0.5bipy: triclinic, space group P1<*>, a = 9.779(4), b = 18.554(7), c = 8.944(3) Angstroem, α = 100.94(3), β = 115.11(3), γ = 86.82(4) deg, Z = 2 and R = 0.044 for 3307 unique reflections.
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