M. Schurmann et F. Huber, ON THE SYNTHESIS AND STRUCTURE OF MONOARYLLEAD AND DIARYLLEAD ACETATES RPB(OCOCH3)(3) AND R2PB(OCOCH3)(2), Journal of organometallic chemistry, 530(1-2), 1997, pp. 121-130
Anhydrous monoaryllead triacetates ArPb(OAc)(3) (Ar = Ph, p-Tolyl, o-T
olyl, 2,5-Xplyl; OAc = OCOMe) were prepared by arylation of Pb(OAc)(4)
with ArSn(C4H9-n)(3) in the presence of Hg(OCOCF3)(2). The procedure
was adapted for the synthesis of diaryllead diacetates Ar2Pb(OAc)(2) (
hr = Ph, p-Tolyl, o-Tolyl, p-ClC6H4, o-ClC6H4) and afforded products w
ith higher purity than other procedures. The crystal structures of PhP
b(OAc)(3), Ph2Pb(OAc)(2) and (o-Tolyl)(2)Pb(OAc)(2) were determined by
X-ray diffraction. PhPb(OAc)(3) and (o-Tolyl)(2)Pb(OAc)(2) are monome
ric. The pentagonal bipyramid around Pb in PhPb(OAc)(3), like the trap
ezoidal bipyramid around Ph in (o-Tolyl)(2)Pb(OAc)(2), is heavily dist
orted, the OAc groups being unsymmetrically chelating. Lead in Ph2Pb(O
Ac)(2) is in a distorted octahedral environment. One OAc group is brid
ging, linking the molecular units to infinite chains, the other OAc gr
oup is symmetrically chelating. IR,H-1,C-13 and (207)pb NMR spectrosco
pic data an reported. The structures of p-TolPb(OAc)(3), o-TolPb(OAc)(
3) and 2,5-XylPb(OAc)(3) are inferred to be similar to that of PhPb(OA
c)(3), and the structure of (o-ClC6H4)(2)Pb(OAc)(2) is inferred to be
similar to that of (o-Tolyl)(2)Pb(OAc)(2).