Synthesis and NMR spectroscopy of [t-Bu 2PHg( μ-PPh 2)M(CO) 5], M = Cr, Mo, W and X-ray structure for M = Cr, W

The title complexes (M = Cr ( 1), Mo ( 2) and W ( 3)) are prepared in almost quantitative yield from [t-Bu 2PHgN(SiMe 3) 2] and [M(HPPh 2)(CO) 5] or in 70% yield by synproportionation of [Hg(t-Bu 2P) 2] and [Hg{( μ-PPh 2)M(CO) 5} 2]. The compounds are crystalline, air-stable in the solid state but o...

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Bibliographic Details
Published in:Journal of organometallic chemistry 1997-08, Vol.541 (1), p.233-236
Main Authors: Eichbichler, Johann, Malleier, Richard, Wurst, Klaus, Peringer, Paul
Format: Article
Language:English
Subjects:
Chromium
Mercury
Molybdenum
Tungsten
X-ray crystallography
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Summary:The title complexes (M = Cr ( 1), Mo ( 2) and W ( 3)) are prepared in almost quantitative yield from [t-Bu 2PHgN(SiMe 3) 2] and [M(HPPh 2)(CO) 5] or in 70% yield by synproportionation of [Hg(t-Bu 2P) 2] and [Hg{( μ-PPh 2)M(CO) 5} 2]. The compounds are crystalline, air-stable in the solid state but oxygen-sensitive in solution. The solid state structures of 1 and 3 consist of dimers containing four-membered (Hg-P) 2 rings with asymmetric phosphido bridges (252.2(2)pm and 268.9(2)pm for 1). The coordination geometry of Hg is almost planar. According to 31P and 199Hg NMR spectroscopy, the solution structure consists of dimers at 173K, whilst dissociation into monomers occurs at ambient temperature.
ISSN:0022-328X
1872-8561
DOI:10.1016/S0022-328X(97)00065-X