The reaction of Fe2(CO)9 in thf with
Ph2SbCH2SbPh2 (dpsm) or
Me2SbCH2SbMe2
(dmsm)
produced [Fe(CO)4(η1-dpsm)] and
[Fe(CO)4(μ-dmsm)Fe(CO)4],
and Co2(CO)8 reacted with
either distibine ligand (L-L) to give
[Co2(CO)4(μ-CO)2(μ-L-L)].
Ni(CO)4 and dpsm gave [Ni(CO)3(η1-dpsm)] and
[Ni(CO)3(μ-dpsm)Ni(CO)3],
while with dmsm only
[Ni(CO)3(μ-dmsm)Ni(CO)3] was isolated.
Mn2(CO)10 reacted slowly with dpsm or
dmsm in the presence of a
[{(Cp)Fe(CO)2}2] catalyst
to give [Mn2(CO)8(L-L)], but no
reaction occurred with
Re2(CO)10
under similar conditions.
cis-[Mn(CO)4X(dpsm)] (X = Cl,
Br, or I) and
[Mn2(CO)8Br2(μ-dmsm)]
were also prepared from the appropriate [Mn(CO)5X],
but iron carbonyl halide derivatives
were too unstable to isolate in the pure state. The complexes have
been characterized by
elemental analysis, IR and multinuclear NMR (1H,
13C{1H}, 55Mn, or
59Co) spectroscopy,
and FAB mass spectrometry. The X-ray structures of dpsm,
[Fe(CO)4(η1-dpsm)], and
[Co2(CO)4(μ-CO)2(μ-dmsm)] have been
determined. No evidence for chelation by dmsm or dpsm
was found, and Sb−C fission does not occur to significant extents in
the reactions studied.
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