Reaction of Me3SiC⋮CC⋮CSiMe3 with RuHCl(CO)(PPh3)3 in CH2Cl2 produced RuCl(η1-C(C⋮CSiMe3)CHSiMe3)(CO)(PPh3)2, which on treatment with dppe gave RuCl(η1-C(C⋮CSiMe3)CHSiMe3)(CO)(PPh3)(dppe). Reaction of RuHCl(CO)(PPh3)3 with HC⋮CC⋮CH
generated in situ from the reaction of Me3SiC⋮CC⋮CSiMe3 with n-Bu4NF/NH4F/H2O
produced [RuCl(CO)(NH3)(PPh3)2]2(μ-CHCHCHCH), whereas the same reaction without
the NH4F afforded [RuCl(CO)(PPh3)2]2(μ-CHCHCHCH). Complex [RuCl(CO)(NH3)(PPh3)2]2(μ-CHCHCHCH) reacted with excess PEt3 and t-BuNC to give [RuCl(CO)(PEt3)3]2(μ-CHCHCHCH) and {[Ru(t-BuNC)3(PPh3)2]2(μ-COCHCHCHCHCO)}Cl2, respectively.
The structure of [RuCl(CO)(PEt3)3]2(μ-CHCHCHCH) has been confirmed by X-ray
diffraction.
Treatment of [CpOs(PPh3)2]BF4 in THF with 0.5 equiv of HC⋮CCH(OH)C⋮CH followed
by Al2O3 gave the C5H-bridged compound [Cp(PPh3)2OsCCCHC⋮COs(PPh3)2Cp]BF4.
The analogous iron complex [Cp(dppe)FeCCCHC⋮CFe(dppe)Cp]BPh4 has been prepared
similarly. The structure of [Cp(PPh3)2OsCCCHC⋮COs(PPh3)2Cp]BF4 has been confirmed by X-ray diffraction. The electrochemical properties of [Cp(dppe)FeCCCHC⋮CFe(dppe)Cp]BPh4, [Cp(PPh3)2RuCCCHC⋮CRu(PPh3)2Cp]BF4, and [Cp(PPh3)2OsCCCHC⋮COs(PPh3)2Cp]BF4 have been studied by cyclic voltammetry.
Reaction of HC⋮CCH(OH)C⋮CH and dppe
with RuHCl(CO)(PPh3)3 produced
[RuCl(CO)(PPh3)(dppe)]2(μ-CHCHCH(OH)CHCH), which
was converted to the C5H5-bridged complex
[(dppe)(PPh3)(CO)ClRuCHCHCHCHCHRuCl(CO)(PPh3)(dppe)]BF4 on treatment with
HBF4·Et2O.
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