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Synthesis and characterisation of diphenylvinylphosphine-substituted osmium and ruthenium carbonyl clusters; crystal and molecular structures of [Os3(CO)11(Ph2PCH=CH2)] and [Os3(μ-H)(CO)9(μ-Ph2PCH=CH)]

DOI: 10.1039/DT9960003825

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 3825 - 3831 (1996)

Update date:2022-08-03

Topics: Synthesis   Characterisation   Crystal structures   Experimental terms   Molecular structures  

Authors:

Johnson, Brian F. G.Johnson, Brian F. G.

Lewis, JackLewis, Jack

Nordlander, EbbeNordlander, Ebbe

Raithby, Paul R.Raithby, Paul R.

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Article abstract of DOI:10.1039/DT9960003825

Reaction of the activated clusters [Os3(CO)12-n(NCMe)n] (n = 1 or 2) with diphenylvinylphosphine (Ph2PCH=CH2) afforded [Os3(CO)12-n(Ph2PCH=CH2) n] (n = 1 1 or 2 2) in good yield. Addition of Ph2PCH=CH2 to [Os3(μ-H)2(CO)10] resulted in the formation of [Os3(μ-H)H(CO)10(Ph2PCH=CH2)] 3. The ruthenium clusters [Ru3(CO)12-n(Ph2PCH=CH2) n] (n = 1 4 or 2 5) have been synthesised by the reaction of [Ru3(CO)12] with an excess of diphenylvinylphosphine in the presence of a catalytic amount of Na-Ph2CO. Thermolysis of 1 led to the formation of [Os3(μ-H)(CO)9(μ3-Ph2PCH=CH)] 6 in which the vinyl moiety has undergone β elimination. Similarly, 4 and 5 are converted into [Ru3(μ-H)(CO)9(μ3-Ph2PCH=CH)] 7 and the known complex [Ru3(μ-H)(CO)8(Ph2PCH=CH 2)(μ3-Ph2PCH=CH)] 8 under mild conditions (thermolysis or photolysis). No intermediate species could be detected during the formation of 6-8. All of the new clusters 2-7 have been fully characterised on the basis of their spectroscopic data and the molecular structures of 1 and 6 have been established by single-crystal X-ray analysis.

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Product name:[Ru3(CO)11(P(C6H5)2CHCH2)]

Cas No:183113-95-3

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