Cluster Chemistry. Part 91. Clusters derived from 1,4-Bis(diphenylphosphino)buta-1,3-diyne and Their Pyrolysis Products: A Route to Complexes containing the Tetracarbon Ligand

DOI: 10.1039/DT9930003299

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Journal of the Chemical Society, Dalton Transactions p. 3299 - 3312 (1993)

Update date:2022-07-30

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Authors:

Adams, Chris J.

Bruce, Michael I.

Horn, Ernst

Skelton, Brian W.

Tiekink, Edward R. T.

White, Allan H.

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Article abstract of DOI:10.1039/DT9930003299

Reactions of n(CO)11(NCMe)> n = Ru3, Os3, Re3(μ-H)3, or Ru4(μ-H4)4> with the linear bis(phosphine) PPh2C2C2PPh2(bdpp) afford the 'barbell' complexes <n(CO)11>2(μ-bdpp)> n = Ru3 1 (38), Os3 2 (68), Re3(μ-H)3 4 (44), or Ru4(μ-H)4 6 (39percent)>.The monosubstituted complexes n(CO)11(bdpp)> n = Os3 3 or Re3(μ-H)3 5> were isolated when an excess of bdpp was used.Reactions of 3 with afforded the mixed-metal complexes <(μ-bdpp)> .In a similar fashion<(μ-bdpp)> 9 was prepared (38percent) from 5 and .When a solution of 1 in CH2Cl2 was gently heated under a nitrogen purge the C4 complex <2(μ3:m3-C4)> 10 was produced in 73percent yield.Without purging, the yield is much reduced; a minor product from the reaction is <<μ4-PPh(C6H4)C2C2PPh2>> 11.Complex 11 contains an Ru3(CO)11 moiety linked via a PPh2C2C2PPh(C6H4) ligand to an Ru-spiked Ru3 cluster.One of the C2 units is attached in a μ-?,?,η²-vinylic mode to the spike Ru and to two of the three Ru atoms in the closed triangular core.When 11 was recrystallised from CH2Cl2-MeOH the complex <<μ4-CCH-μ-η²-C2)> 12 was formed.This complex contains an Ru4 rhombus, opposite faces of which carry μ3-OMe and μ4-vinylidene ligand; the latter is attached via a C-C single bond to the binuclear fragment.The complex <2(μ3:μ3-C4)> 13 was obtained (78percent) by pyrolysis of 2 in refluxing toluene.The structures of complexes 6 and 10-13 were determined by single-crystal X-ray studies.

Full text of DOI:10.1039/DT9930003299

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