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Trirhenium(III) Cluster Alkyls. Synthesis of Tertiary Phosphine Adducts; Cleavage to Rhenium-(III) and -(II) Dimers; Reactions with Carbon Monoxide, Nitric Oxide, and Hydrogen Chloride. X-Ray Structural Determinations of Hexamethylbis(diethylphenylphosphine)tri-ν-methyl-triangulo-tri...

DOI: 10.1039/DT9800000334

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 334 - 344 (1980)

Update date:2022-08-04

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Authors:

Edwards, PeterEdwards, Peter

Mertis, KonstantinosMertis, Konstantinos

Wilkinson, GeoffreyWilkinson, Geoffrey

Hursthouse, Michael B.Hursthouse, Michael B.

Malik, K. M. AbdulMalik, K. M. Abdul

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Article abstract of DOI:10.1039/DT9800000334

A new cluster benzyl, Re3Cl3(CH2Ph)6, and tertiary phosphine (L) adduct of the corresponding cyclohexyl, Re3Cl3(C6H11)6L3, and of the permethyl,Re3Me3L2,3, have been prepared.The structure of the diethylphenyl-phosphine derivative Re3Me9(PEt2Ph)2 has been confirmed by a single-crystal X-ray structure determination.Crystals are monoclinic, space group C2/c, with dimensions a=27.220(4), b=9.817(1), c=26.051(5) Angstroem, and β=102.065(2) deg and the structure was solved by direct methods and refined by least squares to an R of 0.043 using 4982 unique observed intensities.The Re3Me9 unit present in the trinuclear molecule is considerably distorted as a result of steric compression from the two strongly bound phosphines.The tinuclear rhenium(III) phosphine adducts undergo cleavage reactions to give dimeric compounds of rhenium(III) or rhenium(II), examles being Re2Me6(PMe2Ph)2 and Re2Cl2(CH2SiMe3)2(PMe3)4.The reactions of the blue trimethylsilylmethyl cluster Re3Cl3(CH2SiMe3)6 with CO, NO, and HCl are described.Nitric oxide is shown to give an insertion product with an N-(trimethylsilylmethyl)-N-nitrosohydroxylaminato-chelate ring, of formula Re3Cl3(CH2SiMe3)5 whose structure has also been confirmed by X-Ray structure determination.Crystals are monoclinic, space group P21/a, with a=33.33(4), b=11.733(5), c=11.947(6) Angstroem, and β=92.93(4) deg.The structure was solved by direct method and refined by least squares to an R of 0.0067 using 4360 observed data.The nitrosohydroxylaminato-ligand chelates symmetrically (Re-O 0.210 Angstroem X 2) to one of the metal atoms, using one out-of-plane and the in-plane terminal sites.

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Product name:bis(diethylphenylphosphine)hexamethyldirhenium(III)

Cas No:73682-52-7

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