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The Palladium-catalysed Reaction Between and Phosphines and the Crystal and Molecular Structure of Diaxial

DOI: 10.1039/DT9850002277

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2277 - 2282 (1985)

Update date:2022-08-03

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Authors:

Harris, Gillian W.Harris, Gillian W.

Boeyens, Jan C. A.Boeyens, Jan C. A.

Coville, Neil J.Coville, Neil J.

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Article abstract of DOI:10.1039/DT9850002277

The reaction between and PR3 in xylene is catalysed by Pd/C, Pd/CaCO3, and PdO and yields the complexes 10-n(PR3)n> (n=1 or 2) as the major products (15-80percent).Attempts to synthesise 10-n(PR3)n from and PR3 in the presence of NMe3O under milder conditions (e.g. refluxing CH2Cl2) also gave the above products with n=1 or 2 as well as high yields of fac-.An X-ray crystal structure determination of diaxial was carried out: space group C2/c, Z=4, a=22.779(9), b=7.166(3), c=17.249(7) Angstroem, β=95.13(3) deg, R=0.0602.The structure has a staggered geometry with torsion angles deviating by +/-6 deg from the ideal (45 deg).The Re-Re bond length was found to be 3.044(1) Angstroem, cf., 3.041(1) Angstroem for , indicating that this parameter is almost invariant on substitution of CO by PMe2Ph.

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