Organometallic Thiol and Thiolato Complexes of Ruthenium(IV)

DOI: 10.1039/DT9940001949

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1949 - 1962 (1994)

Update date:2022-08-02

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Authors:

Belchem, Gary

Steed, Jonathan W.

Tocher, Derek A.

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Article abstract of DOI:10.1039/DT9940001949

Reaction of the ruthenium(IV) chloro-bridged dimer <3:η³-C10H16)Cl(μ-Cl)>2> 1 with a range of alkane- and arene-thiols in CH2Cl2 resulted in the formation of the simple, bridge-cleaved adducts 3:η³-C10H16)Cl2(HSR)> (R=Et 2, Me 3, iPr 4, tBu 5 or Ph 6).Reaction of 1 with an excess of thiol in methanol gave doubly thiolate-bridged compounds <3:η³-C10H16)Cl(μ-SR)>2> (R=Et 7, Ph 12 or C6F5 13) each of which exists as two diastereoisomers but as a single geometrical isomer.In the case of 7 and 12 separation of the two diastereomeric forms proved possible because of their remarkably different solubilities in methanol, and their kinetic inertness.Reactions of 2 and 3 with 1 gave the mixed-bridge chloro/thiolato complexes <3:η³-C10H16)Cl>2(μ-Cl)(μ-SR)> (R=Me 9 or Et 8).The unusual stereochemistry of these compounds is evident from analysis of their variable-temperature 1H NMR spectra.The crystal structure of 8 has been determined.Reaction of 1 with H2S in CH2Cl2 proceeds via the H2S adduct 3:η³-C10H16)Cl2(SH2)> 10, which rapidly reacts with further 1 with accompanying loss of HCl to give the singly SH-bridged complex <3:η³-C10H16)Cl>2(μ-Cl)(μ-SH)> 11.Reaction of the EtSH compound 2 with a range of Ru(II) and Rh(III)-containing compounds enabled the isolation of a number of unusual mixed-valence and mixed-metal complexes containing one or two bridging ethanethiolate ligands.The ruthenium(IV)-rhodium(III) compounds <(η³:η³-C10H16)ClRu(μ-Cl)(μ-SEt)RhCl(η⁵-C5Me5)> and <(η³:η³-C10H16)ClRu(μ-SEt)2RhCl2(PMe2Ph)2> have been characterized by X-ray crystallography.

Full text of DOI:10.1039/DT9940001949

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