Issue 8, 1994

Synthesis, properties and crystal structures of benzene-1,2-dithiolato complexes of antimony-(III) and -(V)

Abstract

Anaerobic treatment of SbCl3 with 1,2-(LiS)2C6H4 provided a reliable route to [Sb(1,2-S2C6H4)2] which in turn produced [Sb(1,2-S2C6H4)3] on reaction with 1,2-(HS)2C6H4 and O2 in very good yields ([NEt4]+ salt, ca. 82%). Tetraalkylammonium salts of [Sb(1,2-S2C6H4)2] were isolated after metathesis with either [NEt4]Br ([NEt4]+ salt, ca. 72%) or [NBun4]l ([NBun4]+ salt, ca. 90%). Slowly cooling hot MeCN solutions of [Net4][Sb(1,2-S2C6H4)2] gave yellow single crystals. This compound is the first structurally characterized anionic thiolate complex of SbIII. In its structure the stereochemical influence of the lone pair of electrons leads to a distorted Ψ-trigonal-bipyramidal environment [Sax–Sb–Sax 158.95(3), Seq–Sb–Seq 105.08(3)°], however, the degree of distortion is less severe than expected for a complex with a normalized bite (b) of 1.31. Dark purple single crystals of [NEt4][Sb(1,2-S2C6H4)3] were obtained by slowly cooling hot MeCN–MeOH solutions. The co-ordination geometry about Sb is slightly distorted from octahedral with a twist angle of 49.22(3)° and most structural parameters are within 10% of octahedral values.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1994, 1213-1218

Synthesis, properties and crystal structures of benzene-1,2-dithiolato complexes of antimony-(III) and -(V)

J. Wegener, K. Kirschbaum and D. M. Giolando, J. Chem. Soc., Dalton Trans., 1994, 1213 DOI: 10.1039/DT9940001213

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Spotlight

Advertisements