[C5H5(CO)2MnN2H2Cr(CO)5], a Complex with a Diazene Bridge and Two Different Coordination Centers

✍ Scribed by Dr. Dieter Sellmann; Dr. Klaus Jödden

• Publisher: John Wiley and Sons
• Year: 1977
• Tongue: English
• Weight: 218 KB
• Volume: 16
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.197704641

✦ Synopsis

by the molecular weight (determined cryoscopically in benzene) and the mass spectrum, ( ) is monomeric.

The assignment of the substituents at the As=C double bond can be determined only by an X-ray structure analysis. Studies on models suggest the presence of Z isomers in which the aryl and the trimethylsiloxy group are situated at the same site.

Procedure

A solution of phenylbis(trimethy1silyl)arsane (22.4 g, 75.1 mmol) and 2,2-dimethylpropionyl chloride (9.1 g, 75.5mmol) in cyclopentane ( ) is allowed to stand for 12 h at 4°C. The reaction is followed 'H-NMR spectroscopically. After condensing off all components that are volatile at -2O"C, there remains almost pure (5). The rearrangement to (6) is complete after 12 h at 50°C: reddish liquid, b.p. 82 to 86"C/5 x lo-' torr; quantitative yield.