Tetrakis(dimethylamino)ethene: An Extremely Electron-Rich Molecule with Unusual Structure both in the Crystal and in the Gas Phase
✍ Scribed by Prof. Dr. Hans Bock; Dr. Horst Borrmann; Dr. Zdenek Havlas; Prof. Dr. Heinz Oberhammer; Dipl.-Chem. Klaus Ruppert; Prof. Dr. Arndt Simon
- Publisher
- John Wiley and Sons
- Year
- 1991
- Tongue
- English
- Weight
- 548 KB
- Volume
- 30
- Category
- Article
- ISSN
- 0044-8249
No coin nor oath required. For personal study only.
✦ Synopsis
um atoms. Contact ion pairs are presumably also present in CH,CI, and CHCI, solvents since no sharp 19F NMR resonances were observed in freshly prepared solutions of 3. Concentrated solutions of 3 are only metastable at room temperature, however, their blue color disappearing after approximately one week.
The isolation of a Te"' radical cation and the determination of its detailed geometry affords a unique opportunity for a general study of the nature of related species. Furthermore, the unexpected oxidation of 1 by Ag+AsF; strongly suggests that this synthetic method could be generalized to other tellurium compounds.
Experimental Procedure
All manipulations were performed under an inert atmosphere of dry nitrogen gas inside a drybox or on a glass vacuum line. The CH,CI, and CHCI, solvents were dried over P,Ol0 and distilled and stored over molecular sieves (4 A) prior to use. In a typical preparation, 1 (1.13 g, 2.51 mmol) and Ag'AsF; (0.74 g, 2.50 mmol) were loaded into separate arms of an H-shaped glass reaction vessel (equipped with teflon valves and a glass frit). After dissolving the compounds in CH,CI, (30 ml) the solutions were thoroughly mixed at -78 "C and the yellow solution allowed to warm to room temperature. The resulting dark blue solution was then filtered from the white-grey silver metal powder and the solvent slowly condensed off to give large black crystalline blocks of 3. 'H NMR (80 MHz, CDCI,, -50 "C, ext. TMS): 6 = 0.45 (Av,,, =18 Hz). ESR (CDCI,, 10°C): g = 2.0 (Awl,, = 15G). UV/VIS (CH,CI,): A,,,[nm] = 615.