Pd Clusters Containing As and PPh3 Ligands: The Structures of [Pd9As6 (PPh3)8], [Pd2(As2)(PPh3)4], and [Pd20As12 (PPh3)12]

✍ Scribed by Prof. Dr. Dieter Fenske; Dipl.-Chem. Holm Fleischer; Dipl.-Chem. Claudia Persau

• Publisher: John Wiley and Sons
• Year: 1989
• Tongue: English
• Weight: 381 KB
• Volume: 28
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.198916651

✦ Synopsis

homo)cubane or as an oxygen analogue of [4]peristylane." ' 1 Furthermore, this result corroborates the constitutional assignment, based solely on the 'H NMR and IR spectra, of a product obtained after ozonolysis of the syn dimer of tetramethylcyclobutadiene."

Experimental Procedure

Dimethylsilyl bis(trifluoromethanesu1fonate) (2.28 g. 6.4 mmol) was added dropwise at 0 "C to a solution of l-diazo-3,3-dimethyl-2-butanone (1.61 g, 12.8 mmol) and ethyldiisopropylamine (2.23 mL, 12.8 mmol) in 40 mL ofether. After stirring for 5 hat room temperature, the reaction mixture was filtered and the solvent was replaced by 25 mL of cyclohexane. The resulting orange solution of 1 (IR(neat): C (CN,) = 2069 em-') was then treated with copper(1) trifluoromethanesulfonate-benzene complex (90 mg, 0.3 mmo!). After stirring for 12 h. the mixture was filtered, the solvent was removed at 20"C/0.01 Torr, and the product was recrystallized from 4 mL of ether/methanol (1 :l): 0.61 g (38%) of colorless 4 [7], m.p. 135 "C, was obtained.