Crystal structure and electrical properties of κ-((S,S)-DMBEDT–TTF)2ClO4

✍ Scribed by Dr. John S. Zambounis; Dr. Carl W. Mayer; Kurt Hauenstein; Dr. Bruno Hilti; Dr. Walther Hofherr; Jurgen Pfeiffer; Markus Bürkle; Grety Rihs

• Publisher: John Wiley and Sons
• Year: 1992
• Tongue: English
• Weight: 324 KB
• Volume: 4
• Category: Article
• ISSN: 0935-9648
• DOI: 10.1002/adma.19920040106

✦ Synopsis

Additional work is in progress on characterization, physical properties and on varying the central metallic atom, and the size as well as the side chains of the azamacrocyclic ligand.

Experimental

The products were characterized by a combination of techniques. described in detail elsewhere [l6]. Synthesis of 2: To a solution ofthe azamacrocyclic acid amide (1) in dry THF under N, at 0 -C, was dropped under stirring a three fold molar excess of BH,.THF adduct (1 molar, in THF; Janssen). After completlon, the reaction mixture was refluxed for three hours. Then, an excess of conc. HCI was added under additioiial stirring at room temperature for approximately 30 minutes until H,-evolution ceased. Subsequently, the solvent was evaporated, the residue redissolved in THF and, after the addition of an excess of 3 molar NaOH-solution, the mixture was stirred under reflux for 30 minutes. Finally, the solvent was evaporated to a third of its volume and, after the addition of a ten-fold quantity of diethylether, the mixture was shaken with water several times. The combined organic phases were dried with anhydrous sodium sulpate, filtered and evaporated. The residue was purified by column chromatography on neutral A1,0, with hexane/ethyl acetate 1 :I and subsequent recrystalliration from acetone. Yield: 68%; m.p. (DSC): 41.5 "C (first heating), 14.0 -C (second and further heatings). 1R (liquid film on KBr. cm-', Fig. a):