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Coordination Arrays: Tetranuclear Cobalt(II) Complexes with [2 × 2]-Grid Structure

✍ Scribed by Dr. Garry S. Hanan; Dr. Dirk Volkmer; Dr. Ulrich S. Schubert; Prof. Dr. Jean-Marie Lehn; Gerhard Baum; Prof. Dr. Dieter Fenske


Publisher
John Wiley and Sons
Year
1997
Tongue
English
Weight
523 KB
Volume
36
Category
Article
ISSN
0044-8249

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✦ Synopsis


Scheme 2. Schematic representation of the uptake of K + ions by 3 based on molecular mechanics calculations.

Experimental Section

3: A suspension of p-rert-butyl-calix[4]arene (451 mg, 0.70 mmol) and potassium carbonate (480 mg, 3.5 mmol) in dry acetonitrile (100 mL) was stirred under nitrogen. After 2 h at room temperature, 1 (I g, 0.70 mmol) was added and the reaction mixture brought to reflux for five days. The solvent was then removed in vacuo and the solid suspended in a 1 : 1 ethanol-water mixture. The suspension was heated to reflux overnight and hot filtered. The crude mixture was then dissolved in chloroform (50 mL) and the solution carefully paper filtered to yield a clear solution to which acetone (40 mL) was added. Filtration of the microcrystalline material obtained after the solution had been allow to stand for a few hours, followed by its drying in vacuo yielded 3 (500 mg) as an analytically pure product (51 "A). 'H NMR


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