On simply changing the concentration of the reactant, either p-tert-butyldihomooxacalix[5]arene or p-tert-butyltetrahomodioxacalix[10]arene can be obtained as the main product in the thermal dehydration of a bishydroxymethylated pentaphenol. The two compounds are suitable for complexation of uranyl ion in the presence of amines, and the X-ray crystal structures of two such complexes are reported. In the complex with p-tert-butyldihomooxacalix[5]arene, the uranyl ion is sandwiched between two macrocycles, in such a way that each of its two oxo atoms is directed towards the cavity of one homooxacalixarene arranged in a cone conformation. On the other hand p-tert-butyltetrahomodioxacalix[10]arene, in its deca-anionic form, complexes four uranyl ions to give one of the largest species in this family.
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