p-tert-Butylcalix[5]arene: a New Synthetic Pathway and Crystal Structure of the N,N-Dimethylformamide Complex |
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Authors: | I. DUMAZET N. Ehlinger F. VOCANSON S. Lecocq R. LAMARTINE M. Perrin |
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Affiliation: | (1) Laboratoire de Chimie Industrielle, CNRS-ESA, Université, 5078 Claude Bernard Lyon I;(2) Laboratoire de Cristallographie, CNRS-ESA 5078, Université Claude Bernard Lyon I, 43, boulevard du 11 Novembre 1918, 69622 Villeurbanne cedex, France |
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Abstract: | The formation of p-tert-butylcalix[5]arene by the opening ofp-tert-butyldihomooxacalix [4]arene and the addition of a monomer has beenstudied. Various facets, including the effects of bases and the nature ofthe monomer added to the p-tert-butyldihomooxacalix[4]arene, have beeninvestigated. p-tert-Butylcalix[5]arene can be prepared in yields up to30%. The structure of its 1 : 2 complex with DMF has been determinedby X-ray crystallography. Crystals are triclinic, space group P¯1, a =1428.2(3) pm, b = 1837.3(3) pm, c = 1276.1(2) pm, = 108.98(1)°, = 105.02(2)°, = 95.21(1)°, Z = 2, D c = 1.059 kg m-3,final R value = 0.087. The macrocycle adopts a cone conformation, one guestenclosed inside the cavity, the other one outside. |
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Keywords: | p-tert-Butylcalix[5]arene synthesis complexation crystal structure |
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