Alternative methods of modifying the calixarene conformation. The synthesis and molecular structures oft-butylcalix[4]arene methyl ether complexed with aluminum alkyl species |
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Authors: | Simon G. Bott Anthony W. Coleman Jerry L. Atwood |
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Affiliation: | (1) Department of Chemistry, University of Alabama, 35487 Tuscaloosa, AL, USA |
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Abstract: | The configurations of calix[4]arenes may be modified by the formation of donor-acceptor complexes which make use of the basicity of the oxygen atoms of the macrocycle. The complex [t-butylcalix[4]arene methyl ether][AlMe3]2,2, exhibits the previously unseen 1,2-alternate geometry, while [t-butylcalix[4]arene methyl ether][MeAlCl2]2,3, and [t-butylcalix[4]arene methyl ether][EtAlCl2]2,4, show the 1,3-alternate configuration.2 crystallizes in the triclinic space groupPl witha=11.14(1),b=11.60(1),c=12.02(1) Å, =77.32(8), =67.91(8), and =69.34(8)o withDc=1.06 g cm–3 forZ=1. Refinement based on 1270 observed reflections led toR=0.106.3 as the benzene solvate belongs to the monoclinic space groupC2/c witha=12.116(2),b=21.557(7),c=23.470(6) Å, and =104.05(2)o withDc=1.13 g cm–3 forZ=4. Refinement based on 2335 observed reflections led toR=0.075.4 crystallizes in the monoclinic space groupC2/c witha=12.062(4),b=21.175(6),c=21.596(5) Å, and =100.78(4)o withDc=1.18 g cm–3 forZ=4. Refinement based on 2529 observed reflections gaveR=0.082. The Al-O lengths in all three complexes are normal for donor-acceptor interactions.Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82053 (45 pages). |
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Keywords: | Calix[4]arene aluminum alkyl crystal structure |
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