Abstract
Bromocalix[4]arene methyl ether serves as a precursor in the synthesis of the title thiocalixarene via the reagent CuSEt. Ethylthiocalix[4]arene methyl ether crystallizes in the monoclinic space groupP21/c witha = 20.577(9),b, = 10.722(5),c = 20.315(9) Å, β = 120.46(4)°, andD c = 1.24 g cm−3 forZ = 4. Refinement based on 1441 observed reflections led toR = 0.080. The configuration of the calixarene lies between the partial cone and the 1,3-altemate conformations. Bromocalix[4]arene methyl ether crystallizes in the triclinic space groupPI witha = 12.283(7),b = 17.658(9),c = 18.118(6) Å, α = 90.25(6), β = 105.95(4), γ = 105.11(6)°, andD c = 1.68 g cm−3 forZ = 4. Refinement based on 3028 observed reflections led toR = 0.083. The unit cell also contains four CHCl3 molecules which exist pairwise enclathrated by six calixarenes. The partial cone conformation of the bromocalixarene is identical to that of ethylthiocalix[4]arene methyl ether.
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Hamada, F., Bott, S.G., Orr, G.W. et al. Thiocalix[4] arenes. I. Synthesis and structure of ethylthiocalix[4]arene methyl ether and the related structure of bromocalix[4]arene methyl ether. J Incl Phenom Macrocycl Chem 9, 195–206 (1990). https://doi.org/10.1007/BF01053117
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DOI: https://doi.org/10.1007/BF01053117