Abstract
The inclusion complex ofp-tert-butylcalix[5]arene with tetralin has been characterized in the solid state by a single crystal X-ray diffraction study and by13C CP/MAS NMR experiments. A crystallographic mirror plane bisects the calix[5]arene and contains the tetralin molecule (which is dynamically disordered). The guest penetrates the upper rim of the calixarene and the experimental results indicate the saturated ring is imbedded most deeply.p-tert-Butylcalix[5]arene (tetralin) · 2 EtOH belongs to the monoclinic space group C2/m witha = 22.187(6),b = 15.823(6),c = 18.168(5) Å,β = 99.70(2)°, andD c = 1.09 g cm−3 forZ = 4. Refinement based on 1652 observed reflections led to a finalR value of 0.081.
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p-tert-Butylcalix[5]arene was prepared by the method of reference 10. This involved at one stage heating in tetralin at 155° for 6 h. After removal of the tetralin, the substance was recrystallized from ethanol.p-tert-Butylcalix[5]arene (tetralin) · 2 EtOH belongs to the monoclinic space groupC2/m witha = 22.187(6),b = 15.823(6),c = 18.168(5) Å,β = 99.70(2)°, andD c = 1.09 g cm−3 forZ = 4. Refinement based on 1652 observed reflections led to a finalR value of 0.081.
Solid-state13C NMR spectra were obtained using cross-polarization (contact time 1 ms, delay 2 s, decoupling field amplitude 60 kHz) and magic angle spinning (3.25–3.55 kHz) on a Bruker CXP-180 spectrometer equipped with a Doty Scientific probe. Dipolar dephased spectra were obtained by leaving the decoupler off for 40 μs before initiating data acquisition.
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Supplementary Data relating to this article are deposited with the British Library as supplementary publication No. SUP 82/82129 (19 pages).
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Juneja, R.K., Robinson, K.D., William Orr, G. et al. Inclusion of multi-ring compounds byp-tert-butylcalix[5]arene. J Incl Phenom Macrocycl Chem 13, 93–96 (1992). https://doi.org/10.1007/BF01076674
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DOI: https://doi.org/10.1007/BF01076674