Gagnon et al.
1445
tions involving air- or moisture-sensitive reagents were con-
ducted under nitrogen atmosphere. Column chromatography
was performed on 230–400 mesh silica gel (60 Å). All NMR
spectra were acquired (1H 300 MHz, 13C 75 MHz, 31P
121 MHz) using the solvent as chemical shift standard, ex-
cept in 31P NMR, where the chemical shift are relative to
D3PO4 (85% in D2O). All the chemical shifts and the cou-
pling constants are given in ppm and Hz, respectively. The
lower number of signals in 13C NMR spectra is due to
isochronism. Mass spectra were determined at an ionizing
voltage of 70 eV. Compounds 1 (23), 2a (12), 3a (24), 6
(16), and 23 (25) were prepared according to literature pro-
cedures. The syntheses of all new calix[4]arene compouds
are reported in the Supporting Information.2
pour la Formation de Chercheurs et l’Aide à la Recherche
(FCAR) for fundings. J.G. thanks NSERC for a graduate
scholarship.
References
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Crystal data for calix[4]arene 4b and 5
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Acknowledgments
This research was supported by Natural Sciences and En-
gineering Research Council of Canada (NSERC) and Fonds
2 Supplementary material, including syntheses of all compounds and crystallographic data for compounds 4b and 5, may be purchased from
the Depository of Unpublished Data, Document Delivery, CISTI, National Research Council Canada, Ottawa, ON K1A 0S2, Canada. For
deposited with the Cambridge Crystallographic Data Centre (CCDC No. 168 292 and 169 293). Copies of the data can be obtained, free of
charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, U.K. (fax: 44-1223-336033 or e-mail: de-
posit@ccdc.cam.ac.uk).
© 2001 NRC Canada