22
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mmol) was added dropwise with stirring at room
temperature. The formation of two phases and a
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phase d 14.7 (2a), 20.0 (2), dA 22.3 and dB ꢁ
53.0 ppm
/
(no assignment), lower phase: d 12.5 (2a), 17.9 ppm (2);
13C NMR: upper phase: d 5.9 (2), 10.0 ppm (2a); lower
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MeCN). M.p. 243ꢃ
245 8C; (KBr, cmꢁ1): nCÄC: 1670
(s); 13C NMR (D2O): d 41.5, 42.4 (N(CH3)2), d 154.9
ppm (CÃ
C); 1H NMR (D2O): d 3.30, 3.59 ppm
/
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(N(CH3)2) [22], 2.06 ppm (CH3CN); Anal. Calc. for
C12H27Cl2N5 (312.29): C, 46.1; H, 8.7; Cl, 22.7; N, 22.4,
Found: C, 44.8; H, 8.6; Cl, 22.5; N, 18.7%.
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4. Supplementary material
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Crystallographic data (excluding structure factors) for
the structures in this paper have been deposited at the
Cambridge Crystallographic Data Centre, CCDC nos.
[19] Y. Deligiannakis, G. Papavassiliou, M. Fardis, G. Diamanto-
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179841 and 179842 for compounds 5b and 6×
Copies of this information may be obtained free of
charge from The Director, CCDC, 12 Union Road,
/
MeCN.
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Cambridge CB2 1EZ, UK (Fax: ꢀ44-1223-336033; e-
mail: deposit@ccdc.cam.ac.uk or www: http://
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Acknowledgements
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We are grateful to the Deutsche Forschungsge-
meinschaft, the Graduiertenkolleg ‘‘Crystal Engineering
and Crystallisation’’ and Fonds der Chemischen Indus-
trie for financial support. We thank F. Wirbeleit for
carrying out the EPR measurements and B. Kutzner for
recording the NMR spectra.
Weinheim, 1979, pp. 270ꢃ272.
/
[28] Bruker AXS Inc., Madison, WI, USA, 1998.
[29] G.M. Sheldrick, SADABS V2.01, Program for Empirical Absorp-
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