Binuclear copper complexes of bis(1,4,7-triazacyclonon-1-yl) ligands incorporating acetate pendant arms

Abstract

Two new bis(pentadentate) compounds, 1,2-bis[4,7-bis(carboxymethyl)-1,4,7-triazacyclonon-1-yl]ethane (L¹) and 1,4-bis[4,7-bis(carboxymethyl)-1,4,7-triazacyclonon-1-yl]butane (L²), have been prepared by functionalisation of the corresponding alkyl-bridged bis(macrocycles) with acetate pendant arms. Their binuclear copper(II) complexes have been prepared and characterised by X-ray crystallography. Both [Cu₂L¹]·5H₂O and [Cu₂L²]·2H₂O are centrosymmetric about the alkyl bridge with the pentadentate compartments hosting the copper(II) centres oriented away from one another. Each Cu^II exhibits distorted square-pyramidal geometry with an N₂O₂ basal plane and an apical N atom.

References

1. N. Tanaka, Y. Kobayashi and S. Takamoto, Chem. Lett., 1977, 107.
2. K. Wieghardt, I. Tolksdorf and W. Herrmann, Inorg. Chem., 1985, 24, 1230.
3. G. R. Weisman, D. J. Vachon, V. B. Johnson and D. A. Gronbeck, J. Chem. Soc., Chem. Commun., 1987, 886.
4. H. Chang, H. Diril, M. J. Nilges, X. Zhang, J. A. Potenza, H. J. Schugar, D. N. Hendrickson and S. S. Isied, J. Am. Chem. Soc., 1988, 110, 625.
5. J. L. Sessler, J. W. Sibert and V. Lynch, Inorg. Chem., 1990, 29, 4143.
6. J. L. Sessler, J. W. Sibert, A. K. Burrell, V. Lynch, J. T. Markert and C. L. Wooten, Inorg. Chem., 1993, 32, 4277.
7. X. Zhang, W.-Y. Hsieh, T. N. Margulis and L. J. Zompa, Inorg. Chem., 1995, 34, 2883.
8. L. Behle, M. Neuburger, M. Zehnder and T. A. Kaden, Helv. Chim. Acta, 1995, 78, 693.
9. M. J. Young and J. Chin, J. Am. Chem. Soc., 1995, 117, 10577.
10. P. D. Beer, M. G. B. Drew, P. B. Leeson, K. Lyssenko and M. I. Ogden, J. Chem. Soc., Chem. Commun., 1995, 929.
11. A. J. Blake, T. M. Donlevy, P. A. England, I. A. Fallis, S. Parsons and M. Schröder, J. Chem. Soc., Chem. Commun., 1994, 1981.
12. S. J. Brudenell, L. Spiccia and E. R. T. Tiekink, Inorg. Chem., 1996, 35, 1974.
13. P. Chaudhuri and K. Wieghardt, Prog. Inorg. Chem., 1987, 35, 329; R. Bhula, P. Osvath and D. C. Weatherburn, Coord. Chem. Rev., 1988, 91, 89; P. V. Bernhardt and G. A. Lawrance, Coord. Chem. Rev., 1990, 104, 297.
14. S. J. Brudenell, L. Spiccia and D. C. R. Hockless, unpublished work.
15. G. D. Fallon, B. Graham and L. Spiccia, unpublished work.
16. K. Wieghardt, U. Bossek, P. Chaudhuri, W. Herrmann, B. C. Menke and J. Weiss, Inorg. Chem., 1982, 21, 4308.
17. C. K. Johnson, ORTEP II, Report ORNL-5136, Oak Ridge National Laboratory, Oak Ridge, TN, 1976.
18. W. J. Moore, Physical Chemistry, Prentice-Hall, Englewood Cliffs, NJ, 4th edn., 1972.
19. G. B. Deacon and F. Huber, Inorg. Chim. Acta, 1985, 104, 41.
20. D. M. Wambeke, W. Lippens, G. G. Herman and A. M. Goeminne, J. Chem. Soc., Dalton Trans, 1993, 2017.
21. K.-S. Bürger, P. Chaudhuri, K. Wieghardt and B. Nuber, Chem. Eur. J., 1995, 1, 583.
22. G. A. McLachlan, G. D. Fallon, R. L. Martin, B. Moubaraki, K. S. Murray and L. Spiccia, Inorg. Chem., 1994, 33, 4663.
23. N. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158.
24. A. Altomare, M. C. Burla, M. Camalli, M. Cascarano, C. Giacovazzo, A. Guagliardi and G. Polidori, SIR 92, J. Appl. Crystallogr., 1993, 26, 343.
25. G. M. Sheldrick, SHELXS 86, Program for the Automatic Solution of Crystal Structure, University of Göttingen, 1986.
26. TEXSAN, Crystal Structure Analysis Package, Molecular Structure Corporation, Houston, TX, 1985 and 1992.